CN103597556A - New composite iron- based powder mix, powder component and method - Google Patents

New composite iron- based powder mix, powder component and method Download PDF

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Publication number
CN103597556A
CN103597556A CN201280028066.0A CN201280028066A CN103597556A CN 103597556 A CN103597556 A CN 103597556A CN 201280028066 A CN201280028066 A CN 201280028066A CN 103597556 A CN103597556 A CN 103597556A
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iron
layer
weight
powder
compound
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叶舟
H·斯塔凡松
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Hoganas AB
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    • 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

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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)
  • Dispersion Chemistry (AREA)
  • Soft Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)
  • Compounds Of Iron (AREA)

Abstract

The present invention concerns a composite iron- based powder mix suitable for soft magnetic applications such as inductor cores. The present invention also concerns a method for producing a soft magnetic component and the component produced by the method.

Description

NEW TYPE OF COMPOSITE iron-based powder combination, powder component and manufacture method thereof
Technical field
The present invention relates to for the preparation of the soft magnetic composite powder material of soft magnetic part and the soft magnetic part that uses this soft magnetic composite powder to obtain.Particularly, the present invention relates to this type of powder for the preparation of the soft magnetic part material of working under high-frequency, these parts are suitable as inductor or the reactor in power electronics.
Background technology
Soft magnetic material for example, for various uses, the stator of the core in inductor, motor and rotor, driver, transducer and transformer core.Traditionally, soft magnetic core (for example rotor in motor and stator) is made by stacking steel laminated sheet.Soft-magnetic composite material can be based on being generally iron-based soft magnetism particle, on each particle with electric insulation coating layer.By using optionally compacting insulating particle together with lubricant and/or adhesive of prior powder metallurgy method, obtain soft magnetic part.By using powder metallurgy technology, compare with using steel laminated sheet, can be manufactured in design and there is more this base part of high-freedom degree, because this parts portability Three-Dimensional Magnetic flux also can obtain 3D shape by compacting.
The present invention relates to iron-based soft magnetic composite powder, the coating that its core grain is carefully selected applies so that material character is applicable to by powder pressing, then heat treating process is manufactured inductor.
Inductor or reactor are the electrical passive components that can store the energy of the field form producing through the electric current of described parts.Ability---the inductance (L) that the henry (H) of take is unit inductance measuring device storage power.Inductor is normally coiled into the insulated wire of coil.The electric current of flowing through coil produces magnetic field around at coil, and the number of turn/long measure of field intensity and electric current and coil is proportional.The magnetic field that the electric current changing causes change, this causes the voltage contrary with the curent change that causes it.
The electromagnetic force contrary with curent change (EMF) be take volt (V) as unit measurement, and is associated with inductance according to following formula:
v(t)=L?di(t)/dt
(L is inductance, and t is the time, and v (t) is the time time variant voltage through inductor, and i (t) is changing currents with time).
That is to say, inductance is that the inductor of 1 Henry produces the EMF of 1 volt when the electric current through inductor changes with 1 ampere/second.
Ferromagnetic inductor or iron core inductor are used the magnetic core of for example, being made by ferromagnetic or ferrimagnetic material (iron or ferrite), thereby due to the higher magnetic permcability of this core, by improving magnetic field, the inductance of coil are improved thousands of.
The magnetic permeability μ of material indicates it to carry the ability of magnetic flux or the ability being magnetized.Magnetic permeability refers to that (mark is made B and with newton/ampere * rice or with volt * second/rice to induced flux 2for unit is measured) with the ratio of magnetizing force or field intensity (mark is made H and measured with amperes per meter ，A/mWei unit).Therefore the unit of magnetic permeability is volt * second/ampere * rice.Magnetic permeability is typically expressed as the relative permeability μ with respect to permeability of free space r=μ/μ 0, μ 0=4* Π * 10 -7vs/Am.
Magnetic permeability also can be expressed as the inductance of per unit length, Henry/rice.Magnetic permeability not only depends on the material that carries magnetic flux, also depends on extra electric field and frequency thereof.In technological system, it is commonly referred to as maximum relative permeability, and it is the maximum relative permeability recording in the one-period of electric field change.
Inductor core for example can be used on, for filtering the power electronic system of undesired signal (various harmonic waves).For effective work, for the inductor core of this purposes, should there is low maximum relative permeability, this means that relative permeability has the feature more linear with respect to extra electric field, i.e. stable incremental permeability μ Δ(as according to Δ Β=μ Δ *Δ Η defines) and high saturation magnetic flux density.This can make inductor more in wide-range current, more effectively work, and this also can be expressed as this inductor and have good " DC bias voltage ".DC bias voltage can be to specify the percentage of the maximal increment magnetic permeability of (for example, at 4000A/m) under extra electric field to represent.In addition, the combination of low maximum relative permeability and stable incremental permeability and high saturation magnetic flux density can make inductor carry higher electric current, and when size is limiting factor, this is especially useful, therefore can use less inductor.
An important parameter improving soft magnetic part performance is to reduce its core loss characteristic.When magnetic material is exposed in alternating field, because energy loss occurs for magnetic hysteresis loss and eddy current loss.The frequency of magnetic hysteresis loss and alternating magnetic field is proportional, and eddy current loss and this frequency is square proportional.Therefore, under high-frequency, take eddy current loss as main, especially require to reduce eddy current loss and still keep low magnetic hysteresis loss level.This means the resistivity of wishing to improve magnetic core.
In finding the process of the mode of improving resistivity, used and proposed diverse ways.A kind of method is based on provided electric insulation coating layer or film on powder particle before these particles are imposed to compacting.Therefore there are a large amount of patents openly to instruct dissimilar electric insulation coating layer.The example that relates to the publication of inorganic coating is U.S. Patent No. 6,309,748, U.S. Patent No. 6,348,265 and U.S.No.6,562,458.From U.S. Patent No. 5,595,609 for example, know the coating of organic material.From for example United States Patent(USP) Nos. 6,372,348 and 5,063,011 and Deutsche Bundespatent, disclose 3,439, know in 397 and comprise inorganic and coating organic material, open according to these, particle is wrapped up by ferric phosphate layer and thermoplastic.European patent EP 1246209B1 has described feeromagnetic metal based powders, and wherein the surface of this Metal Substrate powder is applied as the coating that the particulate of bentonite or talcum forms by organic siliconresin and the clay mineral with layer structure.
US6,756,118B2 has disclosed the soft magnetic powder metallic composite that comprises the powdered-metal particle that at least two kinds of oxides seal, and described at least two kinds of oxides form at least one common phase.
Patent application JP2002170707A has described the alloyed iron particle being applied by phosphorous layer, and alloying element can be silicon, nickel or aluminium.In second step, by the powder applying and the aqueous solution of sodium metasilicate, then dry.By moulded powder and at the temperature of 500-1000 ℃ this moulded parts of heat treatment manufacture ferrocart core.
In JP51-089198, mention molded by iron powder, use sodium metasilicate as the adhesive of iron particles when then heat treatment moulded parts is manufactured ferrocart core.
In order to obtain efficient soft magnetism composite component, also must under high pressure to electric insulation powder, impose compression molding, because conventionally wish to obtain high density parts.High density is improved magnetic conventionally.Particularly, need high density so that magnetic hysteresis loss remains on low-level and obtains high saturation magnetic flux density.In addition, this electrical insulating material must tolerate required compaction pressure and be not impaired when releasing compression member from mould.This means that again release power must not be too high.
In addition,, in order to reduce magnetic hysteresis loss, need the heat treatment of the release stress of compacting parts.In order to realize effective Stress Release, should be preferably higher than at 300 ℃ and temperature lower than the impaired temperature of insulating coating, heat-treating in for example nitrogen, argon gas or air atmosphere or in a vacuum.
Consider mainly at the needs of the lower powder core using of upper frequency (higher than 2kHz, particularly 5 to 100kHz frequency), made the present invention, wherein higher electric resistivity and lower core loss are basic.The preferably enough height of saturation flux density are so that iron core miniaturization.In addition, should use the temperature compacted metal powder of die wall lubrication and/or rising just can manufacture iron core.Preferably eliminate these steps.
Different from many methods of having used and having proposed that need to low core loss, a special advantage of the present invention is, in powder composition, needn't use any inorganic bond, then by the compacting in compacting step of this powder composition.Therefore the danger that can give birth to the heat treatment of pressed compact and decompose without any organic bond under higher temperature; Higher thermal treatment temperature is also improved flux density and is reduced core loss.Owing to not having organic material in final heat treated iron core, thereby also can in hot environment, use this iron core, and not have due to the softening of organic bond and decompose to make the danger of strength decreased, and realize thus improved temperature stability.
Goal of the invention
An object of the present invention is to provide the new iron-based composite powder that comprises iron-based powder core, the surface of described iron-based powder core is applied by NEW TYPE OF COMPOSITE electric insulation coating layer.This new iron-based composite powder is particularly useful for manufacturing the inductor core of power electronic equipment.
Another object of the present invention is to provide the method for manufacturing this inductor core.
A further object of the present invention is to provide the inductor core with good DC bias voltage, low core loss and high saturation magnetic flux density.
The invention provides can be used for preparation example as there is the inductor of high saturation magnetic flux density, lower core loss and can simplify the iron mixture of its manufacture method and process as described in the method for mixture.
Summary of the invention
Realize as follows at least one these object:
The iron-based powder combination of-coating, described coating comprises first phosphorous layer and the second layer, the combination that the described second layer contains alkaline silicate and particle containing the clay of specific page silicate, the mixture that wherein said iron-based powder combination comprises iron powder and sendust (sendust).According to an embodiment, coating only consists of above-mentioned two layers.
-manufacture the method for inductor core, comprise the steps:
A) provide coated iron powder composition as above,
B) in mould, under 400 to 1200MPa compaction pressure, with unidirectional pressurization campaign by optionally with coated iron/sendust (sendust) mixture of powders compacting of mix lubricant,
C) from mould, release compacting parts,
D) parts of releasing described in heat treatment at the temperature of the highest 800 ℃.
-for example, according to the parts of above making, inductor core.
Detailed Description Of The Invention
Described composition can be the compound iron-based powder combination that comprises core grain, described core grain is contained with the layer of the alkaline silicate of being combined containing the clay mineral of phyllosilicate to be applied, wherein silicon-oxygen tetrahedral layer of its merging and hydroxide octahedral layer are preferably electroneutral, and its SMIS grain is the mixture of following material:
(a) ferroalloy particle, it consists of the iron of 7 % by weight to 13 % by weight silicon, 4 % by weight to 7 % by weight aluminium and surplus substantially, and
(b) iron particle of atomization.
This ferroalloy particle also can be known as " sendust (sendust) " or " sendust (sendust) particle ".
In one embodiment, sendust particle was applied by phosphorous layer before the described alkaline silicate by with being combined containing the clay mineral of phyllosilicate applies.In brief, this coating is known as " alkaline silicate coating " or " clay coating ".This coating can be kaolin based or talcum base for example.
In another embodiment, ferroalloy particle and atomization particle were all applied by phosphorous layer before being applied by described alkaline silicate coating.
In the whole text, term " layer " and " coating " are used interchangeably.
Iron particle can be the straight iron powder form for example, with low pollutant (carbon or oxygen) content.Iron content is preferably higher than 99.0 % by weight, but also can use the iron powder with for example silicon alloy.For straight iron powder or for the iron-based powder of the alloying element alloy with having a mind to add, this powder deironing and the alloying element that may exist also contain the trace element from inevitable impurity being caused by manufacture method outward.Trace element to exist on a small quantity so that they can (or only on bottom line) not affect material character.The example of trace element can be maximum 0.1% carbon, maximum 0.3% oxygen, each sulphur of maximum 0.3% and phosphorus, and maximum 0.3% manganese.
The granularity of iron-based powder depends on desired use, i.e. the applicable frequency of these parts.The particle mean size of iron-based powder (this is also the particle mean size of the powder of coating) is very thin, can be 20 to 300 microns.The example of the particle mean size of suitable iron-based powder is for example 20-80 micron (so-called 200 order powder), 70-130 micron (100 order powder) or 130-250 micron (40 order powder).
This ferroalloy particle can be substantially consists of the iron of 7 % by weight to 13 % by weight silicon, 4 % by weight to 7 % by weight aluminium, surplus, and remainder is impurity.
This powder is known as sendust in the art.Conventionally, by weight, sendust contains 84-86%Fe, 9-10%Si and 5-6%Al substantially.
This iron particle can be water atomization or aerosolization.By the method for iron atomization, it is known in the literature.
Conventionally being administered to phosphorus-containing coatings on naked iron-based powder can be according to United States Patent (USP) 6,348, and the method for describing in 265 is used.This means iron or iron-based powder for example, are mixed with the phosphoric acid being dissolved in solvent (acetone), then dry, to obtain the coating of thin phosphorous and oxygen on powder.The amount of solution of adding especially depends on the granularity of powder; But this amount should be enough to obtain the coating of thickness 20 to 300 nanometers.
Or, can be by iron-based powder be mixed or uses other combination of phosphorus containg substances and other solvent to add thin phosphorus-containing coatings with the ammonium phosphate solution being dissolved in water.Gained phosphorus-containing coatings makes the phosphorus content of iron-based powder improve 0.01 to 0.15%.
As described below alkaline silicate coating is administered on the iron-based powder that phosphorus applies: by the particle of this powder and clay or contain the mix particles of the clay of specific page silicate and the mixture of water-soluble alkaline silicate (being often called waterglass), then carry out drying steps at the temperature of 20-250 ℃ or in a vacuum.Phyllosilicate forms the silicate of following type: wherein silicon tetrahedron is to have formula (Si 2o 5 2-) nlayer form be connected to each other.These layers merge with at least one octahedra hydroxide layer, to form combinatorial construction.Octahedral layer can for example contain aluminium hydroxide or magnesium hydroxide or its combination.Silicon in silicon tetrahedral layer can part be substituted by other atom.The layer structure of these merging can be electroneutral or charged, depends on and has which atom.The type that has been noted that phyllosilicate is most important to realizing object of the present invention.Therefore, this phyllosilicate should be the not charged or electric neutrality layer type with silicon tetrahedral layer and the hydroxide octahedral layer of merging.The example of this phyllosilicate is the pyrofyllit that exists in the kaolinite that exists in clay kaolin, phyllite or containing the mineral talc of magnesium.Should be lower than 15 containing the particle mean size of the clay of the phyllosilicate of appointment, preferably lower than 10, preferably lower than 5 microns, then more preferably less than 3 microns.The amount of the clay containing specific page silicate that will mix with the iron-based powder applying should be the 0.2-5 % by weight of coated compound iron based powders, preferred 0.5-4 % by weight.
The amount of the alkaline silicate calculating as solid alkaline silicate that will mix with coated iron-based powder should be the 0.1-0.9 % by weight of coated compound iron based powders, is preferably the 0.2-0.8 % by weight of iron-based powder.Show, can use various types of water-soluble alkaline silicate, therefore can use sodium metasilicate, potassium silicate and lithium metasilicate.Alkalescence water-soluble silicate is conventionally by its ratio, i.e. SiO 2amount divided by Na optionally 2o, K 2o or Li 2the amount of O (mol ratio or weight ratio) characterizes.The mol ratio of water-soluble alkaline silicate should be 1.5-4, comprises two end points.If mol ratio is lower than 1.5, it is too alkaline that this solution becomes, if mol ratio is higher than 4, SiO 2precipitation.
Can on sendust particle, omit the second kaolin-sodium metasilicate coating and still realize excellent magnetic.But in order further to strengthen magnetic, the second coating is answered aluminium coating ferrosilicon powder and iron powder.
In another embodiment, this alkaline silicate (or clay) coating can be substituted by metal-organic coating (the second coating).
In this case, at least one metal-organic layer is positioned at outside the first phosphorus basic unit.This metal-organic layer is the metal-organic compound with following general formula:
R 1[(R 1) x(R 2) y(MO n-1)] nR 1
Wherein:
M is the central atom that is selected from Si, Ti, Al or Zr;
O is oxygen;
R 1it is hydrolyzable groups;
R 2organic moiety and at least one R wherein 2contain at least one amino;
Wherein n is can number of repeat unit, and it is 1 to 20 integer;
Wherein x is 0 to 1 integer; Wherein y be 1 to 2 integer (x can be therefore 0 or 1, y can be 1 or 2).
This metal-organic compound can be selected from lower group: surface modifier, coupling agent or crosslinking agent.
R in this metal-organic compound 1can be to there is the alkoxyl that is less than 4, is preferably less than 3 carbon atoms.
R 2be organic residue, this means this R 2-group contains organic moiety.R 2can comprise 1-6, preferred 1-3 carbon atom.R 2the hetero-atom that can further comprise one or more N of being selected from, O, S and P.This R 2group can be straight chain, side chain, ring-type or aromatics.
R 2can comprise one or more following functional groups: amine, diamines, acid amides, acid imide, epoxy radicals, hydroxyl, oxirane, urea groups, urethanes, isocyano, acrylate, acrylic acid glyceride, benzyl-amino, vinyl-benzyl-amino.This R 2group can be at any sense R mentioning 2group and containing can change between the hydrophobic alkyl of repetitive.
This metal-organic compound can be selected from derivative, intermediate or the oligomer of silane, siloxanes and silsesquioxane or corresponding titanate, aluminate or zirconates.
According to an embodiment, at least one the metal-organic compound in a metal-organic layer is monomer (n=1).
According to another embodiment, at least one the metal-organic compound in a metal-organic layer is oligomer (n=2-20).
According to another embodiment, the metal-organic layer being positioned at outside ground floor is the monomer of this metal-organic compound, and wherein metal-the organic layer of outermost is the oligomer of this metal-organic compound.The chemical official of this monomer and this oligomer can be not necessarily identical.The weight ratio of the oligomer layer of the monomer layer of metal-organic compound and metal-organic compound can be 1:0 to 1:2, preferably 2:1-1:2.
If this metal-organic compound is monomer, it can be selected from tri-alkoxy and dialkoxy silicane, titanate, aluminate or zirconates.The monomer of this metal-organic compound for example can be selected from 3-aminopropyl-trimethoxy silane, 3-aminopropyl-triethoxysilane, 3-aminopropyl-methyl-diethoxy silane, N-amino-ethyl-3-aminopropyl-trimethoxy silane, N-amino-ethyl-3-aminopropyl-methyl-dimethoxy silane, 1, two (the triethoxysilyl)-4-azaheptan of 7-, triamido-sense propyl group-trimethoxy silane, 3-urea groups propyl group-triethoxysilane, 3-isocyano propyl group-triethoxysilane, three (3-trimethoxy-silylpropyl)-isocyanuric acid ester, 0-(alkynes propoxyl group)-N-(triethoxysilylpropyltetrasulfide)-urethanes, 1-amino methyl-triethoxysilane, 1-amino-ethyl-methyl-dimethoxy silane or its mixture.
The oligomer of this metal-organic compound can be selected from the alkoxy end-capped alkyl-alkoxyl-oligomer of silane, titanate, aluminate or zirconates.The oligomer of this metal-organic compound for example can be selected from amino-silsesquioxane, amino-siloxanes, oligomeric 3-aminopropyl-methoxyl group-silane, 3-aminopropyl/propyl group-alkoxyl-silane, N-amino-ethyl-3-aminopropyl-alkoxyl-silane or N-amino-ethyl-3-aminopropyl/methyl-alkoxyl-silane or its mixture of methoxyl group, ethyoxyl or acetoxyl group-end-blocking.
The total amount of metal-organic compound can be the 0.05-0.6 % by weight of said composition, preferably 0.05-0.5 % by weight, more preferably 0.1-0.4 % by weight, most preferably 0.2-0.3 % by weight.Metal-the organic compound of these kinds can be purchased from companies such as Evonik Ind., Wacker Chemie AG, Dow Corning.
This metal-organic compound has alkalescence, also can comprise coupling character, is coupled to the so-called coupling agent on the first inorganic layer of this iron-based powder.This material should neutralize from the excess acid of ground floor and acidic by-products.If use be selected from aminoalkyl alkoxyl-silane ,-titanate ,-aluminate or-coupling agent of zirconates, this material can be hydrolyzed and partially polymerized (some alkoxyls are hydrolyzed and corresponding formation alcohol).The coupling of this metal-organic compound or crosslinked character are also considered to be coupled on metal or semimetal particulate compounds, and this can improve the mechanical stability of this compacting composite component.
metal or semimetal particulate compounds
The soft magnet based powders of this coating also can contain at least one metal or semimetal particulate compounds.This metal or semimetal particulate compounds should be soft, have and are less than 3.5 Mohs' hardness and form particulate or colloid.This compound preferably have lower than 5 microns, preferably lower than 3 microns, most preferably lower than the particle mean size of 1 micron.This metal or semimetal particulate compounds can have and be greater than 95%, be preferably greater than 98%, be most preferably greater than the purity of 99 % by weight.The Mohs' hardness of this metal or semimetal particulate compounds is preferably 3 or less, and more preferably 2.5 or less.SiO 2, Al 2o 3, MgO and TiO 2be polishing property and there is the Mohs' hardness far above 3.5, and not within the scope of the invention.Grinding agent compound, even if be nanometer particle form, also can cause irreversible breaking to electric insulation coating layer, thereby causes the poor demoulding and worse magnetic and/or the engineering properties of this heat processing unit.
This metal or semimetal particulate compounds can be to be selected from least one of lead, indium, bismuth, selenium, boron, molybdenum, manganese, tungsten, vanadium, antimony, tin, zinc, cerium.
This metal or semimetal particulate compounds can be oxide, hydroxide, hydrate, carbonate, phosphate, fluorite, sulfide, sulfate, sulphite, oxychloride or its mixture.
According to a preferred embodiment, this metal or semimetal particulate compounds are bismuths, more preferably bismuth oxide (III).This metal or semimetal particulate compounds can with the second compound that is selected from alkali metal or alkaline-earth metal, wherein this compound can be carbonate, preferably the carbonate of calcium, strontium, barium, lithium, potassium or sodium.
This metal or semimetal particulate compounds or compound mixture can with the 0.05-0.5 % by weight of said composition, preferably 0.1-0.4 % by weight, most preferably the amount of 0.15-0.3 % by weight exists.
This metal or semimetal particulate compounds adhere at least one metal-organic layer.In one embodiment of the invention, this metal or semimetal particulate compounds adhere on outermost metal-organic layer.
By the alkaline aminoalkyl-alkoxy silane before this from different amounts by this powder
Figure BDA0000432355570000101
after this oligomer of aminoalkyl/alkyl-alkoxy silane
Figure BDA0000432355570000102
(for example use 1:1 relation, all by Evonik Inc., produced) is uniformly mixed, and can form this metal-organic layer.Said composition can from bismuth oxide (III) fine powder (the >99 % by weight of different amounts; D 50～0.3 micron) further mix.
This good saturation flux density realizing by material of the present invention can make inductor components miniaturization and still keep good magnetic.
Compacting and heat treatment
Before compacting, the iron-based compositions of this coating can with suitable organic lubricant for example wax, oligomer or polymer, fatty acid-based derivative or its combined hybrid.The example of proper lubrication agent is EBS, i.e. ethylenebisstearamide can be available from sweden's
Figure BDA0000432355570000112
metallic stearate, as zinc stearate or aliphatic acid or their other derivative.This lubricant can be with the 0.05-1.5% of total mixture, and preferably the amount of 0.1-1.2 % by weight is added.
Can at the temperature of ambient temperature or rising, under the compaction pressure of 400-1200MPa, carry out compacting.
After compacting, the highest 800 ℃, preferably at the temperature of 600-750 ℃, compacting parts are imposed to heat treatment.The example of the appropriate atmosphere in heat treatment is inert atmosphere, for example nitrogen or argon gas, or oxidizing atmosphere, for example air.The pressure forming of the iron-based magnetic powders covering by New insulated coating obtains powder core of the present invention.This magnetic core is with at 2-100kHz, and the low total losses (being approximately less than 12W/kg under 20kHz frequency) in the frequency range of 5-100kHz and 0.05T's is sensed as feature conventionally.In addition, electricalresistivityρ is greater than 1000, is preferably greater than 2000, is most preferably greater than 3000 μ Ω, and saturation flux density Bs is higher than 1.1, preferably higher than 1.2, most preferably higher than 1.3T.In addition, coercive force should be lower than 210A/m, and preferably lower than 200A/m, most preferably lower than 190A/m, and the DC bias voltage under 4000A/m is not less than 50%.
Embodiment
Following embodiment is intended to illustration specific embodiments, and should not be interpreted as limiting the scope of the invention.
Embodiment 1
Use the iron powder of two types as core grain; Have higher than the pure water atomized iron powder of the iron content of 99.5 % by weight and there is the pure sponge iron higher than the iron content of 99.5 % by weight.The particle mean size of this powder of two types is all about 45 microns.Core grain is mixed with the sendust grinding (85%Fe, 9.5%Si and 5.5%Al conventionally), then according to WO2008/069749, with solution containing phosphate, process this mixture of powders.In brief, by 30 milliliter of 85 % by weight phosphoric acid is dissolved in 1000 milliliters of acetone and prepares coating solution, every 1000 grams of powder are used 40 milliliters of-60 milliliters of acetone solns.After mixed phosphate solution and metal dust, make this mixture dry.
By the dry phosphorus of gained apply iron-sendust mixed-powder according to following table 1 further with kaolin and sodium metasilicate fusion.After dry at 120 ℃, by this powder and 0.6%
Figure BDA0000432355570000113
the mixed ring that is compacted into 55 millimeters of 45 millimeters of internal diameters, external diameter and high 5 millimeters under 800MPa that is incorporated in.After this in nitrogen atmosphere, at 700 ℃, compacting parts are imposed to heat treatment 0.5 hour.
By four point measurement methods, measure the ratio resistivity of gained sample.For maximum permeability μ maxand coercivity measurement, this ring is coiled to 100 in primary circuit and turn and in secondary circuit, coil 100 and turn, to can measure magnetic by hysteresis graph Brockhaus MPG100.For core loss, this ring coils 30 by Walker Scientific Inc.AMH-401POD instrument and turns and in secondary circuit, coil 30 and turn in primary circuit
When measuring incremental permeability, this ring is coiled to (third winding) for three times to supply the DC bias current of 4000A/m.Percentage as maximal increment magnetic permeability represents DC bias voltage.
Unless otherwise specified, correspondingly carry out all tests in following embodiment.
In order to show, use the impact that has the character for compacting and heat processing unit of kaolin and sodium metasilicate in sponge or atomization iron, phosphorous layer and the second coating together with the sendust grinding, according to table 1, prepare sample A-H, it also shows the result from unit test.In table 1, also by the present invention with according to US4177089, in the situation that there is no the first phosphor coating, use sponge iron (sample D) to compare.
Table 1
Figure BDA0000432355570000131
As can be seen from Table 1, the combination of atomization iron, sendust, the first phosphor coating and the second coating of consisting of kaolin and sodium metasilicate has significantly improved resistivity and has therefore reduced core loss.It compares with 100% sendust the saturation flux density that also provides good.
Embodiment 2
For the sendust that only has the first phosphor coating the adulterate atomized iron powder that pure phosphorus and kaolin-sodium metasilicate apply the possibility that significantly strengthens the magnetic property of compacting parts for illustration, prepare following sample.Table 2 has also shown the result from unit test.
Table 2
Figure BDA0000432355570000141
As can be seen from Table 2, it is useful on sendust particle, having the first phosphor coating.
Embodiment 3
By changing the sendust content in atomized iron powder, can control the magnetic property through compacting and heat treated parts.Following sample is all processed in the same manner---the first phosphor coating and the second coating being formed by 2% kaolin clay and 0.4% sodium metasilicate, be densified to 800MPa, and heat treatment 0.5 hour at 700 ℃ in nitrogen atmosphere.Difference between sample is, has changed the sendust content in atomized iron powder.Table 3 has also shown the result from unit test.
Table 3
Figure BDA0000432355570000151
As can be seen from Table 3, the even a small amount of sendust in atomized iron powder has also strengthened the magnetic property of compacting and heat treated parts.
Embodiment 4
This embodiment shows that phosphorus-clay of the present invention-silicate coating concept is applicable to the different grain size of iron powder, and sendust powder has the fixedly granularity of about 45 microns.For sample V), use the iron powder of particle mean size～45 micron, for sample W), use the iron powder of particle mean size～100 micron, for sample X), use the iron powder of particle mean size～210 micron.With the first phosphorous layer, apply this iron-sendust mixture of powders.After this some samples are further processed with 1% kaolin and 0.4% sodium metasilicate as mentioned above.In nitrogen, at 700 ℃, heat-treat 0.5 hour.
Sample V-X) test result can be in Table 4.
Table 4
Figure BDA0000432355570000161
Table 4 shows, regardless of the granularity of iron powder, all obtains the resistivity of parts of the present invention and the clear improvement of core loss.
Embodiment 5
Embodiment 5 illustrations can be used dissimilar waterglass and the dissimilar clay containing specific page silicate.60% atomization iron-40% sendust mixture of powders applies as mentioned above, and different is to use various silicate (Na, K and Li) and the various clay that contains the phyllosilicate with electric neutrality layer (kaolin and talcum).In comparative example, use the clay that contains the phyllosilicate with charged layer,
Figure BDA0000432355570000162
and mica. it is the trade name from the clay of smectites.Mica used is muscovite.The second layer in all tests contains 1% clay and 0.4 % by weight waterglass.In nitrogen, at 700 ℃, heat-treat 0.5 hour.
Following table 5 has shown the result from unit test.
Table 5
Figure BDA0000432355570000171
As seen from Table 5, can use various types of waterglass and containing the clay of specific page silicate, condition is that this phyllosilicate is the type with electric neutrality layer.
Embodiment 6
Embodiment 6 illustrations, by changing the amount of second layer medium clay soil and alkaline silicate, can control and optimize the character through compacting and heat treated parts.Prepare as mentioned above and specimen.In nitrogen, at 700 ℃, heat-treat 0.5 hour.
Following table 6 shows test results.
Table 6
As can be seen from Table 6, if the sodium metasilicate content in the second layer surpasses 0.7 % by weight, resistivity decreased.When the content of sodium metasilicate reduces, resistivity also reduces, so the content of silicate should be the 0.2-0.7 % by weight of total 60% atomization iron-40% sendust mixture of powders, preferred 0.3-0,6 % by weight.Clay content in the second layer is further increased to about 4% can improve resistivity, but because the coercive force improving reduces core loss.Therefore, on the clay in the second layer, be limited to 5 % by weight of this composite powder, preferably 4 % by weight.Under clay content, be limited to 1%, be preferably 3%, because too low clay content has adverse effect to resistivity and core loss.
Embodiment 7
Following embodiment 7 illustrations powder manufactured according to the present invention can be real at different compaction pressures and different compaction tool temperatures.Following sample is processed as mentioned above, and 60% atomization iron and 40% sendust apply with phosphorus and clay-sodium metasilicate, 0.4 % by weight that 2 % by weight that the kaolin content in the second layer is compound iron-sendust and sodium metasilicate content are compound iron-sendust.
At 20 ℃ or 60 ℃ of compaction tool temperature by sample o-v) be densified to 400-1200MPa and heat treatment 0.5 hour at 700 ℃ in nitrogen.Test result can be in Table 7.
Table 7
Figure BDA0000432355570000191
Table 7 shows, is densified to different compaction pressures and obtains high resistivity and low core loss at the parts of the present invention of different compaction tool temperatures realities.When compaction pressure is increased to 800MPa from 400, can observe density rising and loss and reduce, but further improve compaction pressure, almost there is no effect.Compaction tool temperature only slightly improves resistivity, and does not realize any further improvement of magnetic.
Embodiment 8
Following embodiment 8 is illustrated in the parts that under different atmosphere and different temperatures, heat treatment is made by powder of the present invention.Following sample is processed as mentioned above, 60% atomization iron and 40% sendust apply with phosphorus and clay-sodium metasilicate, 0.4 % by weight that 2 % by weight that the kaolin content in the second layer is compound iron-sendust and sodium metasilicate content are compound iron-sendust.
Sample w-Dd) heat treatment at 550-750 ℃ in nitrogen and air respectively.Test result can be in Table 8.
Table 8
Figure BDA0000432355570000201
Table 8 shows, in nitrogen atmosphere or in the mixed atmosphere of nitrogen and air, at 650 ℃-750 ℃, heat treated parts of the present invention obtain high resistivity and low core loss.
Embodiment 9
Following embodiment 9 illustrations, by the FeSi of aerosolization is added in this mixture, can be promoted the magnetic property of the parts of being made by powder of the present invention.The second layer that this iron-sendust mixture of powders has the first phosphor coating and consists of 2% kaolin and 0.4% sodium metasilicate.This mixture of powders has been densified to 800MPa and heat treatment 30 minutes at 700 ℃ in nitrogen atmosphere.
Table 9
Figure BDA0000432355570000211
In table 9, can find out, in iron-sendust mixture of phosphorus and the coating of kaolin-sodium metasilicate, add 10%FeSi to improve resistivity and reduced coercive force and core loss.
Embodiment 10
Use has pure water atomized iron powder higher than the iron content of 99.5 % by weight as core grain.The particle mean size of this powder is approximately 45 microns.Core grain is mixed with sendust (85%Fe, 9%Si and 6%Al conventionally), and with solution containing phosphate, process this mixture of powders according to WO2008/069749.The dry phosphorus of gained applies iron powder-sendust mixture and by second (metal is organic) coating, further processes described in WO2009/116938, by stirring by this powder the first alkaline aminoalkyl-alkoxy silane from different amounts
Figure BDA0000432355570000212
after this oligomer of aminoalkyl/alkyl-alkoxy silane
Figure BDA0000432355570000213
(use 1:1 relation, all by Evonik Inc., produced) mixes.Bismuth oxide (III) fine powder (>99 % by weight by said composition from different amounts; D 50～0.3 micron) further mix.
After coating, this powder is mixed with 0.4% amide waxe and be depressed into the ring that 800MPa is compacted into 55 millimeters of 45 millimeters of internal diameters, external diameter and high 5 millimeters.After this in nitrogen atmosphere, at 700 ℃, compacting parts are imposed to heat treatment 0.5 hour.
Unless otherwise specified, correspondingly carry out all tests in following embodiment.
According to table 10, prepare sample Hh-Ii), it also shows the result from unit test.
Table 10
Figure BDA0000432355570000221
As can be seen from Table 10, compare with using 100% atomized iron powder, the combination of atomized iron powder, sendust, the first phosphor coating and second (metal is organic) coating has significantly improved resistivity, DC bias voltage and has reduced core loss and coercive force.
Embodiment 11
By changing the sendust content in atomized iron powder, can control the magnetic of compacting and heat processing unit.Following sample is all processed the-the first phosphor coating and second (metal is organic) coating in the same manner.Difference between sample is, changes the sendust content in atomized iron powder.Sample is all depressed into 800MPa and heat treatment 0.5 hour at 700 ℃ ℃ in nitrogen atmosphere.Table 11 has also shown the result from unit test.
Table 11
Figure BDA0000432355570000231
The atomization iron applying about clay/sodium metasilicate-and sendust-mixture of powders, the sendust share of raising is significantly improved resistivity and DC bias voltage and is therefore reduced core loss and coercive force.

Claims (15)

1. compound iron-based powder combination, it comprises core grain, and wherein said core grain is the mixture of following material:
(a) ferroalloy particle, it consists of the iron of 7 % by weight to 13 % by weight silicon, 4 % by weight to 7 % by weight aluminium and surplus substantially, and
(b) iron particle of atomization,
And wherein said core grain is applied by the first phosphorous layer.
2. according to the compound iron based powders of claim 1, the iron particle of wherein said atomization has the second layer, and this second layer comprises:
(a) with the alkaline silicate of being combined containing the clay mineral of phyllosilicate, silicon-oxygen tetrahedral layer and the hydroxide octahedral layer of the merging of phyllosilicate are electroneutral; Or
(b) metal organic layer.
3. according to the compound iron based powders of claim 2, wherein said ferroalloy particle has the second layer, and this second layer comprises:
(a) with the alkaline silicate of being combined containing the clay mineral of phyllosilicate, silicon-oxygen tetrahedral layer and the hydroxide octahedral layer of the merging of phyllosilicate are electroneutral; Or
(b) metal organic layer.
4. according to the compound iron based powders of claim 3, the iron particle of wherein said ferroalloy particle and described atomization has the identical second layer.
5. according to the compound iron-based powder combination of claim 2-4 any one, the wherein said second layer comprises kaolin and sodium metasilicate.
6. according to the compound iron-based powder combination of claim 1-5 any one, it further comprises the FeSi of atomization,
7. according to the compound iron-based powder combination of claim 1-6 any one, wherein said phosphorous layer has the thickness of 20 to 300 nanometers.
8. according to the compound iron based powders of claim 1-7 any one, wherein by core grain being contacted with the phosphorus compound in solvent, after this providing described phosphor coating by dry except desolventizing.
9. according to the compound iron based powders of claim 1-8 any one, wherein said phosphorus compound is phosphoric acid or ammonium phosphate.
10. according to the compound iron based powders of claim 2-9 any one, wherein the content of alkaline silicate is the 0.1-0.9 % by weight of described compound iron based powders, preferably 0.2-0.8 % by weight.
11. according to the compound iron based powders of claim 2-10 any one, and wherein clay content is the 0.2-5 % by weight of described compound iron based powders, preferably 0.5-4 % by weight.
12. manufacture the method for compacting and heat treated parts, comprise the steps:
A) provide according to the compound iron based powders of claim 1-11 any one,
B) in mould under 400 to 1200MPa compaction pressure with unidirectional pressurization campaign by optionally with the compound iron based powders compacting of mix lubricant,
C) from mould, release compacting parts,
D) parts that are pushed out described in heat treatment at the temperature of the highest 800 ℃ in non-reduced atmosphere.
13. parts of making according to the method described in claim 12.
14. according to the parts of claim 13, and described parts are inductor cores.
15. according to the inductor core of claim 14, and it has and is greater than 1000, is preferably greater than 2000, is most preferably greater than the electricalresistivityρ of 3000 μ Ω; Higher than 1.1, preferably higher than 1.2, most preferably higher than the saturation flux density Bs of 1.3 (T); Under 20kHz frequency, be less than the core loss of 12W/kg; The induction of 0.05T; Lower than 210A/m, preferably lower than 200A/m, most preferably lower than the coercive force of 190A/m; With the DC bias voltage that is not less than 50% under 4000A/m.
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