CN1902719A - Powder composition, method for making soft magnetic components and soft magnetic composite component - Google Patents

Powder composition, method for making soft magnetic components and soft magnetic composite component Download PDF

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Publication number
CN1902719A
CN1902719A CNA2004800394525A CN200480039452A CN1902719A CN 1902719 A CN1902719 A CN 1902719A CN A2004800394525 A CNA2004800394525 A CN A2004800394525A CN 200480039452 A CN200480039452 A CN 200480039452A CN 1902719 A CN1902719 A CN 1902719A
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iron
composition
weight
lubricant
soft magnetic
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CN100533610C (en
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L·谢伦
A·阿赫林
L·胡尔特曼
O·安德森
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Hoganas AB
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/02Apparatus 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
    • H01F41/0206Manufacturing of magnetic cores by mechanical means
    • H01F41/0246Manufacturing of magnetic circuits by moulding or by pressing powder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16Metallic particles coated with a non-metal
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets 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
    • H01F1/14Magnets 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
    • H01F1/20Magnets 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
    • H01F1/22Magnets 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
    • H01F1/24Magnets 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
    • H01F1/26Magnets 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 by macromolecular organic substances
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/105Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing inorganic lubricating or binding agents, e.g. metal salts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • B22F2003/248Thermal after-treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making 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
    • B22F9/082Making 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
    • B22F2009/0824Making 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 with a specific atomising fluid
    • B22F2009/0828Making 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 with a specific atomising fluid with water
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00Aspects linked to processes or compositions used in powder metallurgy
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/22Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • B22F3/225Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/02Making ferrous alloys by powder metallurgy

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  • Metallurgy (AREA)
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Abstract

The invention concerns powder compositions consisting of electrically insulated particles of a soft magnetic material of an iron or iron-based powder and 0.1-2% by weight of a lubricant selected from the group consisting of fatty acid amides having 14-22 C atoms. Optionally a thermoplastic binder such as polyphenylene sulphide may be included in the composition. The invention also concerns a method for the preparation of soft magnetic composite components.

Description

The method of powder composition, manufacturing soft magnetic components and soft magnetic composite component
Technical field
The present invention relates to iron-based powder combination.More specifically, the present invention relates to be used for making the powder composition of soft magnetic composite component by powder metallurgy manufacturing approach.These compositions help making the soft magnetic composite component with high density and valuable magnetic property and mechanical performance.
Background technology
Soft magnetic material is used for following purposes: for example, and the core in the inductor, the stator of generator and rotor, adjuster, transducer and transformer core.Traditionally, soft magnetic core, for example rotor in the generator and stator are made by piling up the steel laminated material.Soft magnetism compound (SMC) material is based on the soft magnetism particle that has electric insulation coating layer on each particle (normally iron-based).Use traditional powder metallurgic method with insulating particle compacting (optional), obtain the SMC parts thus with lubricant and/or adhesive.Compare with the method for using the steel laminated material, the material that uses this powder metallurgy technology to make to have the higher SMC element design degree of freedom because the SMC material can carry three-dimensional magnetic flux, and can obtain 3D shape by pressing.
Two key characteristics of iron-core element are its magnetic permeability and core loss characteristics.The magnetic permeability of material is the indication of the ability of its ability that is magnetized or its carrying magnetic flux.Magnetic permeability is meant the ratio of induced flux and magnetizing force or field intensity.When making magnetic material be exposed in the alternating magnetic field, because magnetic hysteresis loss and eddy current loss and produce power loss, core loss.Magnetic hysteresis loss is by for the essential energy consumption of restraining in the iron-core element of residual magnetic force causes, and proportional with the frequency of alternating field.Eddy current loss causes by producing electric current in the iron-core element, and square proportional with the frequency of alternating field, and the electric current in the iron core produces because of the variations of flux that alternating current (AC) condition causes.Therefore for making the eddy current minimum, high resistivity is desirable, and particularly important under higher frequency.For the magnetic hysteresis loss that reduces the core element that is used for the alternating current purposes and improve its magnetic permeability, need heat-treat the parts of compacting usually.
Exploitation has been pointed in the research of the powder metallurgy manufacturing of the magnetic core element of using the coating iron-based powder improved the iron powder composition that some physics and magnetic property can not damage other performance of final element again.Required element function comprises, for example, and by high magnetic permeability, low core loss, high saturation induction, (high density) and the high strength of the frequency range that enlarges.Usually, the component density of increase has improved all these performances.
Required powder property comprises the applicability for compression molding techniques, this means that powder is molded as high density, high strength components easily, and this element ejects from molding equipment easily, and element has level and smooth surface smoothness.
The present invention relates to a kind of novel powder composition, and this powder composition is used to prepare the purposes of soft magnetic composite component with required powder property.This new compositions can be suppressed the element that (and heat treatment) becomes to have desired properties.
The invention still further relates to method and soft magnetic components itself that a kind of manufacturing has the soft magnet base member of excellent element function.
Brief summary of the invention
In brief, powder composition of the present invention is that electric insulation particle and fatty acid amide lubricant by soft magnetic material constitutes.Randomly, there are thermoplastic adhesives in the composition.Method of the present invention comprises the heat treatment of mixing, compacting and optional gained element, has the soft magnet base member of excellent properties thereby produce.
Detailed Description Of The Invention
This powder preferably substantially pure, water-atomized iron powder or iron sponge powder with irregular shape of particle.In this article, term " substantially pure " is meant that the amount that powder should not contain field trash and impurity O, C and N substantially should remain on minimum.Particle mean size is usually less than 300 microns to being higher than 10 microns.The example of these powder is available from ABC 100.30, the ASC100.29 of Sweden Hoganas AB, AT 40.29, ASC 200, ASC 300, NC 100.24, SC 100.26, MH 300, MH 40.28, MH 40.24.
According to a specific embodiment of the present invention, used powder contains than the normal thick particle of situation in the common mold pressing.In the practice, this means that powder does not contain particulate substantially.Term " do not contain particulate substantially " and be meant be less than about 10%, preferably be less than 5% powder particle and have granularity less than 45 microns, this granularity is to record by the method for describing among the SS-EN 24497.Average grain diameter is generally 106 to 425 microns.Greater than 212 microns particle weights usually above 20%.Maximum particle size can be about 2 millimeters.
The size of iron-based particle commonly used distributes according to Gaussian distribution curve in PM industry, and its average grain diameter is 30 to 100 microns, and the particle of about 10-30% is less than 45 microns.Therefore, powder may have the particle size distribution that departs from powder commonly used used according to the present invention.Powder that can be by removing thin part or have the powder that desired particle size distributes by manufacturing and obtain these meal.Yet, the invention is not restricted to meal, also comprise the powder of the mold pressing granularity commonly used that has in the PM industry among the present invention.
The electric insulation layer of powder particle can be made by inorganic material.What particularly be fit to is disclosed insulating barrier type (being incorporated herein by this reference) among the US 6348265, and it relates to the basic powder particle that the iron by the substantially pure of the separator that contains oxygen and phosphorus that contains insulation constitutes.About coating, should especially propose, coating layer thickness may influence the performance of composite component.The powder that contains insulating particle can be used as Somaloy TM500 and 550 available from Sweden Hoganas AB.
Lubricant is selected from fatty acid amide used according to the present invention.Particularly suitable acid amides is to contain 12-24, preferred 14-22 carbon atom, the primary amide of the saturated or unrighted acid of 18-22 carbon atom most preferably.Lubricant quantity can be lower than 2 weight % of composition weight, preferably is lower than 1.5 weight %.It is 0.05-1 weight % that lubricant is particularly preferably measured, preferred 0.05 to 0.8, more preferably 0.1 to 0.8 weight %, most preferably 0.1 to 0.5 weight %.Particularly preferred lubricant is stearic amide, oleamide, docosanoic acid acid amides, erucic acid (eurcic acid) acid amides, palmitamide, and stearic amide most preferably.At United States Patent (USP) 6,537, in 389, mention the stearic amide that combines with rapeseed methylester as lubricant, also mention as in thermoplastic resin, the polyphthalamide (polyphatalamide) of the adhesive of compacting soft magnetic powder.
Kollag has the density of about 1-2 gram/cubic centimetre usually, and this compares very low with the iron-based powder density of about 7.8 gram/cubic centimetres.Therefore, in composition, comprise the solid density that the lower lubricant of these density can reduce the compacting element.Therefore, lubricant being kept is important for making high density components on a small quantity.Yet the lubricant of low amount is easy to generate (ejection) problem that ejects.Be surprised to find that the lubricant of the above-mentioned type amount of can hanging down is used under the situation that does not produce the problem of ejecting.
By replacing internal lubricant (promptly adding the lubricant in the iron-based powder mix to) with die wall lubrication (DWL), and be used in combination high pressing pressure, can obtain high green density.Yet when pressing down system insulation iron-based powder at high pressing pressure, a shortcoming of this known method is, destroys the insulating barrier of iron-based powder easily, thereby causes the high core loss under upper frequency.In addition, the use meeting of DWL further increases process complexity, and this can prolong circulation timei and reduce production stability in the industrial environment.
According to the present invention, can use fatty acid amide as the unique additive in insulation iron or the iron-based powder, certainly, for some application, it is favourable adding small amount of thermal plastic resin, especially polyphenylene sulfide (PPS).Term " on a small quantity " this be meant be lower than composition weight 2, preferably be lower than 0.8, more preferably less than 0.6, most preferably be lower than 0.5 weight %.When amount is lower than 0.05 weight %, do not observe any effect of PPS.Particularly, the amount of PPS can not wait between 0.1 to 0.5 weight %, preferred 0.2 to 0.5 or 0.4 weight %.When the good frequency stability of needs, the interpolation of PPS is useful especially.
PPS and stearic combination are known from patent application WO01/22448.The embodiment of this application discloses and can make soft magnetic material by the electric insulation iron-based powder is mixed with PPS and stearic acid.This mixture suppressed at elevated temperatures and with the parts of gained compacting in blanket of nitrogen 260 ℃ of heat treatments, then 285 to 300 ℃ of secondary heat treatment.Be surprised to find that,, can obtain some advantages by using this novel powder compositions (it has comprised fatty acid amide but not corresponding aliphatic acid).For example, have been found that novel powder has unexpected improved greasy property, this make will compacting parts to eject the required energy that ejects from mould lower, can obtain higher density, and can obtain better cross-breaking strength.In addition, pressing step can carry out at ambient temperature.In addition, can make heat treatment easier, disclose the first required heat treatment step because can omit according to WO.
The iron-based magnetic that contains insulating particle and combine with thermoplastic resin has been described in U.S. Patent application 2002/0084440.Opposite with particle of the present invention, known particle also contains rare earth element before these.In addition, the consumption of thermoplastic resin is relatively large, i.e. at least 5 weight %.In addition, the granularity of iron-based powder quite little (as an example, having mentioned 3 microns).Can also comprise the lubricant that is selected from the number of chemical compound.These powder compositions preferably can be used for injection moulding according to stating, extrude, injection compression and injection press be with preparation high-weatherability bonding permanent magnet.
In order to prepare composite component of the present invention, single shaft pressed powder composition in the punch die that mustn't lubricate usually at first, but this powder composition also can use in lubricated punch die.Element with compacting ejects from punch die and optional heat-treating then.
Compacting can be in the temperature of ambient temperature or rising and is carried out under the pressure of the highest 1500MPa.
According to preferred embodiment of the present invention, be compressed in the instrument of appropriate heating and carry out, because not only can improve green density thus and eject performance, can also improve maximum relative permeability.The element function that will press down system at the temperature that raises and low pressing pressure with compare with the element function that the higher pressure pressing pressure presses to identical green density in ambient temperature, Ya Zhi element has higher magnetic permeability at elevated temperatures.For bigger element, may also must improve powder temperature to realize improvement of the present invention.
Heat treatment can be carried out in one or several steps.A step heat treatment of recommending is to carry out between 250 to 550 ℃ 30 minutes to 4 hours in oxygen-containing atmosphere (air).
Another selection is to heat-treat 30 minutes to 3 hours at 250-350 ℃ in air or inert gas, heat treatment 15 minutes to 2 hours between 350 to 550 ℃ in containing oxygen (air) atmosphere then.
When comprising PPS in the composition, recommend to use different slightly heat treatment.For example, in this case, heat treatment can be carried out 30 minutes to 4 hours at 250-350 ℃ in oxygen-containing atmosphere (air).Another selection is to heat-treat 30 minutes to 3 hours at 250-350 ℃ in air or inert gas, then in oxygen-containing atmosphere (air) 300 to 500 ℃ of heat treatments 15 minutes to 2 hours.
Can use different atmosphere, time and temperature to heat-treat to obtain to have the final element of desired properties, this makes this novel powder compositions particularly attractive.
By high pressure (for example being higher than 800MPa) down compacting contain the iron-based insulating powder with coarse grain and the composition of lubricant as mentioned above, then repressed element is heat-treated, obtain the soft magnetic composite component of density 〉=7.5 gram/cubic centimetres, maximum relative permeability μ max 〉=600, coercivity H≤250A/m and electricalresistivity 〉=20 μ Ω m.This element can be used in stator in the engine for example and the rotor elements required high request and uses.
Further set forth the present invention by the following example.
Embodiment 1
Use following material.
Use iron-based water atomised powder as raw material, its particle contains thin inorganic coating (Somaloy TM500, can be available from Sweden Hoganas AB).
The PPS powder,
The stearic acid powder, lubricant A,
The stearic amide powder, lubricant B.
According to table 1, with 3 kilograms of basic powder Somaloy TM500 mix with PPS and stearic amide or stearic acid.
Table 1. mixture of powders: lubricant and PPS (weight %)
Sample number PPS Lubricant
A1 0.60% 0.2%A
A2 0.50% 0.3%A
A3 0.50% 0.3%B
A4 0.30% 0.3%B
A5 0.30% 0.4%B
A6 0.30% 0.5%B
A7 0.1% 0.3%B
A8 0.2% 0.3%B
A9 - 0.4%B
Mixture of powders is depressed to 45 millimeters of internal diameters, 55 millimeters of external diameters and high 5 millimeters ring-type sample at 800MPa and ambient temperature (room temperature).The ring-type sample that same compacting is 10 millimeters high, and on these samples, measure ejecting force.Ejecting energy is presented in the table 2.The result shows, uses fatty acid amide to obtain the obviously lower energy that ejects.
Table 2. records on the ring-type sample of h=10 millimeter ejects energy
Sample number PPS Lubricant Eject energy (Jiao/square centimeter)
A1 0.60% 0.2%A 52
A2 0.50% 0.3%A 46
A3 0.50% 0.3%B 38
A4 0.30% 0.3%B 37
A5 0.30% 0.4%B 33
A6 0.30% 0.5%B 30
A7 0.10% 0.3%B 41
A8 0.20% 0.3%B 39
A9 - 0.4%B 35
After the compacting, with parts 290 ℃ of heat treatments 120 minutes in air.The heat treated ring rotation 25 of gained is changeed.According to standard IEC 60404-6, second edition 2003-06 measures relative AC inductance magnetic permeability with LCR-meter (HP4284A).
Table 3 and 4 has shown the decline of initial permeability (frequency stability).The decline of initial permeability be expressed as 10 and 100kHz under the difference of initial permeability divided by the initial permeability under the 10kHz.Table 3 shows, by the amount of fatty acid amide is increased to 0.5% from 0.3, can obtain better frequency stability.Table 4 shows, uses fatty acid amide to replace corresponding aliphatic acid, can obtain better frequency stability.In addition, table 4 shows that when not using PPS, frequency stability descends more.Yet,, be 95 at the initial permeability of 1kHz according to survey, and A3 is 75 for A9.High initial magnetoconductivity under lower frequency is favourable for some application.
The decline of table 3 initial permeability
Dμ10-100kHz(%)
A4 7.4
A5 5.2
A6 4.2
The decline of table 4 initial permeability
Dμ10-100kHz(%)
A2 6.4
A3 3.9
A9 20.9
By four point measurement method measured resistivity and be presented in the table 5.From this table, as can be seen, use fatty acid amide to replace corresponding acid, can obtain obviously higher resistivity.
The resistivity of table 5. ring-type sample
Sample number PPS Lubricant Resistivity, resistance coefficient μ Ohm*m
A2 0.50% 0.3%A 316
A3 0.50% 0.3%B 400
In addition, at 290 ℃ of heat treatments after 120 minutes in air, the cross-breaking strength TRS of specimen.According to ISO 3995 test TRS.On parts, test TRS at 200 ℃ equally.TRS is presented in the table 6.The sample that contains 0.5%PPS and 0.3% stearic amide (A3) is compared with the sample that contains 0.2%PPS+0.6% stearic acid (A1) with the sample that contains 0.5%PPS and 0.3% stearic acid (A2), all shows obviously higher TRS room temperature (RT) and 200 ℃.For the mixture with low organic substance total content, density is higher, and this causes higher induction and magnetic permeability (μ max).
Table 6. is at the density and the TRS of room temperature and 200 ℃
Sample number PPS Lubricant Density gram/cubic centimetre after the heat treatment TRS room temperature MPa TRS 200℃ MPa
A1 0.60% 0.2%A 7.18 68 51
A2 0.50% 0.3%A 7.18 46 30
A3 0.50% 0.3%B 7.19 81 67
A4 0.30% 0.3%B 7.27 88 73
A5 0.30% 0.4%B 7.22 87 73
A6 0.30% 0.5%B 7.17 51 68
A7 0.1% 0.3%B 7.35 85 74
A8 0.2% 0.3%B 7.31 84 71
A9 - 0.4%B 7.33 87 78
Embodiment 2
Use following material.
Use iron-based water atomised powder as raw material, its particle has phosphorous inorganic shallow layer (Somaloy TM500, available from Sweden Hoganas AB).
The PPS powder,
The stearic acid powder, lubricant A,
The stearic amide powder, lubricant B,
The docosanoic acid powder, lubricant C,
The oleamide powder, lubricant D,
Kenolube TM
According to following table 7, with basic powder Somaloy TM500 with PPS and mix lubricant.
Table 7. mixture of powders: lubricant and PPS (weight %)
Sample number PPS Lubricant
B1 0.50% 0.3%A
B2 0.50% 0.3%B
B3 0.50% 0.3%C
B4 0.50% 0.3%D
B5 0.30% 0.3%B
B6 - 0.4%B
B7 - 0.3%B
B8 0.1% 0.3%B
B9 0.2% 0.3%B
B10 - 0.4%Kenolube TM
Mixture of powders is pressed into test-strips according to ISO 3995 under the pressing pressure of 800MPa and ambient temperature.After the compacting, parts are heat-treated in two step heat treatments.The first step was carried out 105 minutes at 290 ℃ in inert nitrogen atmosphere.After this step is at 350 ℃ of heat treatment steps that carry out 60 minutes in air.Cross-breaking strength TRS according to ISO 3995 specimen.
The result of cross-breaking strength test is presented in the table 8.As can be seen from Table 8, the sample made from the mixture of fatty acids acid amides produces enough TRS values.Reach higher density after the heat treatment, this is favourable to induction and magnetic permeability.If PPS content reduces to 0.3% or lower, TRS rises to the above value of 80MPa.Do not contain PPS and contain the sample of stearic amide lubricant even have the above TRS value of 100MPa.The lubricant Kenolube that tradition is used TMUse can not produce required cross-breaking strength.
Density under table 8. room temperature and TRS
Sample number PPS Lubricant Density after the heat treatment TRS-RT
Gram/cubic centimetre MPa
B1 0.50% 0.3%A 7.18 73
B2 0.50% 0.3%B 7.22 68
B3 0.50% 0.3%C 7.23 73
B4 0.50% 0.3%D 7.24 74
B5 0.30% 0.3%B 7.32 83
B6 - 0.4%B 7.37 108
B7 - 0.3%B 7.41 113
B8 0.1% 0.3%B 7.35 88
B9 0.2% 0.3%B 7.32 79
B10 - 0.4%Kenolube TM 7.42 32
Embodiment 3
This embodiment shows, compare with the ethylene bis stearamide lubricant with the zinc stearate that generally uses, when using low amount fatty acid amide lubricant of the present invention and being used in combination meal and during high pressing pressure, eject the low ejecting force of acquisition in the process at the compacting element, and obtain to eject the perfect surface smoothness of element.
Meet US 6,348,265 soft magnetism iron-based meal (wherein particle is surrounded by inorganic insulating material) and the mix lubricant of 0.2 weight % with two kilograms according to table 9.The particle size distribution of iron-based meal is presented in the table 10.Mixture E and F are the Comparative Examples that comprises known lubricants.
Table 9
Mixture Lubricant
A The docosanoic acid acid amides
B Erucyl amide
C Stearmide
D Oleamide
E Zinc stearate
F Ethylene bis stearamide
Table 10
Granularity (micron) Weight %
>425 0.1
425-212 64.2
212-150 34.0
150-106 1.1
106-75 0.3
45-75 0.2
<45 0
The cylindrical specimen (50 gram) of transferring to the gained mixture in the punch die and under the pressing pressure of 1100MPa, moving and be pressed into 25 millimeters of diameters with the single shaft compacting.Used die materials is traditional tool steel.Ejecting in the process of compacting sample, the record ejecting force.Record eject sample required always eject energy/coating (enveloping) area.Following table 11 has shown and has ejected energy, green density and surface smoothness.
Table 11
Mixture Eject energy (Jiao/square centimeter) Green density (gram/cubic centimetre) Surface smoothness
A 90 7.64 Perfect
B 83 7.65 Perfect
C 93 7.63 Perfect
D 70 7.67 Can accept
E 117 7.66 Unacceptable
F 113 7.64 Perfect
Embodiment 4
The following example shows that the particle size distribution of soft magnet based powders is to ejecting the influence of performance and green density.Use is according to " slightly " powder of embodiment 3." carefully " particle size distribution of powder is listed in the table 12.Use 0.2 weight % stearmide to prepare mixture according to the program of embodiment 3.Mixture based on " carefully " powder is made sample H by mark, opens with sample C to compare.
Table 12
Granularity (micron) Weight %
>425 0
425-212 0
212-150 11.2
150-106 25.0
106-75 22.8
45-75 26.7
<45 14.3
According to embodiment 3 used programs mixture is pressed into cylindrical sample.Following table 13 has shown green density and appearance.
Table 13
Mixture Green density (gram/cubic centimetre) Surface smoothness
C 7.63 Perfect
H 7.53 Can accept
As can be seen from Table 13, the composition that contains fine powder produces lower green density and impaired surface smoothness.
Embodiment 5.
This embodiment has compared the known lubricant ethylene bis stearamide (EBS) and the example of lubricant stearmide.Use mixes with EBS and stearmide respectively according to table 14 according to " slightly " powder of embodiment 3.Program according to embodiment 3 prepares sample.
Table 14
Mixture EBS (weight %) Stearmide (weight %)
1 0.20 --
2 0.30 --
3 0.40 --
4 0.50 --
5 -- 0.10
6 -- 0.20
7 -- 0.30
Under 1100MPa, mixture of powders is pressed into 45 millimeters of internal diameters, 55 millimeters of external diameters and high 10 millimeters ring.Ejecting in the process of compacting sample, calculate sample is ejected the required energy/coating area that always ejects from punch die.Following table 15 shown calculate eject energy/area, green density and appearance.
Table 15. ejects energy, green density, appearance
Mixture Eject energy [Jiao/square centimeter] Density [gram/cubic centimetre] Appearance
1 54 7.65 Unacceptable
2 40 7.61 Can accept
3 33 7.56 Perfect
4 28 7.51 Perfect
5 73 7.67 Can accept
6 38 7.64 Perfect
7 37 7.59 Perfect
As can be seen from Table 15, can add and be low to moderate 0.2% novel lubricant, and still can obtain perfect surface smoothness, and for reference lubricant EBS, obtain that perfect surface smoothness is minimum will add 0.4%.
Embodiment 6
This embodiment has compared respectively the magnetic property of realizing similarly ejecting the element that energy value required minimum emollient component stearmide and EBS make with being.Magnetic property after the heat treatment of the element of making by mixture 2 and mixture 6 according to embodiment 5 relatively.
Except that highly being 5 millimeters, according to embodiment 5 compacting ring-type samples.With the green compact sample 300 ℃ of heat treatments 60 minutes in air, then 530 ℃ of heat treatments 30 minutes in air.The ring rotation 100sense that gained is heat treated changes and 100drive changes, and tests in the Brockhaus hysteresisgraph.Following table 16 has shown the sensitivity under the 10kA/m, maximum relative permeability, coercive force H cWith the core loss under 400Hz, 1T.
Table 16. soft magnet performance
Sample 2 Sample 6
Maximum permeability 480 750
The B[T of 10000A/m] 1.58 1.66
Hc[A/m] 218 213
Core loss 400Hz, 1T[W/kg] 78.4 42.1
As can be seen from Table 16, element soft magnet performance excellence of the present invention.
Embodiment 7
The following example has shown the influence that eject performance and green density of punch die temperature to the compacting sample.In this embodiment, select the primary amide stearmide as amide lubricant of the present invention.According to the program of embodiment 3, in 2 kilograms of soft magnetism electric insulation iron-based meal, add 0.2% stearmide.
Under the pressing pressure of 1100MPa, mixture of powders is pressed into 45 millimeters of internal diameters, 55 millimeters of external diameters and high 10 millimeters ring.Write down ejecting force in the process ejecting of compacting sample.Calculating ejects the required energy/coating area that always ejects with sample from punch die.Following table 17 has shown and has ejected energy, green density and appearance at the sample of different punch die temperatures systems.
Table 17. ejects energy, green density, appearance under different punch die temperature
The punch die temperature (℃) Eject energy [Jiao/square centimeter] Green density [gram/cubic centimetre] Appearance
25 38.4 7.64 Perfect
50 31.5 7.66 Perfect
60 30.6 7.67 Perfect
70 29.3 7.67 Perfect
80 27.5 7.69 Perfect
As can be seen from Table 17, the raising meeting of punch die temperature produces positive impact to ejecting energy and green density.
Embodiment 8
This embodiment has compared the element function of element made in accordance with the present invention and by the performance of the element of DWL compacting.In embodiments of the invention and Comparative Examples, all use " slightly " powder of embodiment 3.Use 0.2 weight % stearmide as the lubricant in the embodiment of the invention, and the gained powder composition is become green density 80 ℃ controlled punch die temperatures is the ring-type sample of 7.6 gram/cubic centimetres.In Comparative Examples, do not use internal lubricant, and use DWL.At ambient temperature the ring-type sample is depressed into the density of 7.6 gram/cubic centimetres.Ring-type sample external diameter is 55 millimeters, 45 millimeters of internal diameters and high 5 millimeters.
After the compacting, heat-treat according to table 18.By 4 method measured resistivity.In hysteresis graph, carry out before the magnetic measurement, ring-type sample rotation 100drive is changeed and the 100sense commentaries on classics.From the loop, obtain the DC performance with 10kA/m.Under 1T with different frequency measurement core losss.In Fig. 1, draw the functional arrangement of core loss/circulation and frequency.
Table 18: magnetic property
Sample Heat treatment B 10kA/m He [A/m] ρ [μΩm] 1T, 400Hz[W/kg] time core loss
The present invention 530 ℃, 30 minutes, air 1.65 192 103 41
The DWL method Do not have 1.66 305 60 60
The DWL method 530 ℃, 30 minutes, air 1.66 189 3 109
From table 18 and Fig. 1, as can be seen, compare, because lower H with the DWL method cWith higher resistivity, the present invention produces obviously lower core loss in alternating field.
Embodiment 9
In this embodiment, demonstrate the ferrocart core that can obtain to have the excellent magnetic energy by the present invention.Also demonstrate of the positive impact of the punch die temperature of rising to maximum relative permeability.
With " slightly " powder of embodiment 3 and the mix lubricant of different content and type.Make ring-type sample (OD=55, ID=45, h=5 millimeter) and strip sample (30 * 12 * 6 millimeters) with the process conditions that provide in the table 19.
Measure density by quality and the size of measuring the ring-type sample.By 4 methods measured resistivity on the ring-type sample.In the Brockhaus hysteresisgraph, carry out before the magnetic measurement, ring-type sample rotation 100drive is changeed and the 100sense commentaries on classics.From the loop, obtain μ with 10kA/m MaxAnd H cAnd so on the DC performance, simultaneously measure core loss with 1T and 400Hz.On test-strips, measure the cross-breaking strength (TRS) of heat treated parts by three-point bending method.
Table 19: the process conditions of ring-shaped sample
Sample Lubricant type Amounts of lubrication (weight %) Pressing pressure (MPa) The punch die temperature (℃) Heat treatment
1 Stearmide 0.2 1100 25 300 ℃, 45 minutes, air+520 ℃ *, air
2 Stearmide 0.2 1100 80 300 ℃, 45 minutes, air+520 ℃ *, air
3 Stearmide 0.2 800 80 530 ℃, 30 minutes, air
4 Stearmide 0.2 1100 25 530 ℃, 30 minutes, air
5 Stearmide 0.2 1100 80 530 ℃, 30 minutes, air
6 Stearmide 0.1 1100 85 530 ℃, 30 minutes, air
7 Stearmide 0.3 800 25 300 ℃, 1 hour, air+530 ℃, 30 minutes, air
8 Stearmide 0.3 800 80 300 ℃, 1 hour, air+530 ℃, 30 minutes, air
9 Stearmide 0.3 1100 25 300 ℃, 1 hour, air+530 ℃, 30 minutes, air
10 Stearmide 0.3 1100 80 300 ℃, 1 hour, air+530 ℃, 30 minutes, air
11 Erucyl amide 0.2 1100 25 330 ℃, 2 hours, air+530 ℃, 30 minutes, air
12 Erucyl amide 0.2 1100 25 340 ℃, 2 hours, N 2+ 530 ℃, 30 minutes, air
*In element, improve temperature to 520 ℃ with about 4 ℃/minute
Table 20: the measurement of element function
Sample Density (gram/cubic centimetre) μ max Hc (A/m) Resistivity (μ Ohm*m) Core loss under 1T 400Hz (W/kg) TRS (MPa)
1 7.62 754 209 473 42 93
2 7.63 852 204 230 40 97
3 7.60 718 208 103 43 n.a
4 7.62 602 198 591 39 59
5 7.65 861 178 98 37 68
6 7.71 918 177 66 38 78
7 7.49 669 228 574 46 70
8 7.53 880 202 33 48 81
9 7.56 672 224 515 44 67
10 7.62 860 203 64 43 76
11 7.62 633 192 414 38 54
12 7.68 738 205 614 39 67

Claims (23)

1. powder composition, it comprises the soft magnetic material particle of iron or iron-based powder and the lubricant of 0.05 to 2 weight %, described iron or iron-based powder particle have electric insulation layer, and described lubricant is selected from the primary amide of the saturated or unsaturated straight chain fatty acid that contains 12-24 carbon atom.
2. according to the composition of claim 1, wherein aliphatic acid contains 14-22 carbon atom.
3. according to the composition of claim 1 or 2, it is characterized in that fatty acid amide is selected from stearic amide, oleamide, docosanoic acid acid amides, erucyl amide, palmitamide.
4. according to each composition of claim, it further comprises polyphenylene sulfide.
5. according to the composition of claim 4, wherein the consumption of polyphenylene sulfide is 0.05-2.0 weight %.
6. according to each composition of claim 1-5, wherein the amount of fatty acid amide is 0.05-1, preferred 0.05-0.8, more preferably 0.1-0.8,0.1-0.5 weight % most preferably.
7. according to each composition of claim 1-6, wherein electric insulation layer is made by inorganic material.
8. according to the composition of claim 7, wherein said layer comprises oxygen and phosphorus.
9. according to each composition of aforementioned claim, wherein iron or iron-based powder are made of the iron of substantially pure.
10. according to each composition of aforementioned claim, wherein be less than 10 weight %, preferably be less than the soft magnet of 5 weight % or iron-based powder particle and have granularity less than 45 microns.
11. according to the composition of claim 10, wherein at least 20% particle has and is higher than 212 microns granularity.
12. a method of making soft magnetic components comprises the following steps:
A) with the mix lubricant of soft magnet or iron-based powder and maximum 2 weight %, wherein particle is surrounded by electric insulation layer, and described lubricant is selected from the primary amide of the saturated or unsaturated straight chain fatty acid that contains 12-24 carbon atom,
B) compacting said composition, and
C) optional the gained element is heat-treated.
13. according to the method for claim 12, wherein compacting is carried out at elevated temperatures.
14. according to the method for claim 12 or 13, wherein the amount of lubricant is at 0.05-0.8 weight %, preferred 0.1-0.8 weight %, more preferably between the 0.1-0.5 weight %.
15., wherein suppress being higher than under the pressing pressure of 800MPa according to each method of claim 12-14.
16. according to each method of claim 12-15, wherein be less than 10%, preferably be less than 5% soft magnet or iron-based powder particle and have granularity less than 45 microns.
17. according to each method of claim 12-16, wherein heat treatment is carried out at 250 ℃ to 550 ℃.
18. according to each method of claim 12-16, wherein heat-treat, heat-treat at the highest 550 ℃ then at the highest 350 ℃ first step.
19. according to each method of claim 12-18, wherein heat treatment is carried out in air or inert atmosphere.
20. soft magnetic composite component, it comprises the composition of iron-based insulating powder and lubricant, then the element of compacting is heat-treated and obtained by compacting, its
Density 〉=7.5 gram/cubic centimetres,
Maximum relative permeability μ max 〉=600,
Coercivity H≤250A/m
Electricalresistivity 〉=20 μ Ω m.
21. according to the soft magnetic composite component of claim 19, its density 〉=7.6 gram/cubic centimetres.
22. according to the soft magnetic composite component of claim 20 or 21, its electricalresistivity 〉=100 μ Ω m.
23. according to claim 20,21 or 22 each soft magnetic composite components, its maximum relative permeability μ max 〉=700.
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