EP1700319B1 - Pulverzusammensetzung, verfahren zur herstellung von weichmagnetischen komponenten und zusammengesetzte weichmagnetische komponente - Google Patents

Pulverzusammensetzung, verfahren zur herstellung von weichmagnetischen komponenten und zusammengesetzte weichmagnetische komponente Download PDF

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EP1700319B1
EP1700319B1 EP04809049.2A EP04809049A EP1700319B1 EP 1700319 B1 EP1700319 B1 EP 1700319B1 EP 04809049 A EP04809049 A EP 04809049A EP 1700319 B1 EP1700319 B1 EP 1700319B1
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Prior art keywords
powder
weight
soft magnetic
acid amide
particles
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French (fr)
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EP1700319A1 (de
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Lisa Kjellen
Åsa AHLIN
Lars Hultman
Ola Andersson
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Hoganas AB
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Hoganas AB
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0206—Manufacturing of magnetic cores by mechanical means
    • H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
    • 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
    • H01F1/26—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 by macromolecular organic substances
    • 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
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • 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
    • 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
    • B22F3/14—Both compacting and sintering simultaneously
    • 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
    • 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
    • H01F1/032—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 hard-magnetic materials
    • 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
    • B22F1/105—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing inorganic lubricating or binding agents, e.g. metal salts
    • 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
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
    • 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
    • B22F2009/0824—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 with a specific atomising fluid
    • B22F2009/0828—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 with a specific atomising fluid with water
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • 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
    • B22F3/22—Manufacture 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
    • B22F3/225—Manufacture 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
    • 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

Definitions

  • the present invention relates to iron-based powder compositions. More specifically, the invention concerns powder compositions for producing soft magnetic composite components by the powder metallurgical production route. The compositions facilitates the manufacture of the soft magnetic composite component having high density as well as valuable magnetic and mechanical properties.
  • Soft magnetic materials are used for applications, such as core materials in inductors, stators and rotors for electrical machines, actuators, sensors and transformer cores.
  • soft magnetic cores such as rotors and stators in electric machines, are made of stacked steel laminates.
  • Soft Magnetic Composite, SMC materials are based on soft magnetic particles, usually iron-based, with an electrically insulating coating on each particle. By compacting the insulated particles optionally together with lubricants and/or binders using the traditionally powder metallurgy process, the SMC parts are obtained.
  • the magnetic permeability of a material is an indication of its ability to become magnetised or its ability to carry a magnetic flux. Permeability is defined as the ratio of the induced magnetic flux to the magnetising force or field intensity.
  • the eddy current loss is brought about by the production of electric currents in the iron core component due to the changing flux caused by alternating current (AC) conditions and is proportional to the square of the frequency of the alternating field.
  • a high electrical resistivity is then desirable in order to minimise the eddy currents and is of especial importance at higher frequencies.
  • Desired component properties include e.g. a high permeability through an extended frequency range, low core losses, high saturation induction, (high density) and high strength. Normally an increased density of the component enhances all of these properties.
  • the desired powder properties include suitability for compression moulding techniques, which i.a. means that the powder can be easily moulded into a high density, high strength component which can be easily ejected from the moulding equipment and that the components have smooth surface finish.
  • GB 682 897 discloses a process of preparing magnetic powder for magnetic cores having high resistivity and low power losses when operating at very high frequencies, which comprises impact milling a mixture of carbonyl iron powder, subject to excessive cluster formation, the particle size range of which does not substantially exceed a diameter of 5 microns, with a cluster-penetrating material which forms a solid, non-conductive, inert particle-separating deposit on the particles, the amount of the cluster-penetrating material being such as to yield the deposit in an amount from 0.2 to 5 % of the weight of the iron powder, and continuing impact milling of the mixture until the resulting powder has an apparent density when dry of at least 2.3 g/cm 3 , and the deposit is uniformly distributed throughout the mixture.
  • the present invention concerns a new powder composition having the desired powder properties as well as the use of the powder composition for the preparation of soft magnetic composite components.
  • the new composition can be compacted (and heat treated) to components having the desired properties.
  • the present invention also concerns a method for manufacturing soft magnetic iron-based components having excellent component properties.
  • the powder composition according to the invention is made up by electrically insulated particles of a soft magnetic material and a fatty acid amide lubricant.
  • a thermoplastic binder is present in the composition.
  • the method according to the present invention includes mixing, compaction and optionally heat treatment of the obtained component resulting in a soft magnetic iron-based component having excellent properties.
  • the powder is a substantially pure, water atomised iron powder or a sponge iron powder having irregularly shaped particles.
  • substantially pure means that the powder should be substantially free from inclusions and that the amounts of the impurities O, C an N should be kept at a minimum.
  • the average particle sizes are generally below 300 ⁇ m and above 10 ⁇ m. Examples of such powders are ABC 100.30, ASC 100.29, AT 40.29, ASC 200, ASC 300, NC 100.24, SC 100.26, MH 300, MH 40.28, MH 40.24 available from Hoganas AB, Sweden.
  • the powders used have coarser particles than what is normal in common die pressing. In practice this means that the powders are essentially without fine particles.
  • the term "essentially without fine particles” is intended to mean that less than about 10%, preferably less than 5% the powder particles have a size below 45 ⁇ m as measured by the method described in SS-EN 24 497.
  • the average particle diameter is typically between 106 and 425 ⁇ m.
  • the amount of particles above 212 ⁇ m is typically above 20%.
  • the maximum particle size may be about 2 mm.
  • the size of the iron-based particles normally used within the PM industry is distributed according to a gaussian distribution curve with an average particle diameter in the region of 30 to 100 ⁇ m and about 10-30% of the particles are less than 45 ⁇ m.
  • the powders used according to the present invention may have a particle size distribution deviating from that normally used. These coarse powders may be obtained by removing the finer fractions of the powder or by manufacturing a powder having the desired particle size distribution.
  • the invention is however not limited to the coarse powders but also powders having the particle sizes normally used for die pressing within the PM industry are included in the present invention.
  • the electrical insulation of the powder particles may be made of an inorganic material. Especially suitable are the type of insulation disclosed in the US 634 8265 , which concerns particles of a base powder consisting of essentially pure iron having an insulating oxygen- and phosphorus-containing barrier. As regards the coating it should be especially mentioned that the properties of the composite component may be influenced by the thickness of the coating. Powders having insulated particles are available as SomaloyTM 500 and 550 from Hoganas AB, Sweden.
  • the lubricant used according to the invention is selected from the group consisting of fatty acid amides.
  • Particularly suitable amides are primary amides of saturated or unsaturated fatty acid having 12-24, preferably 14-22 C atoms and most preferably 18-22 C atoms.
  • the lubricants are used in amounts of 0.05-2% and preferably less than 1.5% by weight of the composition.
  • Especially preferred amounts of the lubricant are 0.05-1%, preferably 0.05-0.8 more preferably 0.1-0.8% and most preferably 0.1-0.5% by weight.
  • Especially preferred lubricants are stearic acid amide, oleic acid amide, behenic acid amide, erucic acid amide, palmitic acid amide, the stearic acid amide being most preferred.
  • stearic acid amide seemingly in combination with rapeseed oil methyl ester is mentioned as a lubricant in connection with a termoplastic resin, polyphatalamide as a binder for the compaction of soft magnetic powders.
  • Solid lubricants generally have a density of about 1-2 g/cm 3 which is very low in comparison to the density of the iron- based powder, which is about 7.8 g/cm 3 .
  • inclusions of these less dense lubricants in the compositions will lower the theoretical density of the compacted component. It is therefore essential to keep the amount of lubricant at low levels in order to produce high-density components.
  • low amounts of lubricants tend to give ejection problems. It has now unexpectedly been found that the type of lubricants mentioned above can be used in low amounts without ejection problems.
  • the fatty acid amide may be used as the only additive to the insulated iron or iron-based powder, although for certain applications it is advantageous to add minor amounts of a thermoplastic resin, specifically polyphenylene sulfide (PPS).
  • PPS polyphenylene sulfide
  • the term "minor amounts” should in this context be interpreted as less than 2, preferably less 0.8, more preferably less than 0.6 and most preferably less than 0.5% by weight of the composition. In amounts lower than 0.05 no effects of PPS have been observed. Specifically the amount of PPS could vary between 0.1 and 0.5 and preferably between 0.2 and 0.5 or 0.4% by weight. The addition of PPS is of particular interest when good frequency stability is required.
  • a soft magnetic material can be produced by mixing an electrically insulated iron-based powder with PPS and stearic acid. The mixture is compacted at elevated temperature and the obtained compacted part is heat treated at 260°C in an atmosphere of nitrogen followed by a second heat treatment at 285 to 300°C. It has now unexpectedly been found that by using the new powder composition, which includes a fatty acid amide in stead of a corresponding fatty acid several advantages can be obtained.
  • the new powder has unexpectedly improved lubricating properties, which results in that lower ejection energy is needed to eject the compacted part from the die, that higher densities and that better transverse rupture strength can be obtained.
  • the compaction step can be performed at ambient temperature. Also the heat treatment can be facilitated, as the first heat-treating step, which is required according to the WO publication, can be omitted.
  • Iron-based magnetic powders which have insulated particles and which are combined with thermoplastic resins, are described in the US patent application 2002/0084440 .
  • these previously known particles also include a rare earth element.
  • the thermoplastic resin is used in relatively large amounts, namely at least 5% by weight.
  • the particle size of the iron-based powder is quite small (3 ⁇ m is mentioned as an example).
  • a lubricant selected from a wide variety of chemical compounds may also be included.
  • the powder composition is first uniaxially pressed in a die, which normally must not be lubricated, although the powder composition may also be used in lubricated dies.
  • the compacted component is then ejected from the die and optionally subjected to a heat treatment.
  • the compaction may be performed at ambient or elevated temperatures and at pressures up to 1500 MPa.
  • the compaction is performed in a moderately heated tool as in this way not only the green density and the ejection behaviour but also the maximum relative permeability will be improved.
  • the component compacted at an elevated temperature will have a higher permeability.
  • the heat treatment can be performed in one or several steps.
  • a recommended one step heat treatment is performed for a period of 30 minutes to 4 hours in an oxygen-containing atmosphere (air) at a temperature between 250 and 550°C.
  • Another alternative is to perform the heat treatment at 250-350°C for a period of 30 minutes to 3 hours in a air or inert gas followed by a heat treatment for 15 minutes to 2 hours in an oxygen containing (air) atmosphere at a temperature between 350 and 550°C.
  • the heat treatment may be performed at 250-350°C for 30 minutes to 4 hours in an oxygen-containing atmosphere (air).
  • Another alternative is to perform the heat treatment at 250-350°C for 30 minutes to 3 hours in air or inert gas followed by 300-500°C for 15 minutes to 2 hours in an oxygen containing atmosphere (air).
  • a composition comprising an iron- based insulated powder having coarse particles and a lubricant as described above at high pressures, such as above 800 MPa, followed by heat treatment of the compacted component, soft magnetic composite components having a density ⁇ 7.5 g/cm 3 , a maximum relative permeability, ⁇ max ⁇ 600, a coercive force, Hc ⁇ 250 A/m and a specific resistivity, ⁇ ⁇ 20 ⁇ m.
  • Such components may be of interest for the demanding applications required in e.g. stator and rotor components in electrical machines.
  • the powder mixes were compacted into ring samples with an inner diameter of 45 mm, outer diameter 55 mm and height 5 mm at 800 MPa at ambient (room) temperature. Ring samples with a height of 10 mm were also compacted and the ejection force was measured on these samples.
  • the drop in initial permeability (frequency stability) is shown in tables 3 and 4.
  • the drop in initial permeability is expressed as the difference between the initial permeability at 10 and 100 kHz divided by the initial permeability at 10 kHz.
  • Table 3 shows that by increasing the amount of the fatty acid amid from 0.3 to 0.5% a better frequency stability can be obtained.
  • Table 4 shows that by using the fatty acid amid instead of the corresponding fatty acid a better frequency stability is obtained.
  • table 4 discloses that without PPS a larger drop in frequency stability is obtained.
  • the initial permeability at 1 kHz for A9 was found to be 95 compared with 75 for A3.
  • a high initial permeability at lower frequencies is advantageous for some applications.
  • Table 3 drop in initial permeability D ⁇ 10-100 kHz (%) A 4 7.4 A 5 5.2 A 6 4.2
  • Table 4 drop in initial permeability D ⁇ 10-100 kHz (%) A 2 6.4 A 3 3.9
  • the base powder SomaloyTM 500 was mixed with PPS and lubricants according to the following table 7. Table 7. Powder mixes: Lubricants and PPS, percent by weight. Sample number PPS Lubricant B 1 0.50% 0.3% A B 2 0.50% 0.3% B B 3 0.50% 0.3% C B 4 0.50% 0.3% D B 5 0.30% 0.3% B B 6 - 0.4% B B 7 - 0.3% B B 8 0.1% 0.3% B B 9 0.2% 0.3% B B 10 - 0.4% KenolubeTM
  • the powder mixes were compacted into test bars according to ISO 3995 at a compaction pressure of 800 MPa at ambient temperature. After compaction the parts were heat treated in a two-step heat treatment. The first step was performed at 290°C for 105 minutes in inert nitrogen atmosphere. This step was followed by a subsequent heat treatment step at 350°C for 60 minutes in air. Samples were tested with regard to Transverse Rupture Strength, TRS, according to ISO 3995.
  • results from testing of transverse rupture strength are shown in table 8.
  • samples prepared with mixtures including the fatty acid amide give sufficient TRS-values. A higher density after heat treatment is reached, which is beneficial in terms on induction and permeability. If the PPS content is reduced to 0.3% or less the TRS is increased to values above 80 MPa. The samples without PPS and with the stearic acid amide lubricant even have TRS values above 100 MPa. The use of KenolubeTM, which is a conventionally used lubricant, does not result in the required transverse rupture strength. Table 8.
  • This example shows that, in comparison with the commonly used Zinc Stearate and Ethylene bis stearamide lubricants, low ejection forces during ejection of compacted components and perfect surface finish of the ejected component are obtained, when the fatty acid amide lubricants according to the invention are used in low amount in combination with coarse powders and high compaction pressures.
  • the obtained mixes were transferred to a die and compacted into cylindrical test samples (50 grams) with a diameter of 25 mm, in an uniaxially press movement at a compaction pressure of 1100 MPa.
  • the used die material was conventional tool steel.
  • the total ejection energy/enveloping area needed in order to eject the samples was calculated.
  • the following table 11 show ejection energy, green density and the surface finish.
  • Table 11 Mix Ejection energy (J/cm 2 ) Green density (g/cm 3 ) Surface finish A 90 7.64 Perfect B 83 7.65 Perfect C 93 7.63 Perfect D 70 7.67 Acceptable E 117 7.66 Not Acceptable F 113 7.64 Perfect
  • the following example illustrates the effect of the particle size distribution of the soft magnetic iron-based powder on ejection behaviour and green density.
  • a "coarse" powder according to example 3 was used.
  • the particle size distribution of the "fine” powder is given in table 12.
  • the mixes were prepared using 0.2% stearamide by weight according to the procedure in example 3.
  • the mixture based on the "fine” powder is marked sample H and were compared with sample C.
  • the composition containing fine powder results in a lower green density and deteriorated surface finish.
  • the powder mixes were compacted into rings with an inner diameter of 45 mm, an outer diameter of 55 mm and the height 10 mm at 1100 MPa.
  • the total ejection energy/enveloping area needed in order to eject the samples from the die was calculated.
  • the following table 15 shows the calculated ejection energy/area, green density and the surface appearance.
  • Table 15. Ejection energy, green density, the surface appearance Mix Ejection energy [J/cm2] Density [g/cm 3 ] Surface appearance 1 54 7.65 Not acceptable 2 40 7.61 Acceptable 3 33 7.56 Perfect 4 28 7.51 Perfect 5 73 7.67 Acceptable 6 38 7.64 Perfect 7 37 7.59 Perfect
  • the new lubricant can be added in amount as low as 0.2% and still a perfect surface finish can be obtained whereas the for the reference lubricant, EBS, the lowest addition is 0.4% for obtaining a perfect surface finish.
  • This example compares the magnetic properties of components manufactured with a minimum amount of the lubricating components stearamide and EBS respectively, in order to achieve similar values of ejection energy.
  • Components made from mix 2 and mix 6 according to example 5 were compared regarding magnetic properties after heat treatment.
  • the following example shows the influence of die temperature on the ejection properties and green density of compacted samples.
  • the primary amide stearamide
  • 0.2% of stearamide was added to 2 kg of a coarse soft magnetic electrically insulated iron-based powder according to the procedure of example 3.
  • the powder mixes were compacted into rings having an inner diameter of 45 mm, an outer diameter of 55 mm and a height of 10 mm, at a compaction pressure of 1100 MPa. During ejection of the compacted samples the ejection forces were recorded. The total ejection energy/enveloping area needed in order to eject the samples from the die was calculated.
  • Table 17 shows ejection energy, green density and the surface appearance of the samples compacted at different temperature of the die. Table 17.
  • This example compares component properties of components manufactured according to the present invention to properties of components compacted with the aid of DWL.
  • a "coarse" powder according to example 3 was used.
  • As lubricant in the inventive example 0.2% by weight of stearamide was used and the obtained powder composition was compacted at a controlled die temperature of 80°C into ring samples having a green density of 7.6 g/cm 3 .
  • In the comparative example no internal lubricant was used, instead DWL was applied. Ring samples were compacted to a density of 7.6 g/cm 3 at ambient temperature.
  • the ring samples outer diameter was 55 mm, inner diameter 45 mm and height 5 mm.
  • iron-powder cores with excellent magnetic properties can obtained by the present invention.
  • the positive effect of elevated die temperature on the maximal relative permeability is also shown.
  • the density was determined by measuring the mass and dimensions of the ring samples.
  • the specific electrical resistivity was measured by a 4-point method on the ring samples.
  • Prior to magnetic measurements in a Brockhaus hysterisisgraph the ring samples were wound with 100 drive and 100 sense turns.
  • the DC-properties such as ⁇ max and H c were acquired from a loop at 10kA/m while the core loss was measured at 1T and 400Hz.
  • TRS transverse rupture strength
  • Table 19 Process conditions for ring samples Sample Type of lubricant Amount Lubricant Compacting pressure Die temperature Heat treatment (%wt) (MPa) (°C) 1 Stearamide 0.2 1100 25 300°C 45 min, air+ 520°C*, air 2 Stearamide 0.2 1100 80 300°C 45 min, air+ 520°C*, air 3 Stearamide 0.2 800 80 530°C, 30 min, air 4 Stearamide 0.2 1100 25 530°C, 30 min, air 5 Stearamide 0.2 1100 80 530°C, 30 min, air 6 Stearamide 0.1 1100 85 530°C, 30 min, air 7 Stearamide 0.3 800 25 300°C, 1h, air + 530°C, 30 min, air 8 Stearamide 0.3 800 80 300°C, 1h, air + 530°C, 30 min, air 9 Stearamide 0.3 1100 25 300°C, 1h, air + 530°C, 30 min, air 10 Stearamide 0.3 1100 80 300°C, 1h,

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Claims (18)

  1. Pulverzusammensetzung, die aus unregelmäßig geformten Teilchen eines weichmagnetischen Materials aus im Wesentlichen reinem, mit Wasser zerstäubtem Eisen- oder Eisenschwammpulver besteht, wobei weniger als 10 Gew.-% der Pulverteilchen eine Teilchengröße von weniger als 45 µm aufweisen, und wobei die Pulverteilchen mit einer elektrisch isolierenden Schicht versehen sind, 0,05 bis 2 Gew.-% eines Schmiermittels, das ausgewählt ist aus der Gruppe, bestehend aus primären Amiden gesättigter oder ungesättigter, gerader Fettsäuren mit 12 bis 24 C-Atomen und gegebenenfalls Polyphenylensulfid in einer Konzentration von weniger als 2 Gew.-%, wobei die Pulverzusammensetzung in der Lage ist, durch uniaxiale Verdichtung eine weichmagnetische Komponente herzustellen.
  2. Zusammensetzung nach Anspruch 1, wobei die Fettsäure 14 bis 22 C-Atome aufweist.
  3. Zusammensetzung nach Anspruch 1 oder 2, wobei das Fettsäureamid ausgewählt ist aus der Gruppe, bestehend aus Stearinsäureamid, Oleinsäureamid, Behensäureamid, Eurinsäureamid, Palmitinsäureamid.
  4. Zusammensetzung nach einem der Ansprüche, ferner umfassend Polyphenylensulfid.
  5. Zusammensetzung nach Anspruch 4, wobei das Polyphenylensulfid in einer Menge von 0,05 bis 2,0 Gew.-% verwendet wird.
  6. Zusammensetzung nach einem der Ansprüche 1 bis 5, wobei das Fettsäureamid in einer Menge von 0,05 bis 1, vorzugsweise von 0,05 bis 0,8, besonders bevorzugt von 0,1 bis 0,8, am meisten bevorzugt von 0,1 bis 0,5 Gew.-%, vorliegt.
  7. Zusammensetzung nach einem der Ansprüche 1 bis 6, wobei die elektrisch isolierende Schicht aus einem anorganischen Material zusammengesetzt ist.
  8. Zusammensetzung nach Anspruch 7, wobei die Schicht Sauerstoff und Phosphor umfasst.
  9. Zusammensetzung nach einem der vorhergehenden Ansprüche, wobei weniger als 5 Gew.-% der Pulverteilchen eine Teilchengröße von weniger als 45 µm aufweisen.
  10. Zusammensetzung nach Anspruch 9, wobei mindestens 20 % der Teilchen eine Teilchengröße oberhalb von 212 µm aufweisen.
  11. Verfahren zur Herstellung weichmagnetischer Komponenten, umfassend die Schritte:
    a) Mischen unregelmäßig geformter Teilchen eines weichmagnetischen, im Wesentlichen reinen, mit Wasser zerstäubtem Eisen- oder Eisenschwammpulver, wobei weniger als 10 Gew.-% der Pulverteilchen eine Teilchengröße von weniger als 45 µm aufweisen, und
    wobei die Teilchen mit einer elektrisch isolierenden Schicht umgeben sind, und 0,05 bis 2 Gew.-% eines Schmiermittels, das ausgewählt ist aus der Gruppe, bestehend aus primären Amiden gesättigter oder ungesättigter, gerader Fettsäuren mit 12 bis 24 C-Atomen und gegebenenfalls Polyphenylensulfid in einer Konzentration von weniger als 2 Gew.-%,
    b) uniaxiales Verdichten der sich ergebenden Zusammensetzung, und
    c) gegebenenfalls Unterziehen der erhaltenen Komponente einer Wärmebehandlung.
  12. Verfahren nach Anspruch 11, wobei die Verdichtung bei einer erhöhten Temperatur durchgeführt wird.
  13. Verfahren nach Anspruch 11 oder 12, wobei die Menge des Schmiermittels zwischen 0,05 bis 0,8 %, vorzugsweise 0,1 bis 0,8 und besonders bevorzugt 0,1 bis 0,5 Gew.-% beträgt.
  14. Verfahren nach einem der Ansprüche 11 bis 13, wobei die Verdichtung bei einem Verdichtungsdruck oberhalb von 800 MPa durchgeführt wird.
  15. Verfahren nach einem der Ansprüche 11 bis 14, wobei weniger als 5 Gew.-% der Pulverteilchen eine Teilchengröße von weniger als 45 µm aufweisen.
  16. Verfahren nach einem der Ansprüche 11 bis 15, wobei die Wärmebehandlung zwischen 250 °C und 550 °C durchgeführt wird.
  17. Verfahren nach einem der Ansprüche 11 bis 15, wobei die Wärmebehandlung in einem ersten Schritt bis zu 350 °C durchgeführt wird, gefolgt von einer Wärmebehandlung bis zu 550 °C.
  18. Verfahren nach einem der Ansprüche 11 bis 17, wobei die Wärmebehandlung in Luft oder einer inerten Atmosphäre durchgeführt wird.
EP04809049.2A 2003-12-29 2004-12-15 Pulverzusammensetzung, verfahren zur herstellung von weichmagnetischen komponenten und zusammengesetzte weichmagnetische komponente Active EP1700319B1 (de)

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