EP1131831B1 - Method for producing a weakly magnetic composite material from a mouldable material - Google Patents
Method for producing a weakly magnetic composite material from a mouldable material Download PDFInfo
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- EP1131831B1 EP1131831B1 EP00963959A EP00963959A EP1131831B1 EP 1131831 B1 EP1131831 B1 EP 1131831B1 EP 00963959 A EP00963959 A EP 00963959A EP 00963959 A EP00963959 A EP 00963959A EP 1131831 B1 EP1131831 B1 EP 1131831B1
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- compound
- thermoplastic
- lubricant
- moulding compound
- temperature
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/20—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
Definitions
- the invention relates to a method for producing a soft magnetic composite with a molding compound, according to the preamble of the independent claim
- Soft magnetic composites are needed for the production of temperature, corrosion and solvent resistant magnetic components, especially in electromechanics. These soft magnetic composites or the components produced therewith have certain properties: they should have a high magnetic permeability, a high magnetic saturation, a low coercive force and the highest possible specific electrical resistance. The combination of said magnetic properties with a high electrical resistivity results in a high switching dynamics with low eddy current losses, that is, the magnetic saturation and the demagnetization of such a component take place within a short time.
- thermoplastic resin serves as a lubricant.
- zinc stearate is used as the lubricant.
- thermoplastic materials and fluororesins are added.
- a soft magnetic, moldable composite material and a method for its production is known in which a soft magnetic properties having powder coated with a thermoplastic compound and then pressed into a shaped body. Thereafter, the molded article or molding compound is subjected to a heat treatment under protective gas which exceeds the melting point of the thermoplastic compound. It is also known to perform better mold release of the compressed components from the molding press a surface treatment of the coated powder with a lubricant. The lubricant should be so volatile that it volatilizes in the melting of a polymer in the subsequent heat treatment and does not react chemically with the polymer. Furthermore, it is already known to press unalloyed or alloyed iron powder with thermosetting resins, for example epoxides or phenolic resins, axially.
- thermosetting resins for example epoxides or phenolic resins
- the inventive method for producing a soft magnetic composite material having such a molding compound over the prior art has the advantage that thus a reduction in the previously required temperature during compression of the molding compound in a pressing tool, such as a die, can be achieved, and that at the same time Preheating the molding compound can be dispensed before pressing.
- the better sliding behavior of the molding compound also advantageously allows a reduction in the proportion of the thermoplastic compound in the molding compound.
- the molding compound according to the invention allows the achievement of higher material densities for a given pressing force, and it leads to a lower tool wear.
- dispensing with a preheating of the molding compound prior to compression is also avoided that an undesirable oxidation, for example, of iron powder as soft magnetic properties exhibiting starting powder occurs.
- it can be dispensed with by the reduction of the tool temperature in the inventive method to make the pressing in the press tool under inert gas.
- the molding compound according to the invention and the method according to the invention finally have the advantage of easier processing by substantially simplifying the Warmpreß achieved, and a lower energy consumption in the shaping.
- the production of the soft magnetic composite material or components using this composite advantageously by uniaxial Matrizenpressen the molding compound at temperatures below the melting temperature of the molding compound added thermoplastic compound, and by an adjoining, graduated thermal aging process.
- the added lubricant is advantageously first evaporated or pyrolyzed at temperatures below the melting temperature of the thermoplastic compound, and then melted by a further increase in temperature, the thermoplastic compound.
- the melted thermoplastic compound wets the soft magnetic properties having powder particles of the starting powder, and thus causes after cooling an effective bonding of the powder particles, which leads to a good mechanical strength and high electrical resistance of the resulting composite.
- the molding compound according to the invention as the starting material for the method according to the invention for producing the soft magnetic composite material is based either on a soft magnetic powder which is surface-coated with a thermoplastic compound or alternatively which has been dry-mixed with a fine thermoplastic powder.
- the coating of the powder particles with the thermoplastic compound can be achieved, for example, by adding a solution of a suitable thermoplastic polymer in a solvent.
- thermoplastic compound In the case of the dry mixing of the thermoplastic compound with the soft magnetic powder, a pulverulent, thermoplastic compound is used which preferably has a mean particle size of from 1 .mu.m to 100 .mu.m, in particular from 5 .mu.m to 40 .mu.m.
- a lubricant is particularly advantageously used, which evaporates at a heating of the molding compound under inert gas atmosphere during the two-stage thermal aging process at temperatures below the melting point of the thermoplastic compound used or thermally decomposed and volatilized, with neither the lubricant nor its decomposition products with the thermoplastic compound and / or the soft magnetic properties having starting powder chemically react.
- thermoplastic melt In order to prevent expulsion of the thermoplastic melt from the composite under the pressure of the lubricant originating from the lubricant, it is also very advantageous if the lubricant after pressing at temperatures below the melting point of the thermoplastic compound initially at least almost completely removed again from the molding compound is before then by a further increase in temperature then melting of the thermoplastic compound and wetting of the soft magnetic starting powder occurs.
- the lubricant remains in the microstructure of the resulting soft magnetic composite material, where it can adversely affect its performance properties.
- the lubricant is stearic acid, which also serves as a mold release agent at the same time.
- the stearic acid is added to the molding compound advantageously as micronized powder having an average particle size of 1 .mu.m to 100 .mu.m, in particular from 10 .mu.m to 50 .mu.m.
- thermoplastic compounds are advantageously a variety of polymers, preferably polyphenylene sulfide is used. Particularly advantageous is the combination of stearic acid with polyphenylene sulfide.
- the molding compound according to the invention is free-flowing.
- starting material having soft magnetic properties is phosphated iron powder of types ABM or Somaloy 500 (Höganäs, Sweden) with polyphenylene sulfide powder as a thermoplastic compound.
- polyphenylene sulfide powder for example, the types V0 (Philips Petrolium) or Fortron 0205 B4 / 20 (Ticona) are used.
- this powder mixture stearic acid is added as a lubricant and mold release agent with a mean powder particle size of about 30 microns.
- the lubricant stearic acid is added to the molding compound in a proportion of 0.05 mass% to 1 mass%, especially 0.1 to 0.3 mass%.
- thermoplastic compound is added to the molding compound in a proportion of 0.2% by mass to 10% by mass, in particular 0.3 to 1.5% by mass.
- phosphated iron powder is mixed with 0.6% by mass of polyphenylene sulfide powder and 0.2% by mass of micronized stearic acid.
- the free-flowing molding compound obtained in this way is then further shaped into a component by uniaxial pressing without powder preheating at a mold temperature of 70 ° C. in a die.
- the press tool was preheated to the temperature of 70 ° C.
- the molding compound in the die After pressing the molding compound in the die then follows a two-stage aging process, which comprises a first temperature treatment of the compressed molding compound or the molded component below the melting temperature of the thermoplastic compound used, and then a second temperature treatment of the compressed molding compound above the melting temperature of the thermoplastic compound.
- the first temperature treatment is carried out at a temperature of 260 ° C under nitrogen atmosphere for 2 hours.
- the second temperature treatment joins at 285 ° C to 300 ° C over a period of 30 minutes.
- this lubricant volatilizes at least substantially without residue during the first heat treatment. Furthermore, this lubricant and also its decomposition products are chemically at least substantially inert to the thermoplastic compound polyphenylene sulfide used and the phosphated iron powder, so that no chemical reaction occurs between the lubricant and the other components of the molding compound during the temperature treatment.
- the preparation of the molding compound prior to compression may on the one hand be a mixing of the soft magnetic properties of the iron powder with the powdery thermoplastic compound polyphenylene sulfide and the pulverulent lubricant stearic acid.
- thermoplastic compound for further details on the preparation of the molding compound before the actual pressing in the press tool and other suitable thermoplastic compounds be on the DE 197 35 271 A1 directed.
- thermoplastic compound and polyphthalamides can be used as a thermoplastic compound and polyphthalamides.
- iron-nickel, iron-silicon and iron-cobalt alloys are suitable as starting materials having soft-magnetic properties.
- Thermogravimetric analysis TGA analysis
- DSC analysis differential scanning calorimetry
Abstract
Description
Die Erfindung betrifft ein Verfahren zur Herstellung eines weichmagnetischen Verbundwerkstoffes mit einer Preßmasse, nach der Gattung des unabhängigen AnspruchsThe invention relates to a method for producing a soft magnetic composite with a molding compound, according to the preamble of the independent claim
Weichmagnetische Verbundwerkstoffe werden zur Herstellung von temperatur-, korrosions- und lösemittelbeständigen magnetischen Bauteilen, insbesondere in der Elektromechanik benötigt. Dabei bedürfen diese weichmagnetischen Verbundwerkstoffe beziehungsweise die damit hergestellten Bauteile gewisser Eigenschaften: Sie sollen eine hohe magnetische Permeabilität, eine hohe magnetische Sättigung, eine geringe Koerzitivfeldstärke und einen möglichst hohen spezifischen elektrischen Widerstand aufweisen. Die Kombination der genannten magnetischen Eigenschaften mit einem hohem spezifischen elektrischen Widerstand ergibt eine hohe Schaltdynamik bei geringen Wirbelstromverlusten, das heißt, die magnetische Sättigung und die Entmagnetisierung eines derartigen Bauteils erfolgen innerhalb kurzer Zeit.Soft magnetic composites are needed for the production of temperature, corrosion and solvent resistant magnetic components, especially in electromechanics. These soft magnetic composites or the components produced therewith have certain properties: they should have a high magnetic permeability, a high magnetic saturation, a low coercive force and the highest possible specific electrical resistance. The combination of said magnetic properties with a high electrical resistivity results in a high switching dynamics with low eddy current losses, that is, the magnetic saturation and the demagnetization of such a component take place within a short time.
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Das erfindungsgemäße Verfahren zur Herstellung eines weichmagnetischen Verbundwerkstoffes mit einer derartigen Preßmasse hat gegenüber dem Stand der Technik den Vorteil, daß damit eine Absenkung der bisher erforderlichen Temperatur beim Verpressen der Preßmasse in einem Preßwerkzeug, beispielsweise einer Matrize, erreicht werden kann, und daß gleichzeitig auf eine Vorwärmung der Preßmasse vor dem Verpressen verzichtet werden kann. Das bessere Gleitverhalten der Preßmasse läßt zudem vorteilhaft eine Verminderung des Anteils der thermoplastischen Verbindung in der Preßmasse zu.The inventive method for producing a soft magnetic composite material having such a molding compound over the prior art has the advantage that thus a reduction in the previously required temperature during compression of the molding compound in a pressing tool, such as a die, can be achieved, and that at the same time Preheating the molding compound can be dispensed before pressing. The better sliding behavior of the molding compound also advantageously allows a reduction in the proportion of the thermoplastic compound in the molding compound.
Weiterhin erlaubt die erfindungsgemäße Preßmasse die Erzielung von höheren Werkstoffdichten bei gegebener Preßkraft, und sie führt zu einem geringeren Werkzeugverschleiß. Durch den Verzicht auf eine Vorerwärmung der Preßmasse vor dem Verpressen wird zudem vermieden, daß eine unerwünschte Oxidation beispielsweise von Eisenpulver als weichmagnetische Eigenschaften aufweisendes Ausgangspulver auftritt. Darüber hinaus kann durch die Absenkung der Werkzeugtemperatur kann bei dem erfindungsgemäßen Verfahren darauf verzichtet werden, das Verpressen in dem Preßwerkzeug unter Schutzgas vorzunehmen.Furthermore, the molding compound according to the invention allows the achievement of higher material densities for a given pressing force, and it leads to a lower tool wear. By dispensing with a preheating of the molding compound prior to compression is also avoided that an undesirable oxidation, for example, of iron powder as soft magnetic properties exhibiting starting powder occurs. In addition, it can be dispensed with by the reduction of the tool temperature in the inventive method to make the pressing in the press tool under inert gas.
Die erfindungsgemäße Preßmasse und das erfindungsgemäße Verfahren haben schließlich den Vorteil einer einfacheren Verarbeitung durch wesentliche Vereinfachung der Warmpreßeinrichtung, sowie eines geringeren Energieaufwandes bei der Formgebung.The molding compound according to the invention and the method according to the invention finally have the advantage of easier processing by substantially simplifying the Warmpreßeinrichtung, and a lower energy consumption in the shaping.
Vorteilhafte Weiterbildungen der Erfindung ergeben sich aus den in den Unteransprüchen genannten Maßnahmen.Advantageous developments of the invention will become apparent from the measures mentioned in the dependent claims.
So erfolgt die Herstellung des weichmagnetischen Verbundwerkstoffes bzw. von Bauteilen unter Verwendung dieses Verbundwerkstoffes vorteilhaft durch uniaxiales Matrizenpressen der Preßmasse bei Temperaturen unterhalb der Schmelztemperatur der der Preßmasse zugegebenen thermoplastischen Verbindung, und durch einen sich daran anschließenden, abgestuften thermischen Auslagerungsprozeß.Thus, the production of the soft magnetic composite material or components using this composite advantageously by uniaxial Matrizenpressen the molding compound at temperatures below the melting temperature of the molding compound added thermoplastic compound, and by an adjoining, graduated thermal aging process.
In diesem Auslagerungsprozeß wird vorteilhaft zunächst bei Temperaturen unterhalb der Schmelztemperatur der thermoplastischen Verbindung das zugesetzte Gleitmittel verdunstet oder pyrolisiert, und danach durch eine weitere Temperaturerhöhung die thermoplastische Verbindung aufgeschmolzen. Dabei benetzt die aufgeschmolzene thermoplastische Verbindung die weichmagnetische Eigenschaften aufweisenden Pulverteilchen des Ausgangspulvers, und bewirkt somit nach dem Abkühlen eine effektive Verklebung der Pulverteilchen, was zu einer guten mechanischen Festigkeit und einem hohen elektrischen Widerstand des erhaltenen Verbundwerkstoffes führt. Die erfindungsgemäße Preßmasse als Ausgangsmasse für das erfindungsgemäße Verfahren zur Herstellung des weichmagnetischen Verbundwerkstoffes geht entweder von einem weichmagnetischen Pulver aus, das mit einer thermoplastischen Verbindung oberflächlich beschichtet wird, oder das alternativ mit einem feinen Thermoplastpulver trocken gemischt wurde.In this aging process, the added lubricant is advantageously first evaporated or pyrolyzed at temperatures below the melting temperature of the thermoplastic compound, and then melted by a further increase in temperature, the thermoplastic compound. The melted thermoplastic compound wets the soft magnetic properties having powder particles of the starting powder, and thus causes after cooling an effective bonding of the powder particles, which leads to a good mechanical strength and high electrical resistance of the resulting composite. The molding compound according to the invention as the starting material for the method according to the invention for producing the soft magnetic composite material is based either on a soft magnetic powder which is surface-coated with a thermoplastic compound or alternatively which has been dry-mixed with a fine thermoplastic powder.
Die Beschichtung der Pulverpartikel mit der thermoplastischen Verbindung kann dazu beispielsweise durch Zusetzen einer Lösung eines geeigneten, thermoplastischen Polymers in einem Lösungsmittel erzielt werden.The coating of the powder particles with the thermoplastic compound can be achieved, for example, by adding a solution of a suitable thermoplastic polymer in a solvent.
Im Fall des trockenen Vermischens der thermoplastischen Verbindung mit dem weichmagnetischen Pulver wird eine pulverförmige, thermoplastische Verbindung eingesetzt, die bevorzugt eine mittlere Korngröße von 1 µm bis 100 µm, insbesondere von 5 µm bis 40 µm, aufweist.In the case of the dry mixing of the thermoplastic compound with the soft magnetic powder, a pulverulent, thermoplastic compound is used which preferably has a mean particle size of from 1 .mu.m to 100 .mu.m, in particular from 5 .mu.m to 40 .mu.m.
Als Gleitmittel wird besonders vorteilhaft ein Gleitmittel eingesetzt, das bei einer Erwärmung der Preßmasse unter Inertgasatmosphäre während des zweistufigen thermischen Auslagerungsprozesses bei Temperaturen unterhalb des Schmelzpunktes der eingesetzten thermoplastischen Verbindung verdunstet oder sich thermisch zersetzt und verflüchtigt, wobei weder das Gleitmittel noch seine Zersetzungsprodukte mit der thermoplastischen Verbindung und/oder dem weichmagnetische Eigenschaften aufweisenden Ausgangspulver chemisch reagieren.As a lubricant, a lubricant is particularly advantageously used, which evaporates at a heating of the molding compound under inert gas atmosphere during the two-stage thermal aging process at temperatures below the melting point of the thermoplastic compound used or thermally decomposed and volatilized, with neither the lubricant nor its decomposition products with the thermoplastic compound and / or the soft magnetic properties having starting powder chemically react.
Um ein Austreiben der Thermoplastschmelze aus dem Verbundwerkstoff unter dem Druck der aus dem Gleitmittel stammenden Gase zu vermeiden, ist es weiter sehr vorteilhaft, wenn das Gleitmittel nach dem Verpressen bei Temperaturen unterhalb des Schmelzpunktes der thermoplastischen Verbindung zunächst zumindest nahezu vollständig wieder aus der Preßmasse entfernt wird, bevor durch eine weitere Temperaturerhöhung dann ein Aufschmelzen der thermoplastischen Verbindung und eine Benetzung des weichmagnetischen Ausgangspulvers eintritt.In order to prevent expulsion of the thermoplastic melt from the composite under the pressure of the lubricant originating from the lubricant, it is also very advantageous if the lubricant after pressing at temperatures below the melting point of the thermoplastic compound initially at least almost completely removed again from the molding compound is before then by a further increase in temperature then melting of the thermoplastic compound and wetting of the soft magnetic starting powder occurs.
Insgesamt tritt somit erst beim Abkühlen der Preßmasse bzw. des daraus hergestellten Bauteils eine wesentliche Steigerung der Festigkeit des gleitmittelfreien Verbundes durch Bildung von haftenden Polymerbrücken ein.Overall, therefore, a significant increase in the strength of the lubricant-free composite occurs by the formation of adhesive polymer bridges only on cooling of the molding compound or of the component produced therefrom.
Weiterhin wird damit vorteilhaft vermieden, daß das Gleitmittel im Gefüge des erhaltenen weichmagnetischen Verbundwerkstoffes verbleibt, und dort dessen Gebrauchseigenschaften negativ beeinflussen kann.Furthermore, it is thus advantageously avoided that the lubricant remains in the microstructure of the resulting soft magnetic composite material, where it can adversely affect its performance properties.
Als besonders vorteilhaft hinsichtlich der Temperaturen beim Verpressen und während des thermischen Auslagerungsprozesses hat sich herausgestellt, wenn das Gleitmittel Stearinsäure ist, die überdies gleichzeitig als Formtrennmittel dient. Die Stearinsäure wird dazu der Preßmasse vorteilhaft als mikronisiertes Pulver mit einer mittleren Korngröße von 1 µm bis 100 µm, insbesondere von 10 µm bis 50 µm zugesetzt.It has been found to be particularly advantageous with regard to the temperatures during the pressing and during the thermal aging process, when the lubricant is stearic acid, which also serves as a mold release agent at the same time. The stearic acid is added to the molding compound advantageously as micronized powder having an average particle size of 1 .mu.m to 100 .mu.m, in particular from 10 .mu.m to 50 .mu.m.
Als thermoplastische Verbindungen eignen sich vorteilhaft eine Vielzahl von Polymeren, wobei bevorzugt Polyphenylensulfid eingesetzt wird. Besonders vorteilhaft ist die Kombination von Stearinsäure mit Polyphenylensulfid.As thermoplastic compounds are advantageously a variety of polymers, preferably polyphenylene sulfide is used. Particularly advantageous is the combination of stearic acid with polyphenylene sulfide.
Im übrigen ist sehr vorteilhaft, beispielsweise hinsichtlich einer leichten Verarbeitung und Handhabung, daß die erfindungsgemäße Preßmasse rieselfähig ist.Moreover, it is very advantageous, for example, in terms of ease of processing and handling, that the molding compound according to the invention is free-flowing.
Zunächst wird als weichmagnetische Eigenschaften aufweisendes Ausgangspulver phosphatiertes Eisenpulver der Typen ABM oder Somaloy 500 (Fa. Höganäs, Schweden) mit Polyphenylensulfid-Pulver als thermoplastische Verbindung vermischt. Als Polyphenylensulfid-Pulver werden beispielsweise die Typen V0 (Fa. Philips Petrolium) oder Fortron 0205 B4/20 (Fa. Ticona) eingesetzt. Weiter wird dieser Pulvermischung Stearinsäure als Gleit- und Formtrennmittel mit einer mittleren Pulverkorngröße von ca. 30 µm zugesetzt.Initially, starting material having soft magnetic properties is phosphated iron powder of types ABM or Somaloy 500 (Höganäs, Sweden) with polyphenylene sulfide powder as a thermoplastic compound. As polyphenylene sulfide powder, for example, the types V0 (Philips Petrolium) or Fortron 0205 B4 / 20 (Ticona) are used. Further, this powder mixture stearic acid is added as a lubricant and mold release agent with a mean powder particle size of about 30 microns.
Im einzelnen wird das Gleitmittel Stearinsäure der Preßmasse mit einem Anteil von 0,05 Massenprozent bis 1 Massenprozent, insbesondere 0,1 bis 0,3 Massenprozent, zugesetzt.Specifically, the lubricant stearic acid is added to the molding compound in a proportion of 0.05 mass% to 1 mass%, especially 0.1 to 0.3 mass%.
Die thermoplastische Verbindung wird der Preßmasse mit einem Anteil von 0,2 Massenprozent bis 10 Massenprozent, insbesondere 0,3 bis 1,5 Massenprozent, zugesetzt.The thermoplastic compound is added to the molding compound in a proportion of 0.2% by mass to 10% by mass, in particular 0.3 to 1.5% by mass.
Konkret wird beispielsweise phosphatiertes Eisenpulver mit 0,6 Massenprozent Polyphenylensulfid-Pulver und 0,2 Massenprozent mikronisierter Stearinsäure vermischt.Concretely, for example, phosphated iron powder is mixed with 0.6% by mass of polyphenylene sulfide powder and 0.2% by mass of micronized stearic acid.
Die derart erhaltene, rieselfähige Preßmasse wird im weiteren dann ohne eine Pulvervorwärmung bei einer Werkzeugtemperatur von 70° C in einer Matrize durch uniaxiales Pressen zu einem Bauteil geformt. Dazu wurde das Preßwerkzeug auf die Temperatur von 70° C vorgewärmt.The free-flowing molding compound obtained in this way is then further shaped into a component by uniaxial pressing without powder preheating at a mold temperature of 70 ° C. in a die. For this purpose, the press tool was preheated to the temperature of 70 ° C.
Nach dem Verpressen der Preßmasse in der Matrize folgt dann ein zweistufiger Auslagerungsprozeß, der eine erste Temperaturbehandlung der verpreßten Preßmasse bzw. des geformten Bauteils unterhalb der Schmelztemperatur der eingesetzten thermoplastischen Verbindung, und danach eine zweite Temperaturbehandlung der verpreßten Preßmasse oberhalb der Schmelztemperatur der thermoplastischen Verbindung umfaßt. Im erläuterten Beispiel wird dazu die erste Temperaturbehandlung bei einer Temperatur von 260° C unter Stickstoffatmosphäre über 2 Stunden durchgeführt. Danach schließt sich die zweite Temperaturbehandlung bei 285° C bis 300° C über eine Zeitdauer von 30 Minuten an.After pressing the molding compound in the die then follows a two-stage aging process, which comprises a first temperature treatment of the compressed molding compound or the molded component below the melting temperature of the thermoplastic compound used, and then a second temperature treatment of the compressed molding compound above the melting temperature of the thermoplastic compound. In the illustrated example, the first temperature treatment is carried out at a temperature of 260 ° C under nitrogen atmosphere for 2 hours. Thereafter, the second temperature treatment joins at 285 ° C to 300 ° C over a period of 30 minutes.
Durch die Wahl der Stearinsäure ist gewährleistet, daß sich dieses Gleitmittel während der ersten Temperaturbehandlung zumindest weitgehend rückstandsfrei verflüchtigt. Weiter ist dieses Gleitmittel und auch seine Zersetzungsprodukte gegenüber der verwendeten thermoplastischen Verbindung Polyphenylensulfid und dem phosphatierten Eisenpulver chemisch zumindest weitgehend inert, so daß keine chemische Reaktion zwischen dem Gleitmittel und den übrigen Komponenten der Preßmasse während der Temperaturbehandlung auftritt.The choice of stearic acid ensures that this lubricant volatilizes at least substantially without residue during the first heat treatment. Furthermore, this lubricant and also its decomposition products are chemically at least substantially inert to the thermoplastic compound polyphenylene sulfide used and the phosphated iron powder, so that no chemical reaction occurs between the lubricant and the other components of the molding compound during the temperature treatment.
Die Aufbereitung der Preßmasse vor dem Verpressen kann einerseits ein Mischen des weichmagnetische Eigenschaften aufweisenden Eisenpulvers mit der pulverförmigen thermoplastischen Verbindung Polyphenylensulfid sowie dem pulverförmigen Gleitmittel Stearinsäure sein.The preparation of the molding compound prior to compression may on the one hand be a mixing of the soft magnetic properties of the iron powder with the powdery thermoplastic compound polyphenylene sulfide and the pulverulent lubricant stearic acid.
Alternativ ist es jedoch ebenso möglich, zunächst eine Beschichtung des weichmagnetische Eigenschaften aufweisenden Eisenpulvers mit einer in einem Lösungsmittel gelösten thermoplastischen Verbindung wie Polyphtalamid vorzunehmen, und danach oder gleichzeitig dazu ein Mischen des weichmagnetische Eigenschaften aufweisenden Ausgangspulvers mit dem pulverförmigen Gleitmittel, oder ein Einbringen des in einem Lösungsmittel gelösten Gleitmittels in die Preßmasse vorzunehmen.Alternatively, however, it is also possible to first make a coating of the soft magnetic properties having iron powder with a dissolved in a solvent thermoplastic compound such as polyphthalamide, and then or at the same time mixing the soft magnetic properties having starting powder with the powdered lubricant, or introducing the in one Solvent dissolved lubricant in the molding compound.
Hinsichtlich weiterer Details zur Aufbereitung der Preßmasse vor dem eigentlichen Preßvorgang in dem Preßwerkzeug und weiterer geeigneter thermoplastischer Verbindungen sei auf die
Als weichmagnetische Eigenschaften aufweisende Ausgangspulver eignen sich neben Reineisenpulver auch Eisen-Nickel-, Eisen-Silizium- und Eisen-Kobalt-Legierungen.In addition to pure iron powder, iron-nickel, iron-silicon and iron-cobalt alloys are suitable as starting materials having soft-magnetic properties.
Zur Demonstration der Vorteile der erfindungsgemäßen Preßmasse und des damit durchgeführten Verfahrens zur Herstellung eines weichmagnetischen Verbundwerkstoffes wurde ein Vergleichsversuch vorgenommen, bei dem phosphatiertes Eisenpulver mit 0,8 Massenprozent Polyphenylensulfid-Pulver entsprechend den vorstehenden Ausführungen vermischt wurde. Dieser Preßmasse wurde jedoch kein Gleitmittel zugesetzt.In order to demonstrate the advantages of the molding compound according to the invention and of the process for producing a soft magnetic composite material, a comparative experiment was carried out in which phosphated iron powder was mixed with 0.8 percent by weight polyphenylene sulfide powder in accordance with the above statements. However, no lubricant was added to this molding compound.
Um vergleichbare magnetische und elektrische Eigenschaften der Vergleichsprobe zu dem erfindungsgemäß erhaltenen weichmagnetischen Verbundwerkstoff zu erzielen, war es in diesem Fall erforderlich, zunächst eine Pulvervorwärmung unter Schutzgas auf 130°C vor dem Verpressen vorzunehmen, und die Preßmasse danach bei einer Werkzeugtemperatur von 140°C zu verpressen. Danach schloß sich dann ein einstufiger Auslagerungsprozeß an, der eine Temperaturbehandlung bei 285° bis 300° C über eine Zeitdauer von einer Stunde unter Stickstoffatmosphäre umfaßte.In order to achieve comparable magnetic and electrical properties of the comparative sample to the soft magnetic composite obtained according to the invention, it was necessary in this case to first perform a powder preheating under inert gas to 130 ° C prior to compression, and then the molding compound at a mold temperature of 140 ° C to compress. Thereafter, followed by a single-stage aging process, which included a temperature treatment at 285 ° to 300 ° C over a period of one hour under nitrogen atmosphere.
Somit wird durch die erfindungsgemäße Zugabe des Gleitmittels insgesamt erreicht, daß die Pulvervorwärmung entfallen, und daß die Werkzeugtemperatur deutlich reduziert werden kann.Thus, achieved by the addition of the lubricant according to the invention as a whole that the powder preheating omitted, and that the mold temperature can be significantly reduced.
Durch thermogravimetrische Untersuchungen (TGA-Analyse) und "Differential Scanning Calorimetrie" (DSC-Analyse) konnte weiter nachgewiesen werden, daß das Gleitmittel Stearinsäure durch das Erwärmen der verpreßten Preßmasse während der ersten Temperaturbehandlung verdunstet beziehungsweise sich zumindest weitgehend thermisch zersetzt und verflüchtigt.Thermogravimetric analysis (TGA analysis) and differential scanning calorimetry (DSC analysis) further demonstrated that the lubricant was stearic acid evaporated by the heating of the compressed molding compound during the first temperature treatment or at least largely thermally decomposed and volatilized.
Die erhöhte Festigkeit der erhaltenen Bauteile im Vergleich zu bei einer Werkzeugtemperatur von 140°C hergestellten Teilen zeigt darüber hinaus, daß weder das Gleitmittel noch seine Zersetzungsprodukte mit dem Polyphenylensulfid in nennenswerter Weise chemisch reagierten.The increased strength of the components obtained as compared to parts made at a mold temperature of 140 ° C moreover shows that neither the lubricant nor its decomposition products reacted appreciably chemically with the polyphenylene sulfide.
Claims (9)
- Method for producing a soft-magnetic composite material using a moulding compound, comprising a starting powder which exhibits soft-magnetic properties, comprising a thermoplastic compound and comprising a lubricant added to the moulding compound, said method comprising the following steps:a.) the moulding compound is prepared,b.) the moulding compound is pressed at a temperature below the melting point of the thermoplastic compound, wherein the moulding compound is pressed at a temperature of 50°C to 90°C, in particular 70°C,c.) the pressed moulding compound is subjected to a first heat treatment at a temperature below the melting point of the thermoplastic compound, andd.) the pressed moulding compound is subjected to a second heat treatment at a temperature above the melting point of the thermoplastic compound.
- Method according to Claim 1, wherein the moulding compound is pressed by uniaxial pressing in a pressing tool, in particular a female mould.
- Method according to either of the preceding claims, wherein the moulding compound is pressed at an elevated temperature by preheating the pressing tool to said temperature.
- Method according to one of the preceding claims, wherein the first heat treatment takes place at a temperature of 200°C to 270°C, in particular 260°C, over a period of time of 20 min to 4 h, and the second heat treatment takes place at a temperature of 285°C to 310°C over a period of time of 5 min to 1 h.
- Method according to one of the preceding claims, wherein the first heat treatment and/or the second heat treatment takes place in an inert gas atmosphere, in particular a nitrogen atmosphere.
- Method according to one of the preceding claims, wherein the lubricant is thermally decomposed at least largely without residue and/or evaporates at least largely without residue during the first heat treatment.
- Method according to one of the preceding claims, wherein the lubricant and the decomposition products thereof are at least largely chemically inert towards the thermoplastic compound and the starting powder which exhibits soft-magnetic properties.
- Method according to one of the preceding claims, wherein the preparation of the moulding compound comprises mixing the starting powder which exhibits soft-magnetic properties with the pulverulent thermoplastic compound, or coating the starting powder which exhibits soft-magnetic properties with the thermoplastic compound, which has been dissolved in a solvent.
- Method according to one of the preceding claims, wherein the preparation of the moulding compound comprises mixing the starting powder which exhibits soft-magnetic properties with the pulverulent lubricant, or introducing the lubricant, which has been dissolved in a solvent, into the moulding compound.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19945619A DE19945619A1 (en) | 1999-09-23 | 1999-09-23 | Press compound and method for producing a soft magnetic composite material with the press compound |
| DE19945619 | 1999-09-23 | ||
| PCT/DE2000/003054 WO2001022448A1 (en) | 1999-09-23 | 2000-09-06 | Mouldable material and method for producing a weakly magnetic composite material therewith |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP1131831A1 EP1131831A1 (en) | 2001-09-12 |
| EP1131831B1 true EP1131831B1 (en) | 2010-11-10 |
Family
ID=7923047
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP00963959A Expired - Lifetime EP1131831B1 (en) | 1999-09-23 | 2000-09-06 | Method for producing a weakly magnetic composite material from a mouldable material |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US6706206B1 (en) |
| EP (1) | EP1131831B1 (en) |
| JP (1) | JP4933711B2 (en) |
| CN (1) | CN1322366A (en) |
| DE (2) | DE19945619A1 (en) |
| WO (1) | WO2001022448A1 (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19945619A1 (en) | 1999-09-23 | 2001-04-19 | Bosch Gmbh Robert | Press compound and method for producing a soft magnetic composite material with the press compound |
| US7153594B2 (en) | 2002-12-23 | 2006-12-26 | Höganäs Ab | Iron-based powder |
| US7494600B2 (en) | 2003-12-29 | 2009-02-24 | Höganäs Ab | Composition for producing soft magnetic composites by powder metallurgy |
| SE0303580D0 (en) * | 2003-12-29 | 2003-12-29 | Hoeganaes Ab | Composition for producing soft magnetic composites by powder metallurgy |
| JP4325950B2 (en) * | 2004-03-31 | 2009-09-02 | 住友電気工業株式会社 | Soft magnetic material and dust core |
| US7416578B2 (en) | 2004-09-17 | 2008-08-26 | Höganäs Ab | Powder metal composition |
| US8075710B2 (en) * | 2005-06-15 | 2011-12-13 | Höganäs Ab | Soft magnetic composite materials |
| JP4747918B2 (en) * | 2005-11-04 | 2011-08-17 | 東ソー株式会社 | Polyarylene sulfide composition |
| JP5687323B1 (en) * | 2013-09-30 | 2015-03-18 | 住友理工株式会社 | Sound absorbing cover, sound absorbing assembly, and magnetic induction foam molding apparatus |
| CN109794600B (en) * | 2018-12-27 | 2021-04-27 | 中南大学 | Insulation treatment method of metal soft magnetic powder and preparation method of soft magnetic material |
| CN114231330B (en) * | 2022-01-13 | 2022-11-18 | 鞍钢股份有限公司 | High-calorific-value iron powder composite fuel and preparation method thereof |
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| DE19735271A1 (en) * | 1997-08-14 | 1999-02-25 | Bosch Gmbh Robert | Weakly magnetic deformable composite substance |
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| JPS5364797A (en) * | 1976-11-24 | 1978-06-09 | Tdk Corp | Rubber, plastic magnet and magnetic powder for them |
| JPS56155510A (en) * | 1980-04-30 | 1981-12-01 | Tohoku Metal Ind Ltd | Metal dust magnetic core |
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| JPS6169866A (en) * | 1984-09-12 | 1986-04-10 | Polyplastics Co | Composite material composition |
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- 2000-09-06 US US09/856,763 patent/US6706206B1/en not_active Expired - Fee Related
- 2000-09-06 WO PCT/DE2000/003054 patent/WO2001022448A1/en active Application Filing
- 2000-09-06 CN CN00802030A patent/CN1322366A/en active Pending
- 2000-09-06 JP JP2001525727A patent/JP4933711B2/en not_active Expired - Fee Related
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| DE19735271A1 (en) * | 1997-08-14 | 1999-02-25 | Bosch Gmbh Robert | Weakly magnetic deformable composite substance |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN1322366A (en) | 2001-11-14 |
| JP4933711B2 (en) | 2012-05-16 |
| US6706206B1 (en) | 2004-03-16 |
| EP1131831A1 (en) | 2001-09-12 |
| DE50016026D1 (en) | 2010-12-23 |
| DE19945619A1 (en) | 2001-04-19 |
| JP2003510460A (en) | 2003-03-18 |
| WO2001022448A1 (en) | 2001-03-29 |
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