EP2242602A1 - Method for producing a metal powder and metal powder produced by this method - Google Patents

Method for producing a metal powder and metal powder produced by this method

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Publication number
EP2242602A1
EP2242602A1 EP09707741A EP09707741A EP2242602A1 EP 2242602 A1 EP2242602 A1 EP 2242602A1 EP 09707741 A EP09707741 A EP 09707741A EP 09707741 A EP09707741 A EP 09707741A EP 2242602 A1 EP2242602 A1 EP 2242602A1
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EP
European Patent Office
Prior art keywords
metal
heat treatment
stage
temperature
powder
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EP09707741A
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German (de)
French (fr)
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EP2242602B8 (en
EP2242602B1 (en
Inventor
Bernd Kieback
Gunnar Walther
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Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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Classifications

    • 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
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
    • 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
    • B22F1/14—Treatment of metallic powder
    • B22F1/148—Agglomerating
    • 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

Definitions

  • the invention relates to a process for the production of metal powders and metal powders produced in this way.
  • Metal powders are used, for example, in the production of precision parts by metal injection molding (MIM), as a component of the bonding matrix in diamond tools, for magnetorheological fluids, microwave absorbing materials, coil cores in electronic components, magnetic printing inks and toners.
  • MIM metal injection molding
  • carbonyl iron powders are currently being used for such applications.
  • Their manufacture is costly and must also be critically evaluated in terms of environmental and health aspects, as carcinogenic decomposition products (carbonyls) are formed during the manufacturing process.
  • the reduction of metal oxides with hydrogen is possible even at relatively low temperatures, if the metals do not have too high an affinity for oxygen.
  • iron oxide (Fe 2 ⁇ 3 ) can already be reduced at 500-600 0 C by means of hydrogen to a Fe powder with low oxygen content. This is from W. Schatt, K. -P. Wieters, B. Kieback in "Powder Metallurgy Technologies and Materials", Springer-Verlag Berlin Heidelberg 2007, p 25 have been described.
  • the metal powder thus formed has a very high specific surface area (»Im 2 / g), which causes immediate reoxidation. These metal powders must be classified as pyrophoric and can therefore practically not be used. It is also known that higher reduction temperatures lead to higher oxygen contents, which can only be reduced to acceptable levels at very high temperatures. At these high temperatures (> 1000 0 C) but above all sinter fine powder particles to no more breakable sinter cake. Above all, the production of fine metal powder by H2 ⁇ reduction is not possible in the prior art.
  • this object is achieved by a method having the features of claim 1.
  • a metal powder produced in this way is defined by claim 13.
  • Advantageous embodiments and further developments of the invention can be achieved with features described in the subordinate claims.
  • a two-stage heat treatment in a hydrogen atmosphere is to be carried out.
  • powdered metal oxide is used as the starting material.
  • the metal oxide should preferably be present as an agglomerate.
  • a specific time should initially be maintained at the reduction temperature. In this case, the at least one metal oxide is almost completely reduced, with the relatively high specific surface area of the metal oxide having an advantageous effect.
  • the temperature is raised by further heating at a second stage of the heat treatment, whereby the specific surface area of the metal powder formed upon reduction is reduced.
  • the primary particles contained in the agglomerates can sinter together because of their high sintering activity.
  • the agglomerates do not sinter with each other or only slightly. Trained sinter bridges can be easily broken up mechanically. The reason for the different kinetics of the sintering process is that the sintering activity increases strongly with decreasing particle radius.
  • the metal powder produced according to the invention is not pyrophoric. Depending on the metal oxide used, the particle size can correspond to 50-80% of the size of the original agglomerates.
  • the specific surface should be reduced to a value less than 0.5, preferably less than 0.1 m 2 / g.
  • the first and also the second stage of the heat treatment should each be carried out over a period of at least 900 s, preferably 1800 s and particularly preferably 3600 s.
  • the temperatures in the two stages can be selected.
  • a temperature range of 400 to a maximum of 600 0 C should be complied with in the first stage of the heat treatment, which has a favorable effect especially for a Fe 2 Os powder for the reduction.
  • the temperature should then be increased, wherein a temperature of at least 65O 0 C, preferably 700 0 C should be maintained. However, a temperature increase up to the respective sintering temperature of the metal formed during the reduction should be avoided.
  • the oxygen content should be less than 0.5%.
  • iron oxide (Fe 2 O 3 ) from treated pickle sludge can be used as the raw material, which is obtained in large quantities in the steel industry as a waste product.
  • the iron powder obtained by a subsequent reduction process has a carbonyl iron powder comparable
  • the iron oxide powder used (Fe 2 O 3 ) had an average particle size of 0.3 .mu.m and was in the form of 100 .mu.m agglomerates.
  • the iron oxide powder was heated in an oven in a hydrogen atmosphere to 500 ° C in the first stage of the heat treatment and thereby reduced.
  • the holding time was I h.
  • the temperature was increased to 800 0 C and a holding time of Ih observed.
  • the specific surface area was reduced from about 3 m 2 / g to 0.1 m 2 / g.
  • Cooling to room temperature was also carried out in a hydrogen atmosphere.
  • the obtained iron powder is not pyrophoric.
  • the iron oxide powder was almost completely reduced to iron powder.
  • the oxygen content was about 0.2%.
  • the primary particles of the agglomerates, which were originally 100 ⁇ m in size, were sintered to form spherical particles about 60-70 ⁇ m in size, the spherical particles formed only partially having small sintered contacts with each other, which, however, can easily be mechanically broken up. In this way, a flowable spherical fine iron powder could be prepared.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention relates to a method for producing metal powders and to metal powders thereby produced. The aim of the invention is to provide methods which allow metal powders to be produced a low cost from metal oxides the properties of which allow various uses. The method according to the invention is characterized by subjecting a metal oxide powder in a first step to a heat treatment in a reducing hydrogen atmosphere, the metal oxide being reduced. The temperature is then increased in a second step of the heat treatment and this temperature is maintained over a period, thereby possibly reducing the specific surface of the metal powder obtained previously by reduction.

Description

Verfahren zur Herstellung eines Metallpulvers und mit dem Verfahren hergestelltes MetallpulverProcess for producing a metal powder and metal powder produced by the process
Die Erfindung betrifft ein Verfahren zur Herstellung von Metallpulvern und so hergestellte Metallpulver.The invention relates to a process for the production of metal powders and metal powders produced in this way.
Metallpulver werden z.B. bei der Herstellung von Präzisionsteilen durch Metal Inj^ction Molding (MIM) , als Komponente der Bindematrix in Diamantwerkzeugen, für magnetorheologische Flüssigkeiten, Mikrowellen absorbierende Materialien, Spulenkerne in elektronischen Bauteilen, magnetischen Druckfarben und Toner verwendet. Für solche Anwendungen kommen derzeit z.B, Carbonyleisenpulver zum Einsatz, deren Herstellung kostenintensiv und auch unter Umwelt- und Gesundheitsaspekten kritisch zu bewerten ist, da beim Her- stellungsprozess kanzerogene Zersetzungsprodukte (Carbonyle) entstehen. Die Reduktion von Metalloxiden mit Wasserstoff ist bereits bei relativ geringen Temperaturen möglich, wenn die Metalle keine zu große Affinität zu Sauer- stoff aufweisen. So kann Eisenoxid (Fe2θ3) bereits bei 500-6000C mittels Wasserstoff zu einem Fe-Pulver mit geringem Sauerstoffgehalt reduziert werden. Dies ist von W. Schatt, K. -P. Wieters, B. Kieback in „Pulvermetallurgie-Technologien und Werkstoffe", Springer-Verlag Berlin Heidelberg 2007, S. 25 beschrieben worden.Metal powders are used, for example, in the production of precision parts by metal injection molding (MIM), as a component of the bonding matrix in diamond tools, for magnetorheological fluids, microwave absorbing materials, coil cores in electronic components, magnetic printing inks and toners. For example, carbonyl iron powders are currently being used for such applications. Their manufacture is costly and must also be critically evaluated in terms of environmental and health aspects, as carcinogenic decomposition products (carbonyls) are formed during the manufacturing process. The reduction of metal oxides with hydrogen is possible even at relatively low temperatures, if the metals do not have too high an affinity for oxygen. Thus, iron oxide (Fe 2 θ 3 ) can already be reduced at 500-600 0 C by means of hydrogen to a Fe powder with low oxygen content. This is from W. Schatt, K. -P. Wieters, B. Kieback in "Powder Metallurgy Technologies and Materials", Springer-Verlag Berlin Heidelberg 2007, p 25 have been described.
Das so gebildete Metallpulver hat jedoch eine sehr große spezifische Oberfläche (» Im2/g), die eine so- fortige Wiederoxidation hervorruft. Diese Metallpulver müssen als pyrophor eingestuft werden und können daher praktisch nicht eingesetzt werden. Es ist auch bekannt, dass höhere Reduktionstemperaturen zu höheren Sauerstoffgehalten führen, die erst bei sehr ho- hen Temperaturen wieder auf vertretbare Werte gesenkt werden können. Bei diesen hohen Temperaturen (> 10000C) versintern aber vor allem feine Pulverteilchen zu einem nicht mehr aufbrechbaren Sinterkuchen. Vor allem die Herstellung feiner Metallpulver durch H2~Reduktion ist aber nach dem Stand der Technik nicht möglich.However, the metal powder thus formed has a very high specific surface area (»Im 2 / g), which causes immediate reoxidation. These metal powders must be classified as pyrophoric and can therefore practically not be used. It is also known that higher reduction temperatures lead to higher oxygen contents, which can only be reduced to acceptable levels at very high temperatures. At these high temperatures (> 1000 0 C) but above all sinter fine powder particles to no more breakable sinter cake. Above all, the production of fine metal powder by H2 ~ reduction is not possible in the prior art.
Es ist daher Aufgabe der Erfindung, Möglichkeiten vorzuschlagen, mit denen Metallpulver kostengünstig aus Metalloxiden hergestellt werden können, deren Eigenschaften, einen vielfältigen Einsatz ermöglichen.It is therefore an object of the invention to propose ways in which metal powder can be inexpensively made of metal oxides whose properties allow a diverse use.
Erfindungsgemäß wird diese Aufgabe mit einem Verfahren, das die Merkmale des Anspruchs 1 aufweist, ge- löst. Ein so hergestelltes Metallpulver ist mit dem Anspruch 13 definiert. Vorteilhafte Ausgestaltungen und Weiterbildungen der Erfindung können mit in untergeordneten Ansprüchen bezeichneten Merkmalen erreicht werden.According to the invention, this object is achieved by a method having the features of claim 1. A metal powder produced in this way is defined by claim 13. Advantageous embodiments and further developments of the invention can be achieved with features described in the subordinate claims.
Erfindungsgemäß soll eine zweistufige Wärmebehandlung in einer Wasserstoffatmosphäre durchgeführt werden. Dabei wird pulverförmiges Metalloxid, als Ausgangswerkstoff eingesetzt. Das Metalloxid sollte bevorzugt als Agglomerat vorliegen. In der ersten Stufe der Wärmebehandlung soll zunächst bei Reduktionstemperatur eine bestimmte Zeit eingehalten werden. Dabei wird das mindestens eine Metalloxid nahezu vollständig reduziert, wobei sich die relativ hohe spezifische Oberfläche des Metalloxids vorteilhaft auswirkt.According to the invention, a two-stage heat treatment in a hydrogen atmosphere is to be carried out. In this case, powdered metal oxide is used as the starting material. The metal oxide should preferably be present as an agglomerate. In the first stage of the heat treatment, a specific time should initially be maintained at the reduction temperature. In this case, the at least one metal oxide is almost completely reduced, with the relatively high specific surface area of the metal oxide having an advantageous effect.
Anschließend wird die Temperatur durch ein weiteres Aufheizen bei einer zweiten Stufe der Wärmebehandlung erhöht, wodurch die spezifische Oberfläche des bei der Reduktion gebildeten Metallpulvers verkleinert wird. Dabei können die in den Agglomeraten enthaltenen Primärpartikel aufgrund ihrer hohen Sinteraktivität miteinander versintern. Die Agglomerate versintern untereinander nicht oder nur leicht. Ausgebildete Sinterbrücken lassen sich leicht mechanisch auf- brechen. Die Ursache für die unterschiedliche Kinetik des Sinterprozesses liegt darin, dass die Sinteraktivität stark mit kleiner werdendem Partikelradius zunimmt. Das erfindungsgemäß hergestellte Metallpulver ist nicht pyrophor. Die Partikelgröße kann je nach eingesetztem Metalloxid 50-80% der Größe der ursprünglichen Agglomerate entsprechen.Subsequently, the temperature is raised by further heating at a second stage of the heat treatment, whereby the specific surface area of the metal powder formed upon reduction is reduced. The primary particles contained in the agglomerates can sinter together because of their high sintering activity. The agglomerates do not sinter with each other or only slightly. Trained sinter bridges can be easily broken up mechanically. The reason for the different kinetics of the sintering process is that the sintering activity increases strongly with decreasing particle radius. The metal powder produced according to the invention is not pyrophoric. Depending on the metal oxide used, the particle size can correspond to 50-80% of the size of the original agglomerates.
Bei der zweiten Stufe der Wärmebehandlung sollte die spezifische Oberfläche auf einen Wert kleiner 0,5 bevorzugt kleiner 0,1 m2/g verkleinert werden. Die erste und auch die zweite Stufe der Wärmebehandlung sollten jeweils über einen Zeitraum von mindestens 900 s, bevorzugt 1800 s und besonders bevorzugt 3600 s durchgeführt werden.In the second stage of the heat treatment, the specific surface should be reduced to a value less than 0.5, preferably less than 0.1 m 2 / g. The first and also the second stage of the heat treatment should each be carried out over a period of at least 900 s, preferably 1800 s and particularly preferably 3600 s.
Unter Berücksichtigung eines bei der Erfindung eingesetzten Metalloxids können die Temperaturen in den beiden Stufen gewählt werden. Dabei sollte ein Temperaturbereich von 400 bis maximal 600 0C in der ersten Stufe der Wärmebehandlung eingehalten sein, was sich insbesondere bei einem Fe2Os Pulver günstig für die Reduktion auswirkt.Taking into account a metal oxide used in the invention, the temperatures in the two stages can be selected. In this case, a temperature range of 400 to a maximum of 600 0 C should be complied with in the first stage of the heat treatment, which has a favorable effect especially for a Fe 2 Os powder for the reduction.
Bei der zweiten Stufe sollte die Temperatur dann er- höht werden, wobei eine Temperatur von mindestens 65O0C, bevorzugt 700 0C eingehalten werden sollte. Eine Temperaturerhöhung bis hin zur jeweiligen Sintertemperatur des bei der Reduktion gebildeten Metalls sollte aber vermieden werden.In the second stage, the temperature should then be increased, wherein a temperature of at least 65O 0 C, preferably 700 0 C should be maintained. However, a temperature increase up to the respective sintering temperature of the metal formed during the reduction should be avoided.
Zumindest nach der zweiten Stufe der Wärmebehandlung sollte der Sauerstoffanteil kleiner 0,5 % sein.At least after the second stage of the heat treatment, the oxygen content should be less than 0.5%.
Es ist möglich, Mischungen unterschiedlicher redu- zierbarer Metalloxide (z.B. Fe2θ3, NiO) mit diesemIt is possible to use mixtures of different reducible metal oxides (eg Fe 2 O 3 , NiO) with this
Verfahren zu reduzieren und dabei dann ein legiertes bzw. anlegiertes Metallpulver zu erhalten. Es kann aber auch ein Gemisch in dem mindestens ein pulver- förmiges Metalloxid und mindestens ein pulverförmiges Metall (z.B Al, Cr, Ni, Mo, Co) enthalten sind, bei der Erfindung eingesetzt werden. Bei einem eingesetzten Pulvergemisch sollte der Anteil an Eisenoxid bei mindestens 50 Masse-% liegen.Reduce the process and then get an alloyed or alloyed metal powder. However, it is also possible to use a mixture in which at least one pulverulent metal oxide and at least one powdered metal (for example Al, Cr, Ni, Mo, Co) are used in the invention. For a powder mixture used, the proportion of iron oxide should be at least 50% by mass.
Bei beiden Stufen der Wärmebehandlung sollte der Was- serstoffpartialdruck nahezu konstant gehalten werden, so dass ggf. gebildeter Wasserdampf abgezogen werden sollte .In both stages of the heat treatment, the hydrogen partial pressure should be kept almost constant, so that any formed steam should be removed.
Nachfolgend soll die Erfindung beispielhaft näher er- läutert werden.Below, the invention will be explained in more detail by way of example.
Ausführungsbeispielembodiment
Bei der Anwendung des erfindungsgemäßen Verfahrens zur Eisenpulverherstellung, kann als Rohstoff Eisenoxid (Fe2O3) aus aufbereiteten Beizschlämmen eingesetzt werden, das in großen Mengen in der Stahlindustrie als Abfallprodukt anfällt. Das durch einen anschließenden Reduktionsprozess erhaltene Eisenpul- ver hat eine dem Carbonyleisenpulver vergleichbareWhen using the method according to the invention for the production of iron powder, iron oxide (Fe 2 O 3 ) from treated pickle sludge can be used as the raw material, which is obtained in large quantities in the steel industry as a waste product. The iron powder obtained by a subsequent reduction process has a carbonyl iron powder comparable
Morphologie und ist um mindestens 50 % kostengünstiger.Morphology and is at least 50% less expensive.
Das eingesetzte Eisenoxidpulver (Fe2O3) wies eine mittlere Partikelgröße von 0,3 μm auf und lag in Form von 100 μm großen Agglomeraten vor. Das Eisenoxidpulver wurde in einem Ofen in einer Wasserstoffatmosphä- re bis 500 °C bei der ersten Stufe der Wärmebehandlung aufgeheizt und dabei reduziert. Die Haltezeit betrug I h. Danach wurde bei der zweiten Stufe der Wärmebehandlung die Temperatur auf 8000C erhöht und eine Haltezeit von Ih eingehalten. Ausgehend von der ersten Stufe bis zur zweiten Stufe der Wärmebehandlung wurde die spezifische Oberfläche von ca. 3 m2/g auf 0,1 m2/g verringert.The iron oxide powder used (Fe 2 O 3 ) had an average particle size of 0.3 .mu.m and was in the form of 100 .mu.m agglomerates. The iron oxide powder was heated in an oven in a hydrogen atmosphere to 500 ° C in the first stage of the heat treatment and thereby reduced. The holding time was I h. Thereafter, in the second stage of the heat treatment, the temperature was increased to 800 0 C and a holding time of Ih observed. Starting from the first stage to the second stage of the heat treatment, the specific surface area was reduced from about 3 m 2 / g to 0.1 m 2 / g.
Das Abkühlen auf Raumtemperatur erfolgte ebenfalls in einer Wasserstoffatmosphare .Cooling to room temperature was also carried out in a hydrogen atmosphere.
Das erhaltene Eisenpulver ist nicht pyrophor. Das Ei- senoxidpulver wurde nahezu vollständig zu Eisenpulver reduziert. Der Sauerstoffgehalt lag bei ca. 0,2 %. Die Primärpartikel der ursprünglich 100 μm großen Ag- glomerate wurden zu ca. 60-70 μm großen sphärischen Partikeln versintert, wobei die gebildeten sphärischen Partikel untereinander nur teilweise kleine Sinterkontakte aufwiesen, die sich jedoch leicht mechanisch aufbrechen lassen. Auf diese Weise konnte ein fließfähiges sphärisches feines Eisenpulver hergestellt werden. The obtained iron powder is not pyrophoric. The iron oxide powder was almost completely reduced to iron powder. The oxygen content was about 0.2%. The primary particles of the agglomerates, which were originally 100 μm in size, were sintered to form spherical particles about 60-70 μm in size, the spherical particles formed only partially having small sintered contacts with each other, which, however, can easily be mechanically broken up. In this way, a flowable spherical fine iron powder could be prepared.

Claims

Patentansprücheclaims
1. Verfahren zur Herstellung eines Metallpulvers, bei dem pulverförmiges Metalloxid in einer reduzierenden Wasserstoffatmosphäre bei einer ersten Stufe einer Wärmebehandlung unterzogen wird, bei der das Metalloxid reduziert wird; anschließend die Temperatur in einer zweiten Stufe der Wärmebehandlung erhöht und über einen Zeitraum die Temperatur gehalten und dabei die spezifische Oberfläche des vorab durch Reduktion erhaltenen Metallpulvers verkleinert wird.A process for producing a metal powder in which powdery metal oxide is subjected to a heat treatment in a reducing atmosphere of hydrogen at a first stage, wherein the metal oxide is reduced; Subsequently, the temperature is increased in a second stage of the heat treatment and the temperature is maintained for a period of time while the specific surface area of the metal powder obtained in advance by reduction is reduced.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass die spezifische Oberfläche auf mindestens 0,5 m2/g verkleinert wird.2. The method according to claim 1, characterized in that the specific surface area is reduced to at least 0.5 m 2 / g.
3. Verfahren nach Anspruch 1 oder 2, dadurch ge- kennzeichnet, dass ein Ausgangspulver eingesetzt wird, das mindestens 50 Masse-% Eisenoxid aufweist .3. The method according to claim 1 or 2, character- ized in that a starting powder is used which has at least 50% by mass of iron oxide.
4. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die erste Stu- fe der Wärmebehandlung bei einer Temperatur von mindestens 400 °C und maximal 600 0C durchgeführt wird.4. The method according to any one of the preceding claims, characterized in that the first stage of the heat treatment at a temperature of at least 400 ° C and at most 600 0 C is performed.
5. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass bei der ersten Stufe der Wärmebehandlung die Temperatur über einen Zeitraum von mindestens 900 s gehalten wird. β. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass bei der ersten Stufe der Wärmebehandlung die Temperatur über einen Zeitraum gehalten wird, bis der Sauer- stoffanteil im Metallpulver kleiner als 0,5 % ist.5. The method according to any one of the preceding claims, characterized in that in the first stage of the heat treatment, the temperature over a period of at least 900 s is maintained. β. Method according to one of the preceding claims, characterized in that in the first stage of the heat treatment, the temperature is maintained over a period of time until the oxygen content in the metal powder is less than 0.5%.
7. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass bei der zweiten Stufe der Wärmebehandlung die Temperatur o- berhalb 650 0C gehalten wird.7. The method according to any one of the preceding claims, characterized in that in the second stage of the heat treatment, the temperature above 650 0 C is maintained.
8. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass bei der zweiten Stufe der Wärmebehandlung die Temperatur ü- ber einen Zeitraum von mindestens 900 s gehalten wird.8. The method according to any one of the preceding claims, characterized in that in the second stage of the heat treatment, the temperature Ü is maintained over a period of at least 900 s.
9. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass bei der zweiten Stufe der Wärmebehandlung die Temperatur o- berhalb 700 0C gehalten wird. 10. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass als Ausgangspulver ein Gemisch von mindestens zwei reduzierbaren Metalloxiden eingesetzt wird.9. The method according to any one of the preceding claims, characterized in that at the second stage of the heat treatment, the temperature o- berhalb 700 0 C. 10. The method according to any one of the preceding claims, characterized in that a mixture of at least two reducible metal oxides is used as the starting powder.
11. Verfahren nach einem der vorhergehenden Ansprü- che, dadurch gekennzeichnet, dass als Ausgangspulver ein Gemisch, das mindestens ein Metalloxid und mindestens ein Metall enthält, eingesetzt wird.11. The method according to any one of the preceding claims, characterized in that the starting powder used is a mixture which contains at least one metal oxide and at least one metal.
12. Verfahren nach einem der vorhergehenden Ansprü- che, dadurch gekennzeichnet, dass als zweites in einem Gemisch enthaltenes Metalloxid NiO eingesetzt wird. 12. The method according to any one of the preceding claims, characterized in that the second metal oxide contained in a mixture NiO is used.
13. Metallpulver hergestellt mit einem Verfahren nach einem der Ansprüche 1 bis 12, dadurch gekennzeichnet, dass es eine mittlere Partikelgröße im Bereich 5 μm bis 100 μm und eine spezifi- sehe Oberfläche kleiner 0,5 m2/g aufweist.13 metal powder produced by a method according to any one of claims 1 to 12, characterized in that it has an average particle size in the range 5 microns to 100 microns and a specific surface see less than 0.5 m 2 / g.
14. Metallpulver nach Anspruch 13, dadurch gekennzeichnet, dass es nicht pyrophor ist.14. Metal powder according to claim 13, characterized in that it is not pyrophoric.
15. Metallpulver nach Anspruch 13 oder 14, dadurch gekennzeichnet, dass Eisenpulver mit einem wei- teren Metall zumindest an der Oberfläche legiert ist .15. Metal powder according to claim 13 or 14, characterized in that iron powder is alloyed with a further metal at least on the surface.
16. Metallpulver nach einem der Ansprüche 13 bis 15, dadurch gekennzeichnet, dass der Sauerstoffanteil kleiner 0,5 % ist. 16. Metal powder according to one of claims 13 to 15, characterized in that the oxygen content is less than 0.5%.
EP09707741.6A 2008-02-06 2009-01-28 Method for producing a metal powder and metal powder produced by this method Active EP2242602B8 (en)

Applications Claiming Priority (2)

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DE102008009133A DE102008009133B4 (en) 2008-02-06 2008-02-06 Process for the production of metal powders and metal powder produced in this way
PCT/DE2009/000136 WO2009097835A1 (en) 2008-02-06 2009-01-28 Method for producing a metal powder and metal powder produced by this method

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DE102008009133B4 (en) 2012-04-12
EP2242602B8 (en) 2014-12-31
EP2242602B1 (en) 2014-03-26
DE102008009133A1 (en) 2009-09-24
WO2009097835A1 (en) 2009-08-13

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