EP2242602B1 - 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 Download PDF

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Publication number
EP2242602B1
EP2242602B1 EP09707741.6A EP09707741A EP2242602B1 EP 2242602 B1 EP2242602 B1 EP 2242602B1 EP 09707741 A EP09707741 A EP 09707741A EP 2242602 B1 EP2242602 B1 EP 2242602B1
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Prior art keywords
stage
heat treatment
powder
temperature
metal powder
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German (de)
French (fr)
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EP2242602B8 (en
EP2242602A1 (en
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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 e.g. used 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 powder is used, the production of which is cost-intensive and must also be critically evaluated in terms of environmental and health aspects, since carcinogenic decomposition products (carbonyls) are formed during the manufacturing process.
  • metal oxides with hydrogen are even at relatively low temperatures possible, if the metals do not have too high an affinity for oxygen.
  • iron oxide Fe 2 O 3
  • 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 been described.
  • the metal powder thus formed has a very large specific surface area (>> 1m 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 ° C), however, especially fine powder particles sinter into a sinter cake which is no longer breakable. Above all, the production of fine metal powder by H 2 reduction but not possible in the prior art.
  • 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 due to their high sintering activity with each other.
  • 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.
  • the particle size can correspond to 50-80% of the size of the original agglomerates.
  • the specific surface should be reduced to a value of less than 0.5 m 2 / g, 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 ° C should be maintained in the first stage of the heat treatment, which has a favorable effect especially for a Fe 2 O 3 powder for the reduction.
  • the temperature should then be increased, with a temperature of at least 650 ° C is to be maintained.
  • a temperature above 700 ° C. is preferred.
  • 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%.
  • a mixture of Fe 2 O 3 and NiO can be reduced by this method and thereby to obtain an alloyed metal powder.
  • the proportion of iron oxide should be at least 50% by mass.
  • the hydrogen partial pressure should be kept almost constant so that any water vapor formed should be removed.
  • 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 morphology comparable to the carbonyl iron powder and is at least 50% less expensive.
  • the iron oxide powder (Fe 2 O 3 ) used had a average particle size of 0.3 microns and was in the form of 100 micron large 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 1 h.
  • the temperature was raised to 800 ° C and maintained for a holding time of 1 hour.
  • 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 originally 100 .mu.m large agglomerates were sintered to about 60-70 .mu.m spherical particles, the spherical particles formed with each other only partially had small sintered contacts, however, can be broken easily mechanically. In this way, a flowable spherical fine iron powder could be prepared.

Description

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 Injection 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 Herstellungsprozess kanzerogene Zersetzungsprodukte (Carbonyle) entstehen.Metal powders are e.g. used 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 such applications currently there are e.g. Carbonyl iron powder is used, the production of which is cost-intensive and must also be critically evaluated in terms of environmental and health aspects, since carcinogenic decomposition products (carbonyls) are formed during the manufacturing process.

Die Reduktion von Metalloxiden mit Wasserstoff ist bereits bei relativ geringen Temperaturen möglich, wenn die Metalle keine zu große Affinität zu Sauerstoff aufweisen. So kann Eisenoxid (Fe2O3) bereits bei 500-600°C 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.The reduction of metal oxides with hydrogen is even at relatively low temperatures possible, if the metals do not have too high an affinity for oxygen. For example, iron oxide (Fe 2 O 3 ) can already be reduced by means of hydrogen at 500-600 ° C to form 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 been described.

Das so gebildete Metallpulver hat jedoch eine sehr große spezifische Oberfläche (>> 1m2/g), die eine sofortige 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 hohen Temperaturen wieder auf vertretbare Werte gesenkt werden können. Bei diesen hohen Temperaturen (> 1000°C) 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 large specific surface area (>> 1m 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 ° C), however, especially fine powder particles sinter into a sinter cake which is no longer breakable. Above all, the production of fine metal powder by H 2 reduction but not possible in the prior art.

Aus der DE 1 288 318 A1 und dem US 3,317,285 sind Verfahren für die Herstellung von Metallpulvern bekannt, die für die Weiterverarbeitung zu einem dispersionsgehärtetem Werkstoff geeignet sind. Es sind dabei im Pulver, wie auch im Werkstoff schwer schmelzbare Oxide enthalten. Für die Herstellung wird eine wasserhaltige Verbindung eines Metalls eingesetzt, die in einer Lösung abgeschieden werden soll, in der ein schwer schmelzbares Oxid, wie ThO2, Al2O3 oder ZrO2 enthalten ist. Nach einem Trocknen soll mit Wasserstoff reduziert und ein Metallpulver, in dem das schwer schmelzende Oxid enthalten ist, erhalten werden. Daraus können feste Metallkörper hergestellt werden, in denen Bereiche mit schwer schmelzbarem Oxid neben solchen ohne Oxid vorliegen.From the DE 1 288 318 A1 and the US 3,317,285 Methods are known for the production of metal powders which are suitable for further processing into a dispersion-hardened material. There are in the powder, as well as in the material difficult to melt oxides. For the preparation of a water-containing compound of a metal is used, which is to be deposited in a solution in which a refractory oxide such as ThO 2 , Al 2 O 3 or ZrO 2 is included. After drying it should be reduced with hydrogen and a metal powder in which the hard-melting oxide is contained can be obtained. From this, solid metal bodies can be produced in which areas with refractory oxide are present alongside those without oxide.

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, gelöst. Ein so hergestelltes Metallpulver ist mit dem Anspruch 5 definiert.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 5.

Vorteilhafte Ausgestaltungen und Weiterbildungen der Erfindung können mit in untergeordneten Ansprüchen bezeichneten Merkmalen erreicht werden.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 aufbrechen. 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. In this case, the primary particles contained in the agglomerates due to their high sintering activity with each other. 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 soll die spezifische Oberfläche auf einen Wert kleiner 0,5 m2/g, bevorzugt kleiner 0,1 m2/g verkleinert werden.In the second stage of the heat treatment, the specific surface should be reduced to a value of less than 0.5 m 2 / g, preferably less than 0.1 m 2 / g.

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.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°C in der ersten Stufe der Wärmebehandlung eingehalten sein, was sich insbesondere bei einem Fe2O3 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 ° C should be maintained in the first stage of the heat treatment, which has a favorable effect especially for a Fe 2 O 3 powder for the reduction.

Bei der zweiten Stufe soll die Temperatur dann erhöht werden, wobei eine Temperatur von mindestens 650°C eingehalten werden soll. Bevorzugt ist eine Temperatur oberhalb 700°C. 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, with a temperature of at least 650 ° C is to be maintained. A temperature above 700 ° C. is preferred. 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%.

In einer Alternative der Erfindung kann eine Mischung von Fe2O3 und NiO) mit diesem Verfahren reduziert werden und dabei dann ein legiertes bzw. anlegiertes Metallpulver zu erhalten. Bei einem eingesetzten Pulvergemisch soll der Anteil an Eisenoxid bei mindestens 50 Masse-% liegen.In an alternative of the invention, a mixture of Fe 2 O 3 and NiO) can be reduced by this method and thereby to obtain an alloyed metal powder. In the case of a powder mixture used, the proportion of iron oxide should be at least 50% by mass.

Bei beiden Stufen der Wärmebehandlung sollte der Wasserstoffpartialdruck nahezu konstant gehalten werden, sodass 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 water vapor formed should be removed.

Nachfolgend soll die Erfindung beispielhaft näher erläutert werden.The invention will be explained in more detail by way of example in the following.

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 Eisenpulver hat eine dem Carbonyleisenpulver vergleichbare Morphologie und ist um mindestens 50 % kostengünstiger.When 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 morphology comparable to the carbonyl iron powder 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 Wasserstoffatmosphäre bis 500°C bei der ersten Stufe der Wärmebehandlung aufgeheizt und dabei reduziert. Die Haltezeit betrug 1 h. Danach wurde bei der zweiten Stufe der Wärmebehandlung die Temperatur auf 800°C erhöht und eine Haltezeit von 1h 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 (Fe 2 O 3 ) used had a average particle size of 0.3 microns and was in the form of 100 micron large 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 1 h. Thereafter, in the second stage of the heat treatment, the temperature was raised to 800 ° C and maintained for a holding time of 1 hour. 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 Wasserstoffatmosphäre.Cooling to room temperature was also carried out in a hydrogen atmosphere.

Das erhaltene Eisenpulver ist nicht pyrophor. Das Eisenoxidpulver wurde nahezu vollständig zu Eisenpulver reduziert. Der Sauerstoffgehalt lag bei ca. 0,2 %. Die Primärpartikel der ursprünglich 100 µm großen Agglomerate 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 originally 100 .mu.m large agglomerates were sintered to about 60-70 .mu.m spherical particles, the spherical particles formed with each other only partially had small sintered contacts, however, can be broken easily mechanically. In this way, a flowable spherical fine iron powder could be prepared.

Claims (5)

  1. A method for the production of a metal powder, in which powdered Fe2O3 or a powdered metal oxide which is a mixture of at least 50% by weight iron oxide and NiO as second metal oxide is used as starting powder, and in a reducing hydrogen atmosphere in a first stage is subjected to a heat treatment in which the metal oxide is reduced; then the temperature in a second stage of the heat treatment is increased to above 650°C and the temperature is held over a period of at least 900 s and in so doing the specific surface area of the metal powder which has previously been obtained by reduction is reduced to less than 0.5 m2/g.
  2. A method according to Claim 1, characterised in that the first stage of the heat treatment is carried out at a temperature of at least 400°C and at most 600°C.
  3. A method according to one of the preceding claims, characterised in that in the first stage of the heat treatment the temperature is held over a period of at least 900 s.
  4. A method according to one of the preceding claims, characterised in that in the first stage of the heat treatment the temperature is held over a period until the proportion of oxygen in the metal powder is less than 0.5%.
  5. Iron powder, optionally alloyed with nickel at least on the surface, produced with a method according to one of the preceding claims, with an average particle size in the range 5 µm to 100 µm and a specific surface area smaller than 0.5 m2/g.
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)

Application Number Priority Date Filing Date Title
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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EP2242602B1 true EP2242602B1 (en) 2014-03-26
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DE102019207824A1 (en) * 2019-05-28 2020-12-03 Thyssenkrupp Steel Europe Ag Process for the production of iron powder
WO2022101840A1 (en) * 2020-11-13 2022-05-19 Tata Steel Limited An elemental iron powder, methods and products thereof

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Publication number Priority date Publication date Assignee Title
DE1288318B (en) * 1960-06-10 1969-01-30 Fansteel Metallurgical Corp Process for producing a metal powder with finely dispersed, difficult-to-melt oxide particles
US3317285A (en) * 1964-02-18 1967-05-02 Du Pont Composition comprising iron-group metal and particulate refractory metal oxide
US4414021A (en) * 1982-05-06 1983-11-08 Welbon William W Process for the synthesis of iron powder
DE69523036T2 (en) * 1995-05-03 2002-02-07 Osram Sylvania Inc Process for the production of flowable tungsten / copper composite powder
US5912283A (en) * 1995-07-19 1999-06-15 Toyo Aluminium Kabushiki Kaisha Surface-treated color pigment, colored substrate particles and production process thereof
JP3932336B2 (en) * 1999-03-19 2007-06-20 Ｄｏｗａエレクトロニクス株式会社 Method for producing copper powder for conductive paste
US6881240B2 (en) * 2000-09-18 2005-04-19 Dowa Mining Co., Ltd. Copper powder for electrically conductive paste
DE10332033A1 (en) * 2003-07-15 2005-02-03 Chemetall Gmbh Process for the preparation of metal powders or of metal hydride powders of the elements Ti, Zr, Hf, V, Nb, Ta and Cr
SE0303187D0 (en) * 2003-11-26 2003-11-26 Hoeganaes Ab Food additive

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EP2242602B8 (en) 2014-12-31
WO2009097835A1 (en) 2009-08-13
DE102008009133A1 (en) 2009-09-24
DE102008009133B4 (en) 2012-04-12
EP2242602A1 (en) 2010-10-27

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