EP2242602A1 - Procédé de production d'une poudre métallique et poudre métallique produite au moyen dudit procédé - Google Patents

Procédé de production d'une poudre métallique et poudre métallique produite au moyen dudit procédé

Info

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
Authority
EP
European Patent Office
Prior art keywords
metal
heat treatment
stage
temperature
powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP09707741A
Other languages
German (de)
English (en)
Other versions
EP2242602B8 (fr
EP2242602B1 (fr
Inventor
Bernd Kieback
Gunnar Walther
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
Original Assignee
Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV filed Critical Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
Publication of EP2242602A1 publication Critical patent/EP2242602A1/fr
Application granted granted Critical
Publication of EP2242602B1 publication Critical patent/EP2242602B1/fr
Publication of EP2242602B8 publication Critical patent/EP2242602B8/fr
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

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.

Landscapes

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

Abstract

L'invention concerne un procédé de production de poudres métalliques et des poudres métalliques ainsi produites. L'objectif de l'invention est de permettre de produire des poudres métalliques de manière économique à partir d'oxydes métalliques dont les propriétés permettent une utilisation variée. Selon le procédé de l'invention, un oxyde métallique pulvérulent est placé sous atmosphère d'hydrogène réductrice lors d'une première étape d'un traitement thermique, étape au cours de laquelle l'oxyde métallique est réduit. Ensuite, la température est augmentée au cours d'une seconde étape du traitement thermique et cette température est maintenue pendant un certain laps de temps. Ainsi, la surface spécifique de la poudre métallique obtenue au préalable par réduction peut être réduite.
EP09707741.6A 2008-02-06 2009-01-28 Procédé de production d'une poudre métallique et poudre métallique produite au moyen dudit procédé Active EP2242602B8 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102008009133A DE102008009133B4 (de) 2008-02-06 2008-02-06 Verfahren zur Herstellung von Metallpulvern und so hergestelltes Metallpulver
PCT/DE2009/000136 WO2009097835A1 (fr) 2008-02-06 2009-01-28 Procédé de production d'une poudre métallique et poudre métallique produite au moyen dudit procédé

Publications (3)

Publication Number Publication Date
EP2242602A1 true EP2242602A1 (fr) 2010-10-27
EP2242602B1 EP2242602B1 (fr) 2014-03-26
EP2242602B8 EP2242602B8 (fr) 2014-12-31

Family

ID=40786776

Family Applications (1)

Application Number Title Priority Date Filing Date
EP09707741.6A Active EP2242602B8 (fr) 2008-02-06 2009-01-28 Procédé de production d'une poudre métallique et poudre métallique produite au moyen dudit procédé

Country Status (3)

Country Link
EP (1) EP2242602B8 (fr)
DE (1) DE102008009133B4 (fr)
WO (1) WO2009097835A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020239536A1 (fr) * 2019-05-28 2020-12-03 Thyssenkrupp Steel Europe Ag Procédé de production de poudre de fer

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA3120229C (fr) * 2018-11-23 2023-10-03 Tata Steel Limited Procede de production de poudre de fer spherique et produits associes
EP4038209A1 (fr) * 2019-10-03 2022-08-10 Umicore Procédé de préparation de poudres pré-alliées pour outils diamantés, et poudres ainsi obtenues
WO2022101840A1 (fr) * 2020-11-13 2022-05-19 Tata Steel Limited Poudre de fer élémentaire, procédés et produits associés

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1288318B (de) * 1960-06-10 1969-01-30 Fansteel Metallurgical Corp Verfahren zur Herstellung eines Metallpulvers mit feindispersen, schwer schmelzbarenOxydteilchen
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 (de) * 1995-05-03 2002-02-07 Osram Sylvania Inc., Danvers Verfahren zur Herstellung fliessfähigen Wolfram/Kupfer Verbündpulver
US5912283A (en) * 1995-07-19 1999-06-15 Toyo Aluminium Kabushiki Kaisha Surface-treated color pigment, colored substrate particles and production process thereof
JP3932336B2 (ja) * 1999-03-19 2007-06-20 Ｄｏｗａエレクトロニクス株式会社 導電ペースト用銅粉の製造方法
US6881240B2 (en) * 2000-09-18 2005-04-19 Dowa Mining Co., Ltd. Copper powder for electrically conductive paste
DE10332033A1 (de) * 2003-07-15 2005-02-03 Chemetall Gmbh Verfahren zur Herstellung von Metallpulvern, bzw. von Metallhydridpulvern der Elemente Ti, Zr, Hf, V, Nb, Ta und Cr
SE0303187D0 (sv) * 2003-11-26 2003-11-26 Hoeganaes Ab Food additive

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2009097835A1 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020239536A1 (fr) * 2019-05-28 2020-12-03 Thyssenkrupp Steel Europe Ag Procédé de production de poudre de fer

Also Published As

Publication number Publication date
DE102008009133B4 (de) 2012-04-12
EP2242602B8 (fr) 2014-12-31
EP2242602B1 (fr) 2014-03-26
DE102008009133A1 (de) 2009-09-24
WO2009097835A1 (fr) 2009-08-13

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