EP2242602B1 - 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 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
Authority
EP
European Patent Office
Prior art keywords
stage
heat treatment
powder
temperature
metal 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.)
Active
Application number
EP09707741.6A
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German (de)
English (en)
Other versions
EP2242602B8 (fr
EP2242602A1 (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
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Publication of EP2242602A1 publication Critical patent/EP2242602A1/fr
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Publication of EP2242602B1 publication Critical patent/EP2242602B1/fr
Publication of EP2242602B8 publication Critical patent/EP2242602B8/fr
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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.

Landscapes

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

Claims (5)

  1. Procédé de fabrication d'une poudre métallique, dans lequel on utilise en tant que poudre de départ du Fe2O2 sous forme de poudre ou un oxyde métallique sous forme de poudre, qui est un mélange d'au moins 50 % en masse d'oxyde de fer et de NiO en tant que deuxième oxyde métallique, et, dans une atmosphère d'hydrogène réductrice, est soumis lors d'une première étape à un traitement thermique, au cours duquel l'oxyde métallique est réduit ; puis la température, dans une deuxième étape du traitement thermique, est élevée à une valeur supérieure à 650°C et est maintenue à cette température durant un laps de temps d'au moins 900 s, la surface spécifique de la poudre métallique obtenue préalablement par réduction étant à cette occasion abaissée à une valeur inférieure à 0,5 m2/g.
  2. Procédé selon la revendication 1, caractérisé en ce que la première étape du traitement thermique est mise en oeuvre à une température d'au moins 400°C et d'au plus 600°C.
  3. Procédé selon l'une des revendications précédentes, caractérisé en ce que, dans la première étape du traitement thermique, la température est maintenue durant un laps de temps d'au moins 900 s.
  4. Procédé selon l'une des revendications précédentes, caractérisé en ce que, dans la première étape du traitement thermique, la température est maintenue durant une période de temps allant jusqu'à ce que la proportion de l'oxygène dans la poudre métallique soit inférieure à 0,5 %.
  5. Poudre de fer, en option alliée à du nickel au moins en surface, fabriquée par un procédé selon l'une des revendications précédentes, ayant une taille moyenne de particule comprise dans la plage de 5 à 100 µm et une surface spécifique inférieure à 0,5 m2/g.
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 EP2242602A1 (fr) 2010-10-27
EP2242602B1 true 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)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3883713B1 (fr) * 2018-11-23 2024-07-03 Tata Steel Limited Procédé de production de poudre de fer sphérique
DE102019207824A1 (de) * 2019-05-28 2020-12-03 Thyssenkrupp Steel Europe Ag Verfahren zur Herstellung von Eisenpulver
KR20220078640A (ko) * 2019-10-03 2022-06-10 유미코아 다이아몬드 공구용 예비 합금 분말의 제조 방법, 및 이로 수득된 분말
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
ATE206480T1 (de) * 1995-05-03 2001-10-15 Osram Sylvania Inc 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

Also Published As

Publication number Publication date
EP2242602B8 (fr) 2014-12-31
WO2009097835A1 (fr) 2009-08-13
DE102008009133B4 (de) 2012-04-12
DE102008009133A1 (de) 2009-09-24
EP2242602A1 (fr) 2010-10-27

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