EP2061615A1 - Procédé de préparation de poudres composites et poudres composites correspondantes - Google Patents

Procédé de préparation de poudres composites et poudres composites correspondantes

Info

Publication number
EP2061615A1
EP2061615A1 EP07784634A EP07784634A EP2061615A1 EP 2061615 A1 EP2061615 A1 EP 2061615A1 EP 07784634 A EP07784634 A EP 07784634A EP 07784634 A EP07784634 A EP 07784634A EP 2061615 A1 EP2061615 A1 EP 2061615A1
Authority
EP
European Patent Office
Prior art keywords
composite powder
metals
starting material
compounds
particles
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.)
Withdrawn
Application number
EP07784634A
Other languages
German (de)
English (en)
Inventor
Andreas Bock
Annegret Bicherl
Andreas Schön
Burghard Zeiler
Wolf-Dieter Schubert
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.)
Wolfram Bergbau und Huetten AG
Original Assignee
Wolfram Bergbau-Und Huetten-Gmbh Nfgkg
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 Wolfram Bergbau-Und Huetten-Gmbh Nfgkg filed Critical Wolfram Bergbau-Und Huetten-Gmbh Nfgkg
Publication of EP2061615A1 publication Critical patent/EP2061615A1/fr
Withdrawn legal-status Critical Current

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
    • B22F1/17—Metallic particles coated with metal
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61N—ELECTROTHERAPY; MAGNETOTHERAPY; RADIATION THERAPY; ULTRASOUND THERAPY
    • A61N1/00—Electrotherapy; Circuits therefor
    • A61N1/18—Applying electric currents by contact electrodes
    • A61N1/32—Applying electric currents by contact electrodes alternating or intermittent currents
    • A61N1/36—Applying electric currents by contact electrodes alternating or intermittent currents for stimulation
    • A61N1/372—Arrangements in connection with the implantation of stimulators
    • A61N1/375—Constructional arrangements, e.g. casings
    • A61N1/37512—Pacemakers
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • 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 method according to the preamble of claim 1 and a composite powder produced by this method according to the preamble of claim 15.
  • the invention relates to a method according to the preamble of claim 23 and to a composite powder produced by this method according to the preamble of claim 18.
  • An essential object of the invention is the production of a composite powder in a simple and rapid manner in which the yield of composite powder is as large as possible.
  • the composite powder obtained by the process according to the invention is intended for further
  • the composite powder produced by these process steps according to the invention is characterized in particular by the features of claim 15. It turns out that these powders are good sinterable or can be converted well into hard materials.
  • the composite powders comprise metallic cores or core particles which are overgrown throughout, but at least at least 50%, with a cladding layer of tungsten and / or molybdenum or a compound of these metals, in stoichiometric form or in the form of a metallic phase.
  • a method according to the preamble of claim 22 is inventively characterized by the features cited in the characterizing part of claim 22.
  • the composite powder used to carry out this process is nitrided and / or carburized in a particularly good, rapid and homogeneous manner and gives very good material parameters.
  • the reaction with the corresponding elements carbon and / or nitrogen is advantageously carried out according to the features indicated in claims 23 to 26.
  • Carbides require an optimal distribution of the binder and the
  • Hard material phase in particular by the trend towards ever finer carbides. Likewise, a uniform carbide is required in terms of grain size for good mechanical properties. In conventional hard metal production, the hard material phase (e.g.
  • W-Co composite powders are made by single-stage reduction of the oxide composite powder
  • Phases Co 3 W and Co 7 W 6 are detected. As part of technical
  • W (s) are also shown on the basis of cobalt, among others.
  • the carburization of W-Co mixtures or composite powder offers the advantage of a low carburizing temperature, since cobalt catalyzes the carburization.
  • the 5 carburizing of nanocrystalline W-Co powders occurs already below 900 0 C.
  • the present invention relies predominantly on the fact that the present invention
  • volume ratios of the starting materials is controlled.
  • the composite powders obtained with the invention thus contain a core of 5 Fe and / or Co and / or Ni and / or their alloys, which is at least partially coated with a cladding layer of carbides and / or nitrides of the metals W and / or Mo and / or
  • the intermediate composite powder which is also self-contained for certain uses, e.g. For sintering purposes, comprises particles 0 with a cladding layer of tungsten and / or molybdenum and / or their compounds which at least partially surround a core of iron and / or cobalt and / or nickel and / or their alloys and / or their compounds ,
  • Kerns cobalt is, as by a coating of molybdenum and / or tungsten and / or 5 molybdenum and / or tungsten carbide, the internal oxygen-sensitive metal before
  • Sheath layer by varying the proportions, the particle size and the
  • the hard metal made of the hard metal composite powder has a uniform structure, an optimal distribution of the elements used, no local
  • Another advantage is the good dispersibility of iron and / or cobalt 35. and / or nickel and thus a uniform distribution of elements.
  • the starting material A comprises
  • Oxidic compounds of tungsten and / or molybdenum and / or other compounds and / or alloys of these metals in particular
  • MoO 3 MOO 2 .9 2 , Mo 13 O 38 , Mo 4 Oi 1 or other Mo oxides, H 2 MoO 4 (MoO 3 H 2 O), (NH 4 ) 2 MoO 4 , ammonium dimolybdate ADM ((NH 4 J 2 '2MoO 3 ), (NH 4 ) 2 O • 6MoO 3 ,
  • the starting material B comprises:
  • Co and / or Fe and / or Ni and / or alloys and / or compounds of these metals in particular CoO, Co 3 O 4 , Co 2 O 3 , CoO 2 , Co-hydroxides, Co (OH) 2 , CoOOH, CoWO 4, Co7W6, Co 3 W
  • FeW, Fe 2 W, Fe 3 W 2 , Fe 7 W 6 , NiW, NiW 2 , Ni 4 W, oxides, hydroxides and / or tungstates of Co and / or Fe and / or Ni and / or salts, in particular acetates or Oxalates, of Co and / or Fe and / or Ni, and / or Metal Tungsten Oxi ⁇ brons (Metal Fe, Co, Ni)
  • the starting material A After mixing the starting material A with the starting material B in the predetermined ratio, e.g. by mixing in a tumble mixer and / or wet or dry grinding, e.g. in a ball mill, an attritor, one
  • Planetary ball mill and / or dispersing and / or spraying takes place after any required drying the reduction process.
  • the starting materials A and B dry or wet over a period of 1 to 300 h, preferably 1 to 50 h, in particular homogeneously, are mixed.
  • the reduction process takes place in a hydrogen atmosphere, it being advantageously possible for the duration of the reduction process to be set to 10 minutes to 10 hours.
  • the reduction process is carried out at a temperature of 200 to 1200 0 C.
  • the particle size of the starting material A is 50 nm to 200 ⁇ m, preferably 80 nm to 50 ⁇ m, and the particle size of the starting material B is 10 nm to 50 ⁇ m, preferably 30 nm to 5 ⁇ m.
  • non-pure metals or compounds or alloys of the two starting materials A and B It is also possible to dope the metals of the starting materials or of the compounds used.
  • the metals present in the starting material A, W and / or Mo and / or alloys and / or compounds, in particular metal oxides, of these metals with Cr and / or V and / or Mo and / or Ta and / or Nb in one Extent of 50 ppm to 2 wt .-% of (r) used in the starting material A metal (s) s are doped or if provided in the starting material B metals Co, Fe and / or Ni and / or alloys and / or compounds of these Metals are doped with Cr and / or V and / or Mo and / or Ta and / or Nb in an amount of 50 ppm to 20 wt .-% of (r) used in the starting material B metals (s).
  • the starting materials used can be present in various forms; It is advantageous if the doped metals or the doped metal compounds in the form of pure metals oxides, nitrates, acetates, formates, oxalates, liquid salt solutions and / or solid powders or solid salts, in particular in the form of tungstates or molybdenum, tungsten oxide bronzes and / or molybdenum oxide bronzes, are present!
  • the reduction process can be carried out in different ways.
  • the dumping height of the mixed starting materials present in powder form must be selected as a function of the raw materials and their pouring properties (in particular bulk density, porosity).
  • agglomerates are present in the starting powder of the core particles, ie the starting material B, a completely optimal dispersion of the core component at the crystallite level will no longer be present, nevertheless the agglomerate regions as such are overgrown by tungsten or molybdenum.
  • Transport process are ⁇ 50% of tungsten or molybdenum overgrown.
  • the resulting Co-W composite powders have a particle size in the range of 50 nm -
  • Cobalt acts as a nucleation aid for tungsten metal (or Mo) and causes a redistribution of the tungsten (Mo) with well-distributed Co (Fe, Ni) and thus leads to a very uniform composite powder.
  • Mo tungsten metal
  • Mo well-distributed Co
  • Composite powder corresponds to the macroscopic morphology of the powder of the core component used.
  • Fig. 1 the addition of the starting material B is shown as a cladding layer on the core particle.
  • a particle of the composite powder which is shown in Fig. 1 right.
  • Co 7 W 6 designated 3 WO 2 (OH) 2 and 4 W.
  • Fig. 2 is a mathematical model concerning the structure of the
  • V 2
  • Quantitative ratio of the layer thickness of the shell and the particle size of the composite powder particle can be estimated:
  • R1 mean radius of the particles of the composite powder V A volume of the metals of the starting material A
  • R 2 mean radius of the particles of the starting material B or the Kemteilchen are.
  • Grain size of the starting material B control the grain size of the resulting composite powder, since the thickness of the cladding layer of the resulting composite powder corresponds to the difference of the radii Ri - R 2 .
  • FIG. 3 shows a schematic of the metal composite powders denoted by 4W, 5Co 7W 6 and 6Co.
  • the occurring Co-W or Co-WC composite powder particles are shown schematically.
  • W Co
  • the distribution of the W and Co phases holistic (a) and partially overgrown structures are possible (c).
  • a 2-layer structure can be formed
  • Co-metal core consists of a cladding of intermetallic phase surrounded by tungsten (b).
  • the cobalt powder for the overgrowth is shown in Figure 4 (Umicor ultrafine 0.9 ⁇ m).
  • the mean SEM grain size of the spherical powder is intermediate
  • Figure 4 shows SEM images of Umicor cobalt powder for overgrowth (left) and Co-W composite powder (right).
  • Figure 5 shows SEM images of the co-powder used (left) and the Co-W powder (right); the picture shows the distribution and macroscopic morphology of the powder.
  • Figure 6 shows an X-ray diffractogram of the Co-W powder.
  • Figures 7 and 8 show light micrographs of the Co-W
  • Figure 7 is a photomicrograph of Cu-W Co-W composite powder: etched raised phases (dark) - Co 7 W 6
  • Figure 8 Photomicrograph of Co-W composite powder in Cu
  • Figure 9 SEM images of the Co-W powder in copper ground (Co 7 W 6 -W)
  • Figure 10 SEM images of the Co-W powder in copper ground (Co 7 W 6 -W)
  • the SEM images according to Figure 9 to 10 with the back-scattered detector show the Co-W composite powder in Cu-cut.
  • the areas of the intermetallic phase Co 7 W 6 and light tungsten (black copper (embedding agent)) appear dark.
  • the resulting composite powders generally exhibit a thickness of the cladding layer of 8 nm to 15 ⁇ m.
  • the results of X-ray diffractometry show tungsten in bcc-form and Co 7 W 6 and Co in fcc-form.
  • the oxygen content of the composite powder is ⁇ 5000 ppm.
  • the particle size of the composite powder is about 50 nm to 50 microns determined by scanning electron microscopy.
  • a composite powder is produced which has core particles coated with a cladding layer of a certain thickness and the metals of the starting material A, which are now carburized and / or nitrated, of the metals of the starting material B separated by a phase boundary. Formed phases between cobalt and tungsten are redissolved during nitriding or carburizing.
  • the starting materials or compounds used should have a high degree of purity or impurities should be present in a degree usual in the field of hard metals.
  • the resulting composite powder with carbon preferably in the form of carbon black and / or graphite
  • the resulting composite powder with carbon is mixed and / or in an atmosphere of H 2 and N 2 and / or H 2 / CH 4 and / or CO and / and or CO 2 is heated to a temperature of 800 to 1500 0 C, so that the metals in the cladding layer are converted into the corresponding compounds with carbon and / or nitrogen, in particular nitrides and / or carbides, preferably in tungsten monocarbide.
  • the mixing of the already existing composite powder with carbon black or graphite can be carried out in conventional mixing or milling units, such as e.g. Tumble mixers, ball mills, planetary ball mills, attritors or dispersers.
  • the carburization and / or nitration is carried out at a, in particular constant, temperature for 10 minutes to 50 hours, optionally with a heating rate and / or a cooling rate of 1 to 500 K. / min is set.
  • the atmosphere for the reaction is chosen according to the desired compound; accordingly, the temperatures are set.
  • the composite powder obtained in the course of the reaction comprises cores or core particles of Co and / or Fe and / or Ni, which are overgrown with a cladding layer of W and / or Mo, which are carburized and / or nitrated.
  • Figure 11 illustrates schematically a Co-WC composite powder consisting of a Co core (a cobalt alloy) and a WC jacket, showing a Co-WC composite powder, designated 6 cobalt and 7 tungsten carbide.
  • Figure 12 shows the X-ray diffractogram of the Co-WC composite powder with the occurring phases WC and Co (fcc).
  • Figure 14 clearly shows the co-WC composite powder with a core-shell structure (inside cobalt outside WC).
  • the composite powders obtained by the reaction show that at least 50% of the particles are completely overgrown with the cladding layer containing carbides and / or nitrides. Further, in the composite powder Co in face-centered cubic form and the WC contained in the sheath layer are in hexagonal form.
  • the composite powder has a particle size of 50 nm to 50 microns, wherein the thickness of the cladding layer is 8 nm to 50 microns.
  • At least one of the metals used contains Cr and / or V and / or Mo and / or Ta and / or Nb in an amount of from 50 ppm to 20% by weight. doped of the doped metal.
  • WO 2 (0.5-2 ⁇ m) is intimately mixed with Co metal powder (0.5-1 ⁇ m) in a ratio W: Co of 90:10 by means of a tumble mixer for 40-60 minutes. This mixture is then reduced with hydrogen at a temperature profile of 700-950 0 C.
  • the result is a Co-W composite powder in which Co is present predominantly as an intermetallic phase (Co 7 W 6 ) and is ⁇ 80% of tungsten overgrown, the particle size is in the range of 1-2 microns with a W-layer thickness of 0, 2-0,4 ⁇ m.
  • a Co-WC composite powder is formed, wherein the cobalt is surrounded to> 80% by tungsten carbide, the composite powder Co-WC has an average particle size of 1-2 ⁇ m, whereby the WC layer has a thickness of 0.3 ⁇ m. 0.5 ⁇ m.
  • the co-WC composite powder was then treated in cyclohexane for 2 hours or 24 hours with the addition of pressing aid (paraffin) in the ball mill.
  • the milling medium was then separated on a rotary evaporator, the powder with the aid of a metal sieve (200 .mu.m) granulated and pressed with 200MPa in a laboratory press (25OkN) to rectangular rods.
  • the sintering was carried out under vacuum at 1400 0 C for a period of 60 min.
  • Figure 15 shows SEM images of the WC / 9.4Co hard metal alloy from WC-Co composite powder.
  • Example 2
  • WO 2 (0.5-2 ⁇ m) is intimately mixed with Ni metal powder (2-5 ⁇ m, small proportion 5-8 ⁇ m) in a ratio W: Ni of 80:20 by means of a tumble mixer for 60 minutes. This mixture is then reduced with hydrogen at temperatures of 700-950 0 C.
  • the result is a Ni-W composite powder, in which Ni is predominantly present as an intermetallic phase and is ⁇ 80% of tungsten overgrown, the particle size is in the range of 5-7 microns with a W-layer thickness of about 0.8 microns.
  • Figure 16 shows an SEM absorption of the Ni-W composite powder (80W-20Ni).

Landscapes

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

Abstract

La présente invention concerne un procédé destiné à la préparation d'une poudre composite. Le procédé consiste à mélanger une substance de départ poudreuse A qui comprend au moins du tungstène et/ou du molybdène et/ou des alliages et/ou des composés de ces métaux, avec une substance de départ poudreuse B qui comprend au moins Co et/ou Fe et/ou Ni et/ou des alliages et/ou des composés de ces métaux; à régler un rapport élémentaire du tungstène et/ou du molybdène par rapport à Co et/ou Ni et/ou Fe dans le mélange pour qu'il soit de l'ordre de 99 : 1 (A:B) à 50 :50 (A:B) % en poids; et à soumettre le mélange poudreux à un processus de réduction pendant le déroulement duquel le Co, Fe et/ou Ni utilisés sont recouverts d'une couche de W et/ou Mo. Les poudres composites ainsi obtenues peuvent subir une carburation, nitration ou carbonitration partielle au cours d'une opération de traitement ultérieure.
EP07784634A 2006-09-15 2007-08-24 Procédé de préparation de poudres composites et poudres composites correspondantes Withdrawn EP2061615A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AT0154906A AT504319B1 (de) 2006-09-15 2006-09-15 Verfahren zur herstellung von kompositpulvern sowie kompositpulver
PCT/AT2007/000408 WO2008031122A1 (fr) 2006-09-15 2007-08-24 Procédé de préparation de poudres composites et poudres composites correspondantes

Publications (1)

Publication Number Publication Date
EP2061615A1 true EP2061615A1 (fr) 2009-05-27

Family

ID=38664766

Family Applications (1)

Application Number Title Priority Date Filing Date
EP07784634A Withdrawn EP2061615A1 (fr) 2006-09-15 2007-08-24 Procédé de préparation de poudres composites et poudres composites correspondantes

Country Status (4)

Country Link
EP (1) EP2061615A1 (fr)
JP (1) JP2010503765A (fr)
AT (1) AT504319B1 (fr)
WO (1) WO2008031122A1 (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109136602B (zh) * 2017-06-16 2020-10-30 荆门市格林美新材料有限公司 一种铬掺杂硬质合金的制备方法
WO2019107816A1 (fr) * 2017-11-29 2019-06-06 엔에이티엠 주식회사 Procédé de fabrication d'un alliage tungstène-molybdène
EP3527306A1 (fr) 2018-02-14 2019-08-21 H.C. Starck Tungsten GmbH Particules de matériau dur revêtues contenant de la poudre
CN111069618B (zh) * 2020-01-02 2022-10-25 崇义章源钨业股份有限公司 WC-Co复合粉末及其制备方法和应用
CN115572877B (zh) * 2022-10-08 2023-06-09 郑州大学 一种钼铌或钼钽合金的制备方法
CN115533112B (zh) * 2022-10-17 2023-10-20 北京工业大学 一种复合稀土钨/钼酸盐共晶细化难熔金属的方法

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US3223523A (en) * 1963-07-05 1965-12-14 C K Williams & Co Inc Methods for improving pressed properties and characteristics of sintered powder metal compacts
JPS57152438A (en) * 1981-03-16 1982-09-20 Hitachi Cable Ltd Thermal expansion regulating material
CA1337468C (fr) * 1987-08-01 1995-10-31 Kuniaki Ogura Acier allie pour utilisation en metallurgie des poudres
JPH0356609A (ja) * 1989-07-21 1991-03-12 Awamura Kinzoku Kogyo Kk モリブデン被覆複合粉末の製造法
US5372845A (en) * 1992-03-06 1994-12-13 Sulzer Plasma Technik, Inc. Method for preparing binder-free clad powders
US20070141374A1 (en) * 2005-12-19 2007-06-21 General Electric Company Environmentally resistant disk

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Title
See references of WO2008031122A1 *

Also Published As

Publication number Publication date
AT504319B1 (de) 2010-03-15
AT504319A1 (de) 2008-04-15
WO2008031122A1 (fr) 2008-03-20
JP2010503765A (ja) 2010-02-04

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