WO2008031121A1 - Procédé de préparation de poudres composites w-mo et poudres composites correspondantes - Google Patents

Procédé de préparation de poudres composites w-mo et poudres composites correspondantes Download PDF

Info

Publication number
WO2008031121A1
WO2008031121A1 PCT/AT2007/000407 AT2007000407W WO2008031121A1 WO 2008031121 A1 WO2008031121 A1 WO 2008031121A1 AT 2007000407 W AT2007000407 W AT 2007000407W WO 2008031121 A1 WO2008031121 A1 WO 2008031121A1
Authority
WO
WIPO (PCT)
Prior art keywords
composite powder
starting material
metal
particles
alloy
Prior art date
Application number
PCT/AT2007/000407
Other languages
German (de)
English (en)
Inventor
Andreas Bock
Annegret Bicherl
Andreas Schön
Burghard Zeiler
Wolf-Dieter Schubert
Original Assignee
Wolfram Bergbau- Und Hütten-Gmbh Nfg. Kg
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 Hütten-Gmbh Nfg. Kg filed Critical Wolfram Bergbau- Und Hütten-Gmbh Nfg. Kg
Priority to EP07784633A priority Critical patent/EP2061614A1/fr
Priority to JP2009527644A priority patent/JP2010503764A/ja
Publication of WO2008031121A1 publication Critical patent/WO2008031121A1/fr

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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/6265—Thermal treatment of powders or mixtures thereof other than sintering involving reduction or oxidation
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
    • C04B35/62802—Powder coating materials
    • C04B35/62828—Non-oxide ceramics
    • C04B35/62831—Carbides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
    • C04B35/62897—Coatings characterised by their thickness
    • 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3239—Vanadium oxides, vanadates or oxide forming salts thereof, e.g. magnesium vanadate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3241—Chromium oxides, chromates, or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3256—Molybdenum oxides, molybdates or oxide forming salts thereof, e.g. cadmium molybdate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3258—Tungsten oxides, tungstates, or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
    • C04B2235/3839—Refractory metal carbides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
    • C04B2235/3839—Refractory metal carbides
    • C04B2235/3847—Tungsten carbides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/404—Refractory metals
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron

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 11.
  • the invention relates to a method according to the preamble of claim 18 and to a composite powder produced by this method according to the preamble of claim 24.
  • 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 powders obtained by the process according to the invention are intended for further processing
  • the composite powder produced by these process steps according to the invention is characterized in particular by the features of claim 11. 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 over 50%, by a cladding layer of tungsten or molybdenum.
  • a method according to the preamble of claim 18 is inventively characterized by the features cited in the characterizing part of claim 18.
  • the composite powder used to carry out this process can be nitrided and / or carburized in a particularly good, rapid and homogeneous manner, and produces exceptionally good material parameters.
  • the present invention is based primarily on the fact that the dispersibility and thus uniformity of the distribution of tungsten or molybdenum, especially by the precursors and pre-distribution and the proportions of the starting materials can be controlled.
  • the composite powders obtained with the invention thus contain a core of W or Mo or a W-Mo alloy which is at least partially coated with a sheath layer of Mo or W or a sheath layer of Mo or W containing carbides and / or nitrides of the metals Mo and / or W is surrounded.
  • the core can also be carburized and / or nitrided.
  • the intermediate composite powder which is also self-contained for certain uses, e.g. For sintering purposes, comprises particles with a cladding layer of tungsten or molybdenum, which surround a core of Mo or W or a Mo-W alloy at least partially, advantageously entirely.
  • a composite powder which comprises core particles of W or Mo or of a Mo-W alloy and a cladding layer of W or Mo, wherein in a further embodiment the cladding layer and optionally also the respective core particles in the form of carbides and / or Nitrides may be present or contain.
  • Starting material B in the predetermined ratio for example by mixing in a tumble mixer and / or wet or dry grinding, for example in a ball mill, an attritor, a planetary ball mill and / or dispersing and / or spraying is carried out 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 100 hours.
  • the reduction process is carried out at a temperature of 400 to 1200 0 C. It is envisaged that the particle size of the starting material A and B 0.1 to
  • the metals of the starting materials or the compounds used it is also possible to dope the metals of the starting materials or the compounds used. It is advantageous if the metals or metal alloys present in the starting material A or B 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 ) in the starting material A or in the starting material B provided metal (e) to dope. It is understood that in the case that a starting material contains Mo, doping with Mo is eliminated.
  • the reduction process can be carried out in different ways.
  • one-stage or two-stage reduction operations are feasible.
  • the features of claims 7 and 8 are advantageous.
  • a heating rate and / or a cooling rate between 1 and 500 K / min is set.
  • the bed height of the mixed starting materials present in powder form is selected as a function of the raw materials and their pouring properties (in particular bulk density, porosity). The process of overgrowth of Mo works over the
  • the mathematical model assumes that the powder particles are spherical and ideally uniform and complete as core-shell structures. Likewise, the calculation is based on Mo metal.
  • V 1 (- ⁇ Ri -- ⁇ R 3 2 ) (shell volume V1)
  • V 2 - ⁇ R j (core volume V2)
  • Composite powder is: 0.6 ⁇ X ⁇ R ⁇ 1, 2 X, where
  • R1 mean radius of the particles of the composite powder
  • V 6 volume of the metal of the starting material B (sheath) R2 mean radius of the particles of the starting material A or of the core particles.
  • FIG. 3 shows a schematic representation of the metal composite powders, where 1 W or Mo and 2 Mo or W are used.
  • the occurring Mo-W or W-Mo composite powder particles are shown schematically.
  • W: Mo used and the distribution of the W and Mo phases
  • holistic (a) and partially (b) overgrown structures are possible.
  • (c) and (d) possible overgrowths of non-spherical particles and agglomerates are illustrated.
  • FIGS. 4 and 5 show the X-ray diffractograms of W-Mo (FIG. 4) and Mo-W (FIG. 5) with phases W (bcc) and Mo (bcc).
  • Fig. 6 shows SEM images of Mo-W powder; on the right is an EDS spectrum of the composite powder, on the left is a tungsten crystal with a not completely overgrown molybdenum core to see. On the right side, the corresponding spectrum of the EDS analysis is shown. Based on this SEM image, it can be seen that tungsten epitaxially grows on molybdenum, which is possible due to the very similar lattice parameters (both cubic-centered).
  • Fig. 7 shows electron micrographs of Mo-W; left: Mo-W
  • Fig. 8 shows SEM images of Mo-W composite powder (etched).
  • the copper-ground sections of the MoW powders of FIGS. 7 and 8 clearly show the core-shell structure.
  • the layer thickness of tungsten around the molybdenum appears to be largely uniform.
  • the reverse overgrowth of tungsten with molybdenum shows comparable results ( Figure 9) with a clear core-shell structure.
  • Fig. 9 shows pictures of the W-Mo composite powder, above: REM and below: light microscope.
  • the resulting composite powders generally exhibit a thickness of the cladding layer of 12 nm to 15 ⁇ m, which depends on the ratio of the starting materials and the size of the starting particles.
  • the results of X-ray diffractometry show tungsten and Mo in bcc form.
  • the oxygen content of the composite powder is ⁇ 5000 ppm.
  • the sectioncheng rosse of the composite powder is about 50 nm to 50 microns determined by scanning electron microscopy. It should also be noted that the starting materials or
  • the resulting composite powder with carbon preferably in the form of carbon black and / or graphite, 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 2200 0 C, so that the metals in the cladding layer and0 optionally also in the core particles in the corresponding compounds with carbon and / or nitrogen, in particular nitrides and / or carbides are reacted , Preferably in tungsten mono- and / or Molybdändicarbid, and / or proceed appropriate storage reactions.
  • the mixing of the already existing composite powder with carbon black or graphite 5 can be carried out in conventional mixing or milling units, such as, for example, 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, 0 optionally a heating rate and / or a cooling rate of 2 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 W or Mo or a Mo-W alloy which are overgrown with a cladding layer of 5 Mo or W, the core layer and optionally the cladding layer being carburized and / or nitrided available.
  • the core particles can thus also contain C and / or N inclusions or carbides and / or nitrides.
  • FIG. 10 schematically illustrates a Mo 2 C-WC / WC-Mo 2 C 30 composite powder, consisting of a Mo 2 C or WC core and a WC or Mo 2 C shell, with 3 Mo 2 C or WC and 4 WC or Mo 2 C is designated.
  • Figure 11 shows the X-ray diffractogram of the Mo 2 C-WC composite powder with the occurring phases WC and Mo 2 C.
  • Fig. 12 shows SEM images of a composite powder with 90WC / 1 OMo 2 C (under 35th Cu cut, etched).
  • the composite powders of the invention obtained by the reaction show that at least 50% of the particles are wholly in contact with the carbides and / or nitrides overgrown coat layer are overgrown.
  • the composite powder has a particle size of 50 nm to 15 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 Mo and / or Nb in an amount of from 50 ppm to 2 Wt .-% of each doped metal is doped.
  • Example 1 WO 2 (0.5-2 ⁇ m) is intimately mixed with Mo metal powder (3-4 ⁇ m) in a ratio W: Mo of 90:10 (w%) by means of a tumble mixer for 40-60 minutes. This mixture is then reduced with hydrogen at temperatures of 800-950 0 C. The result is a Mo-W composite powder with a clear core-shell structure in which the molybdenum particles is overgrown by> 90% of tungsten. The particle size is in the range of 5 - 7 microns with a W-layer thickness of 1 - 2 microns.
  • a Mo 2 C-WC composite powder is formed, wherein the molybdenum carbide is> 90% surrounded by tungsten monocarbide and has a distinct core-shell structure.
  • MoO 2 (0.5-2 ⁇ m) is intimately mixed with W metal powder (2-4 ⁇ m) in a ratio Mo: W 1: 1 (w%) by means of a tumble mixer for 40-60 minutes. This mixture is then reduced with hydrogen at temperatures of 900 - 1000 0 C. The result is a W-Mo composite powder with a clear core-shell structure in which the tungsten particles are over> 90% of molybdenum overgrown.
  • the particle size is in the range of 3 - 5 microns with a Mo layer thickness of about 0, 5 microns.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

La présente invention concerne un procédé destiné à la préparation d'une poudre composite contenant Mo et W. Le procédé consiste à : mélanger une substance de départ poudreuse A comprenant de la poudre métallique de Mo ou de W avec une substance de départ poudreuse B qui, dans le cas où la substance de départ A se présente sous la forme de Mo ou d'un alliage Mo-W, comprend des composés oxydiques de W, ou avec une substance de départ poudreuse B qui, dans le cas où la substance de départ A se présente sous la forme de W, comprend des composés oxydiques de Mo; régler le rapport pondéral (V) de Mo par rapport à W dans le mélange pour qu'il soit de l'ordre de 1:99 à 99:1; et soumettre le mélange poudreux à un processus de réduction en au moins une étape, pendant le déroulement duquel les particules du métal ou de l'alliage de métaux contenu dans la substance de départ A se trouvent recouvertes au moins partiellement, de préférence en totalité, par une couche du métal de la substance de départ B utilisée.
PCT/AT2007/000407 2006-09-15 2007-08-24 Procédé de préparation de poudres composites w-mo et poudres composites correspondantes WO2008031121A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP07784633A EP2061614A1 (fr) 2006-09-15 2007-08-24 Procédé de préparation de poudres composites w-mo et poudres composites correspondantes
JP2009527644A JP2010503764A (ja) 2006-09-15 2007-08-24 Ｗ−Ｍｏ複合体粉末の製造方法及び複合体粉末

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AT0155006A AT504302B8 (de) 2006-09-15 2006-09-15 Verfahren zur herstellung von w-mo-kompositpulvern und kompositpulver
ATA1550/2006 2006-09-15

Publications (1)

Publication Number Publication Date
WO2008031121A1 true WO2008031121A1 (fr) 2008-03-20

Family

ID=38704767

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/AT2007/000407 WO2008031121A1 (fr) 2006-09-15 2007-08-24 Procédé de préparation de poudres composites w-mo et poudres composites correspondantes

Country Status (4)

Country Link
EP (1) EP2061614A1 (fr)
JP (1) JP2010503764A (fr)
AT (1) AT504302B8 (fr)
WO (1) WO2008031121A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102284704A (zh) * 2011-07-30 2011-12-21 金堆城钼业股份有限公司 一种小粒度掺钾钼合金粉的制备方法
WO2011124542A3 (fr) * 2010-04-08 2013-01-10 H.C. Starck Gmbh Dispersions ainsi que leur procédé de production et leur utilisation
CN108907218A (zh) * 2018-07-26 2018-11-30 江西理工大学 Co-co2混合气氛还原氧化钨制备超细钨粉的方法
CN110983090A (zh) * 2019-12-31 2020-04-10 金堆城钼业股份有限公司 一种含碳钼合金的烧结方法

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106944629B (zh) * 2016-10-06 2019-04-05 江西理工大学 一种单分散超细/纳米钨粉的制备方法
WO2019107816A1 (fr) * 2017-11-29 2019-06-06 엔에이티엠 주식회사 Procédé de fabrication d'un alliage tungstène-molybdène
CN109182812B (zh) * 2018-09-21 2020-04-10 河南科技大学 一种钨合金前驱复合粉体的制备方法、钨合金及制备方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5885653A (en) * 1995-02-09 1999-03-23 Sandvik Ab Method of making metal composite materials
US5956560A (en) * 1994-12-22 1999-09-21 Osram Sylvania Inc. Tungsten-copper composite powder

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5956560A (en) * 1994-12-22 1999-09-21 Osram Sylvania Inc. Tungsten-copper composite powder
US5885653A (en) * 1995-02-09 1999-03-23 Sandvik Ab Method of making metal composite materials

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
ZOU ZHIQIANG ET AL: "Amine tungstates and their application for tungsten powder production", INTERNATIONAL JOURNAL OF REFRACTORY METALS AND HARD MATERIALS, ELSEVIER PUBLISHERS, BARKING, GB, vol. 9, no. 3, September 1990 (1990-09-01), pages 143 - 145, XP009092316, ISSN: 0263-4368 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011124542A3 (fr) * 2010-04-08 2013-01-10 H.C. Starck Gmbh Dispersions ainsi que leur procédé de production et leur utilisation
CN103108714A (zh) * 2010-04-08 2013-05-15 H.C.施塔克股份有限公司 分散体、其制造方法及其用途
US8815983B2 (en) 2010-04-08 2014-08-26 H. C. Starck Gmbh Dispersion, method for producing same, and use thereof
EP2566638B1 (fr) 2010-04-08 2015-09-02 H.C. Starck GmbH Dispersions comprennant des particules de de carbure de tungstène moulès revetus de carbure de tungstène ainsi que leur procédé de production et leur utilisation
CN102284704A (zh) * 2011-07-30 2011-12-21 金堆城钼业股份有限公司 一种小粒度掺钾钼合金粉的制备方法
CN108907218A (zh) * 2018-07-26 2018-11-30 江西理工大学 Co-co2混合气氛还原氧化钨制备超细钨粉的方法
CN108907218B (zh) * 2018-07-26 2021-11-19 江西理工大学 Co-co2混合气氛还原氧化钨制备超细钨粉的方法
CN110983090A (zh) * 2019-12-31 2020-04-10 金堆城钼业股份有限公司 一种含碳钼合金的烧结方法
CN110983090B (zh) * 2019-12-31 2021-07-13 金堆城钼业股份有限公司 一种含碳钼合金的烧结方法

Also Published As

Publication number Publication date
JP2010503764A (ja) 2010-02-04
EP2061614A1 (fr) 2009-05-27
AT504302B8 (de) 2009-08-15
AT504302A1 (de) 2008-04-15
AT504302B1 (de) 2009-07-15

Similar Documents

Publication Publication Date Title
AT504302B1 (de) Verfahren zur herstellung von w-mo-kompositpulvern und kompositpulver
EP1242642B1 (fr) procede de production de melanges de poudres ou poudres composites
DE60121242T2 (de) Molybdän-Kupfer-Verbundpulver sowie dessen Herstellung und Verarbeitung zu einer Pseudolegierung
DE112008002461B4 (de) Einzelkristall-Feinpulver eines Sulfids oder Sulfidkomplexes und Verfahren zum Herstellen desselben
DE2833015C2 (fr)
EP2010687A2 (fr) Procédé de production d'un corps en métal dur, poudre servant à la production d'un métal dur et corps en métal dur
AT504319B1 (de) Verfahren zur herstellung von kompositpulvern sowie kompositpulver
DE102019130263A1 (de) Allgemeine synthesestrategie zur herstellung von mehrmetallischen nanostrukturen
DE19640788C1 (de) Beschichtungspulver und Verfahren zu seiner Herstellung
EP0572788B1 (fr) Poudre de carbonitrure submicronique, procédé pour sa production et application
DE19704242C1 (de) Carbonitrid-Pulver, Verfahren zu ihrer Herstellung sowie deren Verwendung
DE60223463T2 (de) Feines Wolframcarbidpulver und Verfahren zu dessen Herstellung
WO2000029325A1 (fr) Procede de preparation de carbures de tungstene par carburation en phase gazeuse
EP0232772B1 (fr) Procédé de préparation d'un matériau pulvérulent amorphe par un procédé de broyage
WO2012145773A1 (fr) Carbure de tungstène hexagonal dopé et son procédé de fabrication
DE2910596C2 (de) Verfahren zur Herstellung von Titancarbonitrid
EP4058224A1 (fr) Poudre sphérique pour la fabrication d'objets en 3d
EP1343735B1 (fr) Procede de production de carbure de tungstene
DE112020007343T5 (de) Hoch-Entropie-Legierung und Verfahren zu deren Wärmebehandlung
DE2833016C2 (fr)
DE3100266C2 (de) Verfahren zur Herstellung von Mischcarbiden oder Mischcarbonitriden
DE2115999A1 (de) Verfahren zur Herstellung von gesintertem Hartmetall
DE1295855B (de) Hochtemperaturfeste Werkstoffe und Formteile in Dispersionsform
DE1238219B (de) Verfahren zur Erzeugung von Metallen und Legierungen, in denen nicht reduzierbare Oxyde fein dispergiert sind
EP0464396A1 (fr) Carbonitrures à partir des métaux de transition (M, M*, M**) des groupes 4 (M), 5 (M*) et 6 (M**) du système périodique des éléments, procédé pour leur production et application des carbonitrures

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 07784633

Country of ref document: EP

Kind code of ref document: A1

DPE1 Request for preliminary examination filed after expiration of 19th month from priority date (pct application filed from 20040101)
WWE Wipo information: entry into national phase

Ref document number: 2007784633

Country of ref document: EP

ENP Entry into the national phase

Ref document number: 2009527644

Country of ref document: JP

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE