EP0839920B1 - Procédé de préparation de poudre de départ pour matériau dur à grain fin - Google Patents

Procédé de préparation de poudre de départ pour matériau dur à grain fin Download PDF

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Publication number
EP0839920B1
EP0839920B1 EP97203354A EP97203354A EP0839920B1 EP 0839920 B1 EP0839920 B1 EP 0839920B1 EP 97203354 A EP97203354 A EP 97203354A EP 97203354 A EP97203354 A EP 97203354A EP 0839920 B1 EP0839920 B1 EP 0839920B1
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EP
European Patent Office
Prior art keywords
powder
metal
reaction
cyclone
production
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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.)
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EP97203354A
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German (de)
English (en)
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EP0839920A2 (fr
EP0839920A3 (fr
Inventor
Günter Dr. Kneringer
Wolfgang Dr. Köck
Joachim Dr. Resch
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Plansee SE
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Plansee SE
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C22C1/053—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds
    • C22C1/056—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds using gas
    • 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

Definitions

  • the quality that can be achieved for a type of hard metal depends to a large extent on the nature of the starting powder, which is pressed and processed into a shaped hard metal body by sintering.
  • the chemical-metallurgical composition is just as important as the powder morphology, powder structure and consequently the powder preparation before pressing and sintem.
  • efforts to produce improved carbide grades have focused primarily on achieving fine grain and homogeneity of the carbide in the carbide.
  • the metallic components in the carbide hard material phase of the hard metal are mainly tungsten or titanium, in addition in the form of stabilizing Mixed carbides small amounts of the high-melting metals tantalum, niobium, Molybdenum, vanadium and chrome.
  • Metal oxides or comparable compounds familiar to the person skilled in the art are reduced to pure metal in one or more process stages and then the metal, usually in a separate process step, converted into metal carbide. Reduction and carburization are isolated also carried out in a common, ongoing process.
  • Metal oxides are used for metal oxide reduction in a solid-gas reaction on carrier ships in comparatively thin layers led a reduction furnace.
  • Usual processes for carbide formation are the intimate mixing of metal powder, for example tungsten metal powder, with carbon (soot particles) and subsequent reaction in a carburizing furnace.
  • metal powder for example tungsten metal powder
  • carbon silicates
  • commercial production also plays an important role in commercial production. It is determined by the price of the device in accordance with the complexity of the process, the amount of energy and reaction gas consumed per reaction unit and, above all, the factor of production time.
  • the reaction or throughput times of the powders in the devices listed are without exception in the range of hours, at best 1 to 2 hours, at worst 15 to 20 hours of reaction time.
  • the overall production also includes Reduction and carburization process steps such as grinding and mixing processes, which usually take many hours.
  • Powder preparation processes e.g. granulating the powder by means of Spray drying, largely indispensable in the carbide industry.
  • the object of the present invention is therefore to compare one with the state of the art Technology more economical process for the production of pressable To provide powder mixtures for hard metal production, which the Manufacture of high quality, especially fine-grained carbide grades allowed.
  • the object of the present invention is also to select one for Implementation of the method suitable device, such Devices for the chemical conversion of various organic and inorganic materials are known for the production of hard metal powder batches to achieve homogeneous, fine-grained carbide grades have not been used so far.
  • hard metal in claim 1 also includes materials known under the name of cermet, which in addition to carbides also contain substantial amounts of nitrides or carbonitrides in the hard material phase.
  • the inventive method requires the use of a Term "cyclone" common reaction chamber.
  • Cyclones are characterized in that they generally have axially or rotationally symmetrical chamber walls.
  • the material to be reacted in the form of solid particles is intimately mixed and swirled with carrier and / or reaction gas immediately upon entry into the reaction chamber and continuously blown in as a mixture in a direction deviating from the longitudinal axis of the chamber.
  • the substances introduced in this way move under the action of gravitation and centrifugal forces in accordance with the gas flow conditions prevailing in the chamber on essentially predetermined trajectories, that is to say not in a statistical movement, for example in a fluidized bed furnace.
  • the gas and particle flow is determined by the chamber walls, including any guide elements that may be attached there. There are high flow velocities tangential to these chamber walls. High relative speeds between solid and gaseous substances occur in the reaction chamber. High speed gradients between individual substances mean high turbulence intensities and result in high heat and mass transfer numbers for the individual reactants in the desired chemical reaction.
  • the duration of the reaction material in the chamber is device and process-related small.
  • the stay or reaction times depend on Plant design between tenths of a second and about a minute.
  • a major advantage of the present method over the known methods for producing submicron or nanophase powder for powder press approaches for the production of hard metal is that Raw material powder (metal compounds to be reduced) can be used can, as they do without special additional treatment from the ore processing be provided and after applying this procedure to carbide very uniform and fine-grained structure can be processed.
  • Powder batches allow hard metal qualities to reach those of those correspond to or are even superior to those after the ones above described method, production of nanophase composite powder, Manufacture of submicron carbides.
  • Metal oxides, or standard compounds which are alternatively available for the reduction to metal powder are usually provided in particle sizes between approximately 2 and 30 ⁇ m and, according to the process according to the invention, give metal powders with a particle size approximately comparable to the starting powder size, but with a significant proportion of agglomerated powders. Agglomerated powders are generally not a good starting point for the production of extremely fine-grained carbide. It was completely surprising, however, that the metal powders produced by chemical reduction according to the present invention consistently have an extremely high, sponge-like microporosity in the range of 0.1 ⁇ m. However, this means that the metal powder for further processing to carbide and hard metal has a quality that was previously known only approximately from the nanophase process mentioned as previously known. The entire volume of the metal powder can be completely carburized in a cyclone reaction and leads to a previously unattainable, fine-grained hard metal quality.
  • the chemical process step in Cyclone is the throughput time of the material to be reacted in the solid Phase 0.2 to 10 s, for at least 90% by volume of the solid phase complete chemical conversion to the predetermined reaction state.
  • the individual chemical process step in the cyclone optionally at least in repeated in another run.
  • the Metal oxide powder or the powdery metal compound as that too reducing material before the process step reduction metallic Filler materials added especially those in hard metal as binder metal metals Co and / or Ni used. This is done by adding metallic powder, or by making a solid beforehand Solution, that is, by introducing the filler materials into the solid phase of the good to be reduced.
  • the following result Variants for the invention comprising several partial steps Process for the production of powder press batches for further processing to fine-grain carbide.
  • a first method variant of the method according to the invention consists in the reduction of metal oxide or comparable metal compounds Cyclone metal powder in the cyclone process; at high Purity requirements for the metal powder to be produced also in one Repeat this reduction step.
  • the metal powder thus obtained is in a in Carbide manufacturing commonly used ball mill with carbon particles intimately mixed. In doing so, agglomerates of spongy Crushed metal powder.
  • This mixing and Milling process powdered additional metals (to form mixed carbides as Grain growth inhibitors in hard metal) added.
  • the powder mixture is further converted to metal carbide in the carburizing furnace by conventional methods converted, according to standard procedures with the binding metal (cobalt and / or Nickel powder) mixed and optionally over attritor grinding and Spray drying transferred into a ready-to-press powder batch.
  • the so obtained Powder press approach can be too much using conventional pressing and sintering processes Process fine-grain carbide with very high phase homogeneity.
  • the metal oxides are reduced to metal powder in the cyclone, as above.
  • the metal powder obtained in this way is also further processed in the cyclone to metal carbide by the cyclone process which is essential to the invention, namely in two sub-variants, either following prior external mixing with carbon particles (as above) by simultaneously blowing this mixture together with carrier gas and possibly with reaction gas into the reaction chamber, or according to a second sub-variant, by directly blowing the metal powder into the cyclone reactor together with gaseous carbon compounds, in particular hydrocarbon gases and / or CO.
  • This variant is also supplemented by customary grinding, mixing and granulating processes, with grinding and granulating processes not necessarily having to take place.
  • the Metal oxides together with a reducing gas and a carbon containing gas into the cyclone reaction chamber, or blown in and it takes place during a single overall run a first part of a spatially uniform overall reactor Reduction of the oxide to metal powder and immediately afterwards in one second chamber part to carburize the reduced metal powder Metal carbide.
  • additional metals for mixed carbide formation such as niobium, tantalum, vanadium and chromium, can also be added to the carburizing process in the cyclone and simultaneously converted to carbides with the main metal.
  • additional metals for mixed carbide formation such as niobium, tantalum, vanadium and chromium, can also be added to the carburizing process in the cyclone and simultaneously converted to carbides with the main metal.
  • a cyclone with the features of the present invention and corresponding to the representation in FIG. 1 is used as the device for carrying out the reduction process.
  • the overall system shown in FIG. 1 is composed of a steel reaction chamber designed as a cyclone, which is followed by a second reaction chamber designed as a downpipe for chemical aftertreatment of the reacted material, this aftertreatment and the associated reaction chamber not being part of the invention. It is a pilot plant that is smaller in comparison to plants for industrial production in terms of the throughput quantity of goods to be reduced per unit of time.
  • powdered W 4 O 11 is blown in via a feed device (1) together with reaction and / or carrier gas into the head part of a reaction chamber (2) which is approximately rotationally symmetrical with respect to the direction of fall.
  • the amount of gas is metered by means of a flow meter (7).
  • the reaction chamber is brought to a reaction temperature of 1100 ° C. by means of an electrical heating device (6).
  • the pulverulent reaction product leaves the chamber at the lower end, falls into a storage room with screw conveyor (3) and is introduced into the second reaction chamber (4) with heating device (6).
  • the exhaust gas (8), reaction and / or carrier gas and H 2 O vapor as the end product of the reaction leave the first chamber at the top.
  • the tungsten powder is collected in a container (5).
  • the temperature of the entire two-stage process is controlled by means of a thermocouple (9) at the exhaust outlet of the first reaction chamber.
  • a gas amount of 4000 l H 2 gas is used, ie a large excess of gas based on the stoichiometric reaction amounts.
  • Tungsten oxide as the material to be reduced and H 2 as the carrier or reducing gas are fed to the cyclone separately.
  • the carrier or reducing gas is preferably introduced horizontally into the chamber at the upper end at a high flow rate.
  • the pulverulent material to be reduced is brought up to the gas inlet nozzle in such a way that it is entrained by the gas jet as it enters the chamber, is swirled and mixed intensively with it, and passes through the chamber in accordance with the guidance of the gas flow on predetermined trajectories.
  • the material reduced to tungsten powder leaves the reduction chamber after a passage time of 1-2 s and has a residual oxygen content of 10,500 ⁇ g / g at the outlet.
  • the emerging tungsten powder has a grain size comparable to that of the powder taken in, of the order of 20 ⁇ m in diameter, but the individual powder particles or grains have a large porosity throughout their entire volume.
  • the spatial expansion of the substructure in the tungsten particle is 0.1 ⁇ m.
  • the tungsten powder obtained in this way is converted into carbide by customary methods.
  • the tungsten powder is first intensively mixed in the ball mill with a stoichiometric proportion of fine soot particles for tungsten carbide, WC. Individual agglomerates of the tungsten powder are crushed.
  • the batch obtained in this way is carburized in a graphite furnace with induction heating under an H 2 atmosphere at 1300 ° C. for 3 hours. Pure tungsten carbide with a carbon content of 6.12% and a residual oxygen content of 1200 ⁇ g / g is formed.
  • the carbide is made with binder metal and usual amounts of mixed carbides (Niobium carbide, tantalum carbide) mixed and optionally via attritor grinding and Spray drying processed into free-flowing granules.
  • the device used corresponds to that of Example 1 without a downpipe being connected downstream of the cyclone.
  • Tungsten oxide, blue is reduced to tungsten powder in the cyclone in accordance with the process conditions mentioned in Example 1.
  • the tungsten powder is then further processed into tungsten carbide in a cyclone reactor lined with graphite using carbon-containing gases plus carrier gas (CH 4 / H 2 mixture).
  • Carburization takes place in one step at a cyclone temperature of 1100 ° C.
  • a gas throughput of 6000 l / h is regulated for a tungsten powder throughput of 1000 g / h.
  • the methane concentration in the CH 4 / H 2 mixture is 1.1% by volume.
  • ready-to-press powder batches are produced by mixing the WC with binder material and small proportions of mixed carbides with optional granulation by means of spray drying.
  • the hard metal obtained from these powder batches corresponds in its fine-grained structure and homogeneity to that according to Example 1.
  • the subsequent carburization is again carried out in the cyclone reactor, but in contrast to Example 2, using CO as the carburizing and carrier gas.
  • the tungsten powder obtained from the cyclone reactor is continuously introduced into the chamber at a throughput of 1000 g / h with a gas quantity of 6000 l / h (CO gas) and at 1000 ° C. chamber temperature in a one-step process to produce W 2 C and WC (C content 4.2% by weight) and a residual oxygen content of 3240 ⁇ g / g reacts.
  • the X-ray diffractometer examination shows that in addition to W 2 C, small amounts of WC but no free carbon are present in the end product thus obtained.
  • the throughput time for the particles to be carburized in the cyclone reactor is 1-2 s.
  • the W 2 C-WC powder mixture obtained in this way is reacted in a second process step in the cyclone under approximately the same test conditions as for the first carburization step to pure tungsten carbide WC with only a very small residual oxygen content and without detectable free carbon residues.
  • the powder sets are completed by mixing and optionally granulating as in Examples 1 and 2.
  • a hard metal made from these powder batches by customary processes has a high degree of fine grain and a high degree of material homogeneity.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Claims (5)

  1. Procédé de fabrication de préparations pulvérulentes à comprimer, pour métal dur à grain fin à base de carbures métalliques, en partant d'une poudre d'oxyde métallique ou de composés métalliques pulvérulents réductibles qui inclut les étapes de:
    réduction de l'oxyde métallique ou du composé métallique en métal,
    carburation du métal,
    procédé mécanique-chimique de préparation ou de mélange de poudres,
       caractérisé en ce que
       un dispositif à cyclone et le procédé à cyclone qui présentent la somme des remarques suivantes sont utilisés dans au moins l'une des deux étapes chimiques du procédé, la réduction et la carburation:
    le dispositif est une chambre de réaction réglable en température, à configuration au moins partiellement symétrique en rotation autour d'un axe longitudinal du dispositif, qui comporte des ouvertures d'entrée et de sortie tant pour les produits pulvérulents à réduire et/ou à carburer que pour les matières qui réagissent avec les produits et pour le gaz porteur;
    les produits pulvérulents introduits en continu traversent la chambre de réaction en maintenant l'état de phase solide sur des trajets de vol prédéterminés à des vitesses élevées de poudres au moins partiellement tangentielles à la paroi de la chambre;
    les trajets de vol sont pilotés au moyen de la direction de vol et de la vitesse des produits pulvérulents lors de leur introduction ainsi qu'au moyen de paramètres d'écoulement des gaz porteurs et/ou de réaction; et
    une fraction volumique d'au moins 90% des produits pulvérulents qui quittent le dispositif a réagi en moyenne dans les 0,1 à 60 secondes après l'introduction.
  2. Procédé de fabrication de préparations pulvérulentes à comprimer selon la revendication 1, caractérisé en ce que des produits pulvérulents sont transformés, pour atteindre l'état de réaction prédéterminé, en un temps de parcours de 0,2 à 10 secondes.
  3. Procédé de fabrication de préparations pulvérulentes à comprimer selon la revendication 1 ou 2, caractérisé en ce que des vitesses relatives élevées entre matières solides et gazeuse apparaissent dans le dispositif.
  4. Procédé de fabrication de préparations pulvérulentes à comprimer selon l'une des revendications 1 à 3, caractérisé en ce qu'au moins l'une des étapes, de réduction et de carburation, du procédé est répétée au moins une fois.
  5. Procédé de fabrication de préparations pulvérulentes à comprimer selon l'une quelconque des revendications précédentes, caractérisé en ce que des matières métalliques additionnelles sont ajoutées avant la réduction, sous forme de poudre séparée ou par formation préalable d'une solution solide dans les produits à réduire, à la poudre d'oxyde métallique ou au composé métallique pulvérulent.
EP97203354A 1996-11-04 1997-10-29 Procédé de préparation de poudre de départ pour matériau dur à grain fin Expired - Lifetime EP0839920B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
AT1912/96 1996-11-04
AT191296 1996-11-04
AT0191296A AT404912B (de) 1996-11-04 1996-11-04 Verfahren zur herstellung von pulver-pressansätzen für feinkörniges hartmetall

Publications (3)

Publication Number Publication Date
EP0839920A2 EP0839920A2 (fr) 1998-05-06
EP0839920A3 EP0839920A3 (fr) 2000-03-29
EP0839920B1 true EP0839920B1 (fr) 2002-12-18

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EP97203354A Expired - Lifetime EP0839920B1 (fr) 1996-11-04 1997-10-29 Procédé de préparation de poudre de départ pour matériau dur à grain fin

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US (1) US6113668A (fr)
EP (1) EP0839920B1 (fr)
JP (1) JPH10140216A (fr)
AT (2) AT404912B (fr)
DE (1) DE59709001D1 (fr)
ES (1) ES2186840T3 (fr)

Families Citing this family (6)

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Publication number Priority date Publication date Assignee Title
US6843824B2 (en) * 2001-11-06 2005-01-18 Cerbide Method of making a ceramic body of densified tungsten carbide
JP4619907B2 (ja) * 2005-09-20 2011-01-26 中外炉工業株式会社 粉体製造装置
US20130209308A1 (en) * 2012-02-15 2013-08-15 Baker Hughes Incorporated Method of making a metallic powder and powder compact and powder and powder compact made thereby
JP2013222497A (ja) * 2012-04-12 2013-10-28 Toshiba Corp 真空バルブ用接点材料
CN112390261A (zh) * 2019-08-13 2021-02-23 斯特里特技术有限公司 气相二氧化硅颗粒分离脱氢的系统和方法
CN114853021B (zh) * 2022-05-23 2024-08-23 赣州海盛钨业股份有限公司 纳米碳化钨粉末及其制备方法

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Also Published As

Publication number Publication date
ATE230038T1 (de) 2003-01-15
ATA191296A (de) 1998-08-15
AT404912B (de) 1999-03-25
EP0839920A2 (fr) 1998-05-06
ES2186840T3 (es) 2003-05-16
JPH10140216A (ja) 1998-05-26
EP0839920A3 (fr) 2000-03-29
DE59709001D1 (de) 2003-01-30
US6113668A (en) 2000-09-05

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