EP0966550B1 - Corps fritte en metal dur ou cermet et son procede de production - Google Patents

Corps fritte en metal dur ou cermet et son procede de production Download PDF

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Publication number
EP0966550B1
EP0966550B1 EP98919052A EP98919052A EP0966550B1 EP 0966550 B1 EP0966550 B1 EP 0966550B1 EP 98919052 A EP98919052 A EP 98919052A EP 98919052 A EP98919052 A EP 98919052A EP 0966550 B1 EP0966550 B1 EP 0966550B1
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EP
European Patent Office
Prior art keywords
sintering
microwave
platelets
sintered body
hard
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.)
Expired - Lifetime
Application number
EP98919052A
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German (de)
English (en)
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EP0966550A1 (fr
Inventor
Klaus RÖDIGER
Klaus Dreyer
Monika Willert-Porada
Thorsten Gerdes
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.)
Widia GmbH
Original Assignee
Widia GmbH
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
Priority claimed from DE19725914A external-priority patent/DE19725914A1/de
Application filed by Widia GmbH filed Critical Widia GmbH
Publication of EP0966550A1 publication Critical patent/EP0966550A1/fr
Application granted granted Critical
Publication of EP0966550B1 publication Critical patent/EP0966550B1/fr
Anticipated expiration legal-status Critical
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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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/23—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces involving a self-propagating high-temperature synthesis or reaction sintering step
    • 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
    • C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
    • 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 hard metal or cermet sintered body defined in claim 1, consisting of at least one hard material phase containing WC and a binder phase and embedded WC platelets (platelike reinforcing materials).
  • the invention also relates to a method for producing a hard metal or cermet sintered body as defined in claim 4.
  • a hard metal composite body made of hard material phases, such as tungsten carbide and / or carbides or nitrides of the elements of the IVa or Va group of the periodic table, of reinforcing materials and of a binder metal phase such as cobalt, iron or nickel is known from EP 0 448 572 B1, which as reinforcing materials either single-crystal platelet-shaped reinforcing material made of borides, carbides, nitrides or carbonitrides of the elements of the IVa or VIa group of the periodic table or mixtures thereof or of SiC, Si 3 N 4 , Si 2 N 2 O, Al 2 O 3 , ZrO 2 , AlN and / or BN or single-crystalline needle-shaped reinforcing materials made of SiC, Si 3 N 4 , Si 2 N 2 O, Al 2 O 3 , ZrO 2 , AlN and / or BN.
  • the proportion of the reinforcing materials is 2 to 40% by volume, preferably 10 to 20% by volume.
  • the US-A-3 which is at least 647 401 describes anisodimensional tungsten carbide platelets of maximum dimension between 0.1 to 50 ⁇ m and a largest dimension three times as large as the smallest dimension. These platelets are bound by cobalt, which is present in an amount of 1 to 30% based on the total body weight.
  • the body has a density of 95% of the theoretical maximum density.
  • CH 522 038 describes a cemented cemented carbide body containing tungsten carbide particles, the mean grain size of which is smaller than 1 ⁇ m , at least 60% of the particles being smaller than 1 ⁇ m .
  • the metal phase content is between 1 to 30% and is composed of 8 to 33% by weight of tungsten and 67 to 62% by weight of cobalt.
  • the largest areas of the anisodimensional WC particles should be oriented practically parallel to a reference line.
  • WO 96/22399 describes a multiphase sintered body which has a first hard phase made of carbides, nitrides, carbonitrides or carbooxynitrides of the elements of the IVa, Va or VIa metals of the periodic table.
  • the second phase consists of a solid solution with particle sizes of 0.01 to 1 ⁇ m of carbides, nitrides, carbonitrides and Carbooxinitriden of at least two elements of the IVa to VIa-group of the periodic system.
  • the binder is composed of cobalt, nickel, iron, chromium, molybdenum and tungsten, as well as mixtures thereof.
  • the sintered body can contain WC platelets made of tungsten carbide with a size between 0.1 and 0.4 ⁇ m , which are to be formed in situ.
  • ultra-fine grain alloys Especially in the production of ultra-fine grain alloys but ultrafine and nano-fine starting powders also become clearly that the conventional production process due to problems with processing powders and grain enlargement apparently reach its limits during sintering.
  • microwaves describes electromagnetic radiation in the frequency range from approx. 10 8 to 10 11 Hz (corresponding to a wavelength in a vacuum of around 1 mm to 1 m).
  • Commercially available microwave generators generate monochromatic radiation, ie waves with a certain frequency. Generators with 2.45 ⁇ 10 9 Hz are widespread, which corresponds to a wavelength of 12 cm.
  • thermal radiation (Planckian radiation) has a very large frequency bandwidth and in typical sintering processes it has its energy maximum at a wavelength of 1 to 2 ⁇ m . Matter, which is exposed to electromagnetic radiation, can heat up due to the interaction with the field and thereby withdraw energy from the wave field. Since this interaction is strongly frequency-dependent, matter is also heated in the microwave field and by thermal radiation due to various heating mechanisms.
  • the interaction of matter with a microwave field takes place via the electrical dipoles or free charges present in the material.
  • the range of absorption properties of materials for microwaves ranges from transparent (oxide ceramics, some organic polymers) to partially transparent (oxide ceramics, non-oxide ceramics, filled polymers, semiconductors) to reflective (metals).
  • the behavior of a material in the microwave field depends on the microwave frequency and to a large extent on the temperature: material that is microwave-transparent at room temperature can absorb or reflect strongly at elevated temperatures. For most substances, the penetration depth of the microwaves is much greater than that for infrared radiation, which, depending on the sample size, has the result that the material - in contrast to "skin heating" with infrared radiation - can be heated in volume with microwaves.
  • the penetration depth of microwaves with a frequency of 2.45 GHz at a temperature of 20 ° C differs for different substances and has the following values: 1.7 ⁇ m for aluminum, 2.5 ⁇ m for Cobalt (as an example for metals), 4.7 ⁇ m for WC and 8.2 ⁇ m for TiC (as example for solid semiconductors), 10 m for Al 2 O 3 and 1.3 cm for H 2 O (as example for insulators) and 7.5 cm for WC with 6 M% Co, 31 cm for Al 2 O 3 with 10 M% Al and 36 cm for Al 2 O 3 with 30 M% TiC (as an example for powder metal green parts).
  • Fig. 1 shows schematically the structure of a suitable one Oven.
  • the microwave with a frequency of 2.45 GHz is from generated a magnetron and into the metallic resonator housing guided. Inside the resonator is the cemented carbide batch, the one with a microwave-transparent, thermal Insulation is surrounded. With appropriate interpretation of the The resonators are in a homogeneous magnetic field and is heated homogeneously. The measurement of the batch temperature and the coupled microwave power are used for Control of the microwave sintering process with a microprocessor. Compare the sintering profiles to microwave sintering conventional sintering in comparable sized furnaces have shown that the sintering cycle (without the cooling phase) shortened by a factor of 3 in microwave sintering can be.
  • the consumption of electrical energy the microwave sintering technology here is due to the process time reduction and because of the lower heating output during of sintering is only a fraction of the values for the conventional sintering technology.
  • a microwave sintering hard metals and also cermets with a high binder metal content (e.g. 25% by mass) as well as with a low binder metal content (for example 4% by mass) at temperatures, 50 to 100 K below that of conventional sintering lying, sintering without pressure.
  • the comparison with a conventional one Sintering shows that the bulk of the compaction in microwave sintering at much lower temperatures still takes place below the eutectic temperature.
  • the improved Compression behavior can also be seen in the simultaneous Reduction of open and closed porosity in Microwave sintering. Because of the shorter sintering times and the microwave sintered show lower sintering temperatures Hard metals have a finer structure and thus an increase in hardness up to 10 %. In use as a cutting tool when turning The microwave sintered version of cast iron showed advantages in the open area wear behavior.
  • Tungsten powder no longer in a separate process step be carburized, but in that the carburizing in the Sintering process is integrated.
  • the compacts are on the usual way of shaping made by instead of Tungsten carbide-cobalt powder mixture from a mixture of Tungsten, carbon and cobalt powder is assumed.
  • the exothermic carburization reaction of tungsten and carbon to tungsten carbide, with a heat tone of 38 kJ / mol, takes place after the binder expulsion of the compact at Temperature of around 930 ° C instead.
  • Fig. 2 is thermogravimetry (TG, DTG), dilatometry (DIL, DDIL) and dynamic differential calorimetry (DSC) a reaction sintering of a WC-6 M% Co hard metal for temperatures shown from 500 ° C.
  • the DSC signal is above 750 ° C endothermic reduction of the oxides present in the tungsten powder recognize that with the corresponding mass decrease in thermogravimetry and a first shrinkage stage of the sample in Dilatometer signal corresponds.
  • TG thermogravimetry
  • DIL dilatometry
  • DSC dynamic differential calorimetry
  • the reaction sintering is done using microwave radiation implemented (MWRS), on the one hand is a further refinement of the structure possible, on the other hand the remaining porosity can be compared the conventional reaction sintering (RS) clearly be humiliated.
  • MWRS microwave radiation implemented
  • RS conventional reaction sintering
  • HV30 Vickers hardness was after the conventional one Sintering 1560, after microwave sintering 1630, after conventional reaction sintering 1720 and after microwave reaction sintering 1770.
  • reaction sintering In addition to the material-specific advantages of reaction sintering mentioned, especially microwave reaction sintering, this method offers great potential for simplification and shortening the process flow and saving energy in the production of hard metals. Except at high temperatures carburization that occurs also falls before and after Process steps such as mixing, breaking, crushing etc. continue. A process time gain can also be achieved in this way become.
  • WC-6 M% Co hard metals with differently fine tungsten powders were manufactured using conventional (RS) and microwave heating (MWRS).
  • the tungsten powders used had an average grain size of 0.4 ⁇ m , 1 ⁇ m and 2.4 ⁇ m (in each case FSSS) with doping of 0.2 M% VC or missing VC.
  • FSSS microwave heating
  • the influence of the VC content on the structure is evident most clearly with the fine tungsten powders.
  • the WC crystals especially in the case of the RS samples, apparently have sufficient time to grow out during the sintering phase in the absence of VC.
  • the invention has for its object a simultaneous Increase in hardness and toughness in hard metal or Cemert sintered bodies to bring about the type mentioned.
  • the manufacture the method according to such a sintered body Claim 4 used.
  • the method according to the invention is in no way limited to one limited possible unimodal initial grain size distribution, rather, it can also be used with powders with a wide or bimodal Size distribution to be worked.
  • the reaction sintering of powders, both tungsten and Contain carbon, but also in the starting mixture WC may contain, completely or as a partial Reaction sintering is carried out, the partial proportions of the reaction sintering between 1% and 100% (based on the complete sintering process).
  • the grain growth in the sintered body can be controlled.
  • WC platelet growth can also be controlled via the partial share of reaction sintering, thereby reducing the platelet concentration is controllable in the sintered body.
  • the volume fraction of the WC platelets on the total sintered body volume is preferably up to 25 vol%.
  • the platelet content should be measured as a proportion of the area of a metallographic cut max. 20% amount, with all WC crystals with a length / width ratio, the so-called aspect ratio of greater than 3 be counted.
  • the maximum aspect ratio is preferably Max. 10 ⁇ 1.
  • the rate of growth to be controlled.
  • microwave reaction sintering is that a more homogeneous structure, better compaction, i.e. a smaller residual porosity can be achieved as well as shorter ones Sintering times and lower sintering temperatures. Resulting from this lower manufacturing costs.
  • 0.4 ⁇ m W powder, 0.2% addition of VC, 6% co-powder with a grain size of 1.6 ⁇ m and a stoichiometric addition of carbon in the form of Carbon black mixed and adding acetone for 36 hours in one Ball mill has been ground before then using 2% wax Pressing aids have been added, distilled off and granulated are.
  • the granules were pressed into green bodies by means of die presses and in the microwave sintering oven at 500 ° C / hour to 900 ° C heated up and then with the onset of the carburization reaction to the sintering temperature within 10 min using microwaves heated from 1350 ° C. After a waiting time of 20 min the sample is cooled by turning off the microwave heater.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Claims (7)

  1. Corps fritté en métal dur ou cermet, se composant d'au moins une phase de matière dure contenant du WC et d'une phase liant ainsi que de platelets de WC enrobés,
    caractérisé par le fait
    que les métaux nécessaires à la formation de la ou bien des phase(s) dure(s), le carbone et les proportions de tungstène et de carbone nécessaires à la formation des platelets de WC, ainsi que, le cas échéant, d'autres métaux, carbures et nitrures métalliques et/ou des composés d'azote solides en tant que fournisseurs pour carbone et/ou azote ont été précomprimés au moins en partie respectivement en forme de poudre en un corps formé et ont été soumis ensuite au moins temporairement à un frittage-réaction dans un champ à micro-ondes ayant une densité de flux d'énergie de 0,01 à 10 W/cm3.
  2. Corps fritté en métal dur ou cermet selon la revendication 1, caractérisé par le fait qu'il contient jusqu'à 12 %, de préférence 8 % de VC et/ou de Cr3C2 par rapport à la phase liant.
  3. Corps fritté en métal dur ou cermet selon la revendication 1 ou 2, caractérisé par le fait que les platelets de WC présentent un rapport diamètre/épaisseur de ≥3, de préférence de ≥5, et/ou que la proportion des platelets de WC - par rapport au volume total - est < 25 pourcent volumétrique.
  4. Procédé de fabrication d'un corps fritté en métal dur ou cermet selon l'une des revendications 1 à 3, caractérisé par le fait que les métaux nécessaires à la formation de la ou bien des phase(s) dure(s), le carbone et les proportions de tungstène et de carbone nécessaires à la formation des platelets de WC, ainsi que, le cas échéant, d'autres métaux, carbures et nitrures métalliques et/ou des composés d'azote solides en tant que fournisseurs pour carbone et/ou azote sont précomprimés au moins en partie respectivement en forme de poudre en un corps formé et sont soumis ensuite au moins temporairement à un frittage-réaction dans un champ à micro-ondes ayant une densité de flux d'énergie de 0,01 à 10 W/cm3.
  5. Procédé selon la revendication 4, caractérisé par le fait que la fraction de matière produite par fittage-réaction, en particulier le WC, est comprise entre 1 % et 100 %, les fractions restantes ont été ajoutées dans la forme chimique dans laquelle elles existent plus tard dans le corps fritté fini.
  6. Procédé selon l'une des revendications 4 ou 5, caractérisé par le fait que la croissance des platelets de WC est commandée par la part du frittage-réaction à micro-ondes par rapport à l'ensemble du processus de frittage à micro-ondes.
  7. Procédé selon l'une des revendications 4 à 6, caractérisé par le fait que l'on ajoute au mélange de départ des inhibiteurs de croissance de grains, de préférence jusqu'à 12 %, en outre de préférence jusqu'à 8 % de VC et/ou de Cr3C2.
EP98919052A 1997-03-10 1998-03-06 Corps fritte en metal dur ou cermet et son procede de production Expired - Lifetime EP0966550B1 (fr)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
DE19709527 1997-03-10
DE19709527 1997-03-10
DE19725914 1997-06-19
DE19725914A DE19725914A1 (de) 1997-03-10 1997-06-19 Hartmetall- oder Cermet-Sinterkörper und Verfahren zu dessen Herstellung
PCT/DE1998/000674 WO1998040525A1 (fr) 1997-03-10 1998-03-06 Corps fritte en metal dur ou cermet et son procede de production

Publications (2)

Publication Number Publication Date
EP0966550A1 EP0966550A1 (fr) 1999-12-29
EP0966550B1 true EP0966550B1 (fr) 2001-10-04

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EP98919052A Expired - Lifetime EP0966550B1 (fr) 1997-03-10 1998-03-06 Corps fritte en metal dur ou cermet et son procede de production

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US (1) US6293986B1 (fr)
EP (1) EP0966550B1 (fr)
AT (1) ATE206481T1 (fr)
WO (1) WO1998040525A1 (fr)

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WO1998040525A1 (fr) 1998-09-17
ATE206481T1 (de) 2001-10-15
EP0966550A1 (fr) 1999-12-29

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