EP0396185B1 - Procédé pour la préparation d'outils semi-finis résistant au fluage en métal réfractaire - Google Patents

Procédé pour la préparation d'outils semi-finis résistant au fluage en métal réfractaire Download PDF

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Publication number
EP0396185B1
EP0396185B1 EP90201056A EP90201056A EP0396185B1 EP 0396185 B1 EP0396185 B1 EP 0396185B1 EP 90201056 A EP90201056 A EP 90201056A EP 90201056 A EP90201056 A EP 90201056A EP 0396185 B1 EP0396185 B1 EP 0396185B1
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EP
European Patent Office
Prior art keywords
hot
forming
finished products
producing semi
alloys
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
EP90201056A
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German (de)
English (en)
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EP0396185A1 (fr
Inventor
Ralf Dr. Eck
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.)
Metallwerk Plansee GmbH
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Metallwerk Plansee GmbH
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Publication of EP0396185A1 publication Critical patent/EP0396185A1/fr
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Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • 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
    • C22C1/10—Alloys containing non-metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0031—Matrix based on refractory metals, W, Mo, Nb, Hf, Ta, Zr, Ti, V or alloys thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon

Definitions

  • the invention relates to a process for the production of semi-finished products or molded parts of high creep resistance from sintered or melted precursors from alloys of the high-melting metals vanadium, niobium, tantalum, chromium, molybdenum, tungsten, which are solidified by dispersoidal inclusions of oxides, carbides, silicides, borides and / or nitrides , individually, in groups or as a main component with other metal components.
  • hot forming results in the best possible hot creep strength values in immediately successive, as large as possible forming steps up to very high degrees of deformation of 90% and more. They are like this Formed materials undergo a final recrystallization annealing in order to form a stack structure that is as pronounced as possible. These processes with a large number of forming steps and annealing are very lengthy and expensive, but according to the prevailing teaching opinion, they are essential to achieve the highest hot creep strength.
  • the hot forming to 60-80% forming takes place in a single operation, if necessary with intermediate heating of the workpiece, if, for example, the forming process to the desired degree of deformation or to the desired workpiece shape cannot be carried out quickly enough and without excessive cooling.
  • the heat resistance values of alloys manufactured in this way are significantly lower than the values when a stacked structure is formed.
  • the method is nevertheless said to provide higher heat resistance values, in particular higher heat creep resistance, even at temperature values around and above three quarters of the melting temperature of the main constituent of the alloy, than known materials.
  • the object is achieved by a method according to the present invention, in which sintered or melted preliminary products from the materials mentioned at the outset are processed into semi-finished products, in that the preliminary products are subsequently subjected to two to four times at hot forming temperatures in the range of 900 ° C. which are customary for the respective metallic main component and 1600 ° C by 3 - 25%, but a total of a maximum of 75% thermomechanically and by intermediate annealing between the individual forming steps at temperatures ranging from about the respective hot forming temperature to the respective recrystallization temperature for 1 and 6 hours.
  • semi-finished products are, for. B. to understand forged blanks, rods, circular blanks, sheets and wires.
  • molded parts are parts that are produced from semi-finished products by shaping processes such as machining, but without further influencing the metallic structure and the metallic properties; also those parts that are processed from pre-products in the course of hot forming into ready-to-use molded parts.
  • the most important alloy elements in question in addition to the main constituents mentioned are the metals of subgroup 4 of the periodic table, but also other elements already used in alloys of the refractory metals, in particular rhenium and platinum.
  • the oxides, and especially the rare earths cerium oxide, yttrium oxide, lanthanum oxide, in addition to thorium oxide, manganese oxide, titanium oxide and zirconium oxide have proven particularly effective.
  • carbides, silicides, borides and nitrides are successfully used as dispersoids in high-melting metals.
  • Alkaline earth metals, aluminum and silicon are hardly used in the present case because of their known disadvantages at very high material temperatures, but cannot be completely ruled out.
  • customary hot-forming temperatures is to be understood as the temperatures which are advantageously to be used in hot-forming by forging and / or hammering for the respective high-melting metal.
  • the most favorable temperature for the comparatively low-melting chromium is of course significantly lower than for tungsten, but in any case below the temperature at which recrystallization begins.
  • the degrees of deformation to be used per forming step are to be limited to the area of critical forming, ie to the area in which grain growth occurs due to subsequent temperature treatment. Extrusion and drawing can be mentioned as further applicable hot forming processes.
  • An important advantage of the high-melting alloys produced by the inventive method is the high hot creep resistance values, even in temperature ranges which are around three quarters of the respective melting temperature, where others Process creep-resistant alloys already drop sharply in the corresponding values.
  • Another advantage of the method is that in addition to the heat creep resistance, the other heat resistance values, namely tensile strength with sufficient residual elongation, are comparatively favorable.
  • Dispersion-strengthened alloys according to the present invention are preferably used as molding tools in forging or pressing tools for the high-temperature shaping of metallic moldings, in particular in isothermal high-temperature forging.
  • Another area of application is rotating anodes for X-ray tubes.
  • the ZHM-molybdenum alloy used for comparison was brought to the same overall degree of deformation of approximately 70%, but in a single step, without intermediate annealing after small degrees of deformation according to the invention.
  • the TZM-molybdenum alloy which had long been the leader in terms of high creep resistance, could no longer be cited for comparison, since a corresponding sample under the load values mentioned would crack in less than a minute.
  • Molybdenum metal powder with a grain size of approx. 5 ⁇ m was mixed with fine-grained powder additives, namely with 1.2% by weight Hf, 0.4% by weight Zr, 0.15% by weight C and 1.0% by weight CeO2 with a grain size of approx. 0.8 ⁇ m mixed, the mixture filled in a rubber tube, shaken tightly and cold isostatically pressed with a pressure of 2500 bar under water.
  • the isostatically pressed rod was turned green to a diameter of 75 mm on a lathe and then cut to a height of 55 mm.
  • the cylinders were sintered in a dry H2 atmosphere (TP ⁇ - 35 ° C) for 5 hours at 2000 ° C.
  • the sintered density was 9.50 g / cm3.
  • the forming process involved heating the sintered body to 1200 ° C in an H2-flooded furnace for 20 minutes, further compressing it to a height of 43 mm, the two-period annealing first at 2000 ° C for 1 hour and then at 1500 ° C for 1 hour. This is followed by heating in the forging furnace to 1200 ° C for 20 minutes and forging at approx. 10 degrees of deformation to a height of 39 mm.
  • Annealing and forging are repeated two more times: annealing at 2000 ° C, 1 hour and 1500 ° C, 1 hour, placing in the forging furnace, forging at a height of 35 mm, annealing at 2000 ° C, 1 hour and 1500 ° C 1 Hour, heating to 1200 ° C for 20 minutes and finish forging to a height of 12 mm.
  • Example 1 The process according to Example 1 is repeated with the following alloy composition: Mo - 1.2% by weight Hf, 0.4% by weight Zr, 0.15% by weight C and, deviating from above, 1% by weight Y2O3 with a grain size of 0.25 ⁇ m.
  • Tungsten metal powder which was obtained by H2 reduction of blue tungsten oxide and had a grain size of 3.80 ⁇ m, was with 1.20 wt.% Hf, 0.40 wt.% Zr, 0.10 wt.% C and with 1 wt.% CeO2 of grain size 0.8 microns, mixed in a compulsory mixer and pressed in a die pressing tool with a diameter of 105 mm to a height of 55 mm.
  • the blanks were sintered for 7 hours at 2500 ° C in dry H2 with a dew point of -35 ° C and reached a density of 17.7 g / cm3. After sintering, the dimensions of the blanks were approximately 90 mm in diameter x 48 mm in height.
  • the blanks were first warmed at 1550 ° C. for 20 minutes and then upset to a height of 43 mm by hot forging. There followed an intermediate annealing of the blanks for 2 hours at 1550 ° C in an H2 atmosphere. The blanks were then again heated at 1550 ° C. for 20 minutes and deformed at this temperature in a second forging pass by approx. 10% to a height of 39 mm. The subsequent annealing was again carried out at 1550 ° C for 2 hours in an H2 atmosphere. For the third pass, heating was again carried out at 1550 ° C. for 20 minutes and then forging to a height of 35 mm. Finally, the round blanks were annealed for a fourth time for 2 hours at 1550 ° C. and after a final warming over 20 minutes at 1550 ° C. at 17 mm height, they were forged and cooled from the forging heat in the furnace to room temperature overnight.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Forging (AREA)
  • Powder Metallurgy (AREA)

Claims (9)

  1. Procédé de fabrication de semi-produits ou de pièces de formes à haute résistance au fluage à chaud à partir d'ébauches frittées ou élaborées en alliages des métaux à haut point de fusion : vanadium, niobium, tantale, chrome, molybdène, tungstène, seul ou à plusieurs ou en tant que composant principal avec d'autres composants métalliques, alliages qui sont consolidés par des inclusions de matières dispersées d'oxydes, de carbures, de siliciures, de borures et/ou de nitrures
       caractérisé en ce que,
       les ébauches sont déformées deux à quatre fois de manière thermodynamique, chaque fois de 3 à 25 % mais au maximum de 75 % au total, aux températures habituelles de déformation à chaud du composant métallique principal correspondant dans la zone de 900° à 1600 °C, et dans lequel les ébauches sont recuites de façon intermédiaire pendant 1 à 6 heures entre les étapes individuelles de déformation à des températures situées dans la zone comprise entre la température respective de déformation à chaud et la température respective de recristallisation.
  2. Procédé de fabrication de semi-produits selon la revendication 1, caractérisé en ce que certains des recuits intermédiaires, ou tous ceux-ci, sont respectivement réalisés en deux étapes partielles, la première étape partielle s'effectuant pendant à peu près la moitié du temps de recuit intermédiaire à des températures supérieures à la température de recristallisation, c'est-à-dire à 1300 à 2100°C, et la deuxième étape intermédiaire s'effectuant pendant à peu près la moitié du temps utilisé après le processus de base à la température de déformation à chaud choisie.
  3. Procédé de fabrication de semi-produits selon la revendication 1 ou 2, caractérisé en ce que la déformation à chaud s'effectue par forgeage à chaud.
  4. Procédé de fabrication de semi-produits selon l'une des revendications 1 à 3, caractérisé en ce que l'on soumet au traitement des alliages qui contiennent des matières dispersées à base d'oxydes et/ou de carbures.
  5. Procédé de fabrication de semi-produits selon la revendication 4, caractérisé en ce que l'on utilise, comme matières dispersées, CeO₂, Y₂O₃, La₂O₃ et/ou ThO₂.
  6. Procédé de fabrication de semi-produits selon l'une des revendications 1 à 5, caractérisé en ce que l'on utilise, comme métal à haut point de fusion, un alliage de molybdène contenant des additions de zirconium et de hafnium et, comme matières dispersées finement divisées, des oxydes et des carbures.
  7. Procédé de fabrication de semi-produits selon la revendication 6, caractérisé en ce que la déformation à chaud s'effectue à des températures comprises entre 1250°C et 1350°C.
  8. Utilisation d'alliages consolidés par dispersion, fabriqués selon l'une des revendications 1 à 7, dans des outils de forgeage ou de compression destinés à la déformation à haute température de pièces de formes métalliques.
  9. Utilisation d'alliages consolidés par dispersion, fabriqués selon l'une des revendications 1 à 7, dans des anodes tournantes pour tubes de rayons X.
EP90201056A 1989-05-03 1990-04-26 Procédé pour la préparation d'outils semi-finis résistant au fluage en métal réfractaire Expired - Lifetime EP0396185B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AT1059/89A AT392432B (de) 1989-05-03 1989-05-03 Verfahren zur herstellung von warmkriechfesten halbfabrikaten oder formteilen aus hochschmelzenden metallen
AT1059/89 1989-05-03

Publications (2)

Publication Number Publication Date
EP0396185A1 EP0396185A1 (fr) 1990-11-07
EP0396185B1 true EP0396185B1 (fr) 1993-07-21

Family

ID=3505696

Family Applications (1)

Application Number Title Priority Date Filing Date
EP90201056A Expired - Lifetime EP0396185B1 (fr) 1989-05-03 1990-04-26 Procédé pour la préparation d'outils semi-finis résistant au fluage en métal réfractaire

Country Status (5)

Country Link
US (1) US5051139A (fr)
EP (1) EP0396185B1 (fr)
JP (1) JPH02301545A (fr)
AT (1) AT392432B (fr)
DE (1) DE59002005D1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004010600A1 (de) * 2004-03-02 2005-09-29 Thyssenkrupp Vdm Gmbh Verfahren zur Primäroxidhärtung von Metallschmelzen
DE102005033799B4 (de) * 2005-01-31 2010-01-07 Medicoat Ag Verfahren zur Herstellung eines Drehanodentellers für Röntgenröhren

Families Citing this family (11)

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Publication number Priority date Publication date Assignee Title
US5868876A (en) * 1996-05-17 1999-02-09 The United States Of America As Represented By The United States Department Of Energy High-strength, creep-resistant molybdenum alloy and process for producing the same
AT2017U1 (de) * 1997-05-09 1998-03-25 Plansee Ag Verwendung einer molybdän-/wolfram-legierung in bauteilen für glasschmelzen
US6102979A (en) * 1998-08-28 2000-08-15 The United States Of America As Represented By The United States Department Of Energy Oxide strengthened molybdenum-rhenium alloy
US6478845B1 (en) * 2001-07-09 2002-11-12 Osram Sylvania Inc. Boron addition for making potassium-doped tungsten
JP2003293070A (ja) * 2002-03-29 2003-10-15 Japan Science & Technology Corp 高強度・高靭性Ｍｏ合金加工材とその製造方法
US6830637B2 (en) * 2002-05-31 2004-12-14 Osram Sylvania Inc. Large diameter tungsten-lanthana rod
DE60312012T2 (de) * 2002-09-04 2007-08-09 Osram Sylvania Inc., Danvers Verfahren zur herstellung von sag-beständigen molybdän-lanthanoxid-legierungen
WO2004069453A2 (fr) * 2003-01-31 2004-08-19 H.C. Starck, Inc. Bandes de recuit en métal réfractaire
DE10346464B4 (de) * 2003-10-02 2006-04-27 W.C. Heraeus Gmbh Verfahren zur Kaltumformung von Molybdän durch Rückwärts-Fließpressen und Verwendung von rückwärts-fließgepressten Molybdän-Formteilen
US20080300552A1 (en) * 2007-06-01 2008-12-04 Cichocki Frank R Thermal forming of refractory alloy surgical needles
CN114574822B (zh) * 2022-03-02 2024-01-30 基迈克材料科技（苏州）有限公司 一种银合金靶材制备工艺及应用

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004010600A1 (de) * 2004-03-02 2005-09-29 Thyssenkrupp Vdm Gmbh Verfahren zur Primäroxidhärtung von Metallschmelzen
DE102004010600B4 (de) * 2004-03-02 2008-07-03 Thyssenkrupp Vdm Gmbh Verfahren zur Primäroxidhärtung von Metallschmelzen
DE102005033799B4 (de) * 2005-01-31 2010-01-07 Medicoat Ag Verfahren zur Herstellung eines Drehanodentellers für Röntgenröhren

Also Published As

Publication number Publication date
EP0396185A1 (fr) 1990-11-07
DE59002005D1 (de) 1993-08-26
AT392432B (de) 1991-03-25
ATA105989A (de) 1990-09-15
US5051139A (en) 1991-09-24
JPH02301545A (ja) 1990-12-13

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