EP1574593A1 - cold working of molyddenum by indirect extrusion - Google Patents

cold working of molyddenum by indirect extrusion Download PDF

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Publication number
EP1574593A1
EP1574593A1 EP04021093A EP04021093A EP1574593A1 EP 1574593 A1 EP1574593 A1 EP 1574593A1 EP 04021093 A EP04021093 A EP 04021093A EP 04021093 A EP04021093 A EP 04021093A EP 1574593 A1 EP1574593 A1 EP 1574593A1
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EP
European Patent Office
Prior art keywords
molybdenum
recrystallization
workpiece
carried out
recrystallized
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.)
Granted
Application number
EP04021093A
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German (de)
French (fr)
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EP1574593B1 (en
Inventor
Bernd Spaniol
Wolfgang Günther
Josef Trageser
Jörg Schielke
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WC Heraus GmbH and Co KG
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WC Heraus GmbH and Co KG
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00—Extruding metal; Impact extrusion
    • B21C23/002—Extruding materials of special alloys so far as the composition of the alloy requires or permits special extruding methods of sequences
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00—Extruding metal; Impact extrusion
    • B21C23/02—Making uncoated products
    • B21C23/18—Making uncoated products by impact extrusion
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/02—Manufacture of electrodes or electrode systems
    • H01J9/022—Manufacture of electrodes or electrode systems of cold cathodes

Definitions

  • the present invention relates to the cold working of molybdenum by reverse extrusion.
  • Molybdenum is used in lighting because of its thermal, electrical and chemical properties. It is a brittle material at room temperature, and precursors and semi-finished products are usually hot-formed. Molybdenum molded parts such as pipes or caps for the lighting technology can by deep drawing. 1 made of sheets and strips at room temperature.
  • Fig. 1 shows the longitudinal section of a produced by the process according to the invention Molybdenum coping in the scale 50: 1.
  • Such caps can be used as emitter electrodes in CCFL lamps.
  • the material used is converted to 100% waste-free.
  • the microscopic longitudinal section through a cap produced according to this method in FIG. 1 shows that crack-free rotationally symmetrical molded parts can be produced in this way.

Abstract

Process for cold deforming molybdenum comprises completely recrystallizing the molybdenum before deforming.

Description

Die vorliegende Erfindung betrifft die Kaltverformung von Molybdän durch Rückwärts-Fließpressen.The present invention relates to the cold working of molybdenum by reverse extrusion.

Molybdän kommt in der Lichttechnik wegen seiner thermischen, elektrischen und chemischen Eigenschaften zum Einsatz. Es ist ein bei Raumtemperatur spröder Werkstoff, und Vorprodukte und Halbzeuge werden üblicherweise heiß umgeformt. Molybdän-Formteile wie etwa Rohre oder Kappen für die Lichttechnik können durch Tiefziehen1 aus Blechen und Bändern bei Raumtemperatur hergestellt werden.Molybdenum is used in lighting because of its thermal, electrical and chemical properties. It is a brittle material at room temperature, and precursors and semi-finished products are usually hot-formed. Molybdenum molded parts such as pipes or caps for the lighting technology can by deep drawing. 1 made of sheets and strips at room temperature.

Die Umformung von Vorprodukten und Halbzeugen geschieht gewöhnlich in der Hitze, also zweckmäßig unmittelbar nach dem Sintern (US 5,158,709) - oder bei elektronenstrahler-schmolzenem Molybdän nach dem Heißschmieden - oder durch thermomechanisches Umformen (US 5,051,139). Es gibt auch kalte Umformungsverfahren, bevorzugt bei dünnen Abmessungen, wobei das Molybdän allerdings nicht vollständig rekristallisiert wird, damit es nicht zu Rissen oder Brüchen bei der Bearbeitung unter Zugspannung kommt. Die gängige Lehrmeinung lautet, daß das Material nicht vollständig rekristallisiert werden darf, da im rekristallisierten weichgeglühten Zustand die zur Umformung notwendigen Zugspannungen dann zur Zerstörung (Einschnürung, Risse) des Materials führen würden.The transformation of precursors and semi-finished products usually happens in the heat, so expediently immediately after sintering (US Pat. No. 5,158,709) - or in the case of electron-beam molten metal Molybdenum after hot forging - or by thermomechanical forming (US 5,051,139). There are also cold forming processes, preferably with thin dimensions, however, the molybdenum is not fully recrystallized to prevent it from Cracks or breaks in the processing under tension comes. The common doctrine is that the material may not be fully recrystallized, as in the recrystallized soft annealed condition the tensile stresses necessary for forming then destroying (Constriction, cracks) of the material would result.

Ferner sind Verfahren bekannt, bei denen sich Verformung, Rekristallisation und Tempern abwechseln (z.B. US 4,600,446).Furthermore, methods are known in which alternate deformation, recrystallization and annealing (e.g., U.S. 4,600,446).

Ein Verfahren zur Kaltverformung spröder, rekristallisierter bzw. entspannter Materialien - darunter Mo - durch Extrusion ist in US3552996 beansprucht worden. Diese Methode ist auch als Vorwärts-Fließpressen2 bekannt. Das Hauptaugenmerk liegt bei dem in US3552996 beschriebenen Verfahren auf der Vermeidung einer schroffen Abrißkante an der Fließpreßmatrize. Dadurch soll ein sprunghafter Spannungsübergang nach der Umformung verhindert werden. Allerdings ist das vorgestellte Verfahren nur für TZM Legierungen praktisch belegt, und es lassen sich damit allenfalls teilweise rißfreie Formkörper erzeugen (vgl. Beispiele).A process for cold working brittle, recrystallized or relaxed materials, including Mo by extrusion, has been claimed in US3552996. This method is also called forward extrusion 2 known. In the process described in US Pat. No. 3,552,996, the main focus is on avoiding a rugged tear-off edge on the extrusion die. This is intended to prevent a sudden voltage transition after forming. However, the process presented is only practically proven for TZM alloys, and it is thus possible to produce at most partially crack-free shaped bodies (see examples).

Im vorliegenden wird nun ein Verfahren zur Kaltverformung von Molybdän durch Rückwärts-Fließpressen beschrieben. Es wurde gefunden, daß sich Molybdän überraschenderweise trotz seiner Sprödigkeit durch Rückwärts-Fließpressen verformen läßt, ohne daß Risse oder Brüche entstehen. Beim Fließpressen wird die Energie durch Druckspannung aufgebracht. Das Molybdän wird vorher durch eine Wärmebehandlung vollständig rekristallisiert, um mit ausreichend geringer Spannung die Fließgrenze des Materials zu überschreiten. Bei der Rekristallisation sollen sämtliche Gitterspannungen beseitigt werden, die vorher durch Verformen entstanden waren. Das Material erreicht dann bei relativ geringen Kräften seine Fließgrenze. Die Rekristallisation erfolgt vorteilhaft bei Temperaturen oberhalb 1300°C, besonders über 1400°C (der Schmelzpunkt von Mo liegt bei 2623-5°C).In the present, a method for cold deformation of molybdenum by backward extrusion is now described. It was found that molybdenum surprisingly despite its brittleness can be deformed by backward extrusion without cracks or breaks arise. During extrusion, the energy is applied by compressive stress. The molybdenum is completely recrystallized beforehand by a heat treatment to be sufficient low stress exceeds the yield strength of the material. In the recrystallization should all grid voltages are eliminated, which previously arose by deformation were. The material then reaches its yield point at relatively low forces. The recrystallization takes place advantageously at temperatures above 1300 ° C, especially above 1400 ° C (the Melting point of Mo is 2623-5 ° C).

Die Erfindung betrifft somit ein Verfahren zur Kaltverformung von Molybdän durch Rückwärts-Fließpressen, wobei vorher eine vollständige Rekristallisation durchgeführt wird. Das Verfahren wird vorteilhaft folgendermaßen durchgeführt:

  • Ein Molybdän-Draht im Durchmesserbereich des späteren Fertigproduktes wird unter Vakuum oder Schutzgas bei Temperaturen oberhalb 1400°C vollständig rekristallisiert und unter Vakuum oder Schutzgas abgekühlt. Abschnitte aus dem so rekristallisierten Material werden bei Raumtemperatur zu rotationssymmetrischen Fertigteilen fließgepresst.
  • Die wesentlichen Vorteile des Verfahrens sind: Zum einen kann das Material wesentlich besser genutzt werden als beim Tiefziehen. Weiter können Teile mit dickeren oder geformten Böden durch Rückwärts-Fließpressen hergestellt werden. Das Verfahren eignet sich auch für andere spröde Metalle oder deren Legierungen, z.B. für Chrom oder Wolfram.
  • Industriell kann das Verfahren z.B. zur Herstellung von Mo-Kappen für die Lichttechnik angewandt werden. So hergestellte Teile können als Stromdurchführung durch Glas oder Keramik-Kolben und als Emitter-Elektroden bei CCFL Lampen (Cold Cathode Fluorescent Lighting) bzw. Kaltkathodenlampen (KKL)3 eingesetzt werden.
  • Das folgende Ausführungsbeispiel erläutert die Erfindung näher, ohne sie zu beschränken.
    • The invention thus relates to a process for the cold deformation of molybdenum by reverse extrusion, wherein previously a complete recrystallization is carried out. The method is advantageously carried out as follows:
  • A molybdenum wire in the diameter range of the later finished product is completely recrystallized under vacuum or inert gas at temperatures above 1400 ° C and cooled under vacuum or inert gas. Sections of the thus recrystallized material are extruded at room temperature into rotationally symmetric finished parts.
  • The main advantages of the process are: On the one hand, the material can be used much better than in deep drawing. Further, parts with thicker or shaped bottoms can be made by backward extrusion. The method is also suitable for other brittle metals or their alloys, for example for chromium or tungsten.
  • Industrially, the method can be used for example for the production of Mo-caps for lighting technology. Pieces produced in this way can be used as current feedthrough through glass or ceramic bulbs and as emitter electrodes in CCFL lamps (Cold Cathode Fluorescent Lighting) or Cold Cathode Lamps (CCL) 3 be used.
  • The following embodiment explains the invention in more detail without limiting it.

    • Beschreibung der ZeichnungenDescription of the drawings

    Fig. 1 zeigt den Längsschliff eines nach dem erfindungsgemäßen Verfahren hergestellten Molybdän-Käppchens im Maßstab 50:1.Fig. 1 shows the longitudinal section of a produced by the process according to the invention Molybdenum coping in the scale 50: 1.

    Beispiel:Example:

    Aus einem bei > 1400°C unter Vakuum rekristallisierten und unter Vakuum abgekühlten 1 mm Mo-Drahtabschnitt wird unter einem Druck von ca. 1500 MPa bei Raumtemperatur auf einer Presse ein geformtes Käppchen rückwärts fließgepreßt.From a recrystallized at> 1400 ° C under vacuum and cooled under vacuum 1 mm Mo wire section is placed under a pressure of about 1500 MPa at room temperature on a Press a molded coping backwards.

    Solche Kappen können als Emitter-Elektroden in CCFL Lampen eingesetzt werden.Such caps can be used as emitter electrodes in CCFL lamps.

    Nach dem beschriebenen Verfahren wird der eingesetzte Werkstoff zu 100% abfallfrei umgeformt.According to the described method, the material used is converted to 100% waste-free.

    Der mikroskopische Längsschliff durch eine nach diesem Verfahren hergestellte Kappe in Fig. 1 zeigt, daß auf diesem Weg rißfreie rotationssymmetrische Formteile hergestellt werden können.The microscopic longitudinal section through a cap produced according to this method in FIG. 1 shows that crack-free rotationally symmetrical molded parts can be produced in this way.

    Claims (7)

    Verfahren zur Kaltverformung von Molybdän durch Rückwärts-Fließpressen, dadurch gekennzeichnet, daß vor der Kaltverformung eine vollständige Rekristallisation durchgeführt wird.Process for the cold deformation of molybdenum by backward extrusion, characterized in that a complete recrystallization is carried out before cold working. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die Rekristallisation unter Schutzgas und/oder Vakuum durchgeführt wird.A method according to claim 1, characterized in that the recrystallization is carried out under protective gas and / or vacuum. Verfahren nach einem der vorstehenden Ansprüche, dadurch gekennzeichnet, daß die Rekristallisation bei Temperaturen oberhalb 1300°C durchgeführt wird.Process according to one of the preceding claims, characterized in that the recrystallization is carried out at temperatures above 1300 ° C. Verfahren nach mindestens einem der vorstehenden Ansprüche, dadurch gekennzeichnet, daß A) ein Molybdän-Werkstück unter Vakuum und/oder Schutzgas bei Temperaturen oberhalb 1400°C vollständig rekristallisiert wird, B) das Werkstück unter Vakuum und/oder Schutzgas abgekühlt wird, C) Abschnitte aus dem so rekristallisierten Werkstück bei Raumtemperatur zu Fertigteilen fließgepreßt werden. Method according to at least one of the preceding claims, characterized in that A) a molybdenum workpiece is fully recrystallized under vacuum and / or inert gas at temperatures above 1400 ° C, B) the workpiece is cooled under vacuum and / or inert gas, C) sections of the so recrystallized workpiece are extruded at room temperature to finished parts. Verfahren nach Anspruch 4, bei dem die Fertigteile rotationssymmetrisch gepreßt werden. A method according to claim 4, wherein the finished parts are pressed rotationally symmetrical. Verwendung von nach einem der Ansprüche 1 bis 5 fließgepreßten Molybdän-Formteilen in der Lichttechnik.Use of molybdenum molded parts extruded according to any one of claims 1 to 5 the lighting technology. Verwendung nach Anspruch 6 zur Herstellung von Stromdurchführungen durch Glas- oder Keramik-Kolben oder zur Herstellung von Emitter-Elektroden in CCFL- bzw. Kaltkathodenlampen.Use according to claim 6 for the production of current feedthroughs through glass or Ceramic pistons or for the production of emitter electrodes in CCFL or cold cathode lamps.
    EP04021093A 2003-10-02 2004-09-04 cold working of molyddenum by indirect extrusion Not-in-force EP1574593B1 (en)

    Applications Claiming Priority (2)

    Application Number Priority Date Filing Date Title
    DE10346464A DE10346464B4 (en) 2003-10-02 2003-10-02 Method of cold forming molybdenum by reverse extrusion and use of molybdenum back molded extruded parts
    DE10346464 2003-10-02

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    Publication Number Publication Date
    EP1574593A1 true EP1574593A1 (en) 2005-09-14
    EP1574593B1 EP1574593B1 (en) 2008-10-29

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    EP (1) EP1574593B1 (en)
    JP (1) JP4348266B2 (en)
    KR (1) KR100771731B1 (en)
    CN (1) CN100335671C (en)
    AT (1) ATE412786T1 (en)
    DE (2) DE10346464B4 (en)
    TW (1) TWI283609B (en)

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    CN113732219B (en) * 2021-08-12 2023-10-13 宁波复能稀土新材料股份有限公司 Vacuum hot extrusion forming device for rare earth terbium target

    Citations (5)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    US3553996A (en) * 1967-11-13 1971-01-12 Battelle Development Corp Extrusion of brittle materials
    US4462234A (en) * 1980-06-19 1984-07-31 Battelle Development Corporation Rapid extrusion of hot-short-sensitive alloys
    US4600446A (en) * 1983-10-08 1986-07-15 Agency Of Industrial Science & Technology Method for tempering and working high strength low ductile alloy
    US5051139A (en) * 1989-05-03 1991-09-24 Schwarzkopf Development Corporation Process for the manufacture of semi-finished products or preformed parts made of refractory metals and resistant to thermal creep
    US5158709A (en) * 1990-02-01 1992-10-27 Patent Treuhand Gesellschaft Fur Elektrische Gluhlampen Mbh Electric lamp containing molybdenum material doped wtih aluminum and potassium, molybdenum material for such a lamp, and method of its manufacture

    Family Cites Families (4)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    JPS5731408A (en) * 1980-06-19 1982-02-19 Battelle Development Corp Double extruding die and its extruding method
    JPS6075545A (en) * 1983-09-29 1985-04-27 Toshiba Corp Dies and their manufacture
    EP0694084B1 (en) * 1993-04-15 2001-09-19 Luxfer Group Limited Method of making hollow bodies
    JP3079378B1 (en) * 1999-02-10 2000-08-21 東京タングステン株式会社 Mo sputtering target material and method of manufacturing the same

    Patent Citations (5)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    US3553996A (en) * 1967-11-13 1971-01-12 Battelle Development Corp Extrusion of brittle materials
    US4462234A (en) * 1980-06-19 1984-07-31 Battelle Development Corporation Rapid extrusion of hot-short-sensitive alloys
    US4600446A (en) * 1983-10-08 1986-07-15 Agency Of Industrial Science & Technology Method for tempering and working high strength low ductile alloy
    US5051139A (en) * 1989-05-03 1991-09-24 Schwarzkopf Development Corporation Process for the manufacture of semi-finished products or preformed parts made of refractory metals and resistant to thermal creep
    US5158709A (en) * 1990-02-01 1992-10-27 Patent Treuhand Gesellschaft Fur Elektrische Gluhlampen Mbh Electric lamp containing molybdenum material doped wtih aluminum and potassium, molybdenum material for such a lamp, and method of its manufacture

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    Publication number Publication date
    DE502004008340D1 (en) 2008-12-11
    DE10346464A1 (en) 2005-05-04
    CN1611629A (en) 2005-05-04
    TWI283609B (en) 2007-07-11
    ATE412786T1 (en) 2008-11-15
    JP4348266B2 (en) 2009-10-21
    KR20050033001A (en) 2005-04-08
    CN100335671C (en) 2007-09-05
    TW200526336A (en) 2005-08-16
    EP1574593B1 (en) 2008-10-29
    JP2005111562A (en) 2005-04-28
    KR100771731B1 (en) 2007-10-30
    DE10346464B4 (en) 2006-04-27

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