EP1574593B1 - cold working of molyddenum by indirect extrusion - Google Patents

cold working of molyddenum by indirect extrusion Download PDF

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Publication number
EP1574593B1
EP1574593B1 EP04021093A EP04021093A EP1574593B1 EP 1574593 B1 EP1574593 B1 EP 1574593B1 EP 04021093 A EP04021093 A EP 04021093A EP 04021093 A EP04021093 A EP 04021093A EP 1574593 B1 EP1574593 B1 EP 1574593B1
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Prior art keywords
molybdenum
cold
carried out
workpiece
inert gas
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EP04021093A
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German (de)
French (fr)
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EP1574593A1 (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 tubes or caps for the lighting technology can be made by deep drawing 1 of sheets and strips at room temperature.
  • Deep drawing refers to the tensile pressure forming of sheets into a hollow body or the formation of a hollow body with a smaller circumference from a hollow body of larger circumference. The sheet thickness is not deliberately changed.
  • the cut sheet is placed in the receptacle. A hold-down presses the sheet on the drawing die and prevents wrinkling during deep drawing. The dropping punch pushes the sheet into the drawing die and thus shapes it to the desired workpiece.
  • the draw ratio is the ratio of the diameter of the cut sheet to the diameter of the workpiece. Between the deep drawing steps, an intermediate annealing can take place.
  • the compact starting material is either pressed with a punch through a die ( forward ) similar to the extruding or the punch is pressed into the starting material and the material flows backwards along the punch.
  • the differences from extrusion are in the processing temperature and in that by extruding no semi-finished product strands, but individual parts are produced, which are also complex shapes to produce.
  • Advantages of the method are low tool costs, high tool life and a high operating speed with cycle numbers of about 30-150 pieces / min.
  • the surface quality is good and suitable for further surface treatments.
  • the main field of application is aluminum alloys.
  • Fig. 1 shows the longitudinal section of a molybdenum coping produced by the process according to the invention 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 by this method in Fig. 1 shows that crack-free rotationally symmetrical molded parts can be produced in this way.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Thermal Sciences (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Forging (AREA)
  • Extrusion Of Metal (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Vessels And Coating Films For Discharge Lamps (AREA)
  • Discharge Lamp (AREA)

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.
1 Mit Tiefziehen bezeichnet man das Zugdruckumformen von Blechen zu einem Hohlkörper oder die Formung eines Hohlkörpers mit kleinerem Umfang aus einem Hohlkörper größeren Umfangs. Dabei wird die Blechdicke nicht absichtlich verändert. Das zugeschnittene Blech wird in die Aufnahme gelegt. Ein Niederhalter drückt das Blech auf die Ziehmatrize und verhindert während des Tiefziehens damit eine Faltenbildung. Der niedergehende Ziehstempel drückt das Blech in die Ziehmatrize und formt es damit zu dem gewünschten Werkstück. Bei hohen Ziehverhältnissen kann das Tiefziehen in mehreren Schritten durchgeführt werden. Unter Ziehverhältnis versteht man das Verhältnis von Durchmesser des zugeschnittenen Bleches zum Durchmesser des Werkstücks. Zwischen den Tiefziehschritten kann eine Zwischenglühung erfolgen.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 tubes or caps for the lighting technology can be made by deep drawing 1 of sheets and strips at room temperature.
1 Deep drawing refers to the tensile pressure forming of sheets into a hollow body or the formation of a hollow body with a smaller circumference from a hollow body of larger circumference. The sheet thickness is not deliberately changed. The cut sheet is placed in the receptacle. A hold-down presses the sheet on the drawing die and prevents wrinkling during deep drawing. The dropping punch pushes the sheet into the drawing die and thus shapes it to the desired workpiece. At high draw ratios deep drawing can be carried out in several steps. The draw ratio is the ratio of the diameter of the cut sheet to the diameter of the workpiece. Between the deep drawing steps, an intermediate annealing can take place.

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 takes place in the heat, that is expediently immediately after sintering ( US 5,158,709 ) - or with electron beam-molten Molybdenum after hot forging - or by thermomechanical forming ( US 5,051,139 ). There are also cold forming processes, preferably with thin dimensions, but the molybdenum is not fully recrystallized so as not to crack or fracture during machining under tension. The common doctrine is that the material may not be fully recrystallized, since in the recrystallized soft annealed condition, the tensile stresses necessary for forming would then lead to the destruction (constriction, cracks) of the material.

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 (eg US 4,600,446 ).

Ein Verfahren zur Kaltverformung spröder, rekristallisierter bzw. entspannter Materialien - darunter Mo - durch Extrusion ist in US 3553996 beansprucht worden. Diese Methode ist auch als Vorwärts-Fließpressen2 bekannt. Das Hauptaugenmerk liegt bei dem in US 3553996 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).
2 Fließpressen ist ein Kaltumformverfahren zur Herstellung von Hohl- oder Verkörpern. Das kompakte Vormaterial wird entweder ähnlich wie beim Strangpressen mit einem Stempel durch eine Matrize gepreßt (vorwärts) oder der Stempel wird in das Vormaterial gepreßt und das Material fließt rückwärts am Stempel entlang. Die Unterschiede zum Strangpressen liegen in der Verarbeitungstemperatur und darin, daß durch Fließpressen keine Halbzeugstränge, sondern Einzelteile hergestellt werden, wobei auch komplexe Formen herzustellen sind. Vorteile des Verfahrens liegen in geringen Werkzeugkosten, hohen Werkzeugstandzeiten und einer hohen Arbeitsgeschwindigkeit mit Taktzahlen von etwa 30-150 Stück/min. Die Oberflächenqualität ist gut und eignet sich für weitere Oberflächenbehandlungen. Das Hauptanwendungsgebiet sind Aluminiumlegierungen.A process for cold working brittle, recrystallized or relaxed materials - including Mo - by extrusion is in US 3,553,996 been claimed. This method is also known as forward extrusion 2 . The main focus is on the in US 3,553,996 described method on the avoidance of 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).
2 extrusion is a cold forming process for the production of hollow or embodying. The compact starting material is either pressed with a punch through a die ( forward ) similar to the extruding or the punch is pressed into the starting material and the material flows backwards along the punch. The differences from extrusion are in the processing temperature and in that by extruding no semi-finished product strands, but individual parts are produced, which are also complex shapes to produce. Advantages of the method are low tool costs, high tool life and a high operating speed with cycle numbers of about 30-150 pieces / min. The surface quality is good and suitable for further surface treatments. The main field of application is aluminum alloys.

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 case, a method for cold deformation of molybdenum by backward extrusion is now described. Surprisingly, despite its brittleness, molybdenum has been found to deform by backward extrusion without cracking or cracking. During extrusion, the energy is applied by compressive stress. The molybdenum is previously fully recrystallized by a heat treatment to exceed the yield value of the material with sufficiently low stress. In the recrystallization should all grid voltages are eliminated, which were previously caused by deformation. The material then reaches its yield point at relatively low forces. The recrystallization is advantageously carried out 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.
    3 Kaltkathodenlampen bzw. CCFL-Lampen sind Leuchtstofflampen und nutzen das Prinzip der Niederdruckentladung. Dadurch werden verdünnte Gasmischungen angeregt (z.B. Ar/Hg). Die Elektroden werden nicht erwärmt, sondern es wird zunächst eine hohe Spannung an die Röhre angelegt, um die Gasmischung zu ionisieren und elektrisch leitfähig zu machen. Die elektrische Energie regt die Gasatome an, und sie geben die überschüssige Energie in Form von UV- und sichtbarem Licht wieder ab. Eine auf Phosphor basierende Beschichtung an der Innenseite der Röhre wandelt UV-Strahlung in sichtbares Licht um. Die Elektroden werden aus Refraktärmetallen, meist Molybdän hergestellt. Molybdän eignet sich besonders wegen seiner Eigenschaft, leicht Elektronen zu emittieren. Bei Wechselstrombetrieb fungieren die Elektroden wechselweise als Kathoden und Anoden.
  • 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 .
    3 cold cathode lamps or CCFL lamps are fluorescent lamps and use the principle of low-pressure discharge. This stimulates dilute gas mixtures (eg Ar / Hg). The electrodes are not heated, but first a high voltage is applied to the tube to ionize the gas mixture and make it electrically conductive. The electrical energy excites the gas atoms, and they release the excess energy in the form of UV and visible light. A phosphor-based coating on the inside of the tube converts UV radiation into visible light. The electrodes are made of refractory metals, mostly molybdenum. Molybdenum is particularly suitable for its ability to easily emit electrons. In AC operation, the electrodes function alternately as cathodes and anodes.
  • 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 molybdenum coping produced by the process according to the invention 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 1 mm Mo wire section recrystallized at> 1400 ° C. under reduced pressure and cooled under vacuum, a molded coping is pressed backwards under pressure of about 1500 MPa at room temperature on a press.

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 by this method in Fig. 1 shows that crack-free rotationally symmetrical molded parts can be produced in this way.

Claims (6)

  1. Method for cold-forming of molybdenum by indirect impact extrusion, characterized in that complete recrystallisation is carried out prior to the cold-forming.
  2. Method according to Claim 1, characterized in that the recrystallisation is carried out under inert gas and/or in vacuo.
  3. Method according to either of the above claims, characterized in that the recrystallisation is carried out at temperatures above 1300°C.
  4. Method according to at least one of the above claims, characterized in that
    A) a molybdenum workpiece is completely recrystallised in vacuo and/or under an inert gas above 1400°C,
    B) the workpiece is cooled in vacuo and/or under inert gas,
    C) sections of the workpiece thus recrystallised are extruded at room temperature to give finished articles.
  5. Method according to Claim 4, in which the finished articles are rotationally symmetrically pressed.
  6. Method according to Claim 4 or 5, the finished articles being current feedthroughs through glass or ceramic bulbs or emitter electrodes in CCFL or cold cathode lamps.
EP04021093A 2003-10-02 2004-09-04 cold working of molyddenum by indirect extrusion Expired - Lifetime EP1574593B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10346464 2003-10-02
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

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EP1574593A1 EP1574593A1 (en) 2005-09-14
EP1574593B1 true 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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* Cited by examiner, † Cited by third party
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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

Family Cites Families (9)

* 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
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
JPS6082648A (en) * 1983-10-08 1985-05-10 Agency Of Ind Science & Technol Process for forming material having high strength and difficult processability
AT392432B (en) * 1989-05-03 1991-03-25 Plansee Metallwerk METHOD FOR THE PRODUCTION OF WARM-CRAWL-RESISTANT SEMI-FINISHED PRODUCTS OR MOLDED PARTS FROM HIGH-MELTING METALS
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
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

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DE10346464B4 (en) 2006-04-27
KR100771731B1 (en) 2007-10-30
EP1574593A1 (en) 2005-09-14
CN100335671C (en) 2007-09-05
TWI283609B (en) 2007-07-11
CN1611629A (en) 2005-05-04
DE10346464A1 (en) 2005-05-04
DE502004008340D1 (en) 2008-12-11
JP4348266B2 (en) 2009-10-21
KR20050033001A (en) 2005-04-08
ATE412786T1 (en) 2008-11-15
TW200526336A (en) 2005-08-16
JP2005111562A (en) 2005-04-28

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