DE10346464B4 - Method of cold forming molybdenum by reverse extrusion and use of molybdenum back molded extruded parts - Google Patents

Method of cold forming molybdenum by reverse extrusion and use of molybdenum back molded extruded parts Download PDF

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Publication number
DE10346464B4
DE10346464B4 DE10346464A DE10346464A DE10346464B4 DE 10346464 B4 DE10346464 B4 DE 10346464B4 DE 10346464 A DE10346464 A DE 10346464A DE 10346464 A DE10346464 A DE 10346464A DE 10346464 B4 DE10346464 B4 DE 10346464B4
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Prior art keywords
molybdenum
recrystallization
carried out
workpiece
reverse extrusion
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Expired - Fee Related
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DE10346464A
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German (de)
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DE10346464A1 (en
Inventor
Bernd Spaniol
Josef Trageser
Wolfgang Günther
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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Priority to DE10346464A priority Critical patent/DE10346464B4/en
Priority to AT04021093T priority patent/ATE412786T1/en
Priority to DE502004008340T priority patent/DE502004008340D1/en
Priority to EP04021093A priority patent/EP1574593B1/en
Priority to JP2004270451A priority patent/JP4348266B2/en
Priority to KR1020040075439A priority patent/KR100771731B1/en
Priority to TW093128875A priority patent/TWI283609B/en
Priority to CNB2004100803092A priority patent/CN100335671C/en
Publication of DE10346464A1 publication Critical patent/DE10346464A1/en
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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

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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 ein Verfahren zur Kaltumformung von Molybdän durch Rückwärts-Fließpressen und eine Verwendung von rückwärts-fließgepressten Molybdän-Formteilen.The The present invention relates to a method of cold forming molybdenum by backward extrusion and a use of backward-extruded Molybdenum moldings.

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 Tiefziehen 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 tubes or caps for the lighting technology can be made by deep drawing 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 A ) – oder bei elektronenstrahlergeschmolzenem 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.The transformation of precursors and semi-finished products usually takes place in the heat, that is expediently immediately after sintering ( US 5,158,709 A ) Or electron-molten molybdenum after hot forging - or by thermo-mechanical 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.

Aus US 3,553,996 ist eine Methode zum Vorwärts-Fließpressen von Mo-haltigen Werkstoffen bekannt, bei der Risse allerdings nicht vollständig vermieden werden. Durch die Gestaltung der Form, durch die extrudiert wird, wird eine besondere Verteilung der Spannungen erzielt. Im Beispiel 2 ist von rekristallisiertem Material die Rede, dieses ergibt aber noch Risse. Im Beispiel 3 heißt es zum Material "stress relieved". Das Extrusionsergebnis ist in diesem Beispiel zum Teil wegen Rissen unbrauchbar, kann aber aufgeteilt werden, ohne dass diese Risse sich ausbreiten.Out US 3,553,996 is a method for the forward extrusion of Mo-containing materials is known in the cracks, however, are not completely avoided. The shape of the mold used to extrude results in a particular distribution of stress. Example 2 refers to recrystallized material, but this still gives cracks. In example 3 the material is called "stress relieved". The extrusion result is in this example partly unusable due to cracks, but can be split without propagating these cracks.

Die gängige Lehrmeinung lautet trotz diesen Bemühungen, 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 common The dogma, despite these efforts, is that the material is not Completely may be recrystallized, as in the recrystallized annealed condition the tensile stresses necessary for forming then destroying (constriction, cracks) of the material would.

Ferner sind Verfahren bekannt, bei denen sich Verformung, Rekristallisation und Tempern abwechseln (z.B. US 4,600,446 ). Aufgabe der Erfindung ist es, weitere Verfahren zur Kaltverformung von Molybdän und Verwendungen von nach diesen Verfahren hergestellten Formteilen anzugeben. Kaltverformungsverfahren sind z.B. Schlagverformen, Festwalzen oder Fließpressen.Furthermore, methods are known in which alternate deformation, recrystallization and annealing (eg US 4,600,446 ). The object of the invention is to provide further methods for cold working of molybdenum and uses of molded parts produced by these methods. Kaltverformungsverfahren are eg impact molding, deep rolling or extrusion.

Gelöst wird die Aufgabe durch ein Verfahren mit den Merkmalen des Patentanspruches 1 und durch eine Verwendung mit den Merkmalen des Patentanspruches 5.Is solved the object by a method having the features of claim 1 and by use with the features of claim 5th

Es wurde gefunden, dass sich Molybdän überraschenderweise trotz seiner Sprödigkeit durch Rückwärts-Fließpressen verformen lässt, ohne dass Risse oder Brüche entstehen. Beim Rückwärts-Fließpressen wird die Energie durch Druckspannung aufgebracht. Das Molybdän wird wird vorher durch eine Wärmebehandlung vollständig rekristallisiert, um mit ausreichend geringer Spannung die Fließgrenze des Materials zu überschreiten. Die Rekristallisation erfolgt vorteilhaft bei Temperaturen oberhalb 1300°C, besonders über 1400°C (der Schmelzpunkt von Mo liegt bei 2623-5°C).It was found that molybdenum surprisingly, despite its brittleness by backward extrusion deform without cracks or breaks. In reverse extrusion, the energy is applied by compressive stress. The molybdenum is previously completely recrystallized by a heat treatment in order to exceed the yield value of the material with sufficiently low stress. 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. Bei der Rekristallisation sollen sämtliche Gitterspannungen beseitigt werden, die vorher durch Verformen entstanden waren. Das Material erreicht dann bei relativ geringen Kräften seine Fließgrenze.The invention thus relates to a process for the cold deformation of molybdenum by reverse extrusion, wherein previously a complete recrystallization is carried out. During recrystallization, all lattice stresses that were previously caused by deformation should be eliminated. The material then reaches at relatively low Forces its yield point.

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.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.

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 Fließpressen hergestellt werden. Das Verfahren eignet sich auch für andere spröde Metalle oder deren Legierungen, z. B. für Chrom oder Wolfram.The The main advantages of the process are: First, the material be used much better than deep drawing. Next can be parts with thicker or shaped bottoms by extrusion getting produced. The method is also suitable for others brittle Metals or their alloys, eg. For chromium or tungsten.

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) eingesetzt werden.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) be used.

Claims (6)

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 reverse 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.Method according to claim 1, characterized in that that the recrystallization is carried out under protective gas and / or vacuum. Verfahren nach einem der Ansprüche 1 und 2, dadurch gekennzeichnet, dass die Rekristallisation bei Temperaturen oberhalb 1300°C durchgeführt wird.Method according to one of claims 1 and 2, characterized that the recrystallization is carried out at temperatures above 1300 ° C. Verfahren nach einem der Ansprüche 1 bis 3, 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 rotationssymmetrischen Fertigteilen fließgepresst werden.Method according to one of claims 1 to 3, characterized that A) a molybdenum workpiece below Vacuum and / or inert gas completely recrystallized at temperatures above 1400 ° C. becomes, B) the workpiece is cooled under vacuum and / or inert gas, C) sections from the thus recrystallized workpiece at room temperature to rotationally symmetric Finished parts extruded become. Verwendung von nach einem der Ansprüche 1 bis 4 rückwärts-fließgepressten Molybdän-Formteilen in der Lichttechnik.Use of according to one of claims 1 to 4 backward-extruded Molybdenum molded parts in the Lighting technology. Verwendung nach Anspruch 5 zur Herstellung von Stromdurchführungen durch Glas- oder Keramik-Kolben oder zur Herstellung von Emitter-Elektroden in CCFL- oder Kaltkathodenlampen.Use according to claim 5 for the production of current feedthroughs by glass or ceramic flask or for the production of emitter electrodes in CCFL or cold cathode lamps.
DE10346464A 2003-10-02 2003-10-02 Method of cold forming molybdenum by reverse extrusion and use of molybdenum back molded extruded parts Expired - Fee Related DE10346464B4 (en)

Priority Applications (8)

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
DE502004008340T DE502004008340D1 (en) 2003-10-02 2004-09-04 Cold deformation of molybdenum by backward extrusion
EP04021093A EP1574593B1 (en) 2003-10-02 2004-09-04 cold working of molyddenum by indirect extrusion
AT04021093T ATE412786T1 (en) 2003-10-02 2004-09-04 COLD FORMING OF MOLYBDENUM BY BACKWARD EXPRESSION
JP2004270451A JP4348266B2 (en) 2003-10-02 2004-09-16 Method for cold deformation of molybdenum by backward extrusion
KR1020040075439A KR100771731B1 (en) 2003-10-02 2004-09-21 Cold-forming of molybdenum by backward exrusion
TW093128875A TWI283609B (en) 2003-10-02 2004-09-23 Cold-forming of molybdenum by backward extrusion
CNB2004100803092A CN100335671C (en) 2003-10-02 2004-09-28 Method for extrusion cold forming molybdic through back flowing

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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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DE10346464A1 DE10346464A1 (en) 2005-05-04
DE10346464B4 true DE10346464B4 (en) 2006-04-27

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DE502004008340T Expired - Lifetime DE502004008340D1 (en) 2003-10-02 2004-09-04 Cold deformation of molybdenum by backward extrusion

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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 (4)

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Publication number Priority date Publication date Assignee Title
US3553996A (en) * 1967-11-13 1971-01-12 Battelle Development Corp Extrusion of brittle materials
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 (5)

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JPS5731408A (en) * 1980-06-19 1982-02-19 Battelle Development Corp Double extruding die and its extruding method
US4462234A (en) * 1980-06-19 1984-07-31 Battelle Development Corporation Rapid extrusion of hot-short-sensitive alloys
JPS6075545A (en) * 1983-09-29 1985-04-27 Toshiba Corp Dies and their manufacture
ES2160628T3 (en) * 1993-04-15 2001-11-16 Luxfer Group Ltd METHOD OF MANUFACTURE OF 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 (4)

* 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
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
ATE412786T1 (en) 2008-11-15
CN1611629A (en) 2005-05-04
TW200526336A (en) 2005-08-16
CN100335671C (en) 2007-09-05
DE10346464A1 (en) 2005-05-04
KR20050033001A (en) 2005-04-08
JP2005111562A (en) 2005-04-28
EP1574593B1 (en) 2008-10-29
KR100771731B1 (en) 2007-10-30
EP1574593A1 (en) 2005-09-14
DE502004008340D1 (en) 2008-12-11
TWI283609B (en) 2007-07-11
JP4348266B2 (en) 2009-10-21

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