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EP0947595A2 - Process for preparing a welded workpiece, in particular a tube, from dispersion-hardened platinum material - Google Patents

Process for preparing a welded workpiece, in particular a tube, from dispersion-hardened platinum material Download PDF

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Publication number
EP0947595A2
EP0947595A2 EP99104851A EP99104851A EP0947595A2 EP 0947595 A2 EP0947595 A2 EP 0947595A2 EP 99104851 A EP99104851 A EP 99104851A EP 99104851 A EP99104851 A EP 99104851A EP 0947595 A2 EP0947595 A2 EP 0947595A2
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EP
European Patent Office
Prior art keywords
platinum
alloy
base metal
dispersion
tube
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Application number
EP99104851A
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German (de)
French (fr)
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EP0947595A3 (en
EP0947595B1 (en
Inventor
Franz Braun
Wulf Dr. Kock
David Francis Dr. Lupton
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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
    • 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
    • C22C32/0021—Matrix based on noble metals, Cu or alloys thereof
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12861—Group VIII or IB metal-base component
    • Y10T428/12875—Platinum group metal-base component

Definitions

  • the invention relates to a method for producing a from finely divided, small particles welded, in particular made of base metal oxide dispersion-tested platinum material at least one molded body having an inner wall, in particular a tube, a molded body, in particular a tube, and the use of such a tube.
  • Suitable base metals are, for example, chromium, beryllium, magnesium, aluminum, Silicon, the rare earths, thorium, uranium and metals of the first, second and third subgroup period, Calcium to nickel, strontium to molybdenum and barium to tantalum.
  • the High temperature resistant compound can be an oxide, a carbide, a nitride, a silicide Boride, a sulfide, or any other compound created by interaction between a gaseous phase and the base metal can be formed.
  • sheet metal a metal of the platinum group or their alloys with an addition of the above non-metallic Substances can be dispersion-hardened.
  • Platinum materials with a fine-grained equi-axis structure are usually used in production used by components. This structure is created by a melted and cast one Ingots formed (e.g. by forging, rolling) and then recrystallization annealing is subjected. When the material is subsequently welded after solidification of the metal in the weld seam, a structure that is more likely to be undesirable Structure in cast ingots is comparable to the fine recrystallized structure of the other material. By reshaping the weld seam with the rest of the material a homogenization of the structure can be achieved after a recrystallization annealing treatment becomes visible, d. that is, the reformed and recrystallized weld material corresponds essentially to the rest of the material.
  • the solidifying effect of the dispersoids will no longer be present.
  • the structure becomes different during an annealing treatment or when used at high temperature (Grain size) in the largely oxide-free weld seam is considerably coarser than in the rest Material.
  • the presence of the dispersoids leads to a considerable stabilization of the Grain structure).
  • a blank of any shape is made from yttrium and zirconium and / or cerium-doped platinum-base metal alloy, initially in one Brought preform, in particular a sheet rounded to a tube and the respective Ends are welded together.
  • the welding can either be done without additional metal or with an additional metal of the same type.
  • Additional metal of the same type means that if the addition of welding metal is required during welding, this metal should be similar to the base material, d. i.e. with the specified base metal doping elements, here: zirconium and yttrium, cerium, should be alloyed.
  • the molded body still in the preform is in an oxidizing Medium heat-treated up to a minimum oxidation level of the base metal of 75% by weight, preferably an atmosphere of air, oxygen, water vapor or a mixture from water vapor and hydrogen, noble gas, especially helium or argon, or nitrogen is used.
  • Air is usually used as the oxidizing medium. Because the oxide-forming base metal components are very reactive, they can be used to form the oxides Take oxygen from other oxygen-containing compounds, such as. B. water vapor. The medium containing the oxygen must release it to the base metal components can, d. H. thermodynamically seen that the zirconium-yttrium and cerium oxides are more stable must be as the oxygen-containing species in the medium. To make sure that not that Oxygen supply from the medium, but the diffusion in the platinum material determines the speed sufficient concentration of the oxygenated species should be given be.
  • the doped, non-oxidized material is thus first welded and then the oxide dispersoids are heat-treated in one oxidizing medium generated.
  • the formation of the oxide particles is only slightly affected by the grain structure of the platinum material influenced, d. that is, the only significant difference between the weld and the Base material lies in the grain structure and not in the distribution of the oxide particles.
  • the molded body in the preform is made according to the desired one Final shape, for example, appropriately formed by rolling, forging or drawing, the roll-pressing method has proven itself in the drawing process.
  • platinum material composed of dispersion-strengthened materials can be used Tubes of almost any size can be made.
  • the formed preform is advantageously subjected to a recrystallization annealing treatment subjected to minimize dimensional changes in use.
  • a recrystallization annealing treatment subjected to minimize dimensional changes in use.
  • the Uniformity of the structure between the weld seam and the base material thanks to this treatment more obvious.
  • the welded structure treated in this way and the dispersion-hardened one Platinum materials differ only slightly in their properties from each other.
  • the annealing treatment at a minimum temperature of 600 ° C and a maximum temperature of 1400 ° C is carried out.
  • the annealing treatment can be used with any oxide-strengthened, otherwise unalloyed platinum Temperature ⁇ 600 ° C.
  • PtRh, Pt-Au and PtIr alloys - these are the ones platinum-precious metal alloys - temperatures ⁇ 900 ° C, often ⁇ 1000 ° C, are required.
  • the annealing treatment can also be carried out in principle even higher temperatures are carried out because the oxide dispersoids are too strong Prevent grain enlargement.
  • the deformed one shows Preform body on a uniform structure.
  • the base metal content of the platinum-base metal alloy 0.005 to 1% by weight and that the dispersion-strengthened platinum material from dispersion-strengthened Platinum-rhodium alloy, dispersion-strengthened platinum-iridium alloy or dispersion-strengthened platinum-gold alloy.
  • the platinum-base metal alloy with 0.1 to 0.2% by weight of zirconium and 0.01 to 0.05% by weight of yttrium and / or with 0.05 - 0.2 Weight% cerium is doped and that the platinum-rhodium alloy is a PtRh10 alloy
  • Platinum-gold alloy is a PtAu5 alloy and the platinum-iridium alloy is one PtIr (1-10) -, in particular a PtIr (3-10) alloy, is (PtXn means: (100-n)% by weight Pt and n% by weight of element X).
  • the moldings produced by the process according to the invention in particular pipes, have the surprising and advantageous properties indicated above.
  • a sheet (dimensions: 400 mm long, 350 mm wide, 3 mm thick) made of one with 0.18% by weight zirconium and 0.017% by weight of yttrium-doped, unoxidized platinum material is rounded and welded along the length without additional metal in order to create a down tube with a Length of 400 mm and an inner diameter of approx. 111 mm.
  • This The front pipe is subjected to a heat treatment in an oxidizing medium that is composed from dry air, subjected to a temperature of 1000 ° C for a period of 300 hours, until the oxygen content of the material is 0.073% by weight on a cylindrical Mandrel with a diameter of 110 mm drawn from hardened tool steel and finally stretched to the desired length and wall thickness. The stretching is done through a mandrel.
  • the front pipe is made to a wall thickness of 0.7 mm and a length formed from 1500 mm.
  • the pipe can be several longitudinal or also Include round welds. You can use standard roll spinning machines to do this Wise pipes up to a diameter of approx. 650 mm and a length of approx. 8000 mm are produced, whereby this information is not to be regarded as limiting.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Arc Welding In General (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

A welded hollow article of oxide dispersion strengthened platinum is produced by shaping and welding a base metal-containing platinum alloy prior to internal oxidation. Production of a welded hollow article, especially a tube, of platinum material dispersion strengthened by base metal oxide particles of yttrium, zirconium and/or cerium oxide comprises shaping and welding one or more base metal-containing platinum alloy parts to a preform body, thermally oxidizing to achieve ≥ 75 wt.% oxidation and then shaping the preform body. An Independent claim is also included for an article, especially a tube, produced by the above process. Preferred Features: The platinum-base metal alloy is a Pt-Rh, Pt-Ir or Pt-Au alloy doped with 0.1-0.2 wt.% Zr and 0.01-0.05 wt.% Y and/or 0.05-0.2 wt.% Ce.

Description

Die Erfindung betrifft ein Verfahren zur Herstellung eines aus durch feinverteilte, kleine Teilchen aus Unedelmetalloxid dispersionsvertestigtem Platinwerkstoff bestehenden, geschweißten, insbesondere mindestens eine Innenwand aufweisenden Formkörpers, insbesondere eines Rohres, einen Formkörper, insbesondere ein Rohr, und die Verwendung eines solchen Rohres.The invention relates to a method for producing a from finely divided, small particles welded, in particular made of base metal oxide dispersion-tested platinum material at least one molded body having an inner wall, in particular a tube, a molded body, in particular a tube, and the use of such a tube.

Aus dem Stand der Technik ist es bekannt (siehe DE-OS 15 33 273), daß Platin, Palladium und Rhodium bzw. Legierungen davon, die eine kleine Menge eines oder mehrerer gelöster unedler Metalle enthalten, unter Erzeugung eines dispersionsgehärteten Materials der inneren Oxidation unterworfen werden können.From the prior art it is known (see DE-OS 15 33 273) that platinum, palladium and Rhodium or alloys thereof, which contain a small amount of one or more dissolved base Contain metals, producing a dispersion-hardened material of the internal oxidation can be subjected.

Hierbei wird in Platin, Palladium oder Rhodium bzw. Legierungen dieser Metalle mit einem oder mehreren anderen Metallen der Platingruppe eine kleine Menge wenigstens eines unedlen Metalls einlegiert, das zur Ausbildung einer stabilen hochtemperaturbeständigen Verbindung befähigt ist, und der Legierungszusatz in diese, über die Legierung dispergierte Verbindung überführt. Geeignete Unedelmetalle sind beispielsweise Chrom, Beryllium, Magnesium, Aluminium, Silicium, die seltenen Erden, Thorium, Uran und Metalle der ersten, zweiten und dritten Nebengruppenperiode, Kalzium bis Nickel, Strontium bis Molybdän und Barium bis Tantal. Die hochtemperaturbeständige Verbindung kann ein Oxid, ein Carbid, ein Nitrid, ein Silicid, ein Borid, ein Sulfid oder irgendeine andere Verbindung sein, die durch Wechselwirkung zwischen einer gasförmigen Phase und dem unedlen Metall gebildet werden kann.Here is in platinum, palladium or rhodium or alloys of these metals with one or several other platinum group metals, a small amount of at least one base metal alloyed, which enables the formation of a stable high-temperature resistant connection and the alloy additive is converted into this compound dispersed over the alloy. Suitable base metals are, for example, chromium, beryllium, magnesium, aluminum, Silicon, the rare earths, thorium, uranium and metals of the first, second and third subgroup period, Calcium to nickel, strontium to molybdenum and barium to tantalum. The High temperature resistant compound can be an oxide, a carbide, a nitride, a silicide Boride, a sulfide, or any other compound created by interaction between a gaseous phase and the base metal can be formed.

Weiterhin ist es aus dem Stand der Technik bekannt (siehe DE-OS 15 33 273), daß Bleche aus einem Metall der Platingruppe oder deren Legierungen mit einem Zusatz obiger nicht metallischer Substanzen dispersionsgehärtet vorliegen können.Furthermore, it is known from the prior art (see DE-OS 15 33 273) that sheet metal a metal of the platinum group or their alloys with an addition of the above non-metallic Substances can be dispersion-hardened.

Darüber hinaus ist es bekannt (Mechanical properties of metallic composits, edited by Shojiro Ochiai, 1993, Seiten 352 - 353), daß beim Schweißen von oxiddispersionsgehärteten Platinwerkstoffen die Oxiddispersionshärtung zum größten Teil verloren geht, da der Schmelzprozeß beim Schweißen zum Agglomerien und Ausschwemmen der Oxiddispersoide und damit zu einem Verlust der günstigen Eigenschaften führt.It is also known (Mechanical properties of metallic composits, edited by Shojiro Ochiai, 1993, pages 352-353) that when welding oxide dispersion-hardened platinum materials the oxide dispersion hardening is largely lost because of the melting process during welding to agglomerate and flush out the oxide dispersoids and thus to one Loss of beneficial properties leads.

Üblicherweise werden Platinwerkstoffe mit einem feinkörnigen Äquiachsgefüge bei der Herstellung von Bauteilen eingesetzt. Dieses Gefüge wird erzeugt, indem ein geschmolzener und gegossener Barren umgeformt (z. B. durch Schmieden, Walzen) und anschließend einer Rekristallisationsglühung unterzogen wird. Bei anschließendem Schweißen des Materials entsteht nach Erstarrung des Metalls in der Schweißnaht ein Gefüge, das eher mit dem unerwünschten Gefüge in gegossenen Barren vergleichbar ist, als mit dem feinen rekristallisierten Gefüge des übrigen Materials. Durch Umformen der Schweißnaht zusammen mit dem restlichen Material kann eine Homogenisierung des Gefüges erzielt werden, die nach einer Rekristallisationsglühbehandlung sichtbar wird, d. h., daß das umgeformte und rekristallisierte Material der Schweißnaht im wesentlichen dem übrigen Material entspricht.Platinum materials with a fine-grained equi-axis structure are usually used in production used by components. This structure is created by a melted and cast one Ingots formed (e.g. by forging, rolling) and then recrystallization annealing is subjected. When the material is subsequently welded after solidification of the metal in the weld seam, a structure that is more likely to be undesirable Structure in cast ingots is comparable to the fine recrystallized structure of the other material. By reshaping the weld seam with the rest of the material a homogenization of the structure can be achieved after a recrystallization annealing treatment becomes visible, d. that is, the reformed and recrystallized weld material corresponds essentially to the rest of the material.

Bislang war es jedoch nicht möglich, das Schweißverfahren bei oxiddispersionsgehärteten Werkstoffen anzuwenden, ohne daß die spezifischen Eigenschaften der Dispersionshärtung verloren gehen.So far, however, it has not been possible to weld the oxide dispersion-hardened welding process Materials without using the specific properties of dispersion hardening get lost.

Da der Schweißvorgang, wie schon oben ausgeführt, zum Ausschwemmen der Dispersoide führt, unterscheidet sich die Schweißnaht grundlegend vom restlichen Material.Since the welding process, as already explained above, to flush out the dispersoids leads, the weld seam differs fundamentally from the rest of the material.

Zum einen wird die verfestigende Wirkung der Dispersoide nicht mehr vorhanden sein. Zum anderen wird bei einer Glühbehandlung oder beim Einsatz bei hoher Temperatur das Gefüge (Korngröße) in der weitgehend oxidfreien Schweißnaht wesentlich gröber als im restlichen Material sein. (Die Anwesenheit der Dispersoide führt zu einer erheblichen Stabilisierung der Kornstruktur). Das vergröberte Korn in der Schweißnaht, auch nach Umformung und Glühbehandlung, führt u. a. zu einer verstärkten Korrosionsanfälligkeit, da der Korrosionsangriff hauptsächlich entlang der Korngrenze erfolgt.For one thing, the solidifying effect of the dispersoids will no longer be present. To the the structure becomes different during an annealing treatment or when used at high temperature (Grain size) in the largely oxide-free weld seam is considerably coarser than in the rest Material. (The presence of the dispersoids leads to a considerable stabilization of the Grain structure). The coarsened grain in the weld seam, even after forming and Annealing, leads u. a. increased susceptibility to corrosion because of the corrosion attack mainly along the grain boundary.

Darüber hinaus war es bislang nicht möglich, relativ dicke, insbesondere mehrere Millimeter starke, Halbzeuge aus Platinwerkstoffen bis zu einem hohen Anteil innerlich zu oxidieren. Aus diesem Grund mußten diese Halbzeuge aus einem Material hergestellt werden, das die Oxiddispersoide bereits enthält und somit zu den oben geschilderten Problemen beim Schweißen führt.In addition, it was previously not possible to use relatively thick, in particular several millimeters Strong, semi-finished products made of platinum materials to oxidize internally. Out for this reason, these semi-finished products had to be made from a material that is the oxide dispersoids already contains and thus to the problems with welding described above leads.

Aus dem Vorgenannten ergibt sich das Problem, mit Hilfe eines neuartigen Verfahrens, eines neuartigen Formkörpers und einer Verwendung die oben genannten Nachteile zumindest teilweise zu beseitigen.The problem arises from the above, with the help of a novel method, one novel moldings and a use the disadvantages mentioned above at least partially to eliminate.

Dieses Problem wird erfindungsgemäß durch ein Verfahren nach Anspruch 1, einen Formkörper nach Anspruch 11 und eine Verwendung nach Anspruch 12 gelöst.This problem is solved according to the invention by a method according to claim 1, a molded body solved according to claim 11 and a use according to claim 12.

Beim erfindungsgemäßen Verfahren wird ein Rohling beliebiger Gestalt, der aus mit Yttrium und Zirkonium und/oder Cer dotierter Platin-Unedelmetall-Legierung besteht, zunächst in eine Vorform gebracht, wobei insbesondere ein Blech zu einem Rohr gerundet und die jeweiligen Enden miteinander verschweißt werden. Das Schweißen kann entweder ohne Zusatzmetall oder mit einem artgleichen Zusatzmetall durchgeführt werden. "Artgleiches Zusatzmetall" bedeutet, daß, wenn beim Schweißen die Zugabe von Schweißmetall erforderlich ist, dieses Metall ähnlich dem Grundwerkstoff sein sollte, d. h., mit den angegebenen Unedelmetalldotierungselementen, hier: Zirkonium und Yttrium, Cer, legiert sein sollte. Prinzipiell wäre es denkbar, einen Platin (Zirkonium, Yttrium)-Grundwerkstoff mit einem Platin(Cer)-Zusatzmetall zu schweißen. Normalerweise ist es besser, ein Zusatzmetall mit denselben Haupt- und Dotierungsbestandteilen wie im Grundwerkstoff zu verwenden. Auf diese Art und Weise ist sichergestellt, daß die Oxidationskinetik in der Schweißnaht und im Grundwerkstoff sowie das entstehende Gefüge weitestgehend gleich sind.In the method according to the invention, a blank of any shape is made from yttrium and zirconium and / or cerium-doped platinum-base metal alloy, initially in one Brought preform, in particular a sheet rounded to a tube and the respective Ends are welded together. The welding can either be done without additional metal or with an additional metal of the same type. "Additional metal of the same type" means that if the addition of welding metal is required during welding, this metal should be similar to the base material, d. i.e. with the specified base metal doping elements, here: zirconium and yttrium, cerium, should be alloyed. In principle it would be conceivable, a platinum (zirconium, yttrium) base material with a platinum (cerium) additional metal to weld. It is usually better to use an additional metal with the same main and doping components as used in the base material. This way it is ensured that the oxidation kinetics in the weld seam and in the base material as well as the resulting Structures are largely the same.

Anschließend wird der sich noch in der Vorform befindende Formkörper in einem oxidierenden Medium bis zu einem Mindestoxidationsgrad des Unedelmetalls von 75 Gewichts-% wärmebehandelt, wobei bevorzugt eine Atmosphäre aus Luft, Sauerstoff, Wasserdampf oder ein Gemisch aus Wasserdampf und Wasserstoff, Edelgas, besonders Helium oder Argon, oder Stickstoff zur Anwendung kommt. Then the molded body still in the preform is in an oxidizing Medium heat-treated up to a minimum oxidation level of the base metal of 75% by weight, preferably an atmosphere of air, oxygen, water vapor or a mixture from water vapor and hydrogen, noble gas, especially helium or argon, or nitrogen is used.

In der Regel wird als oxidierendes Medium Luft verwendet. Da die oxidbildenden Unedelmetallbestandteile sehr reaktionsfreudig sind, können sie den zur Bildung der Oxide erforderlichen Sauerstoff auch anderen sauerstoffhaltigen Verbindungen entnehmen, wie z. B. Wasserdampf. Das den Sauerstoff enthaltende Medium muß diesen an die Unedelmetallbestandteile abgeben können, d. h. thermodynamisch gesehen, daß die Zirkonium-Yttrium- und Cer-Oxide stabiler sein müssen als die sauerstoffhaltigen Spezies im Medium. Um sicherzustellen, daß nicht das Sauerstoffangebot aus dem Medium, sondern die Diffusion im Platinmaterial geschwindigkeitsbestimmend ist, sollte eine ausreichende Konzentration der sauerstoffhaltigen Spezies gegeben sein.Air is usually used as the oxidizing medium. Because the oxide-forming base metal components are very reactive, they can be used to form the oxides Take oxygen from other oxygen-containing compounds, such as. B. water vapor. The medium containing the oxygen must release it to the base metal components can, d. H. thermodynamically seen that the zirconium-yttrium and cerium oxides are more stable must be as the oxygen-containing species in the medium. To make sure that not that Oxygen supply from the medium, but the diffusion in the platinum material determines the speed sufficient concentration of the oxygenated species should be given be.

Beim erfindungsgemäßen Verfahren wird somit zunächst der dotierte nicht oxidierte Werkstoff geschweißt und anschließend werden die Oxiddispersoide durch die Wärmebehandlung in einem oxidierenden Medium erzeugt.In the method according to the invention, the doped, non-oxidized material is thus first welded and then the oxide dispersoids are heat-treated in one oxidizing medium generated.

Durch die Verwendung der Unedelmetalle Yttrium, Zirkonium und Cer wird die innere Oxidation soweit beschleunigt, daß die Oxidationsbehandlung am geformten und geschweißten Vorformkörper durchgeführt werden kann.By using the base metals yttrium, zirconium and cerium the internal oxidation accelerated so far that the oxidation treatment on the molded and welded preform body can be carried out.

Die Bildung der Oxidteilchen wird nur geringfügig von der Kornstruktur des Platinwerkstoffes beeinflußt, d. h., daß der einzige wesentliche Unterschied zwischen der Schweißnaht und dem Grundwerkstoff in der Kornstruktur und nicht in der Verteilung der Oxidteilchen liegt.The formation of the oxide particles is only slightly affected by the grain structure of the platinum material influenced, d. that is, the only significant difference between the weld and the Base material lies in the grain structure and not in the distribution of the oxide particles.

Danach wird der sich in der Vorform befindende Formkörper entsprechend der gewünschten Endform beispielsweise durch Walzen, Schmieden oder Abstrecken entsprechend umgeformt, wobei sich besonders das Walzdrückverfahren beim Abstrecken bewährt hat.Then the molded body in the preform is made according to the desired one Final shape, for example, appropriately formed by rolling, forging or drawing, the roll-pressing method has proven itself in the drawing process.

Mit dem erfindungsgemäßen Verfahren können aus dispersionsverfestigtem Platinwerkstoff bestehende Rohre beinahe beliebiger Größe hergestellt werden.With the method according to the invention, platinum material composed of dispersion-strengthened materials can be used Tubes of almost any size can be made.

Vorteilhafterweise wird der umgeformte Vorformkörper einer Rekristallisationsglühbehandlung unterworfen, um dimensionale Änderungen im Einsatz zu minimieren. Darüber hinaus wird die Gleichmäßigkeit des Gefüges zwischen Schweißnaht und Grundwerkstoff durch diese Behandlung offensichtlicher. Das auf diese Art und Weise behandelte Schweißgefüge und der dispersionsverfestigte Platinwerkstoff unterscheiden sich in ihren Eigenschaften nur noch unwesentlich voneinander. The formed preform is advantageously subjected to a recrystallization annealing treatment subjected to minimize dimensional changes in use. In addition, the Uniformity of the structure between the weld seam and the base material thanks to this treatment more obvious. The welded structure treated in this way and the dispersion-hardened one Platinum materials differ only slightly in their properties from each other.

Es hat sich als vorteilhaft herausgestellt, wenn die Glühbehandlung bei einer Mindesttemperatur von 600 °C und einer Maximaltemperatur von 1400 °C durchgeführt wird. Die Glühbehandlung kann bei oxiddispersionsverfestigtem, ansonsten unlegierten Platin bei jeder beliebigen Temperatur ≥ 600 °C erfolgen. Bei PtRh-, Pt-Au- und PtIr-Legierungen - bei diesen handelt es sich um Platin-Edelmetall-Legierungen - sind Temperaturen ≥ 900 °C, häufig ≥ 1000 °C, erforderlich. Um eine gleichmäßige, relativ feine rekristallisierte Kornstruktur zu erhalten, geht man normalerweise nicht über 12000 °C. Allerdings kann die Glühbehandlung prinzipiell auch bei noch höheren Temperaturen durchgeführt werden, weil die Oxiddispersoide eine zu starke Kornvergrößerung verhindern. Als praktikable Obergrenze hat sich eine Temperatur von 1400 °C erwiesen. Wird das Material einer zu hohen Temperatur ausgesetzt, bevor sich die Oxiddispersoide durch innere Oxidation gebildet haben, kann es zu unerwünschter Grobkornbildung kommen.It has proven to be advantageous if the annealing treatment at a minimum temperature of 600 ° C and a maximum temperature of 1400 ° C is carried out. The annealing treatment can be used with any oxide-strengthened, otherwise unalloyed platinum Temperature ≥ 600 ° C. With PtRh, Pt-Au and PtIr alloys - these are the ones platinum-precious metal alloys - temperatures ≥ 900 ° C, often ≥ 1000 ° C, are required. To get a uniform, relatively fine recrystallized grain structure, one goes usually not above 12000 ° C. However, the annealing treatment can also be carried out in principle even higher temperatures are carried out because the oxide dispersoids are too strong Prevent grain enlargement. A temperature of. Has become a practicable upper limit Proven 1400 ° C. If the material is exposed to too high a temperature before the Oxide dispersoids formed by internal oxidation can lead to undesirable coarse grain formation come.

Weiterhin ist es vorteilhaft, daß beim Umformen des Vorformkörpers, insbesondere beim Abstrecken, eine Reduzierung der Wandstärke von mindestens 50 % erreicht wird, da die Eigenschaften des Schweißgefüges und des dispersionsgehärteten Platinwerkstoffs sich quasi nicht mehr voneinander unterscheiden.Furthermore, it is advantageous that when the preform is deformed, in particular when it is stretched, a reduction in wall thickness of at least 50% is achieved because of the properties the weld structure and the dispersion-hardened platinum material are practically not differentiate more from each other.

Bei konventionell hergestellten Vorformkörpern würde man normalerweise erwarten, daß nach dem Schweißen eines dispersionsgehärteten Werkstoffs eine Wandstärkenreduzierung von mindestens 50 % zu Bereichen führen würde, die sehr unterschiedlich auf eine Hochtemperaturauslagerung (Glühbehandlung oder Einsatzbedingungen) reagieren. Man würde weiterhin erwarten, daß die kornstabilisierende Wirkung der Dispersoide in der Schweißnaht quasi nicht mehr vorhanden wäre und es zur Grobkornbildung käme.With conventionally produced preforms one would normally expect that after the welding of a dispersion hardened material a reduction in wall thickness of at least 50% would lead to areas that vary widely on high temperature exposure (Annealing or operating conditions) react. One would continue do not expect the grain-stabilizing effect of the dispersoids in the weld seam to be virtually non-existent would be available and coarse grain would form.

Da die Dispersoide jedoch erst nach dem Schweißen erzeugt werden, weist der umgeformte Vorformkörper ein gleichmäßiges Gefüge auf.However, since the dispersoids are only created after welding, the deformed one shows Preform body on a uniform structure.

Weiterhin hat es sich bewährt, daß der Unedelmetallgehalt der Platin-Unedelmetall-Legierung 0,005 bis 1 Gewichts-% beträgt und daß der dispersionsverfestigte Platinwerkstoff aus dispersionsverfestigter Platin-Rhodium-Legierung, dispersionsverfestigter Platin-Iridium-Legierung oder dispersionsverfestigter Platin-Gold-Legierung besteht.Furthermore, it has proven useful that the base metal content of the platinum-base metal alloy 0.005 to 1% by weight and that the dispersion-strengthened platinum material from dispersion-strengthened Platinum-rhodium alloy, dispersion-strengthened platinum-iridium alloy or dispersion-strengthened platinum-gold alloy.

Schließlich hat es sich in vorteilhafterweise bewährt, daß die Platin-Unedelmetall-Legierung mit 0,1 bis 0,2 Gewichts-% Zirkonium und 0,01 bis 0,05 Gewichts-% Yttrium und/oder mit 0,05 - 0,2 Gewichts-% Cer dotiert ist und daß die Platin-Rhodium-Legierung eine PtRh10-Legierung, die Platin-Gold-Legierung eine PtAu5-Legierung ist und die Platin-Iridium-Legierung eine PtIr(1-10)-, insbesondere eine PtIr(3-10)-Legierung, ist (PtXn bedeutet: (100-n)Gewichts-% Pt und n Gewichts-% Element X).Finally, it has proven advantageous that the platinum-base metal alloy with 0.1 to 0.2% by weight of zirconium and 0.01 to 0.05% by weight of yttrium and / or with 0.05 - 0.2 Weight% cerium is doped and that the platinum-rhodium alloy is a PtRh10 alloy Platinum-gold alloy is a PtAu5 alloy and the platinum-iridium alloy is one PtIr (1-10) -, in particular a PtIr (3-10) alloy, is (PtXn means: (100-n)% by weight Pt and n% by weight of element X).

Die nach dem erfindungsgemäßen Verfahren hergestellten Formkörper, insbesondere Rohre, weisen die oben angegebenen überraschenden und vorteilhaften Eigenschaften auf.The moldings produced by the process according to the invention, in particular pipes, have the surprising and advantageous properties indicated above.

Entsprechendes gilt auch für die Verwendung eines nach dem erfindungsgemäßen Verfahren hergestellten Rohres zum Läutern von Glas.The same applies to the use of a method according to the invention manufactured tube for refining glass.

Das nachfolgende Beispiel dient zur Erläuterung der Erfindung.The following example serves to explain the invention.

Ein Blech (Maße: 400 mm lang, 350 mm breit, 3 mm dick) aus einem mit 0,18 Gewichts-% Zirkonium und 0,017 Gewichts-% Yttrium dotierten, unoxidierten Platinmaterial wird gerundet und ohne Zusatzmetall über die Länge geschweißt, um auf diese Art und Weise ein Vorrohr mit einer Länge von 400 mm und einem Innendurchmesser von ca. 111 mm herzustellen. Dieses Vorrohr wird einer Wärmbehandlung in einem oxidierenden Medium, das sich zusammensetzt aus trockener Luft, bei einer Temperatur von 1000° C für eine Zeitdauer von 300 Stunden unterzogen, bis der Sauerstoffgehalt des Materials 0,073 Gewichts-% beträgt, auf einen zylindrischen Dorn mit einem Durchmesser von 110 mm aus gehärtetem Werkzeugstahl gezogen und schließlich auf die gewünschte Länge und Wanddicke abgestreckt. Das Abstrecken erfolgt dabei durch einen Ziehdorn. Das Vorrohr wird auf eine Wanddicke von 0,7 mm und eine Länge von 1500 mm umgeformt.A sheet (dimensions: 400 mm long, 350 mm wide, 3 mm thick) made of one with 0.18% by weight zirconium and 0.017% by weight of yttrium-doped, unoxidized platinum material is rounded and welded along the length without additional metal in order to create a down tube with a Length of 400 mm and an inner diameter of approx. 111 mm. This The front pipe is subjected to a heat treatment in an oxidizing medium that is composed from dry air, subjected to a temperature of 1000 ° C for a period of 300 hours, until the oxygen content of the material is 0.073% by weight on a cylindrical Mandrel with a diameter of 110 mm drawn from hardened tool steel and finally stretched to the desired length and wall thickness. The stretching is done through a mandrel. The front pipe is made to a wall thickness of 0.7 mm and a length formed from 1500 mm.

Um Rohre noch größeren Umfangs herzustellen, kann das Rohr mehrere Längs- oder auch Rund-Schweißnähte beinhalten. Mit handelsüblichen Walzdrückmaschinen können auf diese Weise Rohre bis zu einem Durchmesser von ca. 650 mm und einer Länge von ca. 8000 mm hergestellt werden, wobei diese Angaben nicht als limitierend anzusehen sind.In order to manufacture pipes of even greater size, the pipe can be several longitudinal or also Include round welds. You can use standard roll spinning machines to do this Wise pipes up to a diameter of approx. 650 mm and a length of approx. 8000 mm are produced, whereby this information is not to be regarded as limiting.

Claims (13)

Verfahren zur Herstellung eines aus durch feinverteilte, kleine Teilchen aus Unedelmetalloxid dispersionsverfestigtem Platinwerkstoff bestehenden, geschweißten, insbesondere mindestens eine Innenwand aufweisenden Formkörpers, insbesondere eines Rohres, wobei das Unedelmetalloxid ein oder mehrere Oxide der Elemente Yttrium, Zirkonium und Cer ist, mit folgenden Verfahrensschritten: Formen und Verschweißen mindestens eines Teils, inbesondere eines Blechs, einer Platin-Unedelmetall-Legierung zu einem Vorformkörper, insbesondere zu einem Rohr, Wärmebehandlung des Vorformkörpers in einem oxidierenden Medium bis zu einem Mindestoxidationsgrad des Unedelmetalls von 75 Gewichts-%, Umformen des Vorformkörpers. Process for the production of a welded molded body consisting of finely divided, small particles of base metal oxide and strengthened platinum material, in particular having at least one inner wall, in particular a tube, the base metal oxide being one or more oxides of the elements yttrium, zirconium and cerium, with the following process steps: Forming and welding at least one part, in particular a sheet, of a platinum-base metal alloy into a preform, in particular into a tube, Heat treatment of the preform in an oxidizing medium up to a minimum degree of oxidation of the base metal of 75% by weight, Forming the preform body. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß der umgeformte Vorformkörper rekristallisationsglühbehandelt wird. Method according to claim 1, characterized in that the shaped preform body is recrystallization annealed. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß die Glühbehandlung bei einer Mindesttemperatur von 600 °C durchgeführt wird.A method according to claim 1 or 2, characterized in that the annealing treatment is carried out at a minimum temperature of 600 ° C. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß die Glühbehandlung bei einer Maximaltemperatur von 1.400 °C durchgeführt wird.Method according to one of claims 1 to 3, characterized in that the annealing treatment is carried out at a maximum temperature of 1,400 ° C. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß beim Umformen des Vorformkörpers, insbesondere beim Abstrecken, eine Reduzierung der Wandstärke von mindestens 50 % erreicht wird.Method according to one of claims 1 to 4, characterized in that during forming of the preform body, especially when stretching, a reduction in the wall thickness of at least 50% is reached. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß der Unedelmetallgehalt der Platin-Unedelmetall-Legierung 0,005 - 1 Gewichts-% beträgt.Method according to one of claims 1 to 5, characterized in that the base metal content the platinum-base metal alloy is 0.005-1% by weight. Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß der disperionsverfestigte Platinwerkstoff aus dispersionsverfestigter Platin-Rhodium-Legierung, dispersionsverfestigter Platin-Iridium-Legierung oder dispersionsverfestigter Platin-Gold-Legierung besteht.Method according to one of claims 1 to 6, characterized in that the dispersion-strengthened Platinum material made of dispersion-strengthened platinum-rhodium alloy, dispersion-strengthened platinum-iridium alloy or dispersion-strengthened platinum-gold alloy consists. Verfahren nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, daß die Platin-Unedelmetall-Legierung mit 0,1 - 0,2 Gewichts-% Zirkonium und 0,01 - 0,05 Gewichts-% Yttrium und/oder mit 0,05 - 0,2 Gewichts-% Cer dotiert ist.Method according to one of claims 1 to 7, characterized in that the Platinum-base metal alloy with 0.1 - 0.2% by weight of zirconium and 0.01 - 0.05% by weight Yttrium and / or with 0.05 - 0.2% by weight cerium is doped. Verfahren nach einem der Ansprüche 7 bis 8, dadurch gekennzeichnet, daß die Platin-Rhodium-Legierung eine PtRh10-Legierung ist.Method according to one of claims 7 to 8, characterized in that the platinum-rhodium alloy is a PtRh10 alloy. Verfahren nach einem der Ansprüche 7 bis 8, dadurch gekennzeichnet, daß die Platin-Gold-Legierung eine PtAu5-Legierung ist.Method according to one of claims 7 to 8, characterized in that the platinum-gold alloy is a PtAu5 alloy. Verfahren nach einem der Ansprüche 7 bis 8, dadurch gekennzeichnet, daß die Platin-Iridium-Legierung eine PtIr(1-10)-Legierung ist.Method according to one of claims 7 to 8, characterized in that the platinum-iridium alloy is a PtIr (1-10) alloy. Formkörper, insbesondere Rohr, hergestellt nach einem Verfahren nach einem oder mehreren der Ansprüche 1 bis 11.Shaped body, in particular pipe, produced by a process according to one or more of claims 1 to 11. Verwendung eines Rohres nach Anspruch 12 zum Läutern von Glas.Use of a tube according to claim 12 for refining glass.
EP99104851A 1998-03-28 1999-03-11 Process for preparing a welded workpiece, in particular a tube, from dispersion-hardened platinum material Expired - Lifetime EP0947595B1 (en)

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EP3121297A1 (en) 2015-07-23 2017-01-25 Cartier International AG Method for obtaining a trim component in platinum alloy
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