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EP0285741B1 - Process for the production of a highly ductile semi-finished tantalum product - Google Patents

Process for the production of a highly ductile semi-finished tantalum product Download PDF

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Publication number
EP0285741B1
EP0285741B1 EP88100151A EP88100151A EP0285741B1 EP 0285741 B1 EP0285741 B1 EP 0285741B1 EP 88100151 A EP88100151 A EP 88100151A EP 88100151 A EP88100151 A EP 88100151A EP 0285741 B1 EP0285741 B1 EP 0285741B1
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Prior art keywords
block
melt
cold
slab
semi
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German (de)
French (fr)
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EP0285741A1 (en
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Michael Dr. Hörmann
Otto Bach
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WC Heraus GmbH and Co KG
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D27/00Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
    • B22D27/15Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting by using vacuum
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing 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
    • C22F1/18High-melting or refractory metals or alloys based thereon

Definitions

  • the invention relates to a method for producing highly ductile semi-finished tantalum products for use in the field of high-speed forming.
  • the object of the present invention is to provide a method for producing highly ductile semi-finished tantalum product, which is suitable for use in the field of high-speed forming, in particular for projectiles.
  • the melting block which is obtained by melting the body made of powder by pressing, is advantageously melted at a higher melting rate (kg / h) in the electron-beam furnace than the aforementioned body.
  • the melt rate for the melt block has proven to be at least twice as large as the melt rate for the body produced by pressing the powder.
  • the melting block obtained from the last remelting cycle is first cold-forged into a blank, which is divided into block-shaped individual pieces. Then each individual piece is heated to a temperature of about 650 ° in a slightly oxidizing atmosphere and, after removal from the oven, if the individual piece still has a temperature in the range from 450 to 600 ° C., is compressed. After cooling completely to room temperature, the compressed body is cold forged into a slab.
  • a cold rolling step with degrees of deformation of p 1,2 1.2 ( ⁇ ⁇ 70%), which comprises both rolling in the direction of the axis of the last melt block obtained and in a direction transverse thereto . It is expedient to carry out a stress relief annealing at a temperature of about 650 ° C. before the cold rolling step and a recrystallization annealing in the range of about 900 ° C. after the cold rolling step.
  • the tantalum semi-finished products produced according to the invention are texture-free and have a grain size that is finer than 30 ⁇ m (according to ASTM E 112). Their tensile strength is less than 200 N / mm z , their elongation is greater than 60%.
  • the overall purity of the materials according to the invention is calculated by determining the residual resistance ratio (electrical resistance at the temperature of 273 K: by electrical resistance at the temperature of 4.2 K). It is at least 200 for materials according to the invention.
  • a method for producing a highly ductile tantalum semi-finished product according to the invention is described with the aid of the exemplary embodiment below.
  • Sodium-reduced tantalum powder was used to produce the rod-shaped body produced by pressing, the impurity contents ( li g / g) of which are shown in the table below:
  • a rod-shaped body was produced from this tantalum powder by cold isostatic pressing. This body was used as a melting electrode in an electron beam furnace and melted at a melting rate in the range from 25 to 35 kg / h. During the melting process en maintain a pressure of 2 x 10- 4 mbar. The melt was collected in a water-cooled mold and a melting block (ingot) with a diameter of 150 mm was formed. This melting block was then remelted three times in the electron beam furnace by melting, the melting block formed in each case being used again as a melting electrode.
  • the melting rate was in the range of 70 to 100 kg / h.
  • the corresponding values for the second remelting process were 6 x 10- 5 mbar, the melting rate was again in the range from 70 to 100 kg / h, while during the last remelting process the pressure in the electron beam furnace was reduced to 3 x 10- 5 mbar and the melting rate was 120 Kg / h.
  • the diameter of the melting block obtained from the last remelting cycle was 175 mm.
  • the last melt block obtained was then preformed into a slab by thermo-mechanical shaping.
  • the melting block was first cold forged on 150 mm octagon, after which it was cut into block-shaped individual pieces of 350 mm length. Each individual piece was then heated to 650 ° C. in a slightly oxidized atmosphere in a gas-heated hearth furnace and held at this temperature for a period of about 2 to 3 hours. After removal from the hearth furnace, the individual pieces were compressed at a temperature of approx. 550 ° C on a forging hammer. After it had completely cooled to room temperature, the compressed individual piece was cold forged into a slab, up to dimensions in mm of approx. 160 x 65 x 800.
  • the smoothed slab was degreased and first pickled in aqua regia and then in an acid mixture consisting of one part by volume of concentrated hydrofluoric acid, two parts by volume of concentrated nitric acid and two parts by volume of water.
  • the degree of deformation was p ⁇ 1.3 (e ⁇ 75%). After this cold rolling process, the cold-rolled part was degreased and pickled.
  • a stress relief annealing was carried out in an inductively heated furnace in which x 10- 4 mbar was maintained during the heat treatment, a pressure of the second
  • the annealed part was subjected to several cold rolling steps, in which case rolling was again carried out in the direction along and across the axis of the melting block obtained last.
  • This cold rolling process was also carried out with a high number of individual passes. The degree of deformation was p ⁇ 1.9 (e ⁇ 85%).
  • the workpiece was ground, degreased and pickled again, as already described above, and then subjected to recrystallization annealing at 875 ° C. in a resistance-heated vacuum oven.
  • the highly ductile semi-finished tantalum product thus obtained was texture-free and had a grain size finer than 30 f.1m according to (ASTM E 112). Its tensile strength was 192 N / mm 2 , its elongation was 65%, the residual resistance ratio was found to be 220.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Forging (AREA)

Description

Die Erfindung betrifft ein Verfahren zur Herstellung von hochduktilem Tantal-Halbzeug für die Verwendung auf dem Gebiet der Hochgeschwindigkeitsumformung.The invention relates to a method for producing highly ductile semi-finished tantalum products for use in the field of high-speed forming.

Auf dem Gebiet der Hochgeschwindigkeitsumformung, wie sie z. B. bei Geschoßen vorkommt, wird üblicherweise hochduktiles Eisen oder Kupfer verwendet. Die Eindringtiefe der Geschoße ist eine Funktion sowohl der Dichte des verwendeten hochduktilen Werkstoffes als auch der Dichte des Werkstoffes, auf den das Geschoß auftrifft. Man ist daher seit langem bestrebt, einen hochduktilen Werkstoff sehr hoher Dichte herzustellen.In the field of high speed forming, as e.g. B. occurs in the case of bullets, usually highly ductile iron or copper is used. The penetration depth of the projectiles is a function of both the density of the highly ductile material used and the density of the material that the projectile strikes. For this reason, efforts have long been made to produce a highly ductile material of very high density.

Die Aufgabe der vorliegenden Erfindung besteht darin, ein Verfahren zur Herstellung von hochduktilem Tantal-Halbzeug bereitzustellen, das für die Verwendung auf dem Gebiet der Hochgeschwindigkeitsumformung, insbesondere für Geschosse, geeignet ist.The object of the present invention is to provide a method for producing highly ductile semi-finished tantalum product, which is suitable for use in the field of high-speed forming, in particular for projectiles.

Gelöst wird diese Aufgabe erfindungsgemäß durch folgende Verfahrensschritte:

  • a) aus mit direkt-reduziertem Tantal-Pulver, das pro g-Pulver weniger als 100 µg Niob, Wolfram und/oder Molybdän enthält, wird durch Pressen ein stabförmiger Körper hergestellt,
  • b) der Körper wird in einem Elektronenstrahl-Ofen unter Aufrechterhaltung eines Druckes von weniger als 5 x 10-4 mbar abgeschmolzen, die Schmelze in einer gekühlten Kokille gesammelt und ein Schmelzblock gebildet,
  • c) der Schmelzblock wird mindestens zweimal im Elektronenstrahlofen unter Aufrechterhaltung eines Druckes von weniger als 5 x 10-4 mbar durch Abschmelzen umgeschmolzen,
  • d) der vom letzten Umschmelzzyklus erhaltene Schmelzblock wird zu einer Bramme verformt,
  • e) die Bramme wird allseitig spanabhebend mit einer Rauhtiefe von maximal 25 µm geglättet,
  • f) aus der glatten Bramme werden in üblicher Weise Halbzeug durch Verformen hergestellt, wobei in diesen Herstellungsprozeß mindestens eine Wärmebehandlung in einem induktiv und/oder widerstandsbeheizten Ofen unter Aufrechterhaltung eines Druckes von weniger als 5 x 10-4 mbar einbezogen wird.
According to the invention, this object is achieved by the following process steps:
  • a) a rod-shaped body is produced by pressing with directly reduced tantalum powder, which contains less than 100 μg of niobium, tungsten and / or molybdenum per g powder,
  • b) the body in an electron beam furnace, maintaining a pressure of less than 5 x 10- 4 mbar melted, the melt is collected in a cooled mold and forming a cast ingot,
  • c) melting the block is 5 x 10- 4 remelted at least twice in the electron beam furnace, maintaining a pressure of less than mbar by melting,
  • d) the melting block obtained from the last remelting cycle is deformed into a slab,
  • e) the slab is machined on all sides with a maximum roughness depth of 25 µm,
  • f) from the smooth slab, semi-finished products are produced by molding in a conventional manner, in this production process at least one heat treatment in an inductively and / or resistance-heated furnace while maintaining a pressure of less than 5 x 10- 4 mbar is included.

Bewährt hat es sich bei dem erfindungsgemäßen Verfahren Natrium-reduziertes Tantal-Pulver zu verwenden. Der Schmelzblock, der durch Abschmelzen des aus Pulver durch Pressen hergestellten Körpers erhalten wird, wird vorteilhafterweise mit einer höheren Schmelzrate (kg/h) im Elektronenstrahl- ofen abgeschmolzen als der vorerwähnte Körper. Bewährt hat sich dabei die Schmelzrate für den Schmelzblock wenigstens doppelt so groß zu wählen wie die Schmelzrate für den durch Pressen des Pulvers hergestellten Körper.It has proven useful to use sodium-reduced tantalum powder in the process according to the invention. The melting block, which is obtained by melting the body made of powder by pressing, is advantageously melted at a higher melting rate (kg / h) in the electron-beam furnace than the aforementioned body. The melt rate for the melt block has proven to be at least twice as large as the melt rate for the body produced by pressing the powder.

Zur Herstellung der Bramme wird vorteilhafterweise der vom letzten Umschmelzzyklus erhaltene Schmelzblock zunächst durch Kaltschmieden zu einem Rohling verformt, der in blockförmige Einzelstücke zerteilt wird. Danach wird jedes Einzelstück in leicht oxidierender Atmosphäre auf eine Temperatur von etwa 650° aufgeheizt und nach Entnahme aus dem Ofen, wenn das Einzelstück noch eine Temperatur im Bereich von 450 bis 600°C besitzt, gestaucht. Nach vollständiger Abkühlung auf Raumtemperatur wird der gestauchte Körper kalt zu einer Bramme geschmiedet.To produce the slab, the melting block obtained from the last remelting cycle is first cold-forged into a blank, which is divided into block-shaped individual pieces. Then each individual piece is heated to a temperature of about 650 ° in a slightly oxidizing atmosphere and, after removal from the oven, if the individual piece still has a temperature in the range from 450 to 600 ° C., is compressed. After cooling completely to room temperature, the compressed body is cold forged into a slab.

Bewährt hat es sich, in den Herstellungsprozeß für das Halbzeug einen Kaltwalzschritt mit Umformgraden von p ä 1,2 (ε ≥ 70 %) einzuschalten, der sowohl ein Walzen in Richtung der Achse des zuletzt erhaltenen Schmelzblockes als auch in einer dazu quer verlaufenden Richtung umfaßt. Dabei ist es zweckmäßig, vor dem Kaltwalzschritt eine Entspannungsglühung bei einer Temperatur von etwa 650°C und nach dem Kaltwalzschritt eine Rekristallisationsglühung im Bereich von etwa 900°C durchzuführen.It has proven to be useful in the manufacturing process for the semifinished product to use a cold rolling step with degrees of deformation of p 1,2 1.2 (ε ≥ 70%), which comprises both rolling in the direction of the axis of the last melt block obtained and in a direction transverse thereto . It is expedient to carry out a stress relief annealing at a temperature of about 650 ° C. before the cold rolling step and a recrystallization annealing in the range of about 900 ° C. after the cold rolling step.

Als Ergebnis des erfindungsgemäßen Verfahrens erhält man hochduktile Tantal-Halbzeuge, die bezüglich ihrer mechanischen Eigenschaften und ihres Gefügeaufbaus isotrop sind. Die erfindungsgemäß hergestellten Tantal-Halbzeuge sind Textur-frei und besitzen eine Korngröße, die feiner als 30 µm (nach ASTM E 112) ist. Ihre Zugfestigkeit ist kleiner als 200 N/mmz, ihre Dehnung ist größer als 60 %. Die Gesamtreinheit der erfindungsgemäßen Werkstoffe wird durch die Bestimmung des Restwiderstandsverhältnisses (elektrischer Widerstand bei der Temperatur von 273 K : durch elektrischen Widerstand bei der Temperatur von 4,2 K) errechnet. Es beträgt bei erfindungsgemäßen Werkstoffen wenigstens 200.As a result of the process according to the invention, highly ductile semifinished tantalum products are obtained which are isotropic with regard to their mechanical properties and their structure. The tantalum semi-finished products produced according to the invention are texture-free and have a grain size that is finer than 30 μm (according to ASTM E 112). Their tensile strength is less than 200 N / mm z , their elongation is greater than 60%. The overall purity of the materials according to the invention is calculated by determining the residual resistance ratio (electrical resistance at the temperature of 273 K: by electrical resistance at the temperature of 4.2 K). It is at least 200 for materials according to the invention.

Anhand des nachfolgenden Ausführungsbeispiels wird ein Verfahren zur Herstellung eines erfindungsgemäßen hochduktilen Tantal-Halbzeuges beschrieben.A method for producing a highly ductile tantalum semi-finished product according to the invention is described with the aid of the exemplary embodiment below.

Zur Herstellung des durch Pressen erzeugten stabförmigen Körpers wurde Natrium-reduziertes Tantal-Pulver verwendet, dessen Verunreinigungsgehalte (lig/g) sich aus nachstehender Tabelle ergeben:

Figure imgb0001
Aus diesem Tantal-Pulver wurde durch kalt-isostatisches Pressen ein stabförmiger Körper hergestellt. Dieser Körper wurde als Abschmelzelektrode in einen Elektronenstrahlofen eingesetzt und mit einer Schmelzrate im Bereich von 25 bis 35 kg/h abgeschmolzen. Während des Abschmelzprozesses wurde ein Druck von 2 x 10-4 mbar aufrechterhalten. Die Schmelze wurde in einer wassergekühlten Kokille gesammelt und ein Schmelzblock (Ingot) mit einem Durchmesser von 150 mm gebildet. Dieser Schmelzblock wurde anschließend dreimal in dem Elektronenstrahlofen durch Abschmelzen umgeschmolzen, wobei der jeweils gebildete Schmelzblock wieder als Abschmelzelektrode eingesetzt wurde. Während des ersten Umschmelzvorganges wurde in dem Elektronenstrahlofen ein Druck von 8 x 10-5 mbar aufrechterhalten, die Schmelzrate lag im Bereich von 70 bis 100 Kg/h. Die entsprechenden Werte für den zweiten Umschmelzvorgang betrugen 6 x 10-5 mbar, die Schmelzrate lag wiederum im Bereich von 70 bis 100 Kg/h, während beim letzten Umschmelzvorgang der Druck im Elektronenstrahlofen auf 3 x 10-5 mbar abgesenkt war und die Schmelzrate 120 Kg/h betrug. Der Durchmesser des vom letzten Umschmelzzyklus erhaltenen Schmelzblocks betrug 175 mm.Sodium-reduced tantalum powder was used to produce the rod-shaped body produced by pressing, the impurity contents ( li g / g) of which are shown in the table below:
Figure imgb0001
A rod-shaped body was produced from this tantalum powder by cold isostatic pressing. This body was used as a melting electrode in an electron beam furnace and melted at a melting rate in the range from 25 to 35 kg / h. During the melting process en maintain a pressure of 2 x 10- 4 mbar. The melt was collected in a water-cooled mold and a melting block (ingot) with a diameter of 150 mm was formed. This melting block was then remelted three times in the electron beam furnace by melting, the melting block formed in each case being used again as a melting electrode. During the first remelting process, a pressure of 8 x 10-5 mbar was maintained in the electron beam furnace, the melting rate was in the range of 70 to 100 kg / h. The corresponding values for the second remelting process were 6 x 10- 5 mbar, the melting rate was again in the range from 70 to 100 kg / h, while during the last remelting process the pressure in the electron beam furnace was reduced to 3 x 10- 5 mbar and the melting rate was 120 Kg / h. The diameter of the melting block obtained from the last remelting cycle was 175 mm.

Der zuletzt erhaltene Schmelzblock wurde danach durch thermo-mechanische Umformung zu einer Bramme vorformt. Dabei wurde zunächst der Schmelzblock an 150 mm achtkant kaltgeschmiedet, danach wurde er in blockförmige Einzelstücke von 350 mm Länge zerteilt. Jedes Einzelstück wurde dann in leicht oxidierender Atmosphäre in einem gasbeheizten Herdofen auf 650 °C aufgeheizt und bei dieser Temperatur während einer Dauer von etwa 2 bis 3 Stunden gehalten. Nach der Entnahme aus dem Herdofen wurden die Einzelstücke bei einer Temperatur von ca. 550 °C auf einem Schmiedehammer gestaucht. Nach seiner vollständigen Abkühlung auf Raumtemperatur wurde das gestauchte Einzelstück zu einer Bramme kaltgeschmiedet, bis an Abmessungen in mm von ca. 160 x 65 x 800. Hieran schloß sich ein Fräsvorgang mit einer Rauhtiefe von 20 J.Lm zur Glättung der Bramme an. Die geglättete Bramme wurde entfettet und zunächst in Königswasser und danach in einem Säuregemisch, das aus einem Volumenanteil konzentrierter Fluorwasserstoffsäure, zwei Volumenanteilen konzentrierter Salpetersäure und zwei Volumenanteile Wasser bestand, gebeizt. Hieran schloß sich ein Kaltwalzen mit hoher Einzelstichabnahme an, wobei sowohl in Richtung der Achse des zuletzt erhaltenen Schmelzblockes als auch in einer quer dazu verlaufenden Richtung gewalzt wurde. Der Verformungsgrad betrug p ≥ 1,3 (e ≥ 75 %). Nach diesem Kaltwalzvorgang wurde das kaltgewalzte Teil entfettet und gebeizt. Danach wurde eine Entspannungsglühung in einem induktiv beheizten Ofen durchgeführt, in dem während der Wärmebehandlung ein Druck von 2 x 10-4 mbar aufrechterhalten wurde. Nach dieser Entspannungsglühung wurde das geglühte Teil mehreren Kaltwalzschritten unterworfen, wobei wiederum ein Walzen in Richtung längs und quer zur Achse des zuletzt erhaltenen Schmelzblocks durchgeführt wurde. Auch dieser Kaltwalzvorgang wurde mit hoher Einzelstichabnahme durchgeführt. Der Verformungsgrad betrug p ≥ 1,9 (e ≥ 85 %). Im Anschluß an diesen Kaltwalzschritt wurde das Werkstück wieder, wie bereits oben geschildert, geschliffen, entfettet und gebeizt und dann in einem widerstandsbeheizten Vakuumofen einer Rekristallisationsglühung bei 875 °C unterworfen.The last melt block obtained was then preformed into a slab by thermo-mechanical shaping. The melting block was first cold forged on 150 mm octagon, after which it was cut into block-shaped individual pieces of 350 mm length. Each individual piece was then heated to 650 ° C. in a slightly oxidized atmosphere in a gas-heated hearth furnace and held at this temperature for a period of about 2 to 3 hours. After removal from the hearth furnace, the individual pieces were compressed at a temperature of approx. 550 ° C on a forging hammer. After it had completely cooled to room temperature, the compressed individual piece was cold forged into a slab, up to dimensions in mm of approx. 160 x 65 x 800. This was followed by a milling process with a roughness depth of 20 J.Lm to smooth the slab. The smoothed slab was degreased and first pickled in aqua regia and then in an acid mixture consisting of one part by volume of concentrated hydrofluoric acid, two parts by volume of concentrated nitric acid and two parts by volume of water. This was followed by cold rolling with a high single pass reduction, rolling both in the direction of the axis of the last block obtained and in a direction transverse to it. The degree of deformation was p ≥ 1.3 (e ≥ 75%). After this cold rolling process, the cold-rolled part was degreased and pickled. Subsequently, a stress relief annealing was carried out in an inductively heated furnace in which x 10- 4 mbar was maintained during the heat treatment, a pressure of the second After this stress relief annealing, the annealed part was subjected to several cold rolling steps, in which case rolling was again carried out in the direction along and across the axis of the melting block obtained last. This cold rolling process was also carried out with a high number of individual passes. The degree of deformation was p ≥ 1.9 (e ≥ 85%). Following this cold rolling step, the workpiece was ground, degreased and pickled again, as already described above, and then subjected to recrystallization annealing at 875 ° C. in a resistance-heated vacuum oven.

Das so erhaltene hochduktile Tantal-Halbzeug war Textur-frei und wies eine Korngröße feiner als 30 f.1m nach (ASTM E 112) auf. Seine Zugfestigkeit betrug 192 N/mm2, seine Dehnung betrug 65 %, das Restwiderstandsverhältnis wurde mit 220 ermittelt.The highly ductile semi-finished tantalum product thus obtained was texture-free and had a grain size finer than 30 f.1m according to (ASTM E 112). Its tensile strength was 192 N / mm 2 , its elongation was 65%, the residual resistance ratio was found to be 220.

Claims (6)

1. A method for the production of highly ductile tantalum semi-finished products for use in the field of high speed deformation, characterized by the following process steps:
a) from directly reduced tantalum powder, which contains per g of powder less than 100 µg niobium, tungsten and/or molybdenum, a bar-shaped body is produced by pressing,
b) the body is melted off in an electron beam furnace, maintaining a pressure of less than 5 x 10-4mbar, the melt is collected in a cooled chill and a block of melt is formed,
c) the block of melt is remelted at least twice in the electron beam furnace, maintaining a pressure of less than 5 x 10-4 mbar, by melting off,
d) the block of melt obtained from the last remelting cycle is deformed into a slab,
e) the slab is smoothed on all sides by machining, with a peak-to-valley height of a maximum of 25 µm,
f) from the smooth slab, semi-finished products are produced in a conventional manner through deformation, in which in this production process at least one thermal treatment is included, in an inductively- and/or resistance-heated furnace, maintaining a pressure of less than 5 x 10-4 mbar.
2. A method according to Claim 1, characterized in that the block of melt is melted off at a higher melting rate (kg/h) than the body produced by pressing.
3. A method according to Claim 2, characterized in that the melting rate for the block of melt is selected to be at least approximately twice as great as the melting rate for the body produced by pressing.
4. A method according to Claims 1 to 3, characterized in that the block of melt obtained from the last remelting cycle is shaped by cold-forging into a blank which is divided into block-shaped individual pieces, after which each individual piece is heated in a slightly oxidizing atmosphere to a temperature of approximately 650°C, after a slight cooling is pressure-forged at a temperature in the range of 450 to 600° C, and after complete cooling to room temperature, is cold-forged into a slab.
5. A method according to Claims 1 to 4, characterized in that there is included into the manufacturing process for the semi-finished product a cold-rolling with conversion ratios of p ≥ 1.2 (e ≥ 70%), which comprises both a rolling in the direction of the axis of the block of melt last obtained and also in a direction running transversely thereto.
6. A method according to Claim 5, characterized in that before the cold-rolling, a stress-relieving annealing is carried out at a temperature of approximately 650° C and after the cold-rolling a process annealing is carried out in the range of approximately 800 to 900° C.
EP88100151A 1987-04-10 1988-01-08 Process for the production of a highly ductile semi-finished tantalum product Expired - Lifetime EP0285741B1 (en)

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DE19873712281 DE3712281A1 (en) 1987-04-10 1987-04-10 METHOD FOR PRODUCING HIGHLY DUCTILE TANTALE SEMI-FINISHED PRODUCTS
DE3712281 1987-04-10

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Cited By (2)

* Cited by examiner, † Cited by third party
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* Cited by examiner, † Cited by third party
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US5411611A (en) * 1993-08-05 1995-05-02 Cabot Corporation Consumable electrode method for forming micro-alloyed products
US6323055B1 (en) * 1998-05-27 2001-11-27 The Alta Group, Inc. Tantalum sputtering target and method of manufacture
US6348139B1 (en) * 1998-06-17 2002-02-19 Honeywell International Inc. Tantalum-comprising articles
CN1066367C (en) * 1998-11-12 2001-05-30 北京有色金属研究总院 Method for making molybdenum electrode blank and molybdenum head piece blank by using electron-beam smelting method
US20040072009A1 (en) * 1999-12-16 2004-04-15 Segal Vladimir M. Copper sputtering targets and methods of forming copper sputtering targets
US6878250B1 (en) * 1999-12-16 2005-04-12 Honeywell International Inc. Sputtering targets formed from cast materials
US7517417B2 (en) * 2000-02-02 2009-04-14 Honeywell International Inc. Tantalum PVD component producing methods
US6331233B1 (en) 2000-02-02 2001-12-18 Honeywell International Inc. Tantalum sputtering target with fine grains and uniform texture and method of manufacture
IL156802A0 (en) 2001-01-11 2004-02-08 Cabot Corp Tantalum and niobium billets and methods of producing same
RU2205248C2 (en) * 2001-02-19 2003-05-27 Федеральное государственное унитарное предприятие "Всероссийский научно-исследовательский институт неорганических материалов имени академика А.А. Бочвара" Method for manufacture of tantalum tape
US7416697B2 (en) 2002-06-14 2008-08-26 General Electric Company Method for preparing a metallic article having an other additive constituent, without any melting
US7897103B2 (en) * 2002-12-23 2011-03-01 General Electric Company Method for making and using a rod assembly
US7228722B2 (en) * 2003-06-09 2007-06-12 Cabot Corporation Method of forming sputtering articles by multidirectional deformation
US20040256226A1 (en) * 2003-06-20 2004-12-23 Wickersham Charles E. Method and design for sputter target attachment to a backing plate
US7531021B2 (en) 2004-11-12 2009-05-12 General Electric Company Article having a dispersion of ultrafine titanium boride particles in a titanium-base matrix
US7396412B2 (en) 2004-12-22 2008-07-08 Sokudo Co., Ltd. Coat/develop module with shared dispense
US7798764B2 (en) 2005-12-22 2010-09-21 Applied Materials, Inc. Substrate processing sequence in a cartesian robot cluster tool
US7699021B2 (en) 2004-12-22 2010-04-20 Sokudo Co., Ltd. Cluster tool substrate throughput optimization
US7819079B2 (en) 2004-12-22 2010-10-26 Applied Materials, Inc. Cartesian cluster tool configuration for lithography type processes
US7651306B2 (en) 2004-12-22 2010-01-26 Applied Materials, Inc. Cartesian robot cluster tool architecture
US7998287B2 (en) * 2005-02-10 2011-08-16 Cabot Corporation Tantalum sputtering target and method of fabrication
US20070084527A1 (en) * 2005-10-19 2007-04-19 Stephane Ferrasse High-strength mechanical and structural components, and methods of making high-strength components
US20070251818A1 (en) * 2006-05-01 2007-11-01 Wuwen Yi Copper physical vapor deposition targets and methods of making copper physical vapor deposition targets
CN120628214B (en) * 2025-08-08 2025-10-10 四川省第七地质大队 Geological disaster displacement monitoring device based on geological analysis

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2825641A (en) * 1955-09-21 1958-03-04 Robert A Beall Method for melting refractory metals for casting purposes
NL252366A (en) * 1958-06-13
US3285716A (en) * 1964-07-20 1966-11-15 Kawecki Chemical Company Etched tantalum foil
US3497402A (en) * 1966-02-03 1970-02-24 Nat Res Corp Stabilized grain-size tantalum alloy
RO76187A2 (en) * 1980-11-14 1983-08-03 Institutul De Cercetare Stiintifica Inginerie Tehnologica Si Proiectare Sectoare Calde,Ro PROCESS AND INSTALLATION FOR FUSION AND CASTING OF METALS AT HIGH TEMPERATURE OF FUSION
JPS6066425A (en) * 1983-09-22 1985-04-16 Nippon Telegr & Teleph Corp <Ntt> High-purity molybdenum target and high-purity molybdenum silicide target for lsi electrode and manufacture thereof
JPS60124452A (en) * 1983-12-07 1985-07-03 Hitachi Ltd Manufacturing method of high purity metal sleeve
US4722756A (en) * 1987-02-27 1988-02-02 Cabot Corp Method for deoxidizing tantalum material

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7431782B2 (en) 1998-11-25 2008-10-07 Cabot Corporation High purity tantalum, products containing the same, and methods of making the same
US7585380B2 (en) 1998-11-25 2009-09-08 Cabot Corporation High purity tantalum, products containing the same, and methods of making the same
US8382920B2 (en) 2006-03-07 2013-02-26 Global Advanced Metals, Usa, Inc. Methods of producing deformed metal articles
US8974611B2 (en) 2006-03-07 2015-03-10 Global Advanced Metals, Usa, Inc. Methods of producing deformed metal articles

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US4844746A (en) 1989-07-04
DE3860768D1 (en) 1990-11-15
DE3712281A1 (en) 1988-10-27
EP0285741A1 (en) 1988-10-12

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