EP0137315A2 - Process and apparatus for the manufacture of high-purity alloys - Google Patents

Process and apparatus for the manufacture of high-purity alloys Download PDF

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Publication number
EP0137315A2
EP0137315A2 EP84110654A EP84110654A EP0137315A2 EP 0137315 A2 EP0137315 A2 EP 0137315A2 EP 84110654 A EP84110654 A EP 84110654A EP 84110654 A EP84110654 A EP 84110654A EP 0137315 A2 EP0137315 A2 EP 0137315A2
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EP
European Patent Office
Prior art keywords
crucible
melt
plant according
vacuum
melting
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EP84110654A
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German (de)
French (fr)
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EP0137315B1 (en
EP0137315A3 (en
Inventor
Jürgen Dr.-Ing. Hartwig
Johannes Jachowski
Paul Dipl.-Ing. Pant
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Fried Krupp AG
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Fried Krupp AG
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Application filed by Fried Krupp AG filed Critical Fried Krupp AG
Priority to AT84110654T priority Critical patent/ATE34775T1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
    • B22D27/15—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting by using vacuum

Definitions

  • the starting material forming the alloy is melted in an induction crucible, subjected to a vacuum treatment and then poured into a resistance-heated casting funnel, from which it is poured to form a certain metallostatic height and z. B. passes through a spray system into a spray chamber.
  • ceramic particles from the lining of the induction crucible and slag particles - the latter also when the pouring funnel flows empty - can get into the atomization chamber - especially in the initial phase of the pouring, in which no metallostatic height has yet been established in the pouring funnel.
  • the liquid material reacts with the lining of the pouring funnel to form further impurities which also end up in the end product.
  • the invention is based on the object of specifying a method for producing high-purity alloys, the use of which improves the degree of purity of the alloy and can be maintained throughout the entire casting phase. Furthermore, an installation for carrying out the method is to be created.
  • the degree of purity can be influenced even more favorably by the measure according to claim 2.
  • the system comprises an induction melting crucible 1, which is housed in a vacuum vessel 2.
  • a resistance-heated melting furnace 3 which has an outflow nozzle 4 in its bottom.
  • the melting furnace 3 is assigned a closing arrangement 5, which has a stopper rod 6, which is inserted from above through a vacuum guide 7 into the vacuum vessel 2 and can be operated by a control device 8.
  • the plug rod 6 is provided with a casing and / or coating 9.
  • the part of the sealing rod 6 located above the casing, the vacuum guide 7 and / or the control device 8 can be connected to a cooling system (not shown) in order to keep harmful thermal influences as low as possible.
  • nozzles 10 which point into the interior of the melting furnace 3 and which are connected to an inert gas line (not shown) on the outside.
  • the stopper rod 6 has at its lower end laterally directed nozzles 11 into the cavity of the melting furnace 3 and a nozzle 12 directed towards the outflow nozzle 4.
  • the nozzles 11 and 12 are connected to an inert gas supply (not shown).
  • the starting material is first introduced into the induction crucible 1.
  • the alloy is used to adjust the required casting temperature and for refining treatment, i. H. Transferred to the resistance-heated melting furnace 3 to remove all non-metallic impurities due to density-related buoyancy and to set the casting temperature.
  • the density-related buoyancy of the non-metallic impurities can be supported by the inert gas that passes through the nozzles 10 and / or 11 into the melt.
  • the melt is kept at a constant casting temperature for the duration of the refining treatment.
  • the stopper rod 6 is raised by actuating the control device 8 and the outflow nozzle 4 is thereby opened.
  • the inert gas jet emerging through the nozzle 12 can be used to support the atomization of the alloy stream flowing into the atomization chamber 13.
  • the resistance-heated melting furnace 3 can be used for casting the alloy in the form, block and continuous casting process.

Abstract

Process and system for the production of very pure alloys. The starting materials are first melted and vacuum treated in an induction crucible inside a vacuum melt system, and then are poured into a second melt crucible, and there brought to casting temperature and held there. An opening beneath the melt in the second melt crucible is used for pouring out the melt. The system for carrying out the process comprises a vacuum melt crucible assembly containing an induction melt crucible and a second melt crucible. The second melt crucible has an orifice in its lower area which is operated by a sealing arrangement. A chamber is arranged underneath the second melt crucible.

Description

Bei einem bekannten Verfahren wird das die Legierung bildende Ausgangsmaterial in einem Induktionstiegel erschmolzen, einer Vakuumbehandlung unterzogen und anschließend in einen widerstandsbeheizten Gießtrichter abgegossen, aus dem es unter Bildung einer bestimmten metallostatischen Höhe abgegossen und z. B. durch ein Verdüsungssystem in eine Verdüsungskammer gelangt. Bei diesem Verfahren können - insbesondere in der Anfangsphase des Abgießens, in der sich noch keine metallostatische Höhe im Gießtrichter eingestellt hat - keramische Teilchen der Auskleidung des Induktionstiegels und Schlackenteilchen - letztere auch beim Leerfließen des Gießtrichters - in den Verdüsungsraum gelangen. Weiterhin besteht bei diesem Verfahren die Gefahr, daß das flüssige Material mit der Auskleidung des Gießtrichters unter Bildung weiterer Verunreinigungen reagiert, die mit in das Endprodukt gelangen.In a known process, the starting material forming the alloy is melted in an induction crucible, subjected to a vacuum treatment and then poured into a resistance-heated casting funnel, from which it is poured to form a certain metallostatic height and z. B. passes through a spray system into a spray chamber. With this method, ceramic particles from the lining of the induction crucible and slag particles - the latter also when the pouring funnel flows empty - can get into the atomization chamber - especially in the initial phase of the pouring, in which no metallostatic height has yet been established in the pouring funnel. Furthermore, there is a risk with this method that the liquid material reacts with the lining of the pouring funnel to form further impurities which also end up in the end product.

Es ist auch bekannt, das die Legierung bildende Ausgangsmaterial in einem Induktionstiegel mit einer im Boden angeordneten Ausflußöffnung zu erschmelzen, wobei die Bodenöffnung durch eine entsprechende Stopfenanordnung verschließbar ist. Bei diesem Verfahren bleiben zwar die Schlackenteilchen weitgehend an der Oberfläche der Schmelze, es besteht jedoch die Gefahr, daß die Ver- schließanordnung sowohl bei der Beschickung des Tiegels mit dem festen Ausgangsmaterial beschädigt wird, als auch, daß die dichtenden Flächen der Verschließanordnung, d.h. sowohl des schließenden Teils als auch der Ausgußöffnung, bei der ständig im Induktionstiegel erzeugten Durchwirbelung der Schmelze erodiert werden.It is also known to melt the starting material forming the alloy in an induction crucible with an outflow opening arranged in the bottom, the bottom opening being closable by a corresponding plug arrangement. In this method, although the slag to remain largely on the surface of the melt, however, there is the danger that the V ER- damaged with the solid starting material closing arrangement, both for the feeding of the crucible, as also that the sealing surfaces of the closing arrangement, ie both the closing part and the pouring opening, are eroded during the swirling of the melt which is constantly generated in the induction crucible.

Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren zum Herstellen von hochreinen Legierungen anzugeben, bei dessen Anwendung der Reinheitsgrad der Legierung verbessert wird und durchgehend über die ganze Gießphase einhaltbar ist. Weiter soll eine Anlage zum Durchführen des Verfahrens geschaffen werden.The invention is based on the object of specifying a method for producing high-purity alloys, the use of which improves the degree of purity of the alloy and can be maintained throughout the entire casting phase. Furthermore, an installation for carrying out the method is to be created.

Diese Aufgabe wird durch die im Anspruch 1 gekennzeichneten Merkmale gelöst. Während durch die von dem Induktionstiegel in der Schmelze erzeugte Durchwirbelung ständig die zur Vakuumbehandlung erwünschte Bewegung des Schmelzbades vorhanden ist, wird das Material in dem weiteren Schmelztiegel strömungsmäßig in Ruhe gehalten. Dadurch können die nichtmetallischen Verunreinigungen, ihrem Auftrieb entsprechend, an die Oberfläche gelangen und dort verbleiben. Die in dem zweiten Schmelztiegel befindliche Schmelze erfährt also gegenüber den Bedingungen im Induktionstiegel einen höheren Reinheitsgrad. Da sich die Anreicherung der nichtmetallischen Verunreinigungen bereits vor dem Abfließen durch die unten gelegene Ausgußöffnung an der Oberfläche der Schmelze befindet, fließt vom Beginn des öffnens an ein hochreines Legierungsmaterial. Durch rechtzeitiges Betätigen der Verschließanordnung kann das Ausfließen der nichtmetallischen Verunreinigungen verhindert und so . der hohe Reinheitsgrad über die ganze Gießphase eingehalten werden.This object is achieved by the features characterized in claim 1. While the swirl generated by the induction crucible in the melt constantly provides the movement of the melt bath desired for vacuum treatment, the material in the further crucible is kept at rest in terms of flow. As a result, the non-metallic impurities, depending on their buoyancy, can reach the surface and remain there. The melt located in the second crucible therefore has a higher degree of purity than the conditions in the induction crucible. Since the enrichment of the non-metallic impurities is already on the surface of the melt before it flows out through the pouring opening below, a high-purity alloy material flows from the beginning of the opening. By timely actuation of the closure arrangement, the outflow of the non-metallic contaminants can be prevented and so. the high degree of purity can be maintained throughout the casting phase.

Der Reinheitsgrad kann durch die Maßnahme nach Anspruch 2 noch weiter günstig beeinflußt werden. Die weiteren Unteransprüche, die Ansprüche 3 bis 12, stellen eine vorteilhafte Anlage zur Durchführung des erfindungsgemäßen Verfahrens dar.The degree of purity can be influenced even more favorably by the measure according to claim 2. The further subclaims, claims 3 to 12, make an advantageous system for performing the method according to the invention.

Als ein Ausführungsbeispiel des Gegenstandes der Erfindung ist in der Zeichnung eine Anlage zum Inertgasverdüsen von Legierungspulver schematisch dargestellt, die im folgenden näher beschrieben wird. Die Anlage umfaßt einen Induktionsschmelztiegel 1, der in einem Vakuumkessel 2 untergebracht ist. In dem Vakuumkessel befindet sich außerdem ein widerstandsbeheizter Schmelzofen 3, der in seinem Boden eine Ausflußdüse 4 aufweist. Dem Schmelzofen 3 ist eine Verschließanordnung 5 zugeordnet, die eine Stopfenstange 6 aufweist, die von oben her durch eine Vakuumführung 7 in den Vakuumkessel 2 eingeführt ist und von einer Regelvorrichtung 8 bedient werden kann. An ihrem unteren Ende ist die Stopfenstange 6 mit einer Ummantelung und/oder Beschichtung 9 versehen.As an embodiment of the subject of the invention, a plant for the inert gas atomization of alloy powder is schematically shown in the drawing, which is described in more detail below. The system comprises an induction melting crucible 1, which is housed in a vacuum vessel 2. In the vacuum vessel there is also a resistance-heated melting furnace 3, which has an outflow nozzle 4 in its bottom. The melting furnace 3 is assigned a closing arrangement 5, which has a stopper rod 6, which is inserted from above through a vacuum guide 7 into the vacuum vessel 2 and can be operated by a control device 8. At its lower end, the plug rod 6 is provided with a casing and / or coating 9.

Der oberhalb der Ummantelung befindliche Teil der Verschlußstange 6, die Vakuumführung 7 und/oder die Regelvorrichtung 8 können, um schädliche thermische Einflüsse möglichst gering zu halten, an ein (nicht dargestelltes) Kühlsystem angeschlossen sein.The part of the sealing rod 6 located above the casing, the vacuum guide 7 and / or the control device 8 can be connected to a cooling system (not shown) in order to keep harmful thermal influences as low as possible.

Im unteren Bereich des Schmelzofens 3 sind Düsen 10 angeordnet, die in das Innere des Schmelzofens 3 weisen und die nach außen an eine (nicht dargestellte)Inertgasleitung angeschlossen sind.In the lower region of the melting furnace 3 there are nozzles 10 which point into the interior of the melting furnace 3 and which are connected to an inert gas line (not shown) on the outside.

Die Stopfenstange 6 weist an ihrem unteren Ende seitlich in den Hohlraum des Schmelzofens 3 gerichtete Düsen 11 sowie eine in Richtung der Ausflußdüse 4 gerichtete Düse 12 auf. Die Düsen 11 und 12 sind an eine (nicht dargestellte)Inertgaszuführung angeschlossen. Unterhalb der Ausflußöffnung 4 befindet sich eine Verdüsungskammer 13, die an ihrem oberen Ende eine genau unter der Ausflußdüse 4 gelegene Verdüsungsanordnung 14 aufweist.The stopper rod 6 has at its lower end laterally directed nozzles 11 into the cavity of the melting furnace 3 and a nozzle 12 directed towards the outflow nozzle 4. The nozzles 11 and 12 are connected to an inert gas supply (not shown). Below the outflow opening 4 there is a spraying chamber 13 which has at its upper end a spraying arrangement 14 located exactly below the outflow nozzle 4.

Zum Aufschmelzen und zur Vakuumbehandlung wird das Ausgangsmaterial zunächst in den Induktionsschmelztiegel 1 eingegeben. Nach der Vakuumbehandlung wird die Legierung zur Einstellung der erforderlichen Gießtemperatur und zur Raffinationsbehandlung, d. h. zur Entfernung aller nichtmetallischen Verunreinigungen durch dichtebedingten Auftrieb und zur Einstellung der Gießtemperatur in den widerstandsbeheizten Schmelzofen 3 umgefüllt. Der dichtebedingte Auftrieb der nichtmetallischen Verunreinigungen kann durch das durch die Düsen 10 und/oder 11 in die Schmelze gelangende Inertgas unterstützt werden. In dem widerstandsbeheizten Schmelzofen 3 wird die Schmelze für die Dauer der Raffinationsbehandlung auf einer konstanten Gießtemperatur gehalten.For melting and for vacuum treatment, the starting material is first introduced into the induction crucible 1. After the vacuum treatment, the alloy is used to adjust the required casting temperature and for refining treatment, i. H. Transferred to the resistance-heated melting furnace 3 to remove all non-metallic impurities due to density-related buoyancy and to set the casting temperature. The density-related buoyancy of the non-metallic impurities can be supported by the inert gas that passes through the nozzles 10 and / or 11 into the melt. In the resistance-heated melting furnace 3, the melt is kept at a constant casting temperature for the duration of the refining treatment.

Zum Abgießen der Legierung in den Verdüsungsraum 13 wird die Stopfenstange 6 durch Betätigen der Regelvorrichtung 8 angehoben und dadurch die Ausflußdüse 4 geöffnet. Dabei kann der durch die Düse 12 austretende Inertgasstrahl zur Unterstützung der Verdüsung des in die Verdüsungskammer 13 einfließenden Legierungsstromes herangezogen werden.To pour the alloy into the atomization chamber 13, the stopper rod 6 is raised by actuating the control device 8 and the outflow nozzle 4 is thereby opened. The inert gas jet emerging through the nozzle 12 can be used to support the atomization of the alloy stream flowing into the atomization chamber 13.

In Abwandlung des beschriebenen Ausführungsbeispiels kann der widerstandsbeheizte Schmelzofen 3 zum Vergießen der Legierung im Form-, Block- und Stranggußverfahren verwendet werden.In a modification of the described embodiment, the resistance-heated melting furnace 3 can be used for casting the alloy in the form, block and continuous casting process.

Claims (12)

1. Verfahren zur Herstellung hochreiner Legierungen, bei dem die Ausgangswerkstoffe in einer Vakuumschmelzanlage schmelzmetallurgisch behandelt und anschließend vergossen werden,
gekennzeichnet durch folgende Schritte: a) Erschmelzen der Legierung in einem Induktionstiegel und Vakuumbehandlung der Schmelze, b) Umfüllen der Schmelze in einen zweiten in der Vakuumschmelzanlage befindlichen Schmelztiegel, c) Raffinationsbehandlung der Schmelze in diesem Tiegel, wobei die gesamte Schmelze auf eine erforderliche Temperatur gebracht und ohne Badbewegung so lange gehalten wird, bis Verunreinigungen aufgestiegen sind, d) Abgießen der Schmelze bei gleichbleibender Gießtemperatur aus einer unterhalb des Badspiegels befindlichen Ausgußöffnung und e) Beenden des Abgießens, bevor die zum Badspiegel aufgestiegenen Verunreinigungen mit ausfließen können. 1. Process for the production of high-purity alloys, in which the starting materials are melt-metallurgically treated in a vacuum melting plant and then cast,
characterized by the following steps: a) melting the alloy in an induction crucible and vacuum treatment of the melt, b) transferring the melt into a second crucible located in the vacuum melting system, c) refining the melt in this crucible, the entire melt being brought to a required temperature and being held without bath movement until impurities have risen, d) pouring the melt at a constant casting temperature from a spout located below the bath level and e) Stop pouring before the contaminants that have risen to the bathroom mirror can also flow out. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß zur Unterstützung der Raffinationsbehandlung der Schmelze im unteren Bereich des zweiten Schmelztiegels Inertgas zugeführt wird.2. The method according to claim 1, characterized in that inert gas is supplied to support the refining treatment of the melt in the lower region of the second crucible. 3. Anlage zur Durchführung des Verfahrens nach Anspruch 1 mit einem in einer Vakuumschmelzanlage befindlichen Induktionstiegel und einem darunter gelegenerin Raum zur Erstarrung der flüssigen Legierung, dadruch gekennzeichnet, daß die Vakuumschmelzanlage (2) einen zweiten, fest angeordneten Schmelztiegel (3) mit einer in seinem unteren Bereich angeordneten Ausgußöffnung (4) und mit einer Verschleißanordnung (5) enthält.3. Installation for carrying out the method according to claim 1 with a located in a vacuum melting installation I nduktionstiegel and including gelegenerin chamber for solidification of the liquid alloy, dadruch in that the vacuum melting installation (2) a second, fixedly arranged crucible (3) with an in contains pouring opening (4) arranged in its lower region and with a wear arrangement (5). 4. Anlage nach Anspruch 3, dadurch gekennzeichnet, daß der zweite Schmelztiegel (3) als widerstandsbeheizter Schmelzofen ausgebildet ist.4. Plant according to claim 3, characterized in that the second crucible (3) is designed as a resistance-heated melting furnace. 5. Anlage nach Anspruch 3, dadurch gekennzeichnet, daß der zweite Schmelztiegel (3) induktiv über einen Suszeptor beheizbar ist.5. Plant according to claim 3, characterized in that the second crucible (3) can be heated inductively via a susceptor. 6. Anlage nach Anspruch 3, dadurch gekennzeichnet, daß der zweite Schmelztiegel (3) mit Hochfrequenz betreibbar ist.6. Plant according to claim 3, characterized in that the second crucible (3) can be operated at high frequency. 7. Anlage nach einem der Ansprüche 3 bis 6, dadurch gekennzeichnet, daß im unteren Bereich des zweiten Schmelz tieaels (3) Düsen (10) zur Zuführung von Inertgas angeordnet sind.7. Plant according to one of claims 3 to 6, characterized in that in the lower region of the second melting tieaels (3) nozzles (10) are arranged for the supply of inert gas. 8. Anlage nach einem der Ansprüche 3 bis 7, dadurch gekennzeichnet, daß die Verschließanordnung (5) eine metallische Stopfenstange (6) mit einer temperaturbeständigen Umkleidung (9) aufweist.8. Installation according to one of claims 3 to 7, characterized in that the closing arrangement (5) has a metallic plug rod (6) with a temperature-resistant casing (9). 9. Anlage nach Anspruch 8, dadurch gekennzeichnet, daß im unteren Teil der Stopfenstange (6) öffnungen (11, 12) zur Durchführung von Inertgas angeordnet sind.9. Plant according to claim 8, characterized in that in the lower part of the stopper rod (6) openings (11, 12) are arranged for carrying inert gas. 10. Anlage nach Anspruch 9, dadurch gekennzeichnet, daß die im unteren Teil der Stopfenstange (6) angeordneten öffnungen (11) seitlich in den zur Aufnahme der Legie- rung bestimmten Hohlraum des zweiten Schmelztiegels (3) gerichtet sind.10. Plant according to claim 9, characterized in that arranged in the lower part of the stopper rod (6) openings (11) are directed into the tion for receiving the L egie- specific cavity of the second crucible (3) laterally. 11. Anlage nach einem der Ansprüche 9 oder 10, dadurch gekennzeichnet, daß die Stopfenstange (6) eine in die Ausgußöffnung (4) des zweiten Schmelztiegel (3) gerichtete Auslaßöffnung (12) aufweist.11. Plant according to one of claims 9 or 10, characterized in that the stopper rod (6) has an outlet opening (12) directed into the pouring opening (4) of the second crucible (3). 12. Anlage nach einem der Ansprüche 8 bis 11, dadurch gekennzeichnet, daß die Verschließeinrichtung (5) durch ein Kühlmittel kühlbar ist.12. Plant according to one of claims 8 to 11, characterized in that the closing device (5) can be cooled by a coolant.
EP84110654A 1983-09-26 1984-09-07 Process and apparatus for the manufacture of high-purity alloys Expired EP0137315B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT84110654T ATE34775T1 (en) 1983-09-26 1984-09-07 PROCESS AND PLANT FOR PRODUCTION OF HIGH PURITY ALLOYS.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3334733A DE3334733C2 (en) 1983-09-26 1983-09-26 Process and plant for the production of high-purity alloys
DE3334733 1983-09-26

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EP0137315A2 true EP0137315A2 (en) 1985-04-17
EP0137315A3 EP0137315A3 (en) 1985-08-21
EP0137315B1 EP0137315B1 (en) 1988-06-01

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US (1) US4584015A (en)
EP (1) EP0137315B1 (en)
JP (1) JPS6096738A (en)
AT (1) ATE34775T1 (en)
DE (1) DE3334733C2 (en)

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US6340376B1 (en) * 1998-02-17 2002-01-22 Energy Conversion Devices, Inc. Method for combining metals with different melting points
US8061444B2 (en) * 2008-05-22 2011-11-22 Schlumberger Technology Corporation Methods and apparatus to form a well
CN106621429B (en) * 2015-07-20 2019-04-19 中国科学院上海应用物理研究所 The method and distilling apparatus of closed distillation fused salt

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JPS6096738A (en) 1985-05-30
EP0137315B1 (en) 1988-06-01
ATE34775T1 (en) 1988-06-15
DE3334733C2 (en) 1985-08-14
US4584015A (en) 1986-04-22
DE3334733A1 (en) 1985-04-25
EP0137315A3 (en) 1985-08-21

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