EP0471798B1 - Induktivschmelzspinnen von reaktiven metallegierungen - Google Patents

Induktivschmelzspinnen von reaktiven metallegierungen Download PDF

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Publication number
EP0471798B1
EP0471798B1 EP90911041A EP90911041A EP0471798B1 EP 0471798 B1 EP0471798 B1 EP 0471798B1 EP 90911041 A EP90911041 A EP 90911041A EP 90911041 A EP90911041 A EP 90911041A EP 0471798 B1 EP0471798 B1 EP 0471798B1
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EP
European Patent Office
Prior art keywords
crucible
nozzle
orifice
interior
side walls
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Revoked
Application number
EP90911041A
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English (en)
French (fr)
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EP0471798A1 (de
Inventor
Santosh Kumar Das
Richard Lister Bye, Jr.
Alexander Lobovsky
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Honeywell International Inc
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AlliedSignal Inc
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Application filed by AlliedSignal Inc filed Critical AlliedSignal Inc
Publication of EP0471798A1 publication Critical patent/EP0471798A1/de
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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
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
    • B22D11/0637—Accessories therefor
    • B22D11/064—Accessories therefor for supplying molten metal

Definitions

  • This invention relates to a method and apparatus for rapid solidification of reactive metals and metal alloys; and more particularly, to an induction skull melting system having a nozzle through which a molten metal stream is directed onto a rapidly moving chill substrate to form a rapidly solidified continuous metal filament or ribbon.
  • Rapid solidification has become an important process for production of new materials. Properties of materials produced by rapid solidification frequently exceed those of similar materials processed at slower solidification rates. The rapid solidification of materials has enhanced physical, mechanical and corrosion properties of a variety of alloy systems.
  • Rapid solidification processes that have been developed for producing material in quantities sufficient for practical application can be broadly classified in two categories, i.e. atomization and melt spinning.
  • atomization processes a stream of molten metal is broken into fine droplets which cool quickly and solidify as fine powders suitable for subsequent consolidation into bulk shapes.
  • Melt spinning processes which comprise chill block melt spinning and planar flow casting involve directing a stream of molten alloy onto a cooled substrate so that it solidifies as a thin foil or ribbon which is used in foil or ribbon form or mechanically comminuted into powder for subsequent consolidation.
  • Common to the processes of each rapid solidification category is the requirement for a crucible in which the metal is melted and held in the molten state and a flow control device, or nozzle, in which the molten metal stream is formed and controlled.
  • the flow of molten metal is controlled by the size of the orifice and the hearth is pressurized relative to the orifice exit for additional control.
  • the metal stream is then either atomized or directed onto a rapidly moving water cooled substrate to form a rapidly solidified ribbon.
  • Arc melting with controlled pouring from the bottom of the hearth has been frequently used to produce rapidly solidified powders by atomization and rapidly solidified ribbons by melt spinning.
  • S.H. Whang "Rapidly Solidified Ti Alloys Containing Novel Additives", Journal of Metals, April, 1984, pp. 34-40.
  • the slag melts and solidifies between the cold crucible wall and the hot metal, providing both thermal and electrical insulation between the crucible and the hot metal.
  • the initial charge melts forming a solid skull at the crucible walls with a molten pool contained within the skull.
  • the crucible is then tilted to pour the molten alloy or, alternatively, the bottom of the skull can be continuously withdrawn and cooled so as to form a continuously cast ingot of the same dimension as the inside diameter of the crucible.
  • the Clites et al. process has been modified by increasing the number of slits in the crucible, thereby eliminating the need for the slag.
  • the modified process permits melting of up to 75 pounds of titanium or 105 pounds of zirconium. Scale-up to between 400 and 500 pounds is said to be possible, the principle limitation being the size of the power source.
  • D.J. Chronister et al. "Induction Skull Melting Titanium and Other Reactive Alloys, Journal of Metals, Sept., 1986, pp. 51-54.
  • the Clite et al. process offers some advantages over more conventional reactive metal melting processes, it does not address an important requirement of a molten metal delivery system for rapid solidification processing, namely, the requirement for a small, controlled molten metal stream.
  • the apparatus comprises a crucible means for holding a metal charge.
  • the crucible means has side walls, a top and a bottom having an orifice therein. Collectively, the side walls, top and bottom define an interior of the crucible. A portion of the dimensions of the side walls and bottom is divided by longitudinal slits into at least two segments.
  • a nozzle means is disposed partially within the crucible means, and extends through the orifice. The nozzle means comprises a first end in communication with the interior.
  • a second end of the nozzle means further comprises a nozzle orifice for defining a stream of molten metal alloy.
  • a cooling means is provided for cooling the top, side walls and bottom of the crucible means.
  • the apparatus further comprises a first induction means for inducing an alternating electrical current within the metal charge.
  • a second induction means is associated with the nozzle means for inducing an electrical current therewithin.
  • the apparatus has pressure control means for establishing and maintaining positive pressure within the interior of the cruicible, and a quenching means including a rapidly moving chill substrate.
  • a positioning means positions said crucible and nozzle means relative to the quenching means.
  • the crucible nozzle and quenching means are housed within an enclosure means that provides therewithin a controlled atmosphere having positive or negative pressure.
  • the invention provides a process for melting and rapid solidification casting of metal alloys, comprising the steps of:
  • the method and apparatus of the invention provide for melting of reactive metals and their alloys in a cold wall crucible to minimize contamination from melt/crucible reactions.
  • a means to form and direct in a controlled manner a stream of metal onto a rapidly moving water cooled substrate for rapid solidification is provided.
  • the apparatus is capable of producing rapidly solidified materials in larger batches than those currently produced and effects rapid solidification of reactive metals in an efficient, reliable manner.
  • the metal filaments or ribbons that are produced by this process are suitable for use as foils in the as-cast or annealed condition or may be comminuted into a powder appointed for consolidation into bulk articles using conventional powder metallurgy techniques.
  • FIGs. 1-5 of the drawings there is shown a preferred embodiment for an apparatus for melting and rapid solidification casting of reactive metal alloys in a controlled atmosphere or vacuum.
  • the apparatus shown generally at 100 comprises a crucible means shown generally at 2, for holding a metal charge.
  • the crucible means 2 has side walls 3, a top 7 and a bottom 20 having an orifice 5 therein. Collectively, the side walls 3, top 7 and bottom define an interior 22 of the crucible. A portion of the dimension of the side walls 3 and bottom 20 is divided by longitudinal slits 11 into at least two segments.
  • a nozzle means 8 is disposed partially within the crucible means 2, and extends through the orifice 5.
  • the nozzle means 8 comprises a first end 24 in communication with the interior 22.
  • a second end 26 of the nozzle means further comprises a nozzle orifice 28 for defining a stream 6 of molten metal alloy.
  • a cooling means 4 is provided for cooling the top 7, side walls 3 and bottom 20 of the crucible means 2.
  • the apparatus 100 further comprises a first induction means 30 for inducing an alternating electrical current within the metal charge.
  • a second induction means 32 is associated with the nozzle means 8 for inducing an electrical current therewithin.
  • the apparatus 100 has pressure control means 34 for establishing and maintaining positive pressure within the interior 22 of the crucible 2, and a quenching means 36 including a rapidly moving chill substrate.
  • a positioning means 10 positions the crucible and nozzle means relative to the quenching means 36.
  • the crucible, nozzle and quenching means are housed within an enclosure means 1 that provides therewithin a controlled atmosphere having positive or negative pressure.
  • a housing or chamber 1 that is constructed in such a manner to be gas tight.
  • Chamber 1 encloses a crucible 2, a nozzle 8 and a casting substrate 36.
  • Crucible 2 is preferably constructed of a metal having high thermal conductivity such as copper.
  • the crucible 2 contains slits 11 part way up the sides 3 and in the bottom 20 so as to reduce the attenuation or shielding action which would be presented by an electrically continuous crucible.
  • a cooling means 4 for supplying cooling water to the crucible 2 is provided.
  • a water manifold which is an integral part of the crucible 2 is preferred.
  • An induction coil 30 is positioned around the lower, or working portion of the crucible and is connected to a conventional induction power supply (not shown) and a source of cooling water (not shown).
  • the top of the crucible 2 is covered by a cap 7 preferably constructed from a material having high thermal arid electrical conductivity, such as copper or a copper containig alloy.
  • the cap is removable to allow access to interior 22 of the crucible 2 but capable of being tightly sealed to the crucible.
  • the cap 7 is connected to a source of cooling water and contains a connection 34 through which an inert gas can be introduced in order to maintain a relative pressure difference between the crucible interior and the chamber environment.
  • a casting nozzle 8 constructed from a high melting point material such as a ceramic or refractory metal, preferably tungsten or molybdenum, is located beneath the crucible 2.
  • the nozzle 8 preferably cylindrical in shape with an outside diameter smaller than the inside diameter of the crucible 2, is open at the top 24 and positioned in a hole 5 in the bottom of the crucible 2 so that the nozzle top 24 is open to the crucible interior 22.
  • the nozzle 8 is closed at the bottom 26 except for a small orifice 28.
  • An induction coil 32 is located coaxially with the nozzle 8 and is connected to a conventional induction power supply, distinct from that of the crucible 2, and a source of cooling water.
  • the crucible and nozzle assembly is supported by a frame 10 which is capable of adjusting the position of the assembly relative to a rapidly moving casting substrate 36.
  • the casting substrate 36 is preferably a water cooled wheel constructed from material having high thermal conductivity, such as copper or one of its alloys, and is capable of being driven so as to achieve surface speeds of between 2500 and 7500 feet per minute (762 and 2286 meters per minute.
  • FIGURE 2 shows a longitudinal cross section of the crucible and nozzle assembly showing construction details and the relationship between the nozzle 8 and the crucible 2.
  • the crucible bottom 20 and side walls 3 are segmented by slits 11 which extend approximately two thirds of the way up the side walls 1. The metal is melted and held in the lower portion of the crucible 2 only and the slits 11 must extend far enough up to provide for the electrical isolation of individual segments in that area.
  • Internal passages 18 are provided in each segment for cooling water. Cooling water is supplied to the internal passages 18 through a manifold 4 which is an integral part of the crucible 2.
  • the crucible 2 is encased in a cylinder 40 of cast refractory which serves to reduce potential deformation of the crucible 2 due to the slits 11 and to seal the slits 11, allowing the crucible 2 to be pressurized.
  • the crucible assembly rests on an electrically insulating plate 42 which is placed on a holding bracket 44 connected to a support assembly 10.
  • the nozzle 8 is positioned in an orifice 5 in the bottom of the crucible 2 so that it is open to the crucible interior 22.
  • the nozzle 8 is electrically and thermally isolated from the crucible 2 by a series of insulating and clamping rings 46 which are constructed so as to allow the position of the nozzle 8 to be adjusted with respect to the crucible bottom 20.
  • the nozzle 8 and clamping ring assembly 46 are fastened in place by means of a holding plate 48 which is bolted to the holding bracket 44.
  • FIGURE 3 is a bottom view of the crucible showing details of the segmentation.
  • Crucible side walls 3 are divided into segments by longitudinal slits 11. In the embodiment shown, there are 24 segments.
  • the crucible bottom 20 is divided into half the number of segments of the side walls by radial slits 50 extending nearly to the orifice 5 in the center of the bottom 20 leaving a narrow ring 52 of unsegmented material so as to provide for the structural stability of the crucible 2.
  • the bottom slits 50 are extensions of alternating side wall slits. 11.
  • Cooling water passages 38 are placed such that pairs of side wall segments and the bottom segment to which they are connected are cooled by a separate cooling loop.
  • the starting material which may consist of a single pre-alloyed ingot or a master alloy with elemental alloying additions, is placed in the crucible 2 and the cap 7 is sealed to the top of the crucible. Power is then applied to the crucible induction coil 30 and the charge is heated. As heating progresses, the charge starts to melt. Molten metal in contact with the crucible freezes so that a layer or skull 54 of solid alloy against the crucible walls 3 and bottom 20 is formed and maintained. The configuration of the metal charge after heating and melting to form a molten metal pool 56 and skull 54 prior to the start of casting is shown in FIGURE 4. Levitating forces induced by the electrical field distort the molten metal pool 56 into the general shape shown. A skull 54 of solid metal remains in the crucible, sealing the opening at the upper end 24 of the nozzle 8.
  • the crucible 2 and nozzle 8 assembly is located over a moving casting substrate 36.
  • Power to the induction coil 32 surrounding the nozzle 8 is turned on heating the nozzle 8 and melting the solid skull 54 adjacent tothe upper end and 24 of the nozzle 8, allowing molten metal 56 to flow into the nozzle 8, through a passageway 58 in the nozzle interior and out the orifice in the nozzle bottom 26.
  • the metal stream 6 exiting the nozzle 8 impinges on the moving casting substrate 36 where it is rapidly solidified into a thin filament 60.
  • An inert gas is supplied to the crucible 2 through a port 34 in the sealing cap 7 in order to provide a pressure sufficient to maintain a metal stream 6 suitable for formation of filament 60. The gas pressure is controlled during the course of the casting operation to compensate for the reduction in metal head pressure as the crucible empties.
  • a crucible such as that shown in FIGURES 2 and 3 was constructed.
  • the crucible had an inside diameter of 4 3/4 inches (12.065 cm), and inside height of 12 1/2 inches (31.75 cm) and contained a 1 1/2 inch (3.81 cm) diameter hole in the bottom.
  • Longitudinal slits were cut in the bottom 7 1/2 inches (19.05 cm) of the crucible walls, dividing the crucible in that area into 24 segments.
  • the crucible bottom was slit radially from the outside diameter to within 1/2 inch (1.27 cm) of the center hole, dividing the bottom into 12 segments.
  • An induction coil consisting of 11 turns of copper tubing and having an overall height of 6 inches (15.24 cm) was placed coaxially around the bottom portion of the crucible. Power for inductively heating and melting was supplied by a 3 kHz, 135 kW solid state induction power supply.
  • the crucible and coil were placed on a holding bracket and support assembly capable of horizontal and vertical movement inside of a vacuum chamber.
  • the charge material consisting of approximately 10 pounds of 1 inch (2.54 cm) diameter titanium-6% aluminum-4% vanadium rods was placed in the crucible.
  • a water cooled brass cap containing a fitting for the introduction of argon gas into the crucible interior was placed on top of the crucible and clamped down by means of clamps attached to the support bracket.
  • a nozzle fabricated from tungsten having an outside diameter of 1 1/2 inches (3.81 cm), an inside diameter of 1 inch (2.54 cm) and an overall height of 1 1/2 inches (3.81 cm) was inserted into the orifice in the crucible bottom and fastened in place using a series of clamping rings and a holding plate attached to the underside of the crucible support plate.
  • the charge was then heated by applying power to the induction coil. As the charge heated up and melted, molten liquid flowed until it connected the crucible walls or bottom and froze, forming a solid skull. By varying the heating rate and applied power levels, conditions were established which resulted in the entire charge being melted and contained within a solid skull. With this configuration, however, liquid metal flow through the nozzle could not be initiated.
  • Example 1 The apparatus described in Example 1 was modified by the addition of a 3 turn induction coil with an overall height of 1 1/2 inches (3.81 cm) located coaxially with a nozzle similar to that of Example 1 but with a length of 3 inches (7.62 cm). Power to the coil was provided by 10 kHz, 10 kW solid state induction power supply. The general procedures outlined in Example 1 were followed except that power to the nozzle induction coil was applied at the same time that the crucible charge was being heated and melted. When heating rates and power levels were adjusted appropriately, molten metal from the crucible flowed into the nozzle and out of the orifice until the crucible was emptied except for a skull on the crucible bottom.
  • Example 1 The apparatus outlined in Example 1 and the procedures outlined in Examples 1 and 2 were used to make a rapid solidification run.
  • the crucible/nozzle assembly was moved over the casting wheel, which had already been turned on.
  • the molten metal stream impinged on the wheel and solidified, forming thin ribbon which came off the wheel downstream of the impingement point.
  • the rapidly solidified ribbon was approximately 0.17 inches (0.43 cm) wide and 0.002 inches (0.005 cm) thick.
  • the composition was analyzed as 35.0% aluminum, 1.74% vanadium and 63.3% titanium.
  • composition of the ribbon in one cast was 13.9% Al, 19.4% Nb, 3.09% V and 1.9% Mo with the balance being titanium and in the other, 13.8% Al, 19.2% Nb, 3.19% V and 1.87% Mo with the balance being titanium. This demonstrates the reliability and repeatability of the invention.
  • Ribbons prepared as in examples 3 and 4 were examined. It was found that ribbons containing interstitial impurities less than about 700 ppm O2, 420 ppm N2 and 200 ppm C and having a thickness less than about 0.003 inches (0.008 cm) had significant ductility. Ductility was indicated by the capability of bending a ribbon back over upon itself without fracture.
  • Ribbon prepared as in example 4 having a composition of 13.9% Al, 19.4% Nb, 3.09% V, 1.90% Mo with the ballance being titanium was subjected to hammer milling to produce a -35 mesh powder
  • the powder was placed in a 1 inch (2.54 cm) diameter by 6 inch (15.24 cm) long cylindrical stainless steel can, vauum outgassed and then sealed under vacuum. The cans were then hot isostatically pressed to produce a fully dense article after the can was removed.

Claims (2)

  1. Vorrichtung zum Schmelzen und zum Gießen mit Rascher Erstarrung von Metallegierungen, welche aufweist:
    (a) eine Schmelztiegeleinrichtung zum Halten einer Metallcharge, welche Schmelztiegeleinrichtung Seitenwände, einen Deckteil und einen Boden mit einer Ausmündung darin aufweist, wobei die Seitenwände, der Deckteil und der Boden gemeinsam einen Innenraum des Schmelztiegels begrenzen und über einen Teil ihrer Abmessungen durch Längsschlitze in wenigstens zwei Segmente unterteilt sind;
    (b) eine Düseneinrichtung, die teilweise innerhalb der Schmelztiegeleinrichtung angeordnet ist und sich durch die Ausmündung erstreckt, welche Düseneinrichtung ein erstes, mit dem Innenraum in Verbindung stehendes Ende und über einen Durchlaß in der Düse ein zweites Ende aufweist, wobei das zweite Ende ferner eine Düsenmündung zur Begrenzung eines Stromes geschmolzener Metallegierung umfaßt;
    (c) eine Kühleinrichtung zum Kühlen des Deckteiles, der Seitenwände und des Bodens;
    (d) eine erste Induktionseinrichtung zum Induzieren eines elektrischen Wechselstromes innerhalb der Metallcharge;
    (e) eine zweite Induktionseinrichtung zum Induzieren eines elektrischen Stromes in der Düse;
    (f) eine Drucksteuereinrichtung für den Aufbau und die Aufrechterhaltung eines Überdruckes innerhalb des Innenraumes;
    (g) eine Abschreckeinrichtung mit einem sich rasch bewegenden Abschrecksubstrat;
    (h) eine Positioniereinrichtung zum Positionieren der Schmelztiegel- und der Düseneinrichtung relativ zur Abschreckeinrichtung; und
    (i) eine Verkleidungseinrichtung zum Umschließen der Schmelztiegel-, der Düsen- und der Abschreckeinrichtung zur Schaffung einer kontrollierten Atmosphäre mit Über- oder Unterdruck darin.
  2. Verfahren zum Schmelzen und zum Gießen mit Rascher Erstarrung von Metallegierungen, mit den Verfahrensschritten:
    (a) Anordnen einer festen, aus einer Metallegierung zusammengesetzten Charge im Inneren einer Schmelztiegeleinrichtung mit Seitenwänden, einem Deckteil und einem Boden, welcher Boden eine Ausmündung darin besitzt, wobei die Seitenwände, der Deckteil und der Boden gemeinsam das Innere begrenzen und die Seitenwände und der Boden über einen Teil ihrer Abmessungenm durch Längsschlitze in wenigstens zwei Komponenten geteilt sind;
    (b) Schmelzen der Charge innerhalb des Inneren durch Induzieren eines elektrischen Wechselstromes innerhalb derselben;
    (c) fortlaufendes Kühlen der Schmelztiegelwände und des Bodens zum Ausbilden und Aufrechterhalten einer Schicht fester Metallegierung aus der geschmolzenen Charge gegenüber diesen und damit zum Verhindern eines Kontaktes zwischen dem geschmolzenen Metall und den Seitenwänden und dem Boden des Schmelztiegels;
    (d) Beheizen einer Düse, die teilweise innerhalb der Schmelztiegeleinrichtung angeordnet ist und sich durch die Ausmündung hindurch erstreckt, welche Düseneinrichtung ein erstes, mit dem Inneren in Verbindung stehendes Ende und, über einen Durchlaß in der Düse, ein zweites Ende aufweist, welches zweite Ende eine Düsenmündung besitzt, um so einen dem ersten Ende benachbarten Teil der Schicht zu schmelzen und eine Strömung der geschmolzenen Charge durch den Durchlaß und die Düsenmündung zu gestatten;
    (e) unter Druck setzen des Inneren zum Aufbauen und Aufrechterhalten eines Überdruckes innerhalb desselben, um so eine Strömung der geschmolzenen Charge durch die Düsenmündung mit gesteuerter Strömungsgeschwindigkeit vorzusehen; und
    (f) Ausrichten eines durch die Strömung der geschmolzenen Charge gebildeten Strahles durch die Düsenmündung in eine Berührung mit einem sich rasch bewegenden Abschrecksubstrat zum Raschen Erstarren der geschmolzenen Charge.
EP90911041A 1989-05-01 1990-04-30 Induktivschmelzspinnen von reaktiven metallegierungen Revoked EP0471798B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US34525489A 1989-05-01 1989-05-01
US345254 1989-05-01

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EP0471798A1 EP0471798A1 (de) 1992-02-26
EP0471798B1 true EP0471798B1 (de) 1993-06-23

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EP (1) EP0471798B1 (de)
JP (1) JP3054193B2 (de)
DE (1) DE69002059T2 (de)
WO (1) WO1990013377A1 (de)

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JP2002066698A (ja) * 2000-08-31 2002-03-05 Ulvac Japan Ltd 金属薄帯製造装置
US20060291529A1 (en) * 2005-05-26 2006-12-28 Haun Robert E Cold wall induction nozzle
US8858697B2 (en) 2011-10-28 2014-10-14 General Electric Company Mold compositions
US9011205B2 (en) 2012-02-15 2015-04-21 General Electric Company Titanium aluminide article with improved surface finish
US8932518B2 (en) 2012-02-29 2015-01-13 General Electric Company Mold and facecoat compositions
US8906292B2 (en) 2012-07-27 2014-12-09 General Electric Company Crucible and facecoat compositions
US8708033B2 (en) 2012-08-29 2014-04-29 General Electric Company Calcium titanate containing mold compositions and methods for casting titanium and titanium aluminide alloys
US8992824B2 (en) 2012-12-04 2015-03-31 General Electric Company Crucible and extrinsic facecoat compositions
US9592548B2 (en) 2013-01-29 2017-03-14 General Electric Company Calcium hexaluminate-containing mold and facecoat compositions and methods for casting titanium and titanium aluminide alloys
US9192983B2 (en) 2013-11-26 2015-11-24 General Electric Company Silicon carbide-containing mold and facecoat compositions and methods for casting titanium and titanium aluminide alloys
US9511417B2 (en) 2013-11-26 2016-12-06 General Electric Company Silicon carbide-containing mold and facecoat compositions and methods for casting titanium and titanium aluminide alloys
US10391547B2 (en) 2014-06-04 2019-08-27 General Electric Company Casting mold of grading with silicon carbide
IT202100024227A1 (it) * 2021-09-21 2023-03-21 Antonio Alessandro Rossi Crogiolo a freddo ad alta efficienza e metodo di realizzazione dello stesso

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Publication number Publication date
DE69002059T2 (de) 1993-09-30
EP0471798A1 (de) 1992-02-26
DE69002059D1 (de) 1993-07-29
WO1990013377A1 (en) 1990-11-15
JPH04504981A (ja) 1992-09-03
JP3054193B2 (ja) 2000-06-19

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