EP1444065A2 - Procede de production d'alliages intermetalliques (ingots) - Google Patents

Procede de production d'alliages intermetalliques (ingots)

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Publication number
EP1444065A2
EP1444065A2 EP02783083A EP02783083A EP1444065A2 EP 1444065 A2 EP1444065 A2 EP 1444065A2 EP 02783083 A EP02783083 A EP 02783083A EP 02783083 A EP02783083 A EP 02783083A EP 1444065 A2 EP1444065 A2 EP 1444065A2
Authority
EP
European Patent Office
Prior art keywords
melting
crucible
melt
homogenized
cold wall
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.)
Granted
Application number
EP02783083A
Other languages
German (de)
English (en)
Other versions
EP1444065B1 (fr
Inventor
Matthias Blum
Georg Jarczyk
Anita Chatterjee
Willy FÜRWITT
Volker GÜTHER
Helmut Clemens
Heinz Danker
Rainer Gerling
Friedhelm Sasse
Frank-Peter Schimansky
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
GfE Gesellschaft fuer Elektrometallurgie mbH
ALD Vacuum Technologies GmbH
GKSS Forshungszentrum Geesthacht GmbH
Original Assignee
GfE Gesellschaft fuer Elektrometallurgie mbH
ALD Vacuum Technologies GmbH
GKSS Forshungszentrum Geesthacht GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by GfE Gesellschaft fuer Elektrometallurgie mbH, ALD Vacuum Technologies GmbH, GKSS Forshungszentrum Geesthacht GmbH filed Critical GfE Gesellschaft fuer Elektrometallurgie mbH
Publication of EP1444065A2 publication Critical patent/EP1444065A2/fr
Application granted granted Critical
Publication of EP1444065B1 publication Critical patent/EP1444065B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D23/00—Casting processes not provided for in groups B22D1/00 - B22D21/00
    • B22D23/06—Melting-down metal, e.g. metal particles, in the mould
    • B22D23/10—Electroslag casting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D7/00—Casting ingots, e.g. from ferrous metals

Definitions

  • the invention relates to a new melt metallurgical process for the cost-effective production of blocks from metallic and intermetallic alloys (ingots) with high chemical and structural homogeneity, in particular ingots made from ⁇ -TiAl.
  • the ⁇ -TiAI-based intermetallic alloys made the leap from development laboratory to industrial application in the fields of aerospace and automobile racing in 2000.
  • the advantageous high-temperature properties in combination with a low weight enable their use in the aerospace industry.
  • the high temperature and corrosion resistance makes the material for fast moving components in machines, e.g. interesting for valves in internal combustion engines or for blades in gas turbines.
  • the properties of this material depend on the chemical and structural homogeneity to an extent not previously known for structural materials.
  • the production of high-quality ingots is technically very demanding and expensive. Homogeneous ingots are required as starting material for various process routes for the production of further semi-finished products or components made of TiAl (cf. H. Clemens and H.
  • the currently used technical alloys based on ⁇ -TiAl have a multi-phase structure and, in addition to the ordered tetragonal ⁇ -TiAl, contain the ordered hexagonal ⁇ 2 -Ti 3 AI as the main phase, typically with a share of 5-15 vol .-%.
  • Refractory metals as alloying elements can be used to form a lead metastable krz phase, which occurs either as a ⁇ phase (unordered) or as a B2 phase (ordered). These alloy additives improve oxidation resistance and creep resistance.
  • Si, B and C are used in small amounts to increase the strength of the cast structure (cf. B. Inkson and H. Clemens (1999), MRS Symp. Proc.
  • TiAI alloys are usually manufactured as ingots by multiple remelting in a vacuum arc furnace (see FIG. 1) (VAR-Vacuum Are Remelting).
  • a pressed electrode which contains all alloy components, is melted, increasing its diameter.
  • a fundamental problem arises from inhomogeneities in the alloy composition of ⁇ -TiAl ingots.
  • a comparison of the AI content in twice and three times remelted ⁇ -TiAl ingot material shows that local fluctuations of the AI content of ⁇ 2 at.% Are still observed in twice remelted ⁇ -TiAl ingot material (see FIG. 2).
  • To achieve sufficient alloy homogeneity, a three-fold remelting in the VAR system is necessary (cf.V. Güther, A.
  • the object of the present invention is to provide a process for the reproducible production of ⁇ -TiAl ingots of high chemical homogeneity and low porosity, which can be carried out more easily and cost-effectively than the VAR process described above, in which numerous melting steps are necessary to achieve the desired high homogeneity and low porosity.
  • the method should offer the possibility of arbitrarily setting the dimensions of the alloy ingots in the technically sensible area, bypassing the restrictions of the VAR method described above.
  • This object is achieved by a process for the production of metallic and intermetallic alloy ingots by continuous and quasi-continuous extrusion from a cold-wall induction crucible, by continuously or quasi-continuously feeding the alloy material to a cold-wall induction crucible in the molten and pre-homogenized state (see Figure 4).
  • the continuous casting process for the production of metallic and intermetallic alloy ingots of high homogeneity and low porosity is characterized by the following chronologically listed steps: (i) production of electrodes by customary mixing and pressing of the selected starting materials,
  • step (iv) homogenizing the melt obtained in step (iii) in a cold wall induction crucible
  • Step (ii) obtained electrode material by melting in one
  • Induction crucible of stage (iv) in the form of cylindrical blocks with freely adjustable diameters and lengths.
  • the method is preferably used for the production of intermetallic alloy ingots based on ⁇ -TiAl, the alloys generally being described by the following empirical formula:
  • the induction melting of the electrodes in stage (iii) takes place in a high-frequency field with a frequency of preferably 70 to 300 kHz, in particular 70 to 200 kHz and preferably at temperatures of 1400 ° C. to 1700 ° C., in particular 1400 ° C. to 1600 ° C. the electrode is rotated in order to achieve uniform dripping, a speed of 4 rpm being preferred.
  • the lowering speed of the electrode can be varied continuously from 0 to 200 mm / min.
  • the method is preferably carried out quasi-continuously, in that one or more electrodes are fed quasi-continuously, while at the same time a block is withdrawn from the cold wall induction crucible.
  • the melt is homogenized in the cold-wall induction crucible in stage (iv) preferably with superheating from 10 to 100 K, preferably from 40 to 60 K. This corresponds to temperatures from 1400 ° C. to 1750 ° C., preferably 1450 ° C. to 1700 ° C. ever. according to alloy composition.
  • the frequency range of the coil is 4 to 20 kHz, preferably 4 to 12 kHz.
  • the cooling of the melt when the blocks are withdrawn in stage (v) is preferably carried out with the aid of water-cooled copper segments, and the diameters of the blocks are preferably in a range from 40 to 350 mm, particularly preferably 140 to 220 mm.
  • the take-off speeds can be set between 5 and 10 mm / min.
  • the withdrawal rate must be matched to the dripping rate (stage iii). This can be around 50 kg / h.
  • the method according to the invention makes it possible to produce new intermetallic alloy ingots based on ⁇ -TiAl, which are distinguished by a new combination of dimensional dimensions on the one hand and homogeneity on the other.
  • the invention therefore also relates to intermetallic alloy ingots based on ⁇ -TiAl, which are characterized by
  • the core of the method according to the invention consists in the continuous or quasi-continuous feeding of a pre-homogenized melt of the alloy material into a cold wall induction crucible (KIT).
  • KIT cold wall induction crucible
  • the KIT also loses its main function corresponding to the state of the art, namely the melting of material that is always charged into the KIT in the solid state. It is a major advantage of the method according to the invention that the alloys always observed during the melting of solid, multi-phase alloys in the KIT Signs of segregation do not occur as the cause of inhomogeneities in the end material, since the material already reaches the KIT in the liquid state.
  • Another advantage is that the frequency range of the induction coil, which is advantageous for homogenizing the already molten alloy, is higher than the frequency range which is advantageous for melting a solid alloy. Surprisingly, this can significantly reduce the edge porosity of the block removed from the solidifying melt in the KIT and thus increase the block quality.
  • a particular advantage of the method according to the invention is that the dimensions of the cold ingot induction crucible, which are freely selectable in a technically expedient framework, allow all the necessary dimensions of the alloy ingots to be achieved, which is not guaranteed by the VAR technology.
  • the process is preferably carried out in a vacuum or under protective gas, and non-contaminated production waste can be returned to the process.
  • the material loss is still 12% compared to 35% with the conventional VAR technology.
  • Novel combinations of known partial processes corresponding to the state of the art are also considered to be according to the invention, which ensure a continuous or quasi-continuous supply of liquid, pre-homogenized material into a cold wall induction crucible for the purpose of continuous or quasi-continuous strand withdrawal from the KIT ,
  • this relates to the combination of an inductively heated melting device for alloy rods or alloy electrodes (inductive drip melting), a KIT with a strand extraction device and the combination of a plasma cold-wall furnace with a fired channel system, an overflow designed as a skull with said KIT and said strand extraction device.
  • the inductive melting of metals is described, for example, in U.S. Patents 4,923,508, 5,003,551 and 5,014,769.
  • the inductive melting of electrodes has also been described in connection with the production of titanium alloy powder by the so-called EIGA (Electrode Induction Melting Gas Atomization) process (cf. DE-A-41 02 101, DE-A-196 31 582) ,
  • EIGA Electrode Induction Melting Gas Atomization
  • an alloy electrode is immersed in an HF coil that is insulated against flashovers with ceramic.
  • the electrode is completely melted by a surface melting process.
  • the melt is further processed in a gas nozzle in which the drops are atomized. This process is only for powder production and not for the production of ingots.
  • the melt in the KIT is subjected to a further homogenization before the block removal (ingot production) takes place.
  • the energy input in the KIT is used exclusively for further homogenization and to keep the material liquid, while in the specified patent the melting, homogenization and solidification process take place at the same place - the KIT. This increases the likelihood of segregation occurring.
  • the block deduction is also known from the prior art, in particular from the ceramic crucible.
  • the patents concerned with this state of the art mainly concern the block withdrawal of non-ferrous metals (Cu, brass).
  • the patents DE-A-198 52 747 and DE-A-196 50 856 listed above include the block draw from the cold wall induction crucible, but the material from which the block draw takes place is fed to the KIT as a solid and not as a pre-homogenized, molten material , As described above, this fact can lead to differences in homogeneity in the material removed as a block.
  • the electrodes are preferably produced by pressing and / or sintering powdery or granular alloy components (cf. DE-A-196 31 582 to -584, DE-A-198 52 747).
  • Electrode feed (2) furnace chamber, (3) air-cooled
  • Example 4 shows the method according to the invention (example 1) for producing chemically homogeneous ⁇ -TiAl blocks with variable dimensions: (1) rotating electrode, (2) inductive RF coil, (3) cold-wall induction crucible and (4)
  • FIG. 5 shows the method according to the invention (example 2) for producing chemically homogeneous ⁇ -TiAl blocks with variable dimensions: (1) charging ramp, (2) plasma torch, (3) cold stove, (4) cold wall
  • the method according to the invention is a melt metallurgical technology for producing chemically and structurally homogeneous alloy ingots, in particular ⁇ -TiAl blocks as ingot material for the forming route or for remelter stocks for the casting route.
  • the technology includes the combination of:
  • the individual process steps are to be described again in detail below.
  • the electrodes are first manufactured. Using a conventional melt metallurgical process, for example using VAR technology, pressed electrodes, which contain all alloy components (Ti sponge, Al granules, pre-alloy granules), are melted onto rods with a diameter of 150 mm, for example, by increasing the diameter. These are rods that have a low chemical homogeneity and a certain porosity. These serve as electrodes for the subsequent strand withdrawal.
  • the first technological step can be represented in two alternative ways - inductive melting or the PACHM process. Both processes aim to produce a pre-homogenized, molten material.
  • inductive melting the electrode which has been melted according to a customary method is inductively melted into a KIT using an HF coil (in accordance with the EIGA method, see DE-A-41 02 101, DE-A-196 31 582).
  • the coil / draining material system and the shape of the coil interact closely.
  • the frequency range on the external resonant circuit is 70 to 300 kHz.
  • the melting process is carried out by plasma torches.
  • the plasma torches perform two functions: melting the raw material and maintaining constant environmental conditions during the block extraction.
  • Starting material in the form of mechanically comminuted pre-alloyed compact, is successively recharged into the melting chamber via a hydraulic ramp.
  • the cold wall crucible (“cold stove") serves as a "removal tool” for undesirable high-density (trough bottom) and low-density inclusions (floating slag) of the melt and as a "reservoir” for supplying the crucible-block extractor system with molten material.
  • the current of the plasma torch above the cold stove is between 275-550 A, but can vary depending on the type and number of plasma torches used.
  • the melt is fed to the cold wall induction crucible.
  • the stirring effect of the electromagnetic field further improves the homogeneity of the melt in a larger, largely constant, molten volume.
  • the melt remains in the crucible for about 20 minutes to 45 minutes.
  • Skull melting in the cold wall induction crucible (KIT) has been an industrially established technique for years.
  • a field is generated by electromagnetic induction in a water-cooled copper crucible, which is used to heat or melt the materials.
  • the Lorenz forces that occur depress this Part of the melting material from the crucible walls and establish a circulation flow in the melt, which consequently leads to a good mixing of the melting phase.
  • the continuous supply of the KIT with melting material is made possible in the case of inductive melting by the connected electrode magazine, which can hold several electrodes at the same time, which are then melted one after the other.
  • the connected electrode magazine which can hold several electrodes at the same time, which are then melted one after the other.
  • mechanically comminuted pre-alloyed material is recharged via a hydraulic ramp.
  • the bottom skull which depends in its thickness and habit directly on the shape of the induction field, offers the starting point for a possible semi-finished product production. If the soil is lowered during the process, the system reacts in such a way that a new state of equilibrium is formed and a new layer grows on the old soil skull. The continuous lowering of the soil thus leads to a system of constantly adapting equilibrium conditions and consequently to an almost continuously growing soil layer. Since the base area of the floor skull is defined by the base of the crucible, the growth of new layers consequently leads to the creation of a semi-finished product (block). However, the constant mass discharge from the KIT also means the supply of the new molten material.
  • the cooling of the melt when the blocks are removed is preferably carried out with the aid of water-cooled Cu segments.
  • the block deduction from the KIT produces a chemically homogeneous and largely non-porous ingot.
  • the diameter of the KIT can be freely selected in large areas, so that a variable choice in the ingot diameter.
  • the take-off speeds can preferably be in a range from 0 to 50 mm / min.
  • the products produced according to the invention can be used for various purposes. Primarily, they are manufactured from them in a first forming step (extrusion), which are used for further processing in the forming route (forging, rolling). Ingots of high structural and chemical quality are required to manufacture ⁇ -TiAI-based components via the forming route.
  • the components are, for example, valves and turbine blades that have an excellent property profile and have to withstand the highest requirements.
  • the products according to the invention can also serve as remelter stocks for the production of cast blanks via precision casting or centrifugal casting.
  • Remelter stocks are required as starting material for the investment casting and centrifugal casting route.
  • the chemical and structural quality is not the focus here, since the material - in contrast to the ingots - is melted again.
  • step (ii) can be dispensed with in the process according to the invention and the pressed electrodes can be immediately inductively melted or premixed compacts can be melted using the PACHM process.
  • the investment casting route is used to manufacture components with a sophisticated design and complex requirement profiles.
  • One example is the already commercialized turbocharger based on ⁇ -TiAl.
  • Centrifugal casting is an inexpensive process for the production of mass components (e.g. valves) with a simple design and requirement profiles.
  • the production of remelter stocks by means of the process according to the invention leads to products which are significantly more homogeneous than the corresponding products of the prior art, and can be produced in any cylindrical dimension by the block deduction, while the dimensions used in the process used hitherto was dependent on the existing mold.
  • the method according to the invention makes it possible to freely choose the diameter and the length of the remelter stock and thus to be able to take into account every customer request in a simple manner.
  • the following examples for the specific embodiment of the invention serve for a better explanation.
  • the example explains the production of a continuous casting block from a ⁇ -TiAl alloy with the composition Ti -46.5AI -4 (Cr, Nb, Ta, B) (data in at.%) With a diameter of 180 mm and a length of 2,600 mm.
  • the first step consists in the production of 4 simply VAR-melted electrodes with a diameter of 150 mm and a length of 1,000 mm from press electrodes, which contain all alloy components in the form of Ti sponge, Al granules and suitable master alloys for Cr, Nb, Ta and B included.
  • the rods which are not yet homogeneous, serve as electrodes for the production of pre-homogenized, molten material by induction melting in an HF coil.
  • the electrodes are conical at the base, the angle of attack being approximately 45 °.
  • one electrode is fed from the magazine holding all 4 electrodes to the HF-melting coil, which is also conical, and is inductively melted into one.
  • the melt is formed on the entire surface of the cone and converges at the tip of the cone to form a melt jet in which the material is pre-homogenized.
  • the melt gets under
  • the melting coil is 80.6 kHz.
  • Drip-off electrode by means of inductive heating (medium frequency approximately 500 Hz to 1 kHz) via an auxiliary coil attached above the melting coil
  • the electrode is with a
  • the pre-homogenized, molten material falls into a cold wall induction crucible with a removable bottom.
  • the diameter of the crucible is 180 mm.
  • the melt solidifies in the lower region of the crucible and is continuously drawn off downwards.
  • the cooling of the melt when the blocks are removed is carried out using water-cooled copper segments.
  • the take-off speed is approx. 1 mm / min.
  • the average residence time of the melt for homogenization in the cold wall induction crucible is approx. 20 min, which corresponds to a bath height of approx. 160 mm.
  • the bath temperature is 1580 ° C and the frequency at the induction coil surrounding the crucible is 12 kHz.
  • the second electrode is moved into the required position and heated until it melts, during which time the strand withdrawal is interrupted. The process is then continued as described until all 4 electrodes of the magazine have melted.
  • the process can be carried out under vacuum as well as under protective gas.
  • the block obtained has a diameter of approx. 180 mm and a total length of 2,600 mm and is characterized by very good chemical and structural homogeneity.
  • the local fluctuations for aluminum and titanium are less than ⁇ 0.5 at.%, Those of the elements Cr, Nb and Ta less than ⁇ 0.2 at.% And those for B less than ⁇ 0.05 at.%.
  • Embodiment 2 differs from embodiment 1 in the manner in which the molten material is produced and supplied to the KIT.
  • the process is carried out under He protective gas.
  • the PACHM process (Plasma Are Cold Hearth Melting) offers an alternative to inductive melting.
  • the starting material is in the form of simply VAR-melted electrodes according to Example 1 using a He plasma torch (150 kW) in a water-cooled copper crucible melted and continued via a water-cooled trough also fired with a He plasma torch (150 kW).
  • the current of the plasma torch above the cold stove is approx. 500 A.
  • the liquid alloy melt flows in the material's own skull up to an overflow above the KIT, from where it flows continuously into the KIT.
  • the raw material is continuously recharged via a hydraulically controlled ramp.
  • the cold crucible performs two main functions: in addition to a reservoir for pre-homogenized, molten material, it also serves as a deposit for undesired high-density and ceramic inclusions.
  • the technical data given in the examples are not intended to limit the invention in any way.
  • the number, type and power of the plasma torch, the material for the cold crucibles, power and frequency ranges of the induction coils, diameter of the KIT, bath heights of the melts in the KIT and feed and withdrawal speeds can be varied within the framework of the prior art without the invention is thus affected.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Continuous Casting (AREA)

Abstract

L'invention concerne un procédé permettant de produire des alliages métalliques et intermétalliques (ingots) par démoulage de barre continu ou quasi-continu hors d'un creuset à induction à paroi froide. Ledit procédé se caractérise en ce que le matériau d'alliage est acheminé de manière continue ou quasi-continue à l'état fondu et pré-homogénéisé jusqu'à un creuset à induction à paroi froide.
EP02783083A 2001-11-16 2002-11-13 Procede de production d'alliages intermetalliques (ingots) Expired - Lifetime EP1444065B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10156336A DE10156336A1 (de) 2001-11-16 2001-11-16 Verfahren zur Herstellung von Legierungs-Ingots
DE10156336 2001-11-16
PCT/EP2002/012668 WO2003041896A2 (fr) 2001-11-16 2002-11-13 Procede de production d'alliages intermetalliques (ingots)

Publications (2)

Publication Number Publication Date
EP1444065A2 true EP1444065A2 (fr) 2004-08-11
EP1444065B1 EP1444065B1 (fr) 2008-01-09

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP02783083A Expired - Lifetime EP1444065B1 (fr) 2001-11-16 2002-11-13 Procede de production d'alliages intermetalliques (ingots)

Country Status (6)

Country Link
US (1) US20060230876A1 (fr)
EP (1) EP1444065B1 (fr)
JP (1) JP4243192B2 (fr)
AU (1) AU2002346837A1 (fr)
DE (2) DE10156336A1 (fr)
WO (1) WO2003041896A2 (fr)

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JP6234841B2 (ja) * 2014-02-24 2017-11-22 株式会社神戸製鋼所 チタンまたはチタン合金からなる鋳塊の連続鋳造装置
FR3033508B1 (fr) * 2015-03-12 2018-11-09 Safran Aircraft Engines Procede de fabrication de pieces de turbomachine, ebauche et piece finale
CN105033216B (zh) * 2015-08-26 2017-03-29 东北大学 一种厚板坯连铸过程结晶器喂钢带工艺参数的确定方法
CN108251693B (zh) * 2018-03-06 2020-09-22 中国航发北京航空材料研究院 一种高强高塑性三相TiAl合金及其制备方法
CN112746176B (zh) * 2020-12-29 2024-03-22 常州中钢精密锻材有限公司 控制esr铸锭中微量元素分布的方法及其应用
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EP1444065B1 (fr) 2008-01-09
US20060230876A1 (en) 2006-10-19
WO2003041896A2 (fr) 2003-05-22
DE10156336A1 (de) 2003-06-05
DE50211532D1 (de) 2008-02-21
WO2003041896A3 (fr) 2004-06-10
AU2002346837A1 (en) 2003-05-26
JP2005508758A (ja) 2005-04-07
JP4243192B2 (ja) 2009-03-25

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