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Blanketing Atmosphere for Molten Aluminum-Lithium Or Pure Lithium

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Blanketing Atmosphere for Molten Aluminum-Lithium Or Pure Lithium Europaisches Patentamt European Patent Office © Publication number: 0 268 841 Office europeen ctes brevets A1 EUROPEAN PATENT APPLICATION © Application number: 87115574.3 C22C © int. Cl.": 1/02 , C22B 9/05 © Date of filing: 23.10.87 © Priority: 30.10.86 US 925652 © Applicant: AIR PRODUCTS AND CHEMICALS, INC. © Date of publication of application: P.O. Box 538 01.06.88 Bulletin 88/22 Allentown, Pennsylvania 18105(US) © Designated Contracting States: @ Inventor: Zurecki, Zbigniew BE DE ES FR GB IT NL SE 704 S. Jefferson Ave. Apt 11 Allentown, PA 18103(US) © Representative: Kador & Partner Corneliusstrasse 15 D-8000 Munchen 5(DE) ® Blanketing atmosphere for molten aluminum-lithium or pure lithium. © Blanketing of molten aluminum-lithium alloys is performed under a nontoxic and noncorrosive dich- lorodifluoromethane containing gas atmosphere, which produces a thin self-passivating fluxing film on the melt surface. The blanketing atmosphere pro- tects the melt from oxidation, burning, and lithium evaporation, improves alloy cleanliness and can be used in any furnace, transfer or casting operation. The blanketing atmosphere can be applied in the entire range of commercial or master aluminum- lithium alloys including pure lithium melts. The dich- lorodifluoromethane concentration in the blanketing atmosphere can range from 0.05 to 100 vol% with the remainder being an inert gas such as argon. 00 00 CO CM CL 111 Xerox Copy Centre 0 268 841 BLANKETING ATMOSPHERE FOR MOLTEN ALUMINUM-LITHIUM ALLOYS OR PURE LITHIUM continuously monitoring the ingot casting rate and Field of the Invention continuously adding a measured and controlled amount of molten lithium beneath the surface of This invention relates to the production of the molten aluminum stream as it flows to the ingot aluminum-lithium alloys, and more particularly to 5 casting station. At the contact location of the lithium the protective atmospheres for the operations of and aluminum, a mixture of argon and chlorine melting, holding, alloying, stirring, degassing, mold and/or other inert and reactive fluxing gases is casting, and direct chill casting of aluminum-lithium injected through a vaned, rotating dispenser. The alloys. patent further discloses that the introduction of the 70 lithium into the aluminum must be below the sur- face of the aluminum in order to minimize the Background of the Invention occurrence of oxidation, fuming and hydrogen ab- sorption. The production of aluminum-lithium alloys has Both U.S. Patent 4,248,630 and 4,556,535 become of commercial interest, due to the com- 75 counterbalance the detrimental effects of lithium bination of mechanical properties and light weight reactivity by means of minimizing time between the which these alloys exhibit. Unfortunately, molten alloying and casting, neither process deals effec- aluminum-lithium alloys are very reactive with air tively with problems of submerged injection of a which makes their production and fabrication cor- premelted lithium charge, inert blanketing, lithium respondingly difficult. 20 evaporation and melt hydrogen pick-up. Both sys- The surface of an Al-Li bath reveals chemical tems suffer from the lack of proper melt surface behavior of molten lithium rather than aluminum protection for inert gas bubbling and handling oper- thus causing the bath to: (1) burn on contact with ations. air thus forming an excessive dross layer with the Batch processes utilizing molten salt fluxes are generation of toxic fumes resulting in poor lithium 25 an alternative to the continuous systems, discussed recovery and hazardous work conditions; (2) attract above, which are expensive and inflexible in opera- hydrogen from the atmosphere, including traces of tion, particularly when operating ranges or alloy water vapor, which increases hydrogen absorption changes are required. These fluxes, which are and results in higher porosity levels and a loss of comprised primarily of lithium chloride or lithium the desired mechanical properties; and (3) become 30 fluoride, are applied to the surface of the lithium practically unskimmable thus preventing proper containing bath whereby they eliminate a part of stirring and degassing of the melt since any disrup- the problem related to the lithium reactivity and still tion of the generated dross will increase the rate at achieve a lithium recovery of approximately 80 which further quantities of dross are formed. To wt%. Unfortunately, disruptions in the bath surface overcome these enumerated difficulties, several so- 35 whether by stirring or degassing or any other lutions have been offered in the literature. movement in the bath breaks the flux layer and U.S. Patent 4,248,630 discloses a process for exposes the metal to ambient air resulting in violent adding alloying elements, including highly reactive oxidation of the lithium. Also, fluxes are highly metals such as lithium, to molten aluminum so that corrosive to the refractory linings of the furnace normally occurring oxidation reactions of such ele- 40 and related casting equipment and materials of ments with the stmosphere is minimized. Basically, construction. The fluxes are also known to deterio- the process requires that all other alloying ele- rate the metal cleanliness and contaminate the ments except lithium be added to the molten alu- environment as well as the equipment including minum and the melt be degassed and filtered. melting, mixing, holding, and alloying furnaces, Upon completion of the degassing/filtering step the 45 metal transfer troughs, casting stations, direct-chill lithium is introduced into a mixing crucible as the liners and molds. Difficulties associated with stor- final step prior to casting. The desired concentra- age and handling of the fluxes frequently cause a tion of the lithium is achieved by controlling the carry over of moisture into the aluminum-lithium relative amount of lithium and the alloyed melt. melt .and the subsequent oxidation and hydrogen Uniformity of the mixture is achieved by mechani- so pick-up. cal stirring. The mixing crucible and all other cru- Other solutions such as blanketing with a pure cibles in with lithium may be present are kept dry inert atmosphere eliminate the flux method under an argon blanket. drawbacks, however, these require tightly enclosed U.S. Patent 4,556,535 discloses a process for pots and troughs and therefore are not flexible forming aluminum-lithium alloys which comprises enough to be used in various stages of aluminum- 0 268 841 lithium fabrication. Furthermore, inert atmosphere Basically, the CCbFa'Ar blanketing blend is ap- blanketing does not decrease lithium evaporation plied to the molten aluminium-lithium alloys during from the bath, which results in; substantial lithium the melting, holding, alloying, stirring, degassing, losses and creates a potential1 hazard. Inert at- melt transfer and casting processes. As a result of mosphere blanketing does not provide flux layer 5 the application of CCI2F2 reacts with the alloy for- cleaning properties such as preventing the hydro- ming a passivating and self-healing viscous liquid gen just removed from the bath during degassing layer which protects the metal from oxidization, from freely back-diffusing into the uncovered alloy, burning, hydrogen and/or moisture pick-up, hydro- and/or allowing nonmetallic inclusions which have gen back-diffusion, and lithium loss due to an moved to the bath surface during inert gas stirring 10 evaporation effect. The formed liquid layer can be to be intercepted by the flux layer. skimmed without harm to the metal if the process requires a reactive bubbling skimmed operation for degassing and/or inclusion removal. Thus, both an Summary of the Invention inerting and fluxing benefit is achieved. 75 The CCbFyinert gas blend should be applied to The present invention is a protection process the molten aluminium bath while the lithium is for use in melting, holding, alloying, stirring, degas- introduced into the aluminum or at any later mo- melt sing, transfer and casting processes for mol- ment or stage of the aluminum-iithium melt pro- ten aluminum-lithium alloys or lithium. The process cessing. The gas blend (atmosphere) may also be of the present invention comprises blanketing the 20 contained above a pure lithium melt as well. of top a molten aluminum-lithium alloy or lithium CCI2F2 concentration in the blend may be var- bath with an effective amount of a nontoxic, reac- ied in the range of 0.05 to 100 vol%; the result tive, dichlorodifluoromethane containing, gas atmo- being the higher the CCI2F2 concentration the high- sphere. The dichlorodifluoromethane reacts with er the rate at which the resultant fluxing film is primarily the lithium in the melt and rapidly forms a 25 formed. The application of a 100% by volume thin fluxing layer on the surface of the bath. This CCI2F2 atmosphere over the melt will not cause any thin layer prevents oxidation of the melt, hydrogen hazardous conditions. A 0.05-5.0 volume % CCI2F2 absorption into the melt, and the formation of a concentration in the inert gas is preferred. The inert heavy dross layerr the thin layer is easily skimmed gas can be chosen from the group consisting of Ar, from the surface if necessary. The layer develops 30 He, etc. Since nitrogen is slightly reactive and even if not all of the ambient air is evacuated from nonprotective to both lithium and aluminum and above the melt. nitrogen will cause deterioration in melt cleanliness, Alternatively, other substitue blanketing at- in those instances where melt cleanliness is not a mospheres containing an effective amount of a paramount concern, nitrogen can be used as the halogen compound having at least one fluorine 35 inert gas. atom and one other halogen atom selected from The dichlorodifluoromethane could be replaced the group consisting of chlorine, bromine and io- by other reactive gases. These other reactive gas- dine, or an atmosphere comprising fluorine or a es of the blend can consist of any combination of fluorine-containing compound and one other halo- chlorine and fluorine bearing gases.
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