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Patented Mar. 12, 1940 2,193,364 UNITED STATES PATENT OFFICE 2,193,364 PROCESS FOR OBTANING BEEY UMAND BERYLUMAL LOYS Carlo Adamoli, Milan, Italy, assignor to Perosa Corporation, Wilmington, Oel, a corporation of Delaware No Drawing. Application April 17, 1939, Serial No. 268,385. a tally June 6, 1936 16 Claims. (C. 5-84) The present application relates to a process ical method for the production of beryllium and for directly obtaining in a single operation start its alloys by treatment with a decomposing bi ing from halogenated compounds containing be valent metal such as magnesium, of a fluorine ryllium, beryllium as such or in the state of alloys containing compound of beryllium, that is a 5 with one or more alloyed elements capable of double fluoride of beryllium and an alkali metal 5 alloying with beryllium, and is a continuation-in (sodium) less rich in sodium fluoride than the part of my prior application Ser. No. 144,411 filed normal double fluoride BeFa2NaF. on May 24, 1937. The practical impossibility in fact has been In my said prior application, I have disclosed established which is met with in operating with 0 a process for directly obtaining in a single oper the normal double fluoride according to the re o ation beryllium or beryllium alloys starting from action: simple beryllium fluoride anhydrous and free or Substantially free from oxide. The present in which is rendered explosive by reason of the lib vention relates more particularly to a process eration of sodium and this is the reason in par s 5 of manufacture of beryllium or beryllium alloys ticular why instead of the normal double fluo starting from normal double fluoride of beryllium ride BeF2.2NaF the complex fluoride BeFa.NaF and an alkali-metal, the term “normal' being in is treated according to the reaction: tended to designate double fluorides containing ! 2BeFaNaF.--Mg-Be--MgF2--BeF2,2NaF two molecules of alkali fluoride for one molecule 20 of beryllium fluoride. This reaction would seem to be rendered pos 20 It is known how many difficulties of chemical, sible hereby the fact that the sodium fluoride thermal and technical nature are presented by and magnesium fluoride formed are present in a the problem of effecting by direct reaction start ratio such that the reversibility of the reaction ing from beryllium compounds, the production which would lead to the setting free of sodium - 25 of beryllium alloys with determined contents, in is prevented. However, as seen, the reaction 25 particular of a high beryllium content, as well thus effected does not lead to the liberation in as of pure beryllium. the metallic state of more than half the beryl It has never been possible up to now despite lium contained in the compound treated, the numerous attempts, to effect with industrial other half of beryllium remaining in the residue, 30 yields the production of beryllium and of its in the form of a complex compound from which 30 alloys by thermo-chemical treatment of beryl the said beryllium may be extracted for example lium compounds. in the form of double fluoride. From this there The difficulties of chemical and thermal nautre results a large diminution of the yield of the met with in decomposing beryllium compounds operation and a corresponding increase in the net 35 arise in particular from the fact that the ex cost of the manufacture. 35 change reactions which take place are very quick Thus the processes known up to now have not ly checked or give rise to the formation of prod permitted a solution of the problem of the in lucts which hinder them being carried out under dustrial manufacture of beryllium and its alloys. This problem is solved nevertheless in a simple the conditions in which it is desired to operate. 40 40 From the technical point of view these difficul and practical manner by the present invention ties are increased by the lightness of the beryl and that in conditions where there is effected in lium which tends to float upon the slag and to be a direct and complete manner and with a high maintained separate from any heavy metal pres yield practically reaching 100%, the production ent, by the high melting point of beryllium and of beryllium, either as such or in the state of 45 45 by its great tendency to be oxidized or to form alloys with predetermined contents, whatever carbides. these may be, and in particular with a beryllium In the presence of all these difficulties it has content above 25% or as high as is desired. been proposed to use electrolytic processes for Although none of the known processes per replacing thermo-chemical treatments, but none mitted practically complete reactions to be ef the less without arriving, by reason in particular fected, the new process which forms the subject 50 of the necessarily very high cost of the manufac of the invention permits such quantitative reac ture, at obtaining industrial results and being tions to be regularly effected and obtained, while able to effect this manufacture upon an indus allowing alloys of beryllium with determined con tria Scale. tents, or pure beryllium to be obtained with prac 55 one is thus brought back to the thermo-chem tically total maximum yield. ... 2 2,198,864 The process according to the invention con such as a high frequency furnace, though the SistS in bringing together a normal double fluoride invention is not confined to such an operating of beryllium and an alkali metal and a quantity nethod. Which practically corresponds stoichiometrically Instead of using as the Original beryllium con With the beryllium contained in said double fluo pound Cnly a normal double fluoride of beryllium ride, of an element or of a mixture of elements and an alkali metal, one may use a mixture of capable of reducing the beryllium fluoride to be simple beryllium fluoride and such a doubie fluo ryllium, in the presence of or in admixture with ride, provided that the reaction is effected ac a halide of another metal, preferably at least cording to this invention in the presence of a O bivalent, Such as magnesium fluoride or an alka neutralizer preventing the Setting free of the O line earth metal fluoride, and in heating the Whole alkali metal of the double fluoride. It should until the reaction of the beryllium fluoride is be also stated that the beryllium fluoride to be Substantially complete. utilised is an anhydrous fluoride practically free The interest in the presence of Such a fluoride from oxide, as described in our Copending ap s of an alkaline earth netal or magnesium in the plication Serial No. 144,411 above mentioned. s ca.Se Where a nOrnal beryllium and alkali double When the beryllium is required in the state fluoride is treated, may be explained by the fact of an alloy the reaction is performed in the pres that this alkaline earth or other fluoride acts as ence of the element or elements to be alloyed a neutralizer preventing the setting free, during With the beryllium. Said element or elements the reaction, of the alkali metal of the double may be mixed or preferably alloyed with the re 20 fluoride treated, and, due to the fact that just ducing agent, or they may be introduced in the the necessary stoichiometrical proportion of the reaction mixture in the form of compounds re reducing element is caused to act, there is thus ducible by the reducing agent, in which case the effected an integral displacement of the beryl reducing agent is used in a quantity Which corre lium of the compound treated Without danger of sponds Stoichiometrically With the beryllium and 25 setting free alkali metal (for example sodium). with the element or elements to be alloyed With Thus for example, in the case where the normal the beryllium. In the case of obtaining beryllium double fluoride of beryllium and Sodium is treated alloys it may be of interest to add to the Slags in the presence of Calcium fuoride with mag alkali or alkalinised salts which are not oxy nesium as the decomposing element, the opera genated, such for example as fluorides and chlo 30 tion follows the reaction: rides, in order to modify the fusibility of the slags according to the nature of the alloys to be BeNa2F4--Mg--n (CaF2) = obtained. 2NaF2--MgF2--Be-1-n (CaF2) The proportions of reacting materials to be s the (CaF2) added acting as a neutralizer due to employed according to the invention may be 35 Which all the Sodium remains fixed by the fluorine determined by calculation to effect the desired in the form of NaF. quantitative reactions. By thus utilizing for extracting all beryllium If: A, is the quantity of beryllium fluoride from a molecule of BeNa2F4, a single molecule of treated; O Mg (instead of two molecules of Mg which would B, the quantity of beryllium alloy to be ob 40 necessitate the corresponding reaction when tained; liberating Sodium) there has been effected under a, the beryllium content of the b3ryllium the optimum conditions the quantitative reac compound treated; tion: b, the beryllium content of the alloy to be 5 obtained; 45 C, the quantity of reducing element to be to Sun up, the utilization of a fluoride of a Caused to act; bivalent metal, such as an alkaline earth metal E, the chemical equivalent of beryllium; or magnesium, in presence of which the opera e, the chemical equivalent of the reducing O tion is carried out, prevents the setting free of element employed, the necessary propor 50 Sodium or other alkali metal which the compound tions of reacting materials, which should of beryllium treated may contain, due to the be approached as closely as possible are fact that it tends to decompose preferentially the following: to Sodium fluoride and by its tendency to set free 5 fluorine it favours a reaction which ensures the The quantity A of the beryllium compound to 55 fixation of the fluorine by the sodium in the be decomposed is determined by the expression: form of NaF in particular.

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