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By W. C. Lilliendahl, G. Meister

Uranium metal with a purity of about 99.9 pct was produced on a large scale by fused salt electrolysis with a material efficiency of about 90 pct. The material efficiency depends mainly on bath composition, electrolysis temperature, electrode smothering, and elutriation during washing of the powder. RESEARCH and development work on fused salt electrolysis carried on by the Westinghouse Lamp Div. Bloomfield, N. J., was done under the Manhattan District Corps of Engineers and later under the Atomic Energy Commission for the commercialization of uranium production for the first atomic pile at the University of Chicago in 1942. From the conception of the atomic bomb project it was recognized that metals with impurity levels having little metallurgical significance would be required. Permissible impurity levels were based on neutron absorption. Of particular significance was boron, which could not be present in amounts exceeding 1 ppm. The electrolytic method as developed in 1930 by Driggs and Lilliendahl,1,2 and later improved, yielded uranium of very low boron and other deleterious impurity content. No other method was capable at that time of producing uranium metal of the required purity.' The low boron content of uranium produced by the electrolytic process resulted from the availability of the reactants which were low in boron content, and from the inherent elimination of boron in the fused salt bath. Since the heart of any electrolytic process is the electrolysis cell, this paper will deal with the development of the original bath composition for the efficient production of uranium from a batch process to one of continuous operation. Emphasis also will be placed on other factors which will affect the material efficiency of the process. With the laboratory cell the material efficiency of uranium powder recovery in the early electrolysis was relatively low, about 35 pct based on the ratio of uranium recovered to uranium added. This early process also had other defects. The electro- lytic bath could not be used continuously. After three runs from a freshly charged crucible, the deposit showed a tendency to slip off the electrode as it was raised from the bath. This condition necessitated pouring the charge every fourth run and preparing a new bath. It was assumed at that time that this condition was caused by the increasing fluoride concentration with each addition of uranium salt, which adected the mobility of the uranium ions. Experimental The electrolysis cells differed in size only. They were of the floating cathode type. The laboratory cells were 21/2 in. ID and 6 in. deep and operated at 30 amp and 5 volts. Production was about 150 g metal powder per 8 hr. The plant cells (5 units) were 9 in. ID x 21 in. deep and operated at 1800 amp at 12 volts. The total production unit was designed to produce 250 lb of uranium powder per 8 hr day. Because of the tendency of uranium fines toward spontaneous combustion, material efficiencies were based only on the recovery of useful coarser metal which could be safely handled. The reported efficiencies are of particular significance only as related to the same group of experimental procedures. At the start of the project no changes were contemplated until previous data could be definitely confirmed. Therefore, the first experiments were with the 50 pct CaCl2-50 pct NaCl mixture. The material efficiency of uranium deposition as a function of the number of electrolyses is shown in Table I. In Table I, the decrease in efficiency at 800°C with number of runs is apparent and confirmed the earlier data. Operating at 900°C enabled the number of runs to be doubled, but before pouring the charge the efficiency of recovery became poor. This test indicated that the improved efficiency might have been caused by an increase in the fluidity of the bath.

Jan 1, 1958

By V. N. Mackiw

IN the process employed by Sherritt Gordon Mines Ltd. for the production of metallic nickel, a sul-fide concentrate is leached with ammonia and air under pressure. Following the removal of iron, copper, and other impurities, there remains a purified solution having the following analysis: 40 to 50 g per liter Ni, 200 to 400 g per liter (NH4)2 SO 4, and 20 to 30 g per liter NH3. Metallic nickel is reduced from this solution by hydrogen under pressure at 300' to 350°F in mechanically agitated autoclaves. A catalyst, ferrous sulfate, is required to initiate the first reduction. After the reduction, the depleted solution is discharged, leaving the metallic nickel in the autoclave. The nickel produced, being in a finely divided form, is used as a catalyst for the reduction of the next batch of solution. Upon repeated use the metallic nickel particles increase in size and become more compact, resulting in the production of a powder with higher apparent density. For this reason, each reduction is termed densification. Finally, when the burden of metal powder in the autoclave becomes too great to obtain effective agitation, both powder and depleted solution are discharged. The autoclave is then filled with fresh solution, ferrous sulfate catalyst added as before, and a new cycle started. The operation is described in earlier publications.1-6 A comprehensive historical review of the reduction of metals from solutions in general was given in a paper by Schaufelberger.7 The experimental data presented in this paper were taken from the work done in the Research Laboratory of Sherritt Gordon Mines Ltd. in Ottawa during the development of the process in 1951 and 1952. The results of the work were tested on a pilot plant scale in Ottawa in the period 1952 to 1953. Following laboratory and the pilot plant studies a commercial process has operated successfully since 1954 in the Nickel Refinery of Sherritt Gordon Mines Ltd. in Fort Saskatchewan, Alberta. General Experimental Technique The experiments were carried out in a stainless steel, 1-gallon, agitated autoclave designed and manufactured by Autoclave Engineers Inc. The inside dimensions of the vessel were 5 in. diam and 12 in. depth. The stirrer consisted of a 1/2 in. diam shaft 11 in. long fitted, with an axial flow type impeller (three blades bent to throw downwards) and a radial flow

Jan 1, 1958

By Kichizo Niwa

A LTHOUGH studies on the roasting of ferrous A sulfide have been carried out by several investigators, some disagreements still remain among those results. Schwab and Philinis1 have measured the rate of oxidation by a precise thermobalance and have concluded that the rate is controlled by diffu-

Jan 1, 1958

By R. E. Lund, D. E. Warnes

SELECTIVE sulfation of individual constituents in ores or metalliferous products has received increased attention in recent years. The fluid-bed reactor with its advantages of close control of both temperature and atmosphere promises to have ap-

Jan 1, 1958

By Volker Weiss, George Sachs, AE. P. Klier

PHYSICAL chemistry contributes to the understanding and efficient operation of hydrometal-lurgical processes in many ways, among them by providing quantitative answers to the following questions. 1) Can a given chemical reaction or process be made to operate and. if so, under what conditions? 2) what are the' factors which determine the rate of the reaction and how can this rate be regulated in practice? Thermodynamics attempts to answer the first of these questions and kinetics the second. The answer

Jan 1, 1958

By I. L. Barker

ALTHOUGH valuable information has been pub-lished on the important problems of slag losses with which every copper metallurgist has to contend, a great deal of money is still being wasted in copper smelters all over the world, through metal being irretrievably lost in reverberatory slags. When smelting a relatively low-grade pyritic concentrate together with a proportion of direct-smelting oxi- dized ore, as is done in Oroya, slag volumes are of necessity high, and even a relatively clean slag, say of 0.5 pct Cu, means a loss of almost 4 pct of all the copper charged, or over $1,000,000 annually at present output and prices. While it is known that such losses can often be reduced by allowing the slag time to settle, with or without addition of a reducing agent such as coal or pyrite, the facilities for such treatment are not always available in a plant of old design working to capacity under severe space limitations. Nor is it easy under such conditions to run large scale tests which may endanger the smooth flow of production for considerable periods without yielding

Jan 1, 1958

By W. A. Krivsky, R. Schuhmann

PREVIOUS papers in this series on the thermo-•t dynamics of copper-smelting systems have presented a survey of the field and an outline of the overall program: thermodynamic studies of iron silicate slags, 2-4 and thermodynamic data for simple mattes in the Cu-S system.5 Since this program was started, an excellent summary of the whole field of physical chemistry of copper smelting was published by Ruddle. The present paper represents a further step in the study of liquid mattes, and deals specifically with the Cu-Fe-S system. The importance of the Cu-Fe-S system to copper smelting is evident from the fact that these three elements constitute 90 to 99 pct of the totalweight of most commercial mattes. In copper mattes oxygen is an important fourth component. Oxygen was rigorously excluded in the work to be described in this paper. However, the behavior of oxygen in mattes was the subject of a companion research by Lander' which will be described in a subsequent publication. Several studies have been made previously of phase equilibria in the Cu-Fe-S system,8-10 so that the ternary phase diagram is fairly well established in most regions. Also, separate studies have been made of the phase diagrams and thermodynamic properties for the three binary systems: CU-S,5,12-15 CU-Fe,11,14,17 and FeS.11,14,16,17 However, no work has

Jan 1, 1958

By V. F. Leferrer

A new process for the treatment of silver crusts from desilverization of lead has been developed by Societe de Penarroya. The zinc contained in the crusts is recuperated by vacuum distillation at low temperature. The use of special retort crucibles is avoided. AT Noyelles-Godault the Parkes process (zinc addition to a silver-bearing lead melt) is used to desilverize lead bullion from the blast furnace. The crust which rises to the surface of the bath is removed and pressed by a well-known process in a press of the Howard type. The pressed crust, called zinc crust or silver crust, contains 10 pct Ag, 30 pct Zn, and 60 pct Pb. It is melted under a salt bed in a small, narrow, and deep kettle heated only in its upper part. A liquid concentrated alloy is obtained which is called T.A.C. in France (triple alliage concentr6) analyzing approximately 25 pct Ag, 65 pct Zn, 8 to 10 pct Pb, and 1 to 1.5 pct Cu. This T.A.C. is a real metallic alloy, completely deoxidized, and can be stored indefinitely. The process used at Noyelles-Godault consists in distilling this alloy in a tight furnace, under low vacuum and at low temperature, so that only the zinc distills and is condensed into liquid form. The residual silver-bearing lead is almost entirely free from zinc and oxidized dross. The vacuum dezincing equipment, see Figs. 1 and 2, consists of: 1) A furnace, constituted of a casing of steel plate lined with refractory bricks, heated internally by means of graphite resistors. The temperature of the furnace is measured by a thermocouple device and controlled by an automatic temperature regulator which acts upon the flow of the current passing through the resistors. Two doors, numbered 1 and 2 in Fig. 2, are provided for, one for charging the T.A.C., the other for tapping the high silver-bearing lead. 2) A condenser, and an ordinary room lined with good heat conductor refractory material. This condenser is provided with a graphite resistor which serves to bring to temperature when starting the furnace. A thermocouple records the temperature of the zinc melt and controls the temperature in the furnace, that is, the flow of current through the resistors, by means of the above mentioned regulator, so that the distillation rate in the furnace does not exceed that of the condensation. The condenser is connected to the vacuum pump by a filter. The whole equipment should, of course, be fluid-tight. The operation is carried out under a vacuum of about 10 mm Hg.

Jan 1, 1958

By Gerhard Derge

EXTRUSION processes are used in the commercial production of a wide variety of products, as indicated by the review presented a few years ago by D. K. Crampton.1 Most writers have confined themselves to a general description of the equipment and products and the engineer-ing aspects of the process. The few studies that have dealt with the metallurgical side of extrusion have been concerned primarily with an examination of the mode of flow of the metal during extrusion. This has been accomplished by the use of composite billets, by scribing grids on symmetrical sections of billets and observing the change of dimensions in the gridwork, or by examining microstructures in extruded sections.2-8 Another limitation of these original studies is that they were confined to the extrusion of very simple shapes, usually rods having a diameter of about one-fourth that of the billet. Tin is particularly well suited to the extrusion of collapsible tubes and similar shapes in which the extruded section is very small in comparison to the diameter of the billet or slug. In modern production, impact extrusion methods are generally employed, therefore the thickness of the slug is small compared to its diameter. Under these conditions the process differs considerably from the processes that have been most fully described in the literature, and it is known that the quality of the product is very sensitive to slight variations in any one of the many variable factors involved, such as composition and structure of the alloy, rate of extrusion, temperature, shape of punch and die. An exhaustive examination of all of the above-mentioned problems promises to produce so many data that it seems advisable to initiate the reports at this time, even though all of the factors outlined have not been examined fully, and to confine this paper to a description of the apparatus and method. Only tin and its alloys with small amounts of copper have been considered. These are the alloys most commonly used in this country for the production of the type of articles already described.

Jan 1, 1939

By Ira A. Stark

Use of clay-working machinery in the metallurgical industry is by no means new. Extrusion- agglomeration as a basic operation in the non-ferrous field has a history of more than 50 years. This article advocates using the technique in the ferrous field where it might serve a useful purpose in today's operations. Many of the processes involved in production of iron ores result in fine powders, with a considerable percentage running finer than 200 mesh. In many instances, mining and related processing operations are located far from furnace operations. Shipping the powdered ore is impractical since handling losses and furnace losses from dusting would be excessive and powdered material must be agglomerated. The agglomerate must withstand the handling involved in transportation and here the continuous pugmill-extruder can be used to form a strong dense product.

Jan 6, 1959

By W. B. Price

AT the New York meeting of the American Institute of Mining-and Metallurgical Engineers held in February, 1926, W. H. Bassett and J. C. Bradley presented a paper entitled "Exudations on Copper Castings."§ The purpose of the present paper, as the title suggests, is to call attention to somewhat similar phenomena which the authors have encountered in brass and bronze. From a study of the examples given, a more-or-less speculative theory of "inverse segregation" is advanced. PROTUBERANCES ON ADMIRALTY BRASS In the rolling mill of the Scovill Manufacturing Co., there have been found quite commonly bars of certain alloys which had a sort of shaggy roughness on the surface due to slight metallic protuberances. No special attention was paid to these until some bars were found on which these protuberances were heavy enough at the bottom of the bars to produce a blistered appearance. A sample of the protuberances was milled off the surface of the bar illustrated (Fig.. 1a) and upon analysis was found to contain 66.66 percent. copper, 4.02 per cent. tin and .03 . per cent. lead, whereas the average composition of the bar was 70.21 per cent. copper, 1.21 per cent. tin, and .01 per cent. lead. A sample of the shaggy-rough protuberances at the -very top of a bar was also analyzed and was found to contain 2.45 per cent. tin, indicating that it was probably of the same origin as the blistered areas. These results were not entirely unexpected for previous analyses of this alloy had -revealed that the surface was richer in tin than the rest of the bar. This, of course, is contrary to what we would expect from a consideration of the equilibrium diagram and has been called "inverse segregation."

Jan 10, 1926

By W. B. Price

AT the New York meeting of the American Institute of Mining and Metallurgical Engineers held in February, 1926, W. H. Bassett and J. C. Bradley presented a paper entitled "Exudations on Copper Castings."' The purpose of the present paper, as the title suggests, is to call attention to somewhat similar phenomena which the authors have encountered in brass and bronze. From a study of the examples given, a more-or-less speculative theory of "inverse segregation" is advanced. Protuberances on Admiralty Brass In the rolling mill of the Scovill Manufacturing Co., there have been found quite commonly bars of certain alloys which had a sort of shaggy roughness on the surface due to slight metallic protuberances. No special attention was paid to these until some bars were found on which these protuberances were heavy enough at the bottom of the bars to produce a blistered appearance. A sample of the protuberances was milled off the surface of the bar illustrated (Fig. la) and upon analysis was found to contain 66.66 per cent. copper, 4.02 per cent. tin and 0.03 per cent. lead, whereas the average composition of the bar was 70.21 per cent. copper, 1.21 per cent. tin, and 0.01 per cent. lead. A sample of the shaggy-rough protuberances at the very top of a bar was also analyzed and was found to contain 2.45 per cent. tin, indicating that it was probably of the same origin as the blistered areas. These results were not entirely unexpected for previous analyses of this alloy had revealed that the surface was richer in tin than the rest of the bar. This, of course, is contrary to what we would expect from a consideration of the equilibrium diagram and has been called "inverse segregation." Fig. 16 is a cross-section of a bar through the protuberances on the surface. It reveals that there is a decidedly different structure through the raised areas and seems to indicate that the bar originally solidified

Jan 1, 1927

By W. H. Bassett

Beads of metal frequently appear at the ends of cast-copper wire bars and on the sides of wedge cakes near the top. These are richer in cuprous-oxide than the rest of the casting. A micrographical study of these exudations has been made. It is suggested that the material is forced through the surface while the copper is solidifying. If not eliminated in process of manufacture, it shows on the finished polished sheet copper in patches differing in color from the main body of the sheet. FIGURES 1 to 4 show the copper exudations, at different magnifications, as they appear on the ends of cast wire bars, and on the sides, usually near the top, of wedge cakes. Sometimes the exudations are in fine "drops;" at other times, large masses of the material are found. Microscopic examination of the copper exudation indicates that it is high in oxide and of eutectic proportions. Because of the difficulty of securing a suitable sample, the protuberances have not been analyzed chemically; but the spectroscope shows no indication that there are any more metallic impurities present than in the balance of the copper. The lowest copper plus silver content of the coppers studied for this? paper was 99.914 per cent.; the highest, 99.966 per cent.; so the oxygen content of the whole casting would be well under 0.07 per cent.

Jan 2, 1926

By Ronald A. Murdock

INTRODUCTION Exxon's Highland Uranium Operations in eastern Wyoming consists of an open pit, an underground mine and a mill complex. The geology of the deposit is reviewed in this paper, and an overview of the mining operations at both the surface and underground mines is presented. Topics discussed include geology, stripping of overburden and mining of ore in the open pit, and underground development and stoping methods. GEOLOGY The Highland uranium deposit was discovered in 1968 by Exxon Minerals Company, U.S.A., in Converse County, Wyoming, 35 miles north of Douglas. The mine is located at an elevation of about 5,200 ft in a high-plains, sagebrush-covered prairie typical of eastern Wyoming. The deposit is near the southern edge of the Powder River Basin in the Paleocene Fort Union Formation. The Fort Union Formation consists of 1,900 to 3,200 ft of sandstone, siltstone, mudstone, claystone and coal beds. Siltstone, mudstone and claystone are collectively referred to as "shale" at Highland. There are many alternating layers of shale and sandstone in the Fort Union Formation; but in the Highland area, there are only three principal sandstones, known as the Highland Sand Group, which host the uranium. The combined sand thickness is about 150 ft.

Jan 1, 1983

By F. G. Cottrell

AS previously announced, Van. H. Manning has resigned as director of the Bureau of Mines, effective June 1, to become director of research with the newly organized American Petroleum Institute. Doctor Manning has been connected with the Department of the Interior for 34 years, having been civil engineer with the Geological Survey, from 1885 to 1910, previous to his connection with the Bureau of Mines which was organized in the latter year. Doctor Manning was appointed to an administrative position in the new Bureau under Joseph A. Holmes, its first director, and on Jan. 1, 1911, was made assistant director. On Jan. 1, 1914, when Doctor Holmes had to relinquish active

Jan 1, 1920

F. McMillan Stanton was born in New York City on May 23, 1865, the son of an English father and of a mother whose family was linked with that of Peter Stuyvesant. Mr. Stanton took his degree from the School of Mines of Columbia University in 1887, worked for two years as an assayer and surveyor and then went into the mining field on his own account. After a few years, he was offered a position with the Atlantic Mining Co., and began the work which was to continue with marked success for twenty-three years. In 1910, Mr. Stanton retired and went to Europe for a rest. Upon his return in 1914, he was elected treasurer and director of the Mohawk Mining Co., the Wolverine Copper Mining Co. and the Michigan Copper Mining Co., to which group was later added the White Pine Extension, Copper Co., and continued to serve these companies until the time of his death, Sept. 12, 1916.

Jan 12, 1916

The Ural Mountains, which were formerly the dividing line between Asia and Siberia, area chain of low mountains, the highest peaks reaching only a little over 5000 ft. The country has been much eroded and the mountains now appear as rounded hills. In the central and northern parts turf swamps abound. The range is covered with forests except at the extreme southern end. The trees are mostly pine. Birch grows on cut-over areas, but never to large size. The rivers are small or the fall is slight, so no large water powers are available. A series of rivers with a north and south course, and which are navigable for long distances, furnish cheap transportation during the summer months. Railroad communications are very insufficient. The first active exploitation of the mineral wealth was initiated by Peter the Great, who sought iron and copper for use in his wars against the Swedes. He selected a blacksmith named Demidoff to supervise operations and gave him rights to most of the Ural and to the Altai. The Nijni Tagil Estates are still in the possession of the Demidoff family. The original large grant was subsequently subdivided through inheritance and marriage, but the Ural is still a country of very large estates, some of them held as leases only and some of them by actual ownership.

Jan 6, 1919

By G. L. Craig

COPPER containing a small amount of arsenic has been used extensively abroad, and a number of reports, particularly those by English workers, have indicated that such copper is better suited for certain uses than high-conductivity copper. Inasmuch as a large percentage of the copper fabricated is used for nonelectrical purposes where high conductivity is not at all essential, it has been suggested that arsenical copper might be at least as suitable as high-conductivity copper for many purposes. An investigation spon-sored by the Calumet & Hecla Consolidated Copper Co. at Battelle Memorial Institute was therefore undertaken with the object of determin-ing the effect of small amounts of arsenic (up to 0.75 per cent) on the properties of copper. In this work the effect of arsenic on the basic properties of tough-pitch and of phosphorized copper have been critically studied and many data collected from laboratory experiments which have been supplemented by mill-scale tests. The results of these tests, with coppers of the type referred to, in the annealed condition and after various degrees of reduction, show that the basic properties of copper are not greatly affected by small amounts of arsenic, an increase in strength being observed with increasing arsenic with no corresponding decrease in ductility. It is well known that the evaluation of material for plastic deforma-tion, on the basis of laboratory tests, may not be directly comparable with its performance in commercial operations. In order, therefore, to substantiate the data obtained at the Institute, the cooperation of the Wolverine Tube Co. was obtained for a series of production tests on the fabrication characteristics of phosphorized arsenical copper in the manu-facture of seamless copper tubing. In these tests the behavior of the arsenical coppers was carefully observed in comparison with that of representative types of phosphorized arsenic-free copper, which were fabricated under the same conditions.

Jan 1, 1933

By C. S. Sivil

To modern civilization the platinum metals are of inestimable value. Their distinctive properties, both physical and chemical, render them indispensable in an age in which the processes of the laboratory are becoming an essential part of the daily life of the world. Generally, their function, though vital to particular processes, is not spectacular, and so remains unknown to all except the operators. EARLY METHODS OF MANUFACTURE The properties of platinum were recognized as of prime importance for scientific work at. a very early date, probably between 1750 and 1760. The difficulty of making articles from it seemed almost insurmountable, because no means of attaining the temperature necessary to melt it were known at that time. It is true that solid platinum could be obtained by fusing the metal with a more volatile metal such as arsenic, which was subsequently driven off by baking, but such a method, at its best, would give only a very brittle product, which was totally unsuitable for the purposes for which it was intended. Little, if any, progress could be made until it was discovered that platinum sponge, heated to white heat and hammered in an iron or clay mold, would metallize and retain the shape of the mold. This was a process that could not be wholly satisfactory but from it developed the method of pressing the sponge in a mold and forging it at white heat into wire or sheet. At present a somewhat similar process must be used for fabricating articles of tungsten, molybdenum and other metals of high fusing point, as with these metals we face today the same problems that the scientists of the eighteenth century encountered with platinum, but possibly the next significant advance in the metallurgy of these metals will be the devising of means to melt and cast them.

Jan 1, 1931

By D. N. Hedges

This paper discusses the actual recovery and installation of a longwall in a bituminous coal mine in western Pennsylvania. The coal bed mined is in the Lower Freeport seam, which averaged 1.07 m (42 in.) in height locally. Drainage from the mine is about 13.25 ML/day (3.5 million gal per day) of water. This water deteriorates the mine's predominately fire clay bottom making it extremely difficult to move equipment. Support removal is accomplilshed by pulling the 5.44 t (6 st) shields out under their own hydraulic power and transporting them by track 8.05 km (5 miles) to the next longwall panel. This paper also discusses the changes that will be made to aid in the succeeding longwall recoveries and installations.

Jan 1, 1985