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By Theron Wasson

Michigan's production of 17,301,000 bbl. in 1945, which is in line with previous years, has been maintained by extensions to old fields like Deep River, Adams, Fork, and others. There were a number of new discoveries but, as in the past, these are not given very much importance because enough drilling has not been done to develop their potentialities; however, judging by the past, some of them will develop enough production so that 1946 -will probably be in line with other years. Activities in Michigan were confined to the Basin area of the lower Peninsula, which has been under development since 1925.

Jan 1, 1946

By G. Das, S. V. Radcliffe

The substructural features developed in tungsten as a function of annealing temperature (up to 2200°C) and type of material [undoped and doped powder metallurgy (PM) tungsten and electron beam melted tungsten] have been investigated by transmission electron microscopy. For doped PM tungsten wires, characteristic "par-ticulate" substructural features developed rapidly with increase in annealing temperature above 700°C. The features consisted of parallel rows of elongated or circular shapes (500 to 1000A diam) lying along the direction of the wire axis and were identified as internal voids by diffraction contrast experiments. In recrystallized doped PM rod, larger voids were observed and were identified by precision dark field analysis to be cubic in shape and bounded by (100) planes. In marked contrast with both the doped PM materials, recrystallized undoped PM rod exhibited only very occasional and randomly arranged voids. Furthermore, no voids were observed in either material after electron beam melting. The high concentration of voids in the doped PM materials is attributed primarily to vaporization of doping additions or their pvoducts situated at the original grain boundaries , whereas the few voids in undoped material are considered to be traces of microporosity which were not eliminated during sintering. A tentative mechanism is suggested for the dezlelopment of the voids in relation to the processing sequences (sintering and working) and to the subsequent annealing. In recent years, a characteristic substructural feature consisting of rows of small elongated or circular regions of light contrast lying along the direction of working has been seen in thin foil electron microscopy studies of annealed sheet, wire, and rod tungsten. These features were present in the published micrographs of sheet by Weissmann et al.1 and of wire by Meieran and Thomas2, although the authors did not draw attention to them. Wronski and Fourdeux3 observed similar features in sintered rod tungsten (it was not specified whether or not the material was doped*) and interpreted them on the basis of their ap- particles, based on extraction replica evidence from the fracture surface of the initial hot-rolled slab material from which the sheet was prepared. No diffraction contrast experiments on the features were reported in any of these studies. The present investigation was undertaken with the primary objectives of: a) identifying the nature of these substructural features in tungsten by electron diffraction contrast experiments, since the contrast for voids can be expected to differ from that for crystalline or glassy particles, and b) elucidating the origin of the features and their development. For the latter purpose, doped and undoped powder metallurgy tungsten was obtained as rod and wire to represent different stages of reduction during final processing. These materials were examined both in the as-processed condition and after annealing to successively higher temperatures. In addition, the same doped and undoped materials were examined after vacuum melting in rod form. I) MATERIALS AND PROCEDURE Doped powder metallurgy (PM) tungsten wire (commercial purity 99.9 pct W) was obtained in the as-drawn and surface ground condition (0.030 in. diam "ground seal rod"). Doped and undoped tungsten rod (0.075 in. diam) representing an earlier stage of final processing was obtained from the same commercial source (Refractory Metals Division, General Electric Co.). Lengths of both the doped and undoped rod materials were single-pass melted in an electron-beam zone refiner to examine the effect of vacuum melting on the substructure. Annealing was carried out in a tungsten crucible in a tantalum strip resistance furnace under a vacuum of l0-15 mm Hg. Longitudinal sections of the wire and rod materials were examined by light and electron microscopy. The preparation of thin foils suitable for electron transmission from 0.030 in. diam tungsten wire and the rod specimens was carried out by means of a high-precision microjet technique developed to provide lack of jet stability and precise control of the area thinned. The method is described in detail elsewhere.' The foils were examined in a JEM 6A electron microscope using a goniometer stage (±20 deg tilt, 360 deg rotation) and operated at 100 kV. To minimize contamination problems a 200 µ condenser aperture was used in conjunction with a useful beam current of 50 µA. II) RESULTS AND DISCUSSION A) Diffraction Contrast Analysis. In order to determine the optimum conditions for the development of the substructural feature, a series of isochronal 30 min annealing experiments were carried out on specimens of the doped PM tungsten wire. The transmission electron microscopy analysis showed that the as-drawn wire, Fig. 1(a), consists of 'fibers' whose long axis is closely parallel to the wire axis of (110). The fiber width averages some 0.5 µ. Dense disloca-

Jan 1, 1969

By H. Bartholomew, L. Bernstein

Experirmental bonds of Ag-In SLID to gold, copper, nickel, Kovar, Dumet, nickel-plated molybdenum, ALL-Pt vrzetallizing on ceramic, and nickel-plated Mo-Ti metallizing on Al2O3 ceramic have been made and exalnined. Metallographic taper sections were made of all bonds for Phase identification. In addition, failuve temperatltres were determined for bonds heated undev shear load. Sowe bonds were subjected to electvon-probe microanalysis. The ternary SLID system Ag-In-Sn was similarly evaluated. Plwtonticrogaphs and electron-probe data are discussed and related to over-all phase diagrams , diffusion effects, and wetting properties of the liquid. The rates of diffusion andor compound formation of gold, silver, and copper in indium and In-Sn liquids are found to descend in that order, as measured by the relatzve thickness of phase layers in the interfaces of bonds made at 200to 400°C. It is concluded that the SLID process enables one to produce bonds which are stable at high temperatures, after having been fabricated at low temperatures, and meet most requirements for application in interconnection, silicon bonding, or hermetic sealing of electronic devices. In a previous publication by one of the authors, the theory and principle of SLID bonding in simple binary systems was discussed. SLID bonding can be defined as a joining process using a preform with a laminated structure: a low-melting material clad on a high-melting core. During the bonding cycle a metallurgical transformation occurs such that the resultant structure can withstand, without reliquefying, temperatures higher than those at which the bond was made. The phases present in the joint interface region are high-melting compounds or, if equilibrium is reached, solid solution. Properties will depend on the phases present, ultimately approaching those of the solid substrate core of the SLID preform. The high-temperature strength of bonds made in these systems was correlated to phase identification in the interfacial bond regions from metallographic cross sections and electron-probe X-ray microanalysis data. When complex electronic components are assembled, multiphase systems result at the interfaces of bond regions. In these ternary and higher-order systems very little diffusion and phase-diagram data is available with which to predict the nature of the interfacia1 region that will result from conventional fabrication processes and subsequent field use of the component. Clarke and Rhines did early work in the field using the Al-Mg-Zn system as a vehicle. Guy and co-workers studied a portion of the Cu-Zn-Ni system and some mathematical4 and general5 aspects of multiphase diffusion. irkald' and coworkerse recently studied diffusion in the Cu-Zn-Sn system. No diffusion studies have been made on ternary systems directly applicable to this investigation but some phase diagrams are available: g-u-n, u-i-n, and CU-i-n. I) DESCRIPTION AND EXPERIMENTAL PROCEDURE The elements Au, Ag, Cu, Ni, In, and Sn are found in alloy systems commonly used in fabricating and assembling electronic components. Reference to the appropriate phase diagrams9 and the previous publication will indicate that the binary systems of any of the two low-melting elements, indium and tin, with any one of the other four higher-melting elements are capable of producing SLID bonds. It is not unreasonable to assume that any ternary or higher-order alloy system containing at least one of the elements gold, silver, copper, or nickel and one or both of the elements indium and tin could be used to produce bonds which are stable at high temperatures, after having been fabricated at low temperatures. Indeed, the liquidus contours and isothermal sections of those phase diagrams available7 do so indicate. The parameters affecting the bond and the equipment used in evaluating the bond were described in an earlier paper.' The current investigation used the

Jan 1, 1967

By Francis Church Lincoln

I. SITUATION AND SURROUNDINGS. THE Promontorio mine is situated at the northern end of the Sierra San Francisco de Coneto, in the town of Promontorio, Partido of El Oro, State of Durango, Mexico. As shown in the sketch-map, Fig. 1, the nearest railroad station is Chinacates on the Mexican International Railroad, 82 miles north of the city of Durango. The mine is 16 miles north of the station by air-line. It is reached by means of a good wagon-road which first crosses the Guatimapé Plain, passing the ranches of San Antonio and San Julian, to Estacion-a distance of about 15.5 miles-and then entering the mountains crosses the Sierra to Promontorio-a further distance of 11.5 miles¬making in all a distance of 27 miles by road from railroad to mine. Promontorio is just beyond the summit of the range, at an elevation of about 8,000 ft. above sea-level, or 1,350 ft. above the Chinacates station. The Castillo de San Francisco, the highest peak in the Sierra, has an altitude of 10,000 ft., and the Promontorio road crosses the summit of the ridge at an elevation of 9,000 ft. by a pass just below this peak known as the Puerto del Almagre. The Promontorio mill is situated at Santa Ives, 2 miles by tram or 3 miles by wagon-road to the north of Promontorio and about 600 ft. lower. The Sierra San Francisco de Coneto decreases in height towards the north and west till it comes to an end at the Melchor Arroyo on the ranches of Melchor and Ramos. Beyond this arroyo another range, the Sierra de la Candela, begins. In the vicinity of the Promontorio mine the hills are very rugged and the surface is furrowed by ravines which contain running streams during the rainy season-July, August and

Jan 1, 1908

Edward Halse, Puerto Berrio, Colombia, So. Amer. (communication to the Secretary*): The Taviche mining-district is generally known as " Taviches," being named from the two villages called respectively San Pedro Taviche and San Jero-nimo Taviche. It is so called by Jose G. Aguilera, in his paper on the Geographical and Geological Distribution of the Mineral Deposits of Mexico;' and in published reports by the late N. W. Rudston Read ;2 and by Juan de Dios Villarello3 The region is a large one, measuring about 24 miles long and 7 miles wide. Dr. Chance, in his interesting paper, tells us very little about the nature of the ores, and, with regard to the geology of the district, contents himself with observing that " the country, as a rule, consists of eruptive rocks; and no evidences of sedimentary strata appear near the mines." The latter part of the above statement is hardly correct. The formation is mainly

Jan 1, 1906

By D. A. Dahlstrom

Although the liquid-solid cyclone is a relatively recent innovation in the field of coal preparation, various authors have already indicated three distinct applications to operations encountered in the modern tipple. Driessen's articles and work at the Dutch State Mines exhibited its possibilities in the beneficiation of fine coal with apparently high efficiencies down to the 200-mesh fraction. 1 2 3 4 Other publications point out its use as a recoverer, thickener, and preliminary dewatering agent of fine coal which in too many cases is being wasted due largely to former high operating cost limitations 5 6. Finally, certain authors have emphasized the practicability of applying the cyclone to the elimination of coarse and fine solids from water slurries in the tipple in order to produce a water suitable for recycle purposes containing only minute particles far below the 200-mesh size.6 This would result in a closed water system for many cases, with its accompanying economic and operating advantages to locations where water quantity and quality problems are severe; better operation of washing equipment using a consistent water devoid of injurious fine particles; lowered maintenance costs due to the lesser abrasion resulting when the fine abraiding particles are removed; and the greater ease of disposing of refuse streams of reduced volume containing greater percentages of solids.

Jan 1, 1949

By W. J. PRIESTLEY

WHEN during the war the Navy Department decided to build an armor-plate and gun-forging plant of its own at South Charleston, W. Va., one of the most important units of the equipment proposed was a 14,000 gross ton forging-press to be used for forging, bending, and rectifying battleship armor-plate and making hol¬low forgings for large caliber guns. A press suitable for doing this kind of work was put into operation in the fall of 1921 and was operated successfully on armor-plate and large forgings until the closing down of the ordnance plant following the Limitation of Armament Conference held in Washington, February, 1922. PURPOSE OF THE PRESS There are three methods by which armor-plate can be made, namely, hammering, forging, and rolling the ingot. Each method produces a different result in the mechanical working of the steel. The hammer was eliminated as impractical from an operating standpoint. The first armor-plate made in this country was worked under a hammer at the Bethlehem Steel Co., between the years 1891 and 1893, but was superseded by forging when the large press was completed in 1893. Harry T. Morris of the Bethlehem Steel Co. informs me that the 1.25-ton steam hammer began operations in 1891 and was in operation for about two years. The Carnegie Steel Co. and the Midvale Steel and Ordnance Steel Co. also forged armor-plate. Certain European manufacturers rolled the plates from large slab ingots, after removing the sink-head and giving the body of the ingot a light pass under a hydraulic press. While rolling accomplished more mechanical work on the surface of an armor plate, forging, on the other hand, resulted in a greater amount of work in the interior of the plate. Either type of equipment involved an enormous expendi¬ture, so it was deemed advisable to adopt the method which would make it possible to use the equipment for more than one purpose. Since g large rolling-mill could be used only for the single operation of rolling armor-plate, a press was decided on, for the reason that it might be designed so as to forge armor, as well as bend and rectify it, and also be used in the forging of ingots for large caliber guns, both in the form of hollow forgings and also solid shafts.

Jan 1, 1926

By Henry Howe

W. E. RUDER, Schenectady, N. Y.-In 1913 I presented a paper before this society on Grain Growth, and at that time it seemed to me that the only explanation for grain growth was that of critical strain. I do not think I published the photographs at the time, but I made some experiments on the effect of stretching sheets of metal. This allowed for fairly accurate determinations of the amount of cold deformation, At the time I worked-with silicon steel because one could see the change in grain growth with the naked eye. I stretched about 10-samples from 0.5 per cent. to 10 per cent., and, after heating to 1,050° C., I found that the maximum grain growth occurred at about 2 ½ per cent. cold deformation. This I designated "the critical strain" for maximum grain growth. About a year ago I talked with Prof. Jeffries, who explained to me his ideas of grain growth. It occurred to me that it would be a very easy thing to check the strain hypothesis against the strain and temperature hypothesis, if we took a certain number of these strips, strained exactly alike and heated to different temperatures; in that case the maximum grain growth ought to appear at a different percentage of deformation for each temperature. These experiments showed that there was, as Mr. Jeffries shows in his present paper, a decrease in germinative temperature with increased cold deformation. The samples were stretched from ½ to 8 per cent. and heated for 10 hr. in hydrogen. Samples were introduced into a furnace previously heated to temperature. A maximum grain growth was obtained at 5 per cent. deformation, when heated to 750° C.; at 2 ½ per cent. when heated to 800' C.; at 1 1/4 per cent., if heated at 950°C.; and at 5/8 per cent.. when heated at 1,100° C. This shows very clearly that the germinative temperature decreases with the increase in cold deformation. The growth was very much more marked, however, at the high temperature, i.e., the grain grew more rapidly and attained a much larger size than at lower temperature. In considering the photographs (Fig. A) those along the lateral edges should be ignored because.

Jan 4, 1917

By C. WIFLARD HAYES

(New Haven Meeting, February, 1909.) I DESIRE to make it perfectly clear at the outset that I fully realize the hazardous nature of any attempt to estimate the quantity of iron-ore or any other mineral in the ground. I should not have had the temerity to venture upon an inventory of the iron-ore supplies of the United States except for the requirements of the Conservation Commission. During the preparation of this inventory I have been impressed by the wide diversity in estimates of those best qualified to. hold an opinion, and I am therefore prepared in advance for criticism of my figures. Inasmuch as this report was prepared in large part for unprofessional readers, I considered it necessary to classify and describe the commercial iron-ores in a somewhat elementary manner, in order to explain the reasons for the large element of uncertainty in the estimates. I have therefore given a chemical and a geological classification of iron-ores, which place the commercial deposits in six classes: (1) magmatic segregations in basic igneous rocks; (2) contact-deposits formed in connection with igneous intrusions; (3) concentration-deposits; (4) replacement-deposits; (5) bedded-deposits, and (6) gossan-deposits. The iron-ores are further distinguished under two classes available and not available. This classification is in large measure arbitrary, and it, is evident that it will vary front time to time. In the available class are placed those ores which can be worked at a profit under conditions essentially as they exist at present. Since it depends wholly on the question of costs, the various factors which affect cost will determine the classification of any particular deposit. Actual production, * Abstract of Report prepared for the Conservation Commission. t Chief Geologist, United States Geological Survey. .

Apr 1, 1909

By Francis P. Sinn

LOW prices have made 1938 a difficult year for the zinc industry of the world. Particularly in the United States, output had to be radically curtailed to bring production into line with consumption. Despite these unfavorable conditions, some additional plant construction is contemplated. In Jugoslavia, through co-operation with the Government, Trepca Mines is lo build a zinc plant to produce 10,000 metric tons annually, the plant to be ready for operation in July, 1941). Cerro de Pasco is proceeding with its plans for an electrolytic plant in Peru. A pilot plant, to be ready next summer, is under construction. In eastern Canada an electrolytic plant is planned in Quebec to treat concentrates from Yoranda and other mines but no defi-

Jan 1, 1939

By M. D. Everell

A study has been made of the relationships between grinding selection functions and physical properties of rocks, particularly the failure loads of irregular particles and the compressive and tensile strengths of large regular specimens. The rocks used were limestones of various structures and impurity contents, a carbonatite, and a high-purity crystallized calcite. The selection functions were obtained from carefully performed grinding experiments on selected narrow size ranges in various grinding machines-a laboratory batch ball mill, a Hard grove grindability machine, and a mill of the type suggested by Yang, Mempel, and Fuerstenau. The specific rates of breakage during milling and the failure loads of irregular specimens correlated well for the rocks studied. The testing of irregular particles is suggested as a means of predicting the behavior of commercial mills.

Jan 1, 1973

By Worthen Bradley

A BETTER understanding of what is happening in the domestic quicksilver industry, and what is likely to happen, can be had after reviewing some of the highlights of the past four years. Hitting the high spots in chronological order, they are: February 1939-Army and Navy Munitions Board starts investigation on civilian and war needs of certain "strategic materials," including quicksilver, with a view to recommending stock piles. Every known producer is canvassed by the end of the year.

Jan 1, 1942

By J. S. Johnson, W. C. McCulloch

All phases of plant operation must be synchronized so that the A number of interruptions in the flow of material may be reduced to a minimum. In the majority of plants operating under a labor agreement, time lost during the operating shift cannot be made up with overtime. With the work week restricted to 35 hr., the ratio of productive time to total time justifies extra effort in keeping the plant operating at capacity during the productive shift. This does not apply when central plants with adequate storage are operated by multiple shifts. In such installations the problems become similar to those of any factory or mill where added units, parallel circuits, or excess capacity serve to maintain the average production during intervals of maintenance shut- down. These plants, by special agreement, may run continuously, barring mechanical interruptions. The control of plant operation is in those procedures that are practiced to obtain from the run-of-mine product a high recovery of clean coal products to meet adopted trade standards and consumer specifications at the lowest possible cost. Correlation of all factors for continuous operation requires more than mechanical perfection in the plant. The run-of-mine coal must be delivered to the preparation plant without delays and the clean coal and refuse products taken away. Power supply and water requirements must be adequate. Signal systems must be established for emergency stops and to facilitate resumption of coal flow.

Jan 1, 1943

By Max Roseler

THE CHAIRMAN (WILLIAM KELLY, Vulcan, Mich.).-Some 8 or 9 years ago I was at Daiquiri, only a. few miles east of Firmeza, where there are deposits of iron ore of the same general character. There is a great conical hill, perhaps 800 or 1,000 ft. in height and the ore deposit appears to be somewhat in a canoe shape on one side of the hill. The mining has been done by quarrying the ore in benches. These are called levels and to go to the 10th level it was necessary to take mules and ride to the top of the hill, which was to me an upside down arrangement of numbering levels and a novel method of entering and viewing a mine. A little copper ore can be seen in places, and not being a geologist I thought the deposit might possibly be a gossan, but none of the geologists who have written on the subject approve of this hypothesis and the great question seems to be what part, if any, the limestones have played in the origin of ore; whether these deposits are replacements of limestone and whether they are contact ,deposits between the limestone and the other rocks. Examinations have been made by many eminent geologists and the problem has been discussed vigorously on both sides. The deposits are exceedingly interesting from a commercial standpoint and although they have been studied for a number off years the origin of the ore is still a difficult and somewhat controversial question. J. T. SINGEWALD, JR., Baltimore, Md.-I have had the privilege of visiting these deposits and have been very much interested in this paper, of Dr. Roesler's; having been on the ground, I can easily appreciate the difficulties under which he labored in attempting to work out the geology of that region, and he certainly deserves considerable credit for the way in which he has deciphered the geological relations of the Firmeza district. There are several points in his paper 1 ,would like to discuss; first, in regard to the geological interpretations. His differs from previous interpretations in the relative age of the diorite and the granite, but you will note that Prof. Lindgren suggests the probability. that those two rocks are very closely of the same age, and Prof. Kemp actually suggests, although he does not-accept the idea, that the granite is probably later than the diorite, so that there seems to be no particular reason

Jan 4, 1917

By H. J. Rahilly

MINE FIRES, in the Butte District, have been a source of trouble and expense for the past thirty years, for while the actual fire area in most of the mines has been comparatively small, the handling of the gas has generally been a much larger problem than the actual putting out of the fire. The chief causes of these fires have been: Defective electrical equipment, incendiarism or carelessness, and spontaneous combustion. While fires from the first two causes have been numerous, they have generally been discovered and extinguished before they became very serious. Spontaneous combustion has been the cause of most of the large fires. Sufficient heat has been generated by ground movement, high rock temperatures, and decomposition to set fire to inflammable materials (tarred ropes, canvas, dry timber, manure, and hay) left in the gobs some years ago. Also, the heat resulting from the oxidation of the fine broken sulfide ore is sometimes sufficient to set fire to the timbers. In 1906, a fire was discovered on the 1100-ft. level of the Minnie Healy mine about 400 ft. (122 m.) west of the Minnie Healy shaft, which presumably originated, in one of the upper levels, from spontaneous combustion. The fire was walled off by concrete bulkheads and a pillar of ground 100 ft. (30 m.) thick was left below and mining resumed underneath. During subsequent operations, this pillar became cracked and broken and the fire passed into the new workings. It travelled downward and spread rapidly until, in 1917, it had become necessary to wall off portions of the Tramway, Leonard, and West Colusa mines on the 1300, 1400, 1500, 1600, 1800, 1900, and 2000-ft. levels, and the top of the 2200-ft. raises were sealed. The fire area now consists roughly of a block 1000 by 1200 ft. and from the 600-ft. to the 2200-ft. level. This block is composed largely of a series of parallel northwest-southeast nearly vertical veins and stringers that form a large orebody, with no well-defined walls but badly fractured and faulted, and known locally as "Horsetail Ore." These veins, or orebodies, are mined by the square-set or the rill method.

Jan 2, 1922

By W. R. Ingalls

THE present administration has made sincere and effective efforts to reduce the expense of the Federal Government, but it has reached a point beyond which it seems impossible, or anyway extraordi-narily difficult, to go. This is ascribable to the large part of the budget that is represented as war expense. There is no doubt that this spells high taxation for many years to come. Nevertheless, although a large part of the taxation will be attributable to the war, the paying out of the proceeds of that taxation by the government will not be war expense, except in minor part, as will be hereinafter made clear. It will be useful to explain the economic meaning of this situation, for it has bear-ings upon several open questions, such as a bonus to the ex-soldiers, the foreign debt accounts, etc. The expense of the war on the part of the American people was in the main paid concurrently with its prose-cution. This was necessary. Warfare is not conducted with money, but with materials and labor. Except for such previous production as was represented by stocks of goods, the requirements had to be supplied by coincident production. With the end of 1918 our war expense ceased, save for such production, e.g., of ships, that was allowed to run on unchecked, and the indemnities that had to be paid for cancelled contracts. When those matters have been settled we shall be done, barring one important thing. Of course, our war expense began to contract right after the armistice and shrunk rapidly with the demobilization of the troops in 1919. If we had not been able to obtain all needful material from our own sources and had been constrained to borrow it from foreign countries, incurring a foreign debt, we should have been in the quite different posi-tion of having to repay that material, or its equivalent, during subsequent years. The European countries had to come to us for such supplies. This outlines the fundamental difference between their present situations and ours. We were therefore compelled not only to furnish materials and man-power for our own warfare but also much for the Allies.

Jan 3, 1923

By G. R. Lehman

The Inspiration Consolidated Copper Co. had an orebody at Miami, Ariz., of close to 100,000,000 tons of low-grade copper ore, and the method of mining this ore most profitably was of great importance. The selection of a method was practically limited to a "top-slicing," a "shrinkage-stope" or a "caving" method. The "top-slicing" method would give a high extraction of the developed ore, at a high mining cost, and the "shrinkage-stope" or "caving" methods a lower extraction of the developed ore, at a lower mining cost. Ore-Drawing Tests To decide on the method to be used it was necessary to know about what extraction of the ore could be obtained by the "shrinkage-stope" or " caving " methods. As no definite information regarding the,question was available at the time, C. E. Mills, the general manager, thought that some information could be obtained by experimenting in drawing ore, covered with capping, from an experimental box. Some work had already been done along these lines by W. C. Browning for the Inspiration Copper Co. and by myself for the Live Oak Development Co. The idea was to represent as nearly as possible, in the experimental box, the conditions within an area of caved stopes of caved ore all ready for drawing. That is, the area was supposed to represent a semibroken mass with the capping above it in the same condition and ready to follow the ore downward as it was drawn out of the chutes under the ore. To represent the above condition, in the experimental box, crushed ore from the mine was placed in it to a given height, and red barren capping from the mine was placed on top of the ore. The Experimental Box The experimental box shown in Fig. 1 was made of wood and glass. The glass was used for the sides so that the drawing action of the outside row of chutes could be seen and noted, the latter being cut in the center by the glass sides. The length of the box was 30 in., width 20 in. and the

Jan 1, 1917

By W. W. Stephens, W. J. Kroll, H. P. Holmes

THE only two methods for producing commercial quantities of malleable zirconium, up to now, have been using magnesium reduction of the anhydrous chloride under a neutral gas, and using purification of raw zirconium by the iodide dissociation method on a hot filament. The purity of the metal obtained by the latter process is about the same as that resulting from the chloride reduction, with the exception of the oxygen content, which may be about 0.05 pct lower in the iodide metal. Even traces of oxygen have a strong hardening effect on zirconium. Since, in the iodide process, the impurities, Si, Al, Fe, Ni, and Mg in the raw zirconium used, are carried over, it would appear uneconomical to use this method of refining solely to eliminate the traces of oxygen, unless very soft metal is desired. One important step to improve the iodide method, namely, dissociating pure iodide made from carbide and recycling the iodine, which would change this refining process into a method for extracting zirconium from the ore, has not yet been made. The Bureau of Mines, by using the chloride reduction, wanted to produce quantities of a reasonably pure and malleable metal at low cost for large-scale industrial use. This aim has been achieved, and a pilot plant permitting production of 600 lb of malleable zirconium per week will be described (fig. 1). Briefly, the Bureau of Mines process consists of reducing purified gaseous anhydrous zirconium chloride with fused magnesium under a noble-gas atmosphere. The reaction product, magnesium chloride, and any excess magnesium metal present are removed from the sponge zirconium in the next step by fusion and evaporation in a good vacuum at about 925°C. In this process, care is taken to keep air out of contact with the hot metal, which otherwise would contaminate the product with oxygen and nitrogen. Both these impurities embrittle zirconium even when present in an amount as low as 0.1 pct. A number of previous reports1-3 describe the method and the various improvements that finally led to a workable process. The major steps made were the production of large quantities of carbide, which is the raw material for producing the chloride, its chlorination with reasonable efficiencies, and the elimination of iron trichloride contained in the raw chloride, as well as that of the zirconium oxide which is always present in this product. The physical nature of the anhydrous chloride, which sublimes at 331°C at atmospheric pressure and melts at 420°C under a pressure of 25 atm, made it necessary to provide a special safety device on the purification and reduction vessels in the form of a lead-alloy seal, permitting escape of excess gases if pressure tended to build up. The main difficulties encountered in the reduction and in the following step, salt separation in a vacuum at elevated temperature, were caused by the material from which the reaction pot was constructed—iron. This metal reacts with zirconium at about 940°C with formation of a eutectic. The last step, salt separation by evaporation of the magnesium and magnesium chloride in a vacuum, is quite unconventional and has not been used before on such a scale. It is only due to the improved construction of high-vacuum pumps, especially oil-diffusion pumps, that such a method could be used. The various steps of the Bureau of Mines process, as described in the general outline above, may be summarized as follows: (1) production of the carbide, (2) chlorination of the carbide, (3) purification of the raw chloride, (4) reduction of the pure chloride with fused magnesium, (5) separation of excess magnesium and magnesium chloride in vacuum at elevated temperature, and (6) melting of the sponge obtained. Production of Carbide The arc furnace, described in a previous report,' was improved both to reduce the graphite consumption caused by the burning of the bottom plates and to concentrate the heat in order to obtain better power efficiency. This was achieved by providing the bottom with graphite plates entirely embedded in refractory bricks, the contact with the current being made with three water-cooled copper plugs. Figs. 2 and 3 show the arrangement. The crucible, made

Jan 1, 1951

MRS. SIDNEY J. JENNINGS, President, MRS. ARTHUR S.. DWIGHT, First Vice-President, MRS. KARL EILERS, Second Vice-President, MRS. H. W. HARDINGE, Third Vice-President, MRS. BRADLEY STOUGHTON, Recording Secretary, MRS. AXEL 0. IHLSENG, Corresponding Secretary, MRS. ARTHUR S. DWIGHT, Acting Treasurer. Welfare Committee MRS. C. C. BURGER, Chairman, Sub-Committees Americanization Belgian Relief MRS. LEVI HOLBROOK, Chairman, MRS. HENRY H: KNOX, Chairman, Emergency MRS. HERMAN A. PROSSER, Chairman. Since the annual meeting held in February, 1917, when the Woman's Auxiliary to the A. I. M. E., was formed, the work of organization, which of necessity must be slow, has steadily gone forward. Under the Chairmanship of Mrs. C. C. Burger of the Welfare Committee, three active sub-committees have been formed: that of Americanization; under Mrs. Levi Holbrook, who is eminently fitted for such a position, by her active and valuable work in a number of the fine patriotic societies of our country; the Belgian Relief Committee, under Mrs. Henry H. Knox, which has clone phenomenal work in the three months of its existence, and whose report is later given in detail; and the Emergency Committee under Mrs. Herman A. Prosser, which has a fund already established, and is. in close touch with Major Arthur S. Dwight, ready to act when necessity arises. The officers of the Auxiliary feel more than gratified at the response so far received, and in a later issue will print extracts from letters, if permission can be gotten from the writers, showing the interest and enthusiasm that have beer aroused by the formation of a Woman's Auxiliary. Answers have even come from far Korea "the hermit nation," from Australia, from South America, showing what a bond of sympathy and, helpfulness is in process of growth. It is our sad duty to announce the death of our Treasurer, Mrs. George D. Baryon, who, from the very inception of our plan to organize, was an inspiring and valuable co-worker. Her place will be difficult to fill. Mrs. Arthur S. Dwight is Acting Treasurer at present. The Auxiliary wishes to express its heartiest thanks to Mr. Stoughton, the genial and efficient Secretary of the A. I. M. E., for his cooperation and valuable suggestions in the difficult work of organizing. He has indeed been "a guide, philosopher and friend." SUSANNE M. IHLSENG (MRS. AXEL 0.), Corresponding Secretary.

Jan 7, 1917

By R. S. Dean

The commercial production of electrolytic manganese on a small scale commenced in 1939. The writer made a short report on the progress of production and utilization in Mining and Metallurgy for January 1941. Progress during the last two years, naturally, has been more rapid. In June 1940, Congressman (now Senator) Scrugham presented a proposal to Congress for an appropriation authorizing erection of a pilot plant for " the production of metallic manganese by electrolytic or other means." As a result of this, a pilot plant, having a capacity of a few hundred pounds per day was built at Boulder City, Nev. Subsequent appropriations permitted expansion of the plant to about a ton per day. Much has been learned in this plant about electrolytic manganese, and the product even in its small way has found war uses of considerable importance. Meanwhile, the Knoxville plant of the Electro Manganese Corporation, the sole commercial producer, was expanded to about 4 tons per day to supply needed material for the war program. Other proposals for commercial plants have not been favorably received by the War Production Board. The Bureau reported on one such proposal by the American Alloys and Chemical Corporation. Practice at BouldeR City The present practice, as carried out at Boulder City, which is being described in more detail in a current paper by the Bureau staff at Boulder City, starts with a manganese dioxide ore containing about 20 per cent manganese. Currently this ore comes from the Three Kids deposit near Las Vegas. The steps for the production of electrolytic manganese, in general, are as follows: 1. The manganese in the ore is reduced to MnO. 2. The MnO is dissolved from the ore in spent electrolyte, which contains about 38 to 47 grams per liter of free sulphuric acid, 135 grams per liter of ammonium sulphate, and 10 to 12 grams per liter of Mn as sulphate. In the leaching step the manganese is built back up to 32 to 36 grams per liter of Mn as sulphate; the pH is adjusted to neutral by means of gaseous ammonia and passed through thickeners. 3. The electrolyte is purified by adding H2S, which precipitates the heavy metals. After filtering, ferrous sulphate is added to the solution and oxidized with air and the solution is filtered and clarified on a precoat filter. 4. The purified catholyte is electrolyzed in a diaphragm cell using stainless-steel cathodes and lead-silver anodes. The current density is about 45 amp. per sq. ft. Current efficiencies of 60 to 65 per cent are regularly obtained.

Jan 1, 1944