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By R. F. Domagala, M. Hansen, D. J. McPherson

On the basis of metallographic analysis, incipient melting data, thermal analysis work, and X-ray diffraction, phase relationships in the 0 to 50 atomic pct alloy content were carefully resolved. Phase relationships in the higher alloy content regions were outlined. A single intermediate phase, peritectically formed, of the form ZrX2 was established in each system. A eutectic and a eutectoid were found in the zirconium-rich region of both systems. Appreciable solubility of molybdenum and wolfram was found in ß zirconium, but only a slight solubility in a zirconium. PREVIOUS work on these systems was limited to X-ray investigations of the intermediate phases1, 2 and preliminary surveys of the zirconium-rich alloys." The diagrams presented were determined principally by metallographic, thermal analysis, and incipient melting techniques. In accordance with the Atomic Energy Commission contract requirements, phase relationships up to 50 atomic pct molybdenum or wolfram were carefully resolved, while only a limited amount of work was done to outline the 50 to 100 atomic pct alloy region. A description and analysis of the metals used in the preparation of alloys for this study are included in Table I. A "low-hafnium" zirconium crystal bar, produced by the decomposition of a volatile iodide onto a hot filament, was employed for these studies. Westinghouse "Grade 3" crystal bar was used for all alloys. The zirconium, as received, was coated with corrosion product from a standard autoclave test by which its grade designation is determined. This was removed by a sand-blasting and HF-HNO, pickling technique developed by the Atomic Energy Commission. The bars were cold rolled to approximately 1/32 in. sheet, pickled for iron removal, sheared to 1/4 in. squares, washed with acetone, and stored for furnace charge. Molybdenum sheet. 0.003 in. thick, 0.001 to 0.005 in. wolfram wire, and M in. wolfram rod crushed to granular form, from Fansteel Metallurgical Corp., were used as alloying stock. Melting Procedure A nonconsumable electrode arc furnace identical to that described in detail by Hansen et al.4 was used. The source of power for melting Zr-Mo alloys was a 400 amp dc welding generator, while a 900 amp dc generator was used for preparing Zr-W alloys. Electrode tips of the same material as the alloy addition were employed in both systems, i.e., molybdenum tips were used for Zr-Mo alloys, and wolfram tips for Zr-W alloys. This precluded any possible electrode contamination during arc melting. Ingots of 20 to 30 g of Zr-Mo alloys were melted under high purity helium in the cavity of a copper block insert in a spun copper crucible. Homogeneity was insured by remelting all ingots four to six times without opening the furnace. Due to the large difference between the melting points of wolfram and zirconium, direct melting of the charged metals as above generally yielded ingots containing unmelted wolfram particles. This was overcome, after many variations in technique, by melting a pure wolfram charge at high power levels (700 to 900 amp) and slowly adding zirconium to form a master alloy. Such master alloys were sectioned and remelted several times, then crushed to serve as melting stock for alloys of lower wolfram content. Master alloys containing 26, 50, 52, 70, and

Jan 1, 1954

By H. Cecil Spicer

THE results described in this article are based on field work conducted during the periods April-May, 1939, and May-July, 1940. The United States Potash Co. is mining potash on Government land under a permit from the Department of the Interior and the geophysical investigation was completed under a cooperative arrangement made between that company and the Conservation Branch of the Geological Survey. The writer, a member of the Section of Chemistry and Physics of the Geologic Branch, was assigned to this investigation. Four definite objectives were in mind for the geophysical work in the studies over the salt deposits. The first was to determine the measure of success that could be attained in this type of work with the resistivity methods that were to be employed. These methods had been introduced into the work of the Conservation Branch by Benjamin E. Jones for the investigation of dam sites, and have been used under his direction by the author for such work. If the method proved to be applicable, an effort was to be made to contour the top of the salt beds and also the other formation boundaries known to be present in this area. Salt-water aquifers were to be studied in an effort to determine their boundaries, and an attempt was to be made to delineate the potash-bearing beds. EARLIER STUDIES Others have made, and reported, resistivity studies over saliferous deposits in different areas. Friede1 and Messrs. Schlumberger2 reported geophysical work performed in the discovery of the salt domes of Alsace; Carrette and Kelly3 described the geology of the same area. Leonardon and Kelly4 published a resistivity curve obtained over the Hettenschlag dome, and a further discussion of this same area was given by the Messrs. Schlumberger5 in a communication. Messrs. Alty6 described studies on salt deposits in which the single-probe method was used. Sinerez7 mentions that electrical methods were tried over salt deposits in Spain. Geoffrey and Charrin8 show a resistivity curve obtained over marl, gypsiferous marl and salt which is similar to that obtained over the New Mexico salt deposits. Kelly9 reported resistivity work performed with the ground comparator of Zuschlag over the salt deposits near Syracuse, N. Y., where the Salina formation is at a depth of 700 to B00 ft. Some structural studies on the potash basin of Alsace are described by Poldini.10 Another single-probe resistivity study, made over salt deposits in New Mexico, is briefly described by Heiland,11 through the courtesy of Harry Aurand, of the Midwest Refining Co.

Jan 1, 1941

By AIME AIME

A SIDE from the technical sessions held as noted elsewhere, the chairman of the various sub-committees of the Mining Methods Committee, together with a few other specialists, were invited to a conference with President Bradley, which was held on Wednesday afternoon, Feb. 20. The general plan of a comprehensive series of comparable papers descriptive of mining practice in various parts of the country, launched by this committee some seven years ago having been adopted by the U. S. Bureau of Mines, the feeling was general that the Committee could safely 1eave.that part of its work in these capable hands and turn its attention to other matters. The plans of the Bureau were presented as below by Charles William Wright of the Bureau.

Jan 1, 1929

We note with sincere regret the death of H. T. Chen,, who was killed by forest fire in the mountainous re-ion of Kokiu-Chang where he had been operating as Engineer in Chief of the Yunnan Tin Trading Co. Mr. Chen graduated in 1911 from the Department, of Mines, .University of California, being the first Chinese Government scholar in mining to attend that institution; and one of the first in America. He came of a distinguished family, many members of Which are in official life in Peking and in his native province of Hunan, all of whom are noted for their classical scholarship. He was himself a Hsiao-tsai or Bachelor of Arts, a coveted degree of the old literati class, Which he won under the Manchu regime when he was still a stripling. His mining work in Yunnan was carried on with only the most primitive facilities and in a distant province, but was, nevertheless, attended with great success and profit for his company. The region is infested with brigands and rebellious troops. who frequently turn marauders and prey upon the countryside, and Mr. Chen has had to go to the mines always with a large armed guard sometimes aggregating 150 men and some hundreds of miners, also armed. Two armed squads of men keep in touch with his base 'at Kokiu-Chang every day to get supplies and food, and it is feared that the brigands who have thus been prevented from plundering and mobbing his parties have started 'he fires to burn him out, with the disastrous result reported. Mr. Chen has thus given his life to his country in the attempt to win for modern China and Chinese civilization the raw materials of her new industrial life. He did so cheerfully and with full appreciation of the dangers that beset him, and China regards this as one of the most noble sacrifices of her young sons on the altar of patriotism. He is survived by a daughter of two years and by his widow who was also a graduate of the University of California and will be remembered by her classmates as Lucy Kong, 1912.

Jan 7, 1917

By Guy Bjorge

IN recent years the Homestake mine has been served by three shafts, the B. &. M., the B. & M. No; 2 and the Ellison, supplemented by an inside shaft, the Milliken, extending from the 2000-ft. level to the 3200-ft. level. In 1932, when a new operating shaft was under consideration, the bottom of the mine was at the 3200-ft. level. The B: & M. and the B. & M. No. 2 shafts were down to the 1550-ft. level and the Ellison was being deepened from the 2600 to the 3200-ft. level. All ore was hoisted at the B. & M. and-Ellison shafts. Levels below the 2600 level, which were under development only, were served by the Milliken shaft. Below the 1550-ft. level, the mine was served only by the Ellison shaft from the surface. Within a few years, when ore reserves above the 1550-ft. level would be depleted, operation would be limited to the Ellison shaft and the auxiliary underground shaft. The Ellison shaft alone was not adequate for hoisting the entire output from the deeper levels and also handling all men and supplies. Further-more, assurance of safety and uninterrupted operation required- two fully equipped shafts to the deeper levels. Therefore a new operating shaft was authorized in November, 1932, and was named for A. J. M. Ross, the mine superintendent.

Jan 1, 1935

John R. Lucas was born Apr. 15, 1866, at St. Louis, Mo. From his 19th year until his death on his 51st birthday anniversary, he was engaged in the mining industry, in which, however, he made his beginning and achieved his progress after a somewhat unusual fashion. Presumably without previous training as a mining engineer, he became in April, 1885, and remained until the end of 1892, bookkeeper of the Granite Metal Mining Co. at its St. Louis office. Then for a year he served as bookkeeper of the same company at its mine in Montana. This official of a mining company is at the very heart of its operations; and if he possesses ambition and intelligence, may learn the business thoroughly. It is not surprising, therefore, that Mr. Lucas, being that kind of man, assumed, in 1894, a position with the Hope Mining Co., another St. Louis corporation operating in Montana, which he retained for eight years, serving not only in the office, but becoming also successively mill foreman and assayer. This varied practical experience prepared him for important administrative functions. From April, 1902, he was for many years the business agent of the Goodhope Mining Co. In 1903, he became also the assistant superintendent of the Granite Bi-metallic Consolidated Mining Co., and subsequently its superintendent-a position which he retained until his health failed at the end of 1916. In addition to the other Granite Bi-metallic properties, he had charge of the sapphire mines in the west fork of Rock Creek, Mont., the Basin Gulch placer mines, the claims of the former Hope Co., etc., all of which he managed with skill, integrity and recognized business ability.

Jan 6, 1918

By Philip D. Wilson

OF all the metals in the war program the demand for and the production of magnesium have increased percentagewise the most. In the prewar year 1939 the production was 3350 tons. The war program, twice expanded, now provides for nearly one hundred times that amount annually. The goal announced by the War Production Board in February 1942 was 362,500 tons per year. Be- cause of the development during the year of satisfactory types of incendiary bombs other than magnesium this objective has been somewhat reduced but the capacity of the plants already built or under construction will be huge. The Aluminum and Magnesium Division of the W.P.B. has had the responsibility of planning and implementing this expansion and of providing fabricating facilities as well for this greatly increased tonnage of magnesium ingot.

Jan 1, 1943

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

By Herbert Kilburn Scott

The information in this paper was collected by the author during a five years' residence in the State of Minas Geraes. Outside the State itself, very little is known of the gold-field. Such accounts as have been published are antiquated and contained in publications mostly out of print. The increased attention now attracted to the natural resources of Brazil, and the probability that American capital will be, in the near future, largely invested there, will make an up-to-date account specially useful at this time. I. Historical and General. Soon after the Jesuits founded what is to-day the city of S?o Paulo, gold was discovered in the streams of the neighborhood; and this incited the natives, known as paulistas, to look for it farther afield. After many expeditions into the interior, gold was found in quantity in placer-deposits in the vicinity of Ouro Preto, in 1699, by a prospecting party headed by Antonio Dias. The name of Ouro Preto (black gold) was given because of the superficial dark coating of the gold, and the inhabitants of the district were known as mineiros (miners). Later on, the placers of Cuiaba, in the State of Matto Grosso, were discovered in 1718, and those of the State of Goyaz in 1724. All this territory was at the time a private colony, but on account of its increasing importance it was taken over by the Crown, and in 1739 a royal governor was appointed, with his nominal capital in S?o Paulo, though for a number of years the real capital was Ouro Preto. In 1711 Ouro Preto was raised to the rank of a city, with the name of Villa Rica de Ouro Preto (" rich city of black gold"); and in 1720, by reason of administrative difficulties, Minas Geraes was constituted a separate colony from S?o Paulo, with Villa Rica as its capital. The site of this city

Jan 1, 1903

By J. J. Frawley, W. J. Childs

Experiments were carried out to induce grain refinement during solidification by applying vibrational energy (freq 20 kc) to small specimens of bismuth, tin, and bismuth-tin alloys. The results show that if the intensity of the applied sound -field is not great enough to fragment the growing dendrites of a pure metal, no grain refinement is observed and the pain size of the dynamically nucleated specimens is the same as the grain size of a specimen statically supercooled the same amount. Bismuth specimens did not show any grain refinement; whereas, the tin specimens did show grain refinement. This phenomenon is the result of the difference in growth habit between the bismuth and tin dendrites. The bismuth-tin alloys showed grain refinement and, in addition, the segregation pattern was changed. THE solidification process is a change in phase requiring the nucleation of the solid phase from the liquid and the growth of this solid phase at the expense of the liquid phase. Since many physical properties and also the integrity of a casting are dependent on the solidification process, understanding and controlling this process are very important.' A good example in the controlling of a cast structure using heterogeneous nucleation theory is the reduction of grain size in aluminum castings by nucleation catalysis.2 This mechanism of nucleation catalysis has been explained by Turnbull.3 Another technique for grain refinement, which has received much attention but the mechanism has not been fully understood, is to vibrate the solidifying melt. Vibrations can be applied to the melt either by vibrating the mold directly or by introducing a vibrating rod into the melt.4-13 Three mechanisms have been proposed to explain this phenomenon: 1) The mechanical fragmentation of the original dendrites that grew into the melt. These crystals or fragmented dendrites act as new growth sites. 2) The nucleation of new grains in the liquid by the generation of very high pressure pulses caused by cavitation in the liquid. 3) The remelting of the dendrite arms during the solidification process. This mechanism is operative only in alloy systems and would be enhanced by stirring or mechanical vibration. The purpose of this investigation was to determine the mechanism that will increase the number of grains when mechanical energy is introduced into a solidifying melt. APPARATUS The unit used to generate the ultrasonic vibrations was manufactured by the Redford Co., and is similar to the one used in ultrasonic soldering. Fig. 1 is a sketch of the major components used for generating ultrasonic vibrations. The crystal transducer assembly consisted of four lead zirconate ti-tanate piezoelectric crystals in an aluminum holder. An acoustical horn, which was fabricated from stainless steel, was attached to the holder by a set screw. The resonant frequency of this unit was 20,000 cycles per sec. A Pyrex crucible, 4 in. in diam and 4 in. high, was contained in a hole in the top of the horn. The piezoelectric crystals changed volume when excited by an electric signal, thereby generating a sound signal which passed through the horn. The crucible was coupled to the horn by a liquid silicone oil. The purpose of the couplant was to transmit the soundwaves from the horn to the crucible. Without the couplant, much of the sound energy would be lost. The energy transmitted was sufficient at the resonant frequency used, so that acoustical cavitation always occurred in the molten metal. The presence of acoustical cavitation was detected by the characteristic hissing sound emitted from the liquid. EXPERIMENTAL PROCEDURE The influence of ultrasonic vibration on the grain refinement of bismuth, tin, and bismuth-tin alloys was studied. These metals were chosen because of their low melting temperature and the relative ease with which they can be thermally supercooled. The following procedure was used for obtaining large amounts of supercooling. Pure bismuth (99.999+), which was received in bar form, was mechanically broken into pieces small enough to be accommodated in a 50 ml beaker. About 200 to 300 g of bismuth and a few grams of SnCl2 as a flux were placed in the 50 ml beaker and melted by induction heating. The melt was held for 20 min at

Jan 1, 1970

By Hugh Rose

The properties of the company lie within the Pachuca district, State of Hidalgo, Mexico, connected by three railway lines with Mexico City, 55 miles southwest, and by two lines with Vera Cruz, 250 miles southeast. The ores were formerly divided by sorting into two classes, smelting and milling, the former averaging about 2 oz. gold and 335 oz. silver, the latter 0.12 oz. gold and 23 oz. silver. The smelting ores were sold to custom plants, principally the American Smelting & Refining Co. at Aguascalientes. The milling ores were treated by the patio process at the Guadalupe Hacienda, at Pachuca. This patio was probably the largest in existence at the time and continued in active operation up to March, 1910. In January, 1910, the mines and patio were sold to English interests, represented by Camp Bird Limited. Two new companies were formed, the Compania de Santa Gertrudis, S. A., to operate the mines, and the Compania Beneficiadora de Pachuca, S. A., to build and operate a custom cyanide milling plant. (Pig. 1.) Geology The historical geology of the Pachuca district is described by Fred J. Pope as follows: 1. The most recent sedimentary rooks in the district belong to the Cretaceous period. 2. The Cretaceous rocks were penetrated by large intrusions of ande-site (referred to hereafter as primary andesite) which occur as elliptical dome-shaped masses, striking northwest-southeast. These andesite bodies are from 8 to 15 miles long and from 6 to 10 miles wide. 3. A period of erosion during which the contour of the andesite domes was changed. 4. Andesite flows (secondary andesite) which rest unconformably on the primary andesites.

Jan 1, 1917

By F. O. Garrabrant

POWER is furnished to the Climax Molybdenum Co. by the Public Service Co. of Colorado over two 100,000-volt line to a bank of three 3333-kva. Transformers 100/13.8 kv. These transformers arc so designed that with the addition of forced cooling their capacity may be increased 33 1/3 per cent at 12,000-ft. altitude. Under present conditions, these transformers are operated at 140 per cent of their rating with forced air cooling. On the secondary side of this bank there is a 15-kv., 1200- amp. Westinghouse oil circuit breaker provided with automatic reclosing relays allowing three successive short circuits before lockout. From this breaker 13.8-kv. power is transmitted to a central switching station (Fig. I) where all circuits radiate to the different operations of the property. Each circuit is protected by a 23-kv., 600-amp. oil circuit breaker with by-pass and isolating disconnecting switches. MINE Power at 13.8 kv. enters the mine through a ventilation raise over a three-conductor, size 1-0 varnished cambric insulated, leaded, steel-wire armored cable, insulated from 17 kv. This power is received and distributed through one switching station and four underground substations, shown in Fig. 2. No. 370 substation (Fig. 3) contains three 250-kva, 13,800/440-volt, single-phase Pyranol transformers protected on the high-voltage side by a 600-amp. manually operated oil circuit breaker. This station serves 20 slusher-hoist motors, a 45-kw., three-phase, 220-volt electric furnace, a Massco hot miller for tempering and milling Timken detachable bits and a hoist with 175-hp. motor on the No. 3 development shaft. Also at this shaft are three pumps. One two-stage pump, 1200 gal, per min., 100-ft. head, 3600 r.p.m., driven by a 150-hp. motor, is at the bottom of the shaft. Two deep-well pumps, 500 gal. per min., 500-ft. head, are at the collar of the shaft. Under normal operation the one pumping 1200 gal. per min. is controlled by a float switch to take care of the water. If this pump fails, or if its capacity is insufficient, the first 500-gal. pump is automatically started, and if still more capacity is needed the second 500-gal. pump automatically starts. Time delay relays are provided on the deep-well pumps, so that if power fails the column will have time to drain before the pumps restart. On failure of any of these, an alarm is sounded in the train dispatcher's office, so that mechanics can be sent to ascertain the cause of failure and make repairs. The cable from No. 370 substation is run to the switching station, in which are four15-kv., 600-amp. direct-current solenoid-operated oil circuit breakers. The current for operating and tripping is furnished by a 125-volt storage battery. All breakers are operated from the switchboard in the compressor room. One circuit from this switching station goes to the

Jan 1, 1944

By Hugh Rose

THE properties of the company lie within the Pachuca district, State of Hidalgo, Mexico, connected by three railway lines with Mexico City, 55 miles southwest, and by two lines with Vera Cruz, 250 miles southeast. The ores were formerly divided by sorting into two classes, smelting and milling, the former averaging about 2 oz. gold and 335 oz. silver, the latter 0.12 oz. gold and 23 oz. silver. The smelting ores were sold to custom plants, principally the American Smelting & Refining. Co. at Aguascalientes. The milling ores were treated by the patio process at the Guadalupe Hacienda, at Pachuca. This patio was probably the largest in existence at the time and continued in active operation up to March, 1910. In January, 1910, the mines and patio were sold to English interests, represented by Camp Bird Limited. Two new companies were formed, the Compañia de Santa Gertrudis, S. A., to operate the mines, and the Compañia Beneficiadora de Pachuca, S. A., to build and operate a custom cyanide milling plant. (Fig. 1.) GEOLOGY The historical geology of the Pachuca district is described by Fred J. Pope as follows: 1. The most recent sedimentary rocks in the district belong to the Cretaceous period. 2. The Cretaceous rocks were penetrated by large intrusions of ande-site (referred to hereafter as primary andesite) which occur as elliptical dome-shaped masses, striking northwest-southeast. These andesite bodies are from 8 to 15 miles long and from 6 to 10 miles wide. 3. A period of erosion during which the contour of the andesite domes was changed. 4. Andesite flows (secondary andesite) which rest unconformably on the primary andesites.

Jan 8, 1916

By Anthony J. Chasteen

Although geothermal energy has been used by mankind for thousands of years and has even been used to generate electricity since the turn of the century, it is only in the last few years that the threatened energy crisis has focused attention on this resource. Geothermal exploration and development is being carried out in at least thirty-five countries on five continents. The status of geothermal energy production, however, is rudimentary with about 800 MW installed generating capacity worldwide, equal to about 0.1% of the world's total energy production.' The world's first (1904) commercial generating site at Lardarello, Italy, will soon be surpassed by developments at The Geysers, Calif. There are other successfully operating geothermal power projects in New Zealand, Japan, USSR, Mexico and Iceland with pilot plants planned or under construction in Chile, El Salvador, Nicaragua, Turkey and the Philippines. The preponderance of exploration and development is being sponsored or assisted by individual governments, by the UN or by the U.S. Agency for International Development

Jan 10, 1972

By H. Sigurdson, C. H. Moore

Extensive studies have been carried out on electric furnace and blast furnace slags obtained in the winning of iron from its ores. These slags normally consist of elements of the gangue minerals present in the ores, as well as the added flux materials. In consequence, melts of CaO, MgO, Al2O3 and SiO2 can be considered as representing typical slag compositions. When a slag of this composition cools, it usually crystallizes according to predictions possible from an equilibrium diagram of these constituents, providing the melt is not undercooled to form glass. The melt is either viscous or fluid, depending upon the ratio of binary cations to silica, and crystallizes easily or forms a glass for the same reasons. If the melt is not overheated so that carbides of the metal components of the slag are formed and if the composition of the slag is so adjusted that it has a high fluidity, liquid equilibrium is attained and the slag can be held in a liquid state for extended periods of time. Upon tapping, the slag crystallizes into minerals, the type and proportion of which are determined by the melt composition. Since equilibrium is attained, the holding period is not critical. In melts containing a large increment of titanium, however, the normal slag procedures are not applicable. Titanium, as one of the atomic transition elements, is, at elevated temperatures, capable of being reduced to form metalloid compounds much more readily than the refractory oxides present in normal slags. In consequence, an oxide melt containing titanium never reaches equilibrium in a reducing environment, but continues to shift its composition until cooled. If melts of this nature are cooled and samples submitted to metal-lographic and X ray analysis the course of reaction and crystallization in this type of slag can be determined. Preparation of Slag The slags investigated fell into the system CaO-MgO-TiO2-Al2O3-SiO2 and were produced from ilmenite ores reduced by carbon in an electric furnace. Since the equilibrium series1 and the laboratory smelting of ilmenite2 are described in two of the accompanying papers, detailed description of the smelting procedure is not required here. However, certain essentials must be mentioned. Two types of melts were used to produce slags studied in this investigation. The first series of smelts made to determine proper flux addition were produced in a 4 lb Ajax induction furnace. The charge, consisting of ore with the proper flux addition, was heated in a graphite crucible until fluid, held fluid for a sufficient time period to obtain 1-5 pct FeO content, and poured. Because of the small size of the charge only the final sample of these melts could be examined. In the melts made in the 50 lb arc furnace, however, grab samples taken at 10 min. intervals between time of initial melting and final pouring were available for examination. These samples allowed a much clearer picture of the course of reaction and crystallization. amounts of ferrous oxide and reduced titanium compounds is opaque to transmitted light. Therefore, all petro-graphic studies had to be made on polished slag sections. A representative sample of slag was cut or broken, mounted in a thermosetting plastic, ground flat using 400 grit silicon carbide, the coarse scratches removed with 600 grit silicon carbide and polished on billiard cloth using levigated alumina. Rouge was avoided because of the entrainment of the red particles in pores in the slag, causing a possible confusion with some of the mineral phases. In order to prevent sample projection above the plastic surface red bakelite was used to hold the sample, and backed up with clear lucite. In this manner sample labels could be permanently retained in the mounting. The polished samples were examined on a Bausch and Lomb metallograph at magnifications of 250 X, 500 X, 1000 X and 1800 X. The instrument was equipped for examination of specimens under bright field illumination and with crossed nicols. A magenta tint plate to aid in color tone differentiation was also used. Petrology of Slags In order to determine the composition and mineral relatinos of a previously unreported system petrologically, it is essential that the starting composition, reaction temperature and final composition be known. The chemical composition of the ilmenite ore used in these smelts is given in Table 1, and the complete analysis of a typical high titanium, low iron slag is given in Table 2. In the winning of TiO2 from ilmenite by a smelting process it is necessary to produce a slag which will melt at an economically feasible temperature, remain molten as the iron is removed by reduction, be fluid enough to be readily removed from the furnace, contain a high percentage of TiO2 and a low percentage of reduced titanium com-

Jan 1, 1950

By Luis Toron, Salvador Cortes-Obregon

John D. Price (Colorado Fuel and Iron Corp., Pueblo, Colo)—The paper on the coal fields of the Oaxaca district as prepared by engineers Toron and Cortes-Obregon of the staff of the Bank of Mexico bears witness to the thorough and careful way in which the men associated with this organization perform their work. There is little to be added to their paper in way of discussion other than to confirm and amplify some of their statements. Since the only extensive and well-developed field of coking coal lies in the northeastern section of the country adjacent to Sabinas in the state of Coahuila, it follows that blast furnace plants would be located in that same region. Two such plants are now operating at Monterrey and Monclova, using coke produced at the Sabinas district mines. But the nearer of these two plants is 600 miles from Mexico City and even farther from the center of population. Transportation of products from these mills to the market area is therefore expensive, both because of the distance and the difficulty of the terrain over which it must be carried. The development of an integrated steel industry closer to the center of population has therefore long been a goal toward which the Mexican technicians have been striving. While the presence of coal of some grade has been reported in many of the states, and many ideas have been advanced regarding its possible uses in iron and steel production, deposits of anthracite in Sonora and the various coals of the Oaxaca district as reported on in this paper are the only ones that have been explored in a serious manner. The coking coal from the Mix-tepec zone appears to offer promise of producing a coke which could be used in a standard blast furnace. Several problems are indicated, however: 1—The ash in the coal is high as mined, but indications are that it can be washed to an ash content of 15 pct with a recovery of 70 pct of washed coal. 2—Such washing would increase the volatile content from 17.4 pct to about 20 pct, and in a byproduct oven this should give a coke yield of close to 80 pct with an ash content of coke under 20 pct. 3—A free swelling index of 5 appears low for a good coking coal, and below that of the coals from the Sabinas district, which show between 6 and 9. But washing of the coal should result in an improvement in this regard; in the United States coals from Utah with an index even lower than 5 have made a usable coke. 4—A coal with volatile as low as 17.4 in raw coal and 20 in washed coal would come close to being classed as a low-volatile rather than medium-volatile coal, and low-volatile coals are notorious for their high expansion properties. Several plants in the United States are making coke from straight medium-volatile coal of 26 to 28 volatile content, and one at Rosita,, Mexico, from coal of 25 volatile. But no plants to my knowledge are using coal as low as 20 volatile. Since the Rosita coal appears to be a borderline coal from the angle of its expansion properties the coking of one of the straight lower volatile must be approached with caution. 5—There are few coals possessing any degree of coking properties which cannot be used in coke production by careful attention to its preparation and blending. The fact that coals of other types are available in this same region make improvement through blending very possible. 6—There are other workable methods of reducing iron ore other than the conventional coke-blast-furnace method. These will not be discussed here but it is known that their use has been considered. The technicians of not only Mexico but also of the other Latin American countries are keenly aware of their natural resources and their national needs. This paper emphasizes the fact that the Mexican technicians are working on their problem and attempting to speed the day of self-sufficiency for their country. Salvatore Cortes-Obregon (author's reply)—I wish to thank Mr. Price for his kind remarks. The Mixtepec coal as shown in Table II has 30 pct ash and a free swelling index of 5, but when the same coal is washed to 15 pct ash it has a free swelling index of 8 to 9 and the volatiles increased from 17.4 to 20.7 pct. A satisfactory coke has been produced from blends made in the Mexican laboratory using at least 40 pct of the Mixtepec coking coals with the other Oaxaca non-coking coals. Koppers in Germany report good coke obtained from the Oaxaca coal with a blend of 80 pct Mixtepec coal. Consideration is being given the possibility of using methods other than the conventional blast furnace for the reduction of iron ore near the Oaxaca area; electric furnaces appear promising. The non-coking coals could be used to produce cheap electric energy and the coking coals to make metallurgical coke.

Jan 1, 1955

By P. Chiotti, J. T. Mason

Thermal, X-ray, metallographic, and resistivity data were obtained to establish the phase diagram for the Yb-Zn system. Six intermetallic compounds and five eutectics have been identified. The compounds position at 695°C. No evidence for the compound YbZn,, was observed. Whether this compound is stabilized or inhibited by small amounts of impurities is uncertain. SEVERAL aspects of the Yb-Zn system have been reported in the literature. Much of this work deals with the crystallographic identification of some of the compounds. The YbZn compound has been reported by Iandelli and palenzonal and the YbZn, structure and thermal data for the composition range between YbZn and Yb3Znll have been reported by Michel et al. A compound of uncertain stoichiometry in the range 60 to 68 wt pct Zn with a cubic structure has been reported by Kuz'ma et aL4 The YbzZn17, YbZn,,, and YbZn13 compounds have been reported by both Kuz'ma et a1 and Iandelli and Palenzona.' YbnZn17 has also been identified by Laube. This investigation was undertaken to establish the phase diagram of this system. Ytterbium in many respects behaves as an alkaline earth rather than a rare earth metal6 and it is of interest to note the resemblance between the Yb-Zn system, the Ca-Zn,' and typical rare earth-zinc systems.g'10 MATERIALS AND EXPERIMENTAL PROCEDURES The materials used in this investigation were Ames Laboratory ytterbium and Bunker-Hill slab zinc, 99.99 pct pure. Analyses of the ytterbium showed 38 ppm Ta, 82 ppm 0, and 15 ppm N with Ca, Cu, C, Mg, Al, Si, Cr, Fe, Ni, Sc, Y, Er, Tm, and Lu all less than 50 ppm. The ytterbium was dehydrogenated by heating in tantalum under vacuum for 8 hr at 900°C. The metal was kept under argon except when being cut with shears and when being weighed. Tantalum was found to be a suitable container for alloys in the composition range between ytterbium and Yb2Zn17. With higher zinc concentrations the tantalum was penetrated by the alloy and failed after several days at temperatures of 600" to 700°C. Approximately 20 g of zinc and ytterbium metal were sealed under argon in *-in.-diam tantalum cruci- bles equipped with thermocouple wells. The crucibles were in turn sealed in stainless-steel jackets. The alloys were equilibrated in an oscillating furnace and given various heat treatments in a soaking furnace. The steel jackets were removed and differential thermal analysis data were obtained under an atmosphere of argon. The thermal analysis apparatus was calibrated against the melting points of pure zinc, aluminum, silver, and copper and found to give thermal arrests within 1°C of the accepted melting temperatures for these elements. The thermal analysis apparatus has been described in an earlier paper.g Alloys were further heat-treated as necessary and subjected to metallographic examination and X-ray diffraction analysis. Most alloys were etched with Nital (0.5 to 10 pct nitric acid in alcohol). EXPERIMENTAL RESULTS The results of the thermal analysis are summarized by the points on the phase diagram, Fig. 1. Six compounds and five eutectics were observed. The eutectic temperature and compositions in weight percent zinc are 491°C and 12 pct, 645°C and 32 pct, 687°C and 54 pct, 742°C and 67 pct, and 750°C and 77 pct. The compounds YbZn, YbZn2, Yb2Zng, Yb2Zn17, and YbZnll melt congruently at 650°, 751°, 75Z°, 754", and 755"C, respectively. The compound Yb3Znll undergoes a peritectic decomposition at 695°C. The transformation and melting temperatures for the ytterbium were observed to be 797" and 817°C. re-

Jan 1, 1969

By Franz Wever

ACCORDING to Tammann,1 the explanation of the effect of mechanical deformation in producing changes in the properties of metals is one of the most important problems of physical metallurgy, taking rank with the study of the constitution of alloy systems; and this problem has long attracted-the attention of practitioner and scientist alike. Its solution was not advanced materially until Tammann2 set up his translation hypothesis with its crystallographic basis, while other hypotheses, such as the amorphous metal hypothesis of Beilby3 and Rosenhain,4 have been shown by more intensive studies to be less and less satisfactory. The principles of the Tammann translation hypothesis have proved to be useful even up to today and in spite of all of the recent accumulation of experimental data, while the differences of opinion which have arisen relate to the extent to which the hypothesis accounts for the observed changes in properties and to what extent further assumptions are necessary. Stimulated by the proposals of Tammann, there soon developed a lively experimental activity which aimed at the elucidation of the structural or crystallographic changes produced by the mechanical deformation of metals. Parallel movements of crystal "blocks" along definite crystal slip planes had already been observed by lowing and Rosenhain5 in 1900, in metals which had been moderately deformed but without shedding light on the crystallographic nature of the processes accompanying more severe deformation. The solution of this important problem was not advanced until a much later date, or until the methods of X-ray crystal analysis had become available. Shortly after the discovery of the diffraction of X-ray by crystals, symmetrical diffraction effects were

Jan 1, 1931

By B. S. Butler

The principal ore deposits of Arizona are in the southern, cen-tral, and western portions of the state, which physiographically are part of the Basin and Range province, southwest of the Colo-rado Plateau (Pl. I). The Basin and Range province is characterized by numerous subparallel mountain ranges separated by plains or valleys. Most of these ranges trend northwest to north, parallel to the margin of the Colorado Plateau; but in southeastern Arizona, southern New Mexico, and northeastern Sonora, they trend northward, transverse too the edge of the Plateau. The mountains rise abruptly from plains or valleys, the margins of which in many places are pediments cut on hard rock. Some of the plains form closed basins (bolsons, playas), but most of them are drained. The Basin and Range province in Arizona is divisible into the Mountain Region and the Desert Region4 (Pls. I and II). The Mountain Region forms a belt 60 to 100 miles wide that contains most of the large ore deposits. Its longest range measures about 55 miles, the widest 20 miles, and the highest peak more than 10,000 feet above sea level or 7,000 feet above adjacent valleys or plains. Broad plain-forming valleys are exceptional, but several with maximum widths of 20 to more than 30 miles appear in the southeastern portion. In the Desert Region the mountains are relatively low, narrow, serrated, and steep, with sharply angular profiles. There are a few exceptionally large ranges of which the longest measures nearly 100 miles and the widest 18 miles. The highest peak is some 7,000 feet above sea level, and the maximum local relief amounts to about 5,400 feet. Broad and comparatively low desert plains form 50 to 75 per cent of the area.

Jan 1, 1939

By S. F. Emmons

Jan 1, 1899