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By M. F. Goudge

Production of many industrial minerals reached all-time records in 1965. In keeping with the high level of industrial activity throughout the nation, producers of many industrial minerals operated at capacity or near capacity, notably the producers of phosphate, potash and sulfur. In the case of sulfur, the demand exceeded production and orders were filled, in part, from stocks accumulated in previous years. Industrial minerals as a group continued to increase both in value and quantity at a faster percentage rate than metallic minerals and fuels, The U.S. Bureau of Mines estimated that the value of industrial minerals produced in 1963 was $4318 million vs. $2006 million for metals. Preliminary estimates for 1965 indicate that current value of production was again more than 2% times that of metals, thus making apparent their importance to the industrial life of the nation.

Jan 2, 1966

By N. S. Stoloff, R. G. Davies

The annealing behavior of a heavily cold-worked FeCo-V alloy has been studied at temperatures both above and below Tc, the critical temperature for ordering. It was found that re crystallization and grain growth can take place below Tc in the ordered state and that, in agreement with results for fcc alloys, order retards grain growth. The activation energy for pain growth is -55 kcal per mole in the disordered condition; it was not possible to assign a value to the activation energy for grain growth below Tc because the degree of order is changing rapidly over the temperature interval investigated. Precipitation of an fcc y phase was observed upon annealing the cold-worked alloy at temperatures of 675°C and below. SINCE it is known that diffusion constants are greatly affected by long-range order,' it is not unreasonable to anticipate that order will influence the diffusion-controlled phenomena of recrystallization and grain growth. In the course of a study of strain aging of ordering alloys around the composition Ni3Fe Vidoz, Lazarevic, and cahn2 noted that a disordered cold-worked alloy annealed at a temperature T1 just below Tc will order but not recrystallize; Tc is the critical temperature for order. The same alloy annealed at a temperature T2 just above Tc, or an alloy of different (nonordering) composition annealed at either T1 or T2, will recrystallize after equivalent amounts of cold work. Initially Selisskii and coworkers,3,4 who examined a series of cold-worked and annealed bcc Fe- Co alloys, reported that alloys forming the B2 FeCo super lattice could not be recrystallized below Tc. However in a later paper5 it was shown that FeCo ordered alloys could be recrystallized below Tc. Thus the first question to be answered by the present investigation was whether or not a heavily cold-worked Fe-Co-V alloy could be recrystallized below Tc. When it was found that the alloy would indeed re-crystallize below Tc, the influence of long-range order upon subsequent grain growth was studied. EXPERIMENTAL PROCEDURE The grain-growth measurements were made upon FeCo-2 pct V wire of 0.031 in. diam; the alloy was the same as that used in an earlier study of the mechanical properties of FeCO-v.6 The wire was produced by cold swageing and drawing a rod 0.125 in. diam that had been quenched into iced brine from 850°C to disorder the alloy; the initial grain size was 0.05 mm. Rates of grain browth were measured after isother-mally annealing the wire in the temperature range 675° to 825°C; T, is -720°C. Grain diameters were measured on the transverse cross section of the wires. The line-intercept method of determining the grain diameter was used; conventional light photomicrographs were taken when the grain size was greater than 10 . Carbon replicas were produced and examined in the electron microscope if the grain size was less than Dislocation configurations after recrystallization anneals were studied by electron transmission microscopy of foils produced by cold rolling a 0.125-in.-thick strip of the quenched material to 0.012 in. The foils, after heat treatments similar to the wire samples, were thinned by electropolishing in a chromic-

Jan 1, 1967

By William B. Plank

A NEW record-a quarter million students in the engineering schools of the United States and Canada-has resulted from the great demand for engineers following World War II. The figures released by the American Society for Engineering Education and which appeared in detail in the Journal of Engineering Education for January 1948, show that, on Nov. 1, 1947, 252,250 students were studying engineering in 149 engineering schools of both countries. There are 244,390 in the 143 schools canvassed in the United States, and 7860 in six schools in Canada. These figures include both undergraduate and graduate students and are therefore comparable with the figures in previous presentations on this subject. This unprecedented engineering student body

Jan 1, 1948

By E. T. Turkdogan, L. S. Darken

Calcium ferrite melts were equilibrated with sulfur and oxygen-bearing gases at temperatures within the range 1290°C to 1620°C. The results show that at oxygen partial pressures below 10-4 atm the sulfide-reaction occurs and at higher oxygen pressures the sulfur dissolves in the melt principally as sulfate ion. It is also observed that when the product increases, sulfate ions are converted to pyrosulfate ions and the results permit the evaluation of the pyrosulfate/sulfate ratio. It is shown that the ratio y CaSO,/rCaO increases with decreasing concentration of calcium oxide in calcium ferrite, silicate and aluminate melts. Indications are that oxy-acids, e.g. silica, alumina and ferric oxide, increase yCaS0,. A few experiments were carried out within the sul-tide range and the results are in accord with those obtained by other investigators on aluminate and silicate melts. BECAUSE of the industrial importance and theoretical interest, many investigators have studied the reactions between molten oxides, silicates or alumi-nates, and gases containing oxygen and sulfur. The early work reviewed by Schenckl and studies made by Bardenheuer and Geller2 indicates that solution of gaseous sulfur in an oxide melt resulted in the replacement of the oxide ions by the sulfide ions. Measurements made by Grant and Chipman3 on the equilibrium partition of sulfur between molten iron and complex silicate melts also demonstrated that, for a given temperature and silicate composition, the distribution of sulfur between slag and metal increased with decreasing oxygen content of the metal. Fincham and Richardson4 studied the effects of temperature and partial pressures of sulfur and oxygen on the solubility of sulfur in simple silicate and alumino-silicate melts. They observed that at oxygen partial pressures below about 10-5 atm sulfur in the gas dissolved in the melt as sulfide ions, replacing an equal number of oxide ions of the melt. At oxygen partial pressures higher than 10-3 atm, sulfur entered the melt as sulfate ions. Similar studies were made by St. Pierre and Chipman5 using calcium ferrite and calcium silico-ferrite melts. The experimental data presented in this paper were obtained in this Laboratory about 10 years ago; this is the first formal presentation although a preliminary report was given previously.6 In each of these experiments, a pure synthetic CaO-Fe2O3 melt in a platinum crucible was equilibrated with a gas mixture (SO2-O2, SO,-air, SO2-CO, or SO2-CO2-CO) at a temperature ranging from 1296°to 1620°C. The experimental technique was essentially the same as that reported by Darken and Gurry,7 the main difference being that the atmosphere in the reaction chamber contained sulfur dioxide together with oxygen, or carbon dioxide-carbon monoxide

Jan 1, 1962

By C. C. Whittier

CIVILIZATION'S PROGRESS, which has multiplied man's comforts, conveniences, a n d happiness, is based upon the extensive employment of natural minerals and sources of energy. Mineral resources are basic factors in modern economic development, machine industry, international trade and world power. A survey of mineral consumption shows that the United States leads the world in the production and consumption of energy materials, of metals, and of the large and diverse array of earth materials that fall in the nonmetallic mineral group. The use of nonrnetallic minerals exceeded both the metals and the fuels in the long period before the industrial age, but it is only in the last two decades that consumption of non- metals has kept pace with and approximated in value the output of metals. Although the data of production in the first half of the last century are meager and fragmentary, the record of the past fifty years-the period of most rapid growth-is available, and reveals an astounding growth.

Jan 1, 1933

By Bernard K. Asdell

Georgia, a state seldom considered to be an important mineral producer, has one surprising feature-it is the nation's largest producer of kaolin. Kaolin is a highly important raw material in the paper, rubber, ceramic whiteware, paint and chemical industries. In 1965, more than 2.7 million tons of kaolin were produced in this state, a 150,000-ton increase over the preceding year, and production continues to climb. Strictly defined, the term "kaolin" applies to a group of hydrous aluminum silicates in which kaolinite is the predominant mineral. Kaolinite is inherently white, non-abrasive, chemically inert, and of a very fine particle size, ranging from sub-micron to 40-microns equivalent spherical diameter. An electron-micrograph of kaolinite is shown in Fig. 1. The particles finer than about 2 microns are thin, elongated plates, hexagonal in outline. The larger particles, coarser than 2 microns, are predominantly vermicular in outline with a foliated structure. Table I shows a typical chemical analysis of commercial, wet-processed kaolin compared to pure kaolinite.

Jan 11, 1967

By John Wulff

In a previous paper Burwell and Wulff1 have shown by electron diffraction studies that allotropic transformations can be induced in 18-8 stainless steel by polishing to a depth of about 5 X 10-5 cm. The development of a successful etching technique, which removes accountable amounts of metal from the surface without pitting and without changing the root-mean-square profile as measured with an Abbot pro-filometer, led to the application of the whole technique and material to an investigation of various mechanical methods of surface preparation, such as grinding, lapping, superfinishing and cold-rolling. Ideally suited to such a study is 18-8 of low carbon and nitrogen content. The material can be heat-treated to produce a coarse-grained single-phase structure. On cold deformation there occurs not only a reduction in grain size but, at regions of maximum stress, a change of face-centered material to body-centered material, provided the metal is worked below about 200°C. When worked between 200"about and 415°C., diffraction studies evidence a reduction in grain size without the appearance of any new body-centered ferrite. Ferrite, which can be referred also to strains induced by carbide precipitation, is evident when the material is worked at temperatures between 4150 and 800°C. Stainless steel is advantageous because the usual surface-finishing operations do not readily oxidize it to any appreciable depth. In order to produce detectable oxide films on the surface of austenitic 18-8 in a time equivalent to that required to produce, for example, a fine ground finish on 1/2 sq. in., the sample must be held in a furnace or oxygen stream above 600°C. By using longer heating times, it is possible to achieve measurable oxide films on samples , whose surface temperatures exceed only about 250°C. Experimental Procedure The apparatus, material, and technique described in the previous paper1 were employed in this investigation. Samples of 18-8, I by I cm. by 4 mm., were carefully annealed in the austenitic range to produce a coarse-grained structure. They were then quenched and pickled to remove scale, On a lapping machine of the Graton2 type, both sides of each sample were polished to a a of 1/6 a wave length of sodium D light. Thereafter they were electrolytically etched to remove at least 1 X 10-3 cm. of the surface, a depth that is well below that of any defermations induced by surface preparation. samples of this material, carefully mounted in steel holders, were then sent to various industrial organizations known for special finishing techniques. In the instrue ment shops at the Massachusetts Institute of Technology check samples were finished by the same methods, as far as they were available. Abbot profilometer3 readings Were made on all the samples, which were then carefully degreased in double distilled benzine and alcohol, dried in a hot-filtered air blast, and kept in a desiccator. SUC-

Jan 1, 1941

By John Wulff

In a previous paper Burwell and Wulff1 have shown by electron diffraction studies that allotropic transformations can be induced in 18-8 stainless steel by polishing to a depth of about 5 X 10-5 cm. The development of a successful etching technique, which removes accountable amounts of metal from the surface without pitting and without changing the root-mean-square profile as measured with an Abbot pro-filometer, led to the application of the whole technique and material to an investigation of various mechanical methods of surface preparation, such as grinding, lapping, superfinishing and cold-rolling. Ideally suited to such a study is 18-8 of low carbon and nitrogen content. The material can be heat-treated to produce a coarse-grained single-phase structure. On cold deformation there occurs not only a reduction in grain size but, at regions of maximum stress, a change of face-centered material to body-centered material, provided the metal is worked below about 200°C. When worked between 200"about and 415°C., diffraction studies evidence a reduction in grain size without the appearance of any new body-centered ferrite. Ferrite, which can be referred also to strains induced by carbide precipitation, is evident when the material is worked at temperatures between 4150 and 800°C. Stainless steel is advantageous because the usual surface-finishing operations do not readily oxidize it to any appreciable depth. In order to produce detectable oxide films on the surface of austenitic 18-8 in a time equivalent to that required to produce, for example, a fine ground finish on 1/2 sq. in., the sample must be held in a furnace or oxygen stream above 600°C. By using longer heating times, it is possible to achieve measurable oxide films on samples , whose surface temperatures exceed only about 250°C. Experimental Procedure The apparatus, material, and technique described in the previous paper1 were employed in this investigation. Samples of 18-8, I by I cm. by 4 mm., were carefully annealed in the austenitic range to produce a coarse-grained structure. They were then quenched and pickled to remove scale, On a lapping machine of the Graton2 type, both sides of each sample were polished to a a of 1/6 a wave length of sodium D light. Thereafter they were electrolytically etched to remove at least 1 X 10-3 cm. of the surface, a depth that is well below that of any defermations induced by surface preparation. samples of this material, carefully mounted in steel holders, were then sent to various industrial organizations known for special finishing techniques. In the instrue ment shops at the Massachusetts Institute of Technology check samples were finished by the same methods, as far as they were available. Abbot profilometer3 readings Were made on all the samples, which were then carefully degreased in double distilled benzine and alcohol, dried in a hot-filtered air blast, and kept in a desiccator. SUC-

Jan 1, 1941

By R. C. Buehl, M. B. Royer

High manganese slags of low phosphorus and iron content are produced by air oxidation of high phosphorus spiegeleisen in a basic-lined converter. Control of phosphorus and iron within specification limits for ferromanganese ore feed is obtained by a unique cyclic operating procedure. Various types of slags, or synthetic manganese ore, can be made. AN affiliated paper' describes the production of high phosphorus spiegeleisen containing 14 to 23 pct Mn and up to 4 pct P in an experimental blast furnace from open-hearth slag or manganiferous iron ore. This phosphorus content is too high for use of the spiegel in normal steel-production operations. Consequently, a preferential separation must be effected whereby the manganese is concentrated in a product that is usable in industrial operations. The preferential separation methods being investigated for this phase of the work are confined to pyrometal-lurgical processes for ready incorporation into steel-plant operations. It is fortunate that manganese is more actively oxidizable than iron or phosphorus, and therein lies a preferential separation method for isolating manganese from these two elements. Silicon is more strongly oxidizable than manganese, and its oxidation precedes, or occurs simultaneously, with manganese. Therefore, manganese and silicon are separable into a high manganese oxide slag phase while the phosphorus and iron remain in the molten metallic state. Complete separation of these elements represents an ideal condition which is not generally attainable in actual operations. This pyro-metallurgical method for separating manganese from phosphorus and iron by preferential oxidation was investigated by blowing 500 lb of metal in a basic-lined vessel to obtain preliminary information on the effectiveness of the procedure. Certain conditions of attainment in the separation process are desirable in any method for removing manganese from high phosphorus spiegeleisen, such as: 1—High recovery of manganese in the oxidation product; 2—the product to be of equal or better quality than ferromanganese-grade ore—48 pct Mn minimum, less than 10 pct SiO2, and Mn-P ratio of 300:1; and 3—attainment of the enumerated objectives in a product amenable to industrial handling, such as a slag of high manganese content that will flow from the processing vessel and of sufficient fluidity for ready separation of metallic granules that may have become mixed with the manganese slag phase. Previous Work Recovery of manganese from low grade ores and industrial byproduct slags by smelting to spiegeleisen, with subsequent oxidation to synthetic ferro-manganese-feed ores, has been a subject for periodic investigation during the past four or five decades in the United States and Germany. Joseph' and associates of the Bureau of Mines North Central Experiment Station, Minneapolis, Minn., smelted manganiferous iron ores of the Cuyuna range, Minn., to spiegeleisen and subsequently tried air and ore oxidation procedures for concentrating the manganese into synthetic ferrograde manganese ore. Joseph's results on the operation of a side-blown basic-lined converter for air oxidation of manganese from molten spiegeleisen were so discouraging that the procedure was abandoned after 11 blowing tests. Much slag was thrown from the converter vessel; phosphorus content was four to five times the maximum allowable for ferro ore; and a manganese-iron ratio of only 2 or 3:1 was obtained in the slag instead of the required 8:1. Oxidation of manganese from spiegeleisen with about 0.5 pct P, by adding iron ore to molten spiegel in an experimental open-hearth furnace, proved moderately successful in Joseph's experiments. The main drawback to the operation was the necessity for over-oreing for effective oxidation of the manganese with consequent too high iron oxide residual in the slag. Furthermore, the phosphorus content was proportional to the iron concentration and therefore much too high, so that several hours of reduction by a carbonaceous material were required to adjust the iron and phosphorus to the desired content of high grade ferro feed. A troublesome feature of the slag product of the spiegel oxidation process was its lack of fluidity if the silica content was less than 10 pct, the concentration considered desirable for the synthetic ore. Approximately twice the desired concentration of silica was required to impart enough fluidity for transfer from the vessel by pouring. The acute shortage of manganese in Germany

Jan 1, 1953

By G. W. Ostroot, S. Shryock

Cementing deep, high-temperature oil wells where static temperatures range from 350 to 400F has become routine in the part decade. In the United States there were 271 wells drilled deeper than 15,000 ft during 1963. Many of these wells had static temperatures higher than 400F. Bottom-hole static temperatures near 700F are now realities in the geother-mal (steam producing) wells of California's Salton Sea area. The detailed planning initiated prior to drilling the wells is discussed together with the methods, materials and equipment used in solving the cementing problems which are encountered. Data are also presented that lead to development of cementing compositions that provide adequate thickening time, do not retrogress in strength, and maintain low permeability under these extreme temperature conditions. Field data include the cementing programs used on eight relatively trouble-free geothermal steam wells in the Salton Sea area. INTRODUCTION Not too many years ago cementing oil wells with temperatures in the range of 300F caused considerable anxiety. In some areas of the United States it is now fairly common to cement wells having bottom-hole static temperatures in excess of 400F. We are now confronted with the problem of cementing wells with temperatures ranging from 500 to 700F. Temperatures in this order of magnitude are often found in geothermal steam wells. From where does this extreme heat emanate? There are many theories as to the source of this steam flow. The most widely held views are: (1) heat- ing of ground water fairly close to the surface by an intrusive mass of hot rock; (2) steam generation from a reservoir of metamorphic rock, normally found below 25,000 ft and not at the shallower depths of the Salton Sea reservoir; and (3) high-temperature gases (water vapor) escaping and migrating from molten or semi-molten rock (magma) at a considerable depth. Of these. No. 3 seems to be the most generally acceptable explanation. Heat from springs and fumaroles has been used for years as a means of heating and cooking; however, significant progress in harnessing the vast power of underground steam reservoirs has been relatively slow. The first large-scale attempt to use the heat generated by steam from wells was made in Italy around the beginning of the 20th century. In excess of 250,000 kw of electrical power is now being produced from holes around Larde-rello, Italy. Another very active drilling program was initiated in the volcanic area of New Zealand in 1949.' Natural steam for power projects in the United States began in the early 1920's. An early commercial steam field is located at the Geysers, approximately 75 miles north of San Francisco, an area discovered in 1847 and used for many years as a health resort. Steam originates from 15 wells that have been drilled since 1957. The present output from this project is 25,000 kw. Success of the Geysers operation has been responsible for several companies taking a careful look at the feasibility of producing steam for power generation in the Salton Sea area of Southern California's Imperial Valley. Geothermal steam activity in this latter area began in 1961 when O'Neill, Ashmun and Hilliard completed Sportsman No. 1, at that time the hottest wellbore in the world.' Since its References given at end of paver. completion seven additional wells have been successfully completed in this area. Many problems encountered in drilling steam wells had to be overcome to make the ventures successful. Formation temperatures encountered in the Salton Sea seemed to be a straight-line function (a gradient of 13F per 100 ft of depth).' This imposed severe conditions on all aspects of drilling and completion. This varied, to some extent, from gradients in the older geothermal areas. Not to be overlooked is the effect of these temperatures on casing creep or elongation by thermal expansion (Table I), because standard API flanged wellhead equipment makes no provision for this kind of performance. Floating equipment was redesigned, and changes in types of downhole equipment were made in an effort to eliminate anticipated problems. In the later completed wells, standard oil-well cementing equipment has been used. During the early development of geothermal steam wells there were some problems resulting from blowouts. However, these were eliminated in the deeper Salton Sea wells and no problems were encountered with the drilling mud. A sodium surfactant mud was used on the Sportsman No. 1 to drill from 2,690 to total depth. Nevertheless, it was necessary that a cooling system be added and the mud cooled before circulating it back into the well. The difficulty in evaluating the size of the steam area and its potential in terms of pounds of steam and years of productivity still has not been resolved. Economic complexities have also entered into the steam play in the Salton Sea. The wells at the Geysers were drilled at a cost of $15,000 to $20,-000, whereas the Salton Sea wells will cost more than $150,000. This cost differential has to some extent been accounted for because of the heavily

Jan 1, 1965

Belting worth thousands of dollars can be ruined in a few minutes because of careless maintenance or lack of maintenance. Proper belt conveyor maintenance means having a clean conveyor system at all times. The belt line should be visually inspected during each shift. Equipped with proper maintenance instructions, one belt man can patrol a belt line of 2 to 3 km (1.5 to 2 miles). His duties would be to lubricate drives and idlers (except sealed-for- life type), maintain belt and conveyor frame alignment, detect sticking idlers, and maintain an unobstructed right-of-way.

Jan 3, 1978

By Walter Miller

ALTHOUGH confident of its ability to meet any demands which may be made, the petroleum refining industry is not complacent about the situation and realizes that the quantities of petroleum products to be furnished are so enormous and so far beyond what was previously estimated that the full co-operative effort of the industry must be exerted. Establishment by the President in May of the Office of Petroleum Coordinator for Defense with Secretary of the Interior Ickes at its head, plus the formation of the Petroleum Industry Council for Defense, in November, provide the channels for united endeavor within the industry and the means for gearing that endeavor within the industry and the means for gearing that endeavor in full harmony with the nation?s needs. Great strides have been made and a rapid understanding of the situation and the magnitude of the task is being attained by all concerned.

Jan 1, 1942

By C. W. Allen, B. D. Cullity, H. S. Choi

The torsional deformation of aluminum and magnesium crystals is investigated, with particular reference to the dependence of proportional limit on crystal orientation. The proportional limit is found to be governed by the average value of the resolved shear stress on the most highly stressed slip systems, but the proportional limit does not strictly obey a critical-resolved-shear-stress law. The behavior of a cylindrical single crystal stressed in tension is well known: plastic flow begins when the resolved shear stress on the most highly stressed slip system reaches a critical value. There is much less understanding of the effect of torsion on such a crystal and on the way in which the critical-resolved-shear-stress law should be applied to torsional deformation. In the present paper particular attention is paid to the dependence of plastic yielding on crystal orientation and lesser attention to the mechanism of flow after yielding has occurred. New work on aluminum and magnesium crystals is presented, and previous results obtained in this laboratory on magnesium1 are re-examined. STRESS DISTRIBUTION The problems involved in torsional deformation of single crystals are due entirely to the complexity of the stress distribution. In tension, if loading conditions are perfect, the shear stress on any particular slip plane is completely uniform over the entire area of that plane. In torsion, on the other hand, the stress on any selected plane in a particular direction varies not only from center to edge of the specimen but also around its perimeter. It is convenient to express the stress at any point in terms of t0, which is the shear stress acting at the surface of a cylindrical specimen on a plane normal to the axis and in a direction tangential to the cylinder. At point P of Fig. 1 this stress acts in the direction of axis 2 and is given by To = 2T/pr3 [1] where T is the applied torque and r the specimen radius. This stress can be resolved on any chosen slip system, and details are given in the Appendix. Let P be the point on the specimen surface where the stress is to be evaluated; P is defined by its angular distance A from an arbitrary reference line through 0 normal to the axis. his line is usually taken as the direction of incidence of the X-ray beam used to determine the crystal orientation.) Then the shear stress t, acting at P in direction Dona plane whose normal is N is given by Ts/TO = sin ? 0, cos ?d sin (?0, - ?) + cos ?, sin ?d sin (?d - ?) [2] where 0, and Od are the angles between N and D, respectively, and the axis, ?0 and ?d are the angles between the projections of N and D, respectively, on the transverse plane and the reference line through 0. By means of Eq. [2], the stress 7, acting in any given slip direction can be computed. In the previous work on magnesium1 only gross slip tangential to the specimen surface was considered, and this

Jan 1, 1963

By H. W. Peirce

Identified and utilized Arizona salt deposits are of two ages: 1) Permian in the Colorado Plateau, and 2) Tertiary in the Basin and Range country. Uses include: a) storage of energy fluids in man-made solution cavities in both Permian (Supai Formation) and Tertiary (Luke salt body) salt and b) production of marketable products by solution and evaporation of tertiary salt. The two liquid petroleum storage Projects have a combined storage capacity in excess of 380 million L (100 million gal). Current production of salt products approximates 32 kt/a (32,000 stpy). Increasing demand for both storage and salt products is anticipated.

Jan 1, 1983

By R. C. Himes, K. Zanio, J. B. Wagner, J. W. Moody, J. F. Miller, W. Johnson

The recent research with which this paper deals has been concerned with the preparation of pure PbTe crystals suitable for control of radiative processes and othe.v electronic applications. The research has been directed toward the developrnent of methods for the preparation of puve, homogeneous, loul-ca,wier-density PbTe crystals suitable for use in the fabrication of optically pumped and electrically pumped diode lasers. Steps in the preparation of the crystals include 1) purification of the starting materials, 2) synthesis and purification of the PbTe, 3) growoth of PbTe crystals, and 4) adjustt~zertt of composition of the crystals This Paper describes the general preparation procedure employed and discusses some investigntiotzs of purification processes. THE as-received lead and tellurium are nominally 99.999 to 99.9999 pct pure. Assays furnished by the suppliers, obtained by emission spectrographic analysis, show only the presence of about 2 ppm Mg in the tellurium. Such analyses are not very informative, however, since they give no information on the concentrations of normally gaseous impurity elements such as oxygen. Both the lead and the tellurium in the as-received state usually contain appreciable concentrations of oxygen—primarily in the form of oxides on the surfaces of the material. To reduce the oxygen content, the lead is held in the molten state in hydrogen at -700°C for several hours. For this treatment, the lead is contained in a graphite boat which is rf-heated, and the hydrogen is passed through a liquid-nitrogen trap prior to use. Tellurium is subjected to multiple distillation in hydrogen to remove oxygen and other foreign impurities. If, in conducting the distillation, approximately the last 10 pct of the charge at each "stage" is left as the discard cut, purification of the tellurium proceeds as indicated in Fig. 1.l Tellurium used in this work has been distilled two or three times to reduce carrier concentration to about 10" per cu cm. The PbTe is prepared from the purified elements by reacting them in the molten state in sealed, evacuated, or hydrogen-filled silica ampoules. The charge is usually held above the melting point of PbTe (923°C) at 1000 C for 24 hr to ensure that it has been homogenized. Two methods have been employed for the growth of the required single crystals of PbTe: growth from the melt, which will be discussed first, and growth from the vapor phase. Large single crystals of p-type PbTe can be grown readily from the melt by the Bridgman method. For this method of crystal growth, the PbTe is synthesized in situ from proper proportions of the purified elements. Growth (dropping) rates in the range 1.3 to 6.5 mm per hr are employed. Material near the maximum melting composition (about 50.012 at. pct Te) is utilized to avoid composition change on freezing, and thus to obtain crystals of nearly uniform composition. Crystals prepared by use of procedures described up to this point were sufficiently pure and perfect that they could be used for the preparation of laser crystals in studies at Lincoln Laboratory.2-5 ADJUSTMENT OF COMPOSITION Good n-type crystals of PbTe cannot readily be grown from the melt. Further, growth from the melt of crystals of any compositions (n or p type) other than those near the maximum melting composition is difficult because of the large composition changes that must occur on freezing.'" However, melt-grown crystals can rapidly be brought to other desired compositions by isothermal equilibration through the vapor phase with a two-phase Pb-Te stock material, essentially as described by Brebrick and Allgaier.1 The work to be discussed has been concerned with the preparation of n-type crystals; thus, the two-phase stock which was employed contained excess lead, and all ensuing discussion is of the preparation and properties of n-type crystals. The equilibration was designed to the shift composition to the lead-rich limit of stability at the selected temperature. Initial treatment of the crystals at high temperature was employed to minimize the total time required for the equilibration. Final adjustments of the composition and state of the crystals were made by use of low-temperature heat treatment at temperatures in the range 200" to

Jan 1, 1968

By AIME AIME

HEREWITH is presented a preliminary report of a special committee, consisting of Erle V. Daveler, Paul D. Merica, and C. H. Mathewson (chairman), dealing with sundry matters of which many are of vital interest to all members of the American Institute of Mining and Metallurgical Engineers. As the report states, the initial purpose of the investigation was to determine ways and means to stimulate "the welfare and growth" of the Institute of Metals and Iron and Steel Divisions. However, it soon became apparent to the committee that most of the problems and possible correctives were of no less vital concern 1o members of the other Divisions and to the "unattached" group of members. Consequently, the Committee has authorized publication of the report and invites written comment from any member on the specific recommendations or on any other phase of the broad subject.

Jan 1, 1943

By Karl Cohen

The question of attainment of competitive nuclear electric power is of interest to uranium producers because the rate of attainment of this goal determines the date when there will be a solid, non-political, domestic uranium market. It is a burning question to those of us in the civilian nuclear power business, because our entire business future hinges on how well, and how soon, we can make electricity from nuclear reactions at prices comparable to electricity from coal. For an idea of the magnitudes involved, consider that the first fuel load of the Dresden (Illinois) nuclear power station, plus spares, will be about 90 tons of 1.5 pct UO2. This requires about two-and- a-half times as much natural uranium oxide feed to the diffusion plant, or 225 tons. This, in turn, represents about a month's production from the nearby Uranium Reduction Co. mill. Note also that the 180,000 kw electric output of the Dresden station will be about 0.1 pct of the national electric generating capacity in 1960.

Jan 12, 1958

By Paul F. Kerr

The insufficiencies of our mineral resources are becoming well known, and the national political conscience seems to be troubled at last by our dependence upon mineral commodities which must come from other lands. This realization places increased responsibility upon the industrial, educational, and governmental groups whose task it will be to solve the problems of mineral supply. As we all know, from the time that man first sought mineral deposits until recent years, prospectors have been largely responsible for mineral discoveries. Today the era of the prospector is almost over. The human ants that have literally examined all accessible outcrops and have tested the gravels of nearly all stream beds in the United States have left undiscovered few worthwhile mineral deposits within the scope of their recognition. The pages in the history of mineral exploration are now being turned from the era of the surface prospect to the era of the hidden de- posit.

Jan 1, 1949

By R. D. Caudle, Yoginder P. Chugh, V. K. Agarwala

Longwall coal mining is a growing mining technique in the United States. However, very little premining exploration data are collected presently by coal companies to 1) select coal winning equipment, 2) select and design face supports and supports in gate and tail entries, or 3) optimize operational parameters such as length, width, and orientation of face. The authors are of the opinion that much of the data needed for mine planning and design for longwall mining can be obtained during exploration. In this paper, the authors identify the data requirements, discuss how these data can be obtained during exploration, propose an exploration program and estimate the cost to obtain the necessary data.

Jan 1, 1982

By John D. Morgan

Prior to World War I there was no Government stockpiling program. Prior to World War I1 relatively few items were included in Government stockpiling and the start of that war found most objectives for even these few materials far from complete. Profiting from the experience of materials shortages in two wars, Congress in 1946 passed the Strategic and Critical Materials Stock Piling Act, which stated that it is the policy to decrease and prevent wherever possible a dangerous and costly dependence of the U. S. upon foreign nations for supplies of strategic and critical materials in times of national emergency. However, as of mid-1950 few stockpile objectives had been achieved. Shortly after the start of the Korean War it was obvious that in the absence of adequate stockpiles, the defense program could not be successfully carried out without broad authority to expand supplies of strategic and critical metals and minerals and at the same time to channel limited supplies of these materials to essential defense purposes. Accordingly, in September 1950 Congress passed the Defense Production Act, which provided broad powers for allocating materials and for making arrangements, including financial, to expand supplies.

Nov 1, 1955