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By E P. Graham

Orebodies occur in an infinite variety of grades, shapes and sizes, and take many millions of years to grow. When extraction starts there is only one possible end -the mine sooner or later will run out of ore and shut down. If the mineral industry is to supply the ever increasing demands of modern civilizations, more and more metals must be found and mined. This will require a never-ending search for ore, and the development of every economic body, large or small. To justify the mining of a small orebody, it first of all must pay its way. If the size of the burden imposed by the capital cost estimates is not carefully worked out, an otherwise promising situation could be killed. The very nature of mining, as a transient industry, re-leases a steady stream of good used equipment, and the trained personnel to install and operate it. All manner of plans and layouts, which can be utilized at a new property, are available. Working these and other economies into the estimates will sometimes make enough difference to give a prospect the green light.

Jan 1, 1964

By G. Venturello, C. Antonione, G. Della Gatta

Results from work on the effect of inferstitials on recovery and recrystallization of' very pure iron (99.995 pet) doped with nilrogen up to 400 ppm are reported. Nitrided specimens were obtained by heating the iron in a static atmosphere of NH3 + H2. The samples were cold-rolled 80 pet, subjected to a series of isochronal and isothermal anneals, and submitted to examination by X-rays, micrographs, and hardness tests. Small additions of nitrogen show a strong effect in reducing recovery of' the mechanical properties of high-purity iron. At the temperatures of. the experiments, this effect proved greater than in the case of carbon. At 400°C pure iron recovers more than 50 pet of the total hardness increase, carburized iron vecovers 25 pet, and nitrided iron only 10 pet. On the other hand. the addition of nitrogen has, similarly to carbon, a very small effect on recrystallization; the effect is, however, slightly higher than that of carbon. When the concentration Of nitrogen is above the solubility limit in a iron at the temperattue of the experiments, an increase in the frequency of nu -cleation is also observed. THE object of the present work is to improve knowledge on the effect of interstitials both on recovery and on primary recrystallization of pure iron. In fact. at present there are no available data on the effect of nitrogen on high-purity iron. The only work which at present can be somewhat related to this problem is a work of Leak et al.1 in which grain boundary internal friction at high temperature in the presence of increasing amounts of nitrogen is studied by a torsion pendulum. The present work is a continuation of a previous one2 on the effects of carbon. EXPERIMENTAL PART Preparation of the Material. Pure iron was prepared following the same methods used in the pre- vious work2 and was nitrided using controlled quantities of ammonia in an apparatus similar to that used for carburizing. The apparatus consists essentially of a gas-tight quartz tube containing the specimens. The tube, maintained at constant pressure by means of a mercury seal, is placed in a resistance furnace. For nitriding, the NH3 + H2 atmosphere with a suitable concentration of NH3 was introduced into the tube, which had been previously carefully evacuated and degassed by heating at 600°C. The hydrogen used was carefully purified by passing it through a palladium filter. The ammonia required was prepared with the following reaction: CaO + 2NH4CI —CaCl2 + H2O + 2NH3 by heating the mixture of CaO and NH4C1 in a glass flask and then collecting the ammonia in a graduated Hempel burette. For each nitriding program a given amount of NH3 prepared by this method was introduced together with the H2 into the tube previously evacuated. Nitriding of the sample was then performed at 570°C for 48 hr. After this, to ensure a homogeneous distribution of nitrogen, the samples were further heated for 72 hr at 800°C. With this method which uses a static nitriding atmosphere, carefully controlled conditions of purity are obtained. Contrarily, with the conventional continuous-flow methods, using large quantities of circulating gas, there is a greater risk of introducing impurities into the samples. Furthermore, the required nitrogen concentration in the specimen is easily predetermined and obtained. A plot of the relation observed between the initial concentration of NH3 in the gas and the quantity of nitrogen introduced into the iron samples is given in Fig. 1. The data refer to samples of 1.2-mm thickness and to the nitriding conditions previously described. Furthermore, as a comparison, the data relative to two 0.5-mm-thick samples are reported. The presence of a reservoir in the cold zone of the reaction bulb made possible the gradual dissociation of ammonia on the sample in the hot zone. Internal-friction methods were used to determine the content of nitrogen dissolved in the iron samples. Some analyses were also carried out with chemical methods. The following table, Table I, shows a comparison of data obtained with chemical and internal-friction methods. The correspondence between chemical methods and internal-friction

Jan 1, 1964

By S. Leber, R. F. Hehemann

This investigation describes the kinetics of alloying in a (Cb-15 wt pct W. 5 wt pct Mo, 1 wt pct Zr) powder-metallurgy alloy. The degree of homogeneity obtained in hydrostatic ally pressed and vacuum-sintered samples is described by composition distributions resulting from analysis of X-ray dvfraction line profiles. Sintering variables and degvee of powder dispersion were evaluated. The utility of single-value parameters obtained from composition distributions is disaissed. The spatial distribution of composition, as revealed by anodically tinted metallographic sarrzples, was used to provide diffision models based on a concentric-sphere geometry. Diffusion equations developed from these models were found to be in general agreement with experimental results. The powder-metallurgy method for the production of refractory metal alloys has the ability to produce an inherently fine-grained, fabricable structure. The more general use of this method is inhibited, in part, by the presumed difficulty in obtaining homogeneity on a microscale. The degree of homogeneity therefore is an important, but usually neglected, variable in specifying the quality of a powder-metallurgy alloy. Convenient techniques for measuring the degree of homogeneity are now available,' and have been used to develop a model describing the process of alloying in a simple binary mixture.' In this investigation, the process of alloy formation has been studied in a more complex system. PROCEDURE The columbium-based F-48 mixture was prepared from the constituent powders shown in Table I. The particle sizes tabulated were provided by the vendors of the individual powders. Standard laboratory techniques utilizing a jar mill were employed for blending. The blended powders were hydro-pressed into 1-in. diam rods which were then sliced into thin discs for vacuum sintering. All samples were given a preliminary treatment at 1700°C for 2 hr. Varying degrees of homogeneity were obtained using additional treatments at higher temperatures. The degree of homogeneity obtained by a specific sintering treatment was evaluated metallographi-cally using the anodic-tinting technique described by olff,' and quantitatively by the analysis of X-ray diffraction line profiles using the X-ray diffraction technique developed by udman.' The diffraction technique is strictly valid only for binary systems. However, the relatively small difference between the lattice parameters of tungsten and molvbdenum when compared with columbium permitted the treatment of the complex composition of F-48 as a (W, Mo)-Cb pseudobinary. Calculations were weighted in accord with the W-Mo ratio in the F-48 composition. The contribution of the 1 pct Zr was ignored since it could not even be detected in the blended powder. Two factors are required to convert an X-ray line profile into a composition distribution. The variation of these factors with composition is shown in Fig. 1. Curve A was used to convert angular posi-

Jan 1, 1964

By Frank L. Wideman

THE TREND towards larger quantities of waste in materials handled at metal and nonmetal mines (excluding fuels) continued. A gain of 10 percent from 1962 in the tonnage of waste removed in mineral operations reflects the kind of technological problems being encountered. Technology has a major role in the mineral industry in the task of supplying raw materials obtained from resources occurring beneath the surface of the earth and used in manufacturing commodities essential to modern living. Changes in technology are often brought about by such factors as variations in economic conditions, differences in physical properties of raw material and changes in mineralogical compositions of ore. Mining is usually begun on the richest and most accessible of known deposits, and when these are exhausted, is continued with leaner ores or with less accessible deposits that are either lying at greater depths or are more remote from markets. The increasing difficulties of extraction and depletion of reserves are offset by improvements in extraction technology, improved transportation, and exploration for new deposits. Although depletion has prevailed at many individual mines and in many districts, technology has been the means of providing for increasing demands of an expanding economy with adequate supplies of minerals despite either the changing character or decreasing grade of certain ores. This has been accomplished by various methods applicable to minerals. Among the implements of technology are utilization of lower grade or more complex refractory ores by mass mining, concentration, processing, recovery of byproducts, and mechanization. Better methods to find concealed deposits or to penetrate to greater depths also have been helpful in maintaining a supply of particular minerals.

Jan 1, 1964

By W. F. Hosford

A quantitative explanation is offered for the peculiar curled grain shapes found in the microstructures of drawn wires of bcc metals and compressed aluminum specimens. It is shown that once an [011] fiber texture is developed, the slip system are so oriented that further slip tends to produce plane strain rather than axially symmetric flow of individual grains. With plane -strain flow, however, compatibility of neighboring grains can be maintained only by a bending of grains about one another. PROBABLY the most obvious microstructural feature of heavily worked metals is the distorted shapes of grains. In the course of deformation, the shape change of each grain must be compatible with that of neighboring grains; otherwise holes would be formed at grain boundaries. In analyses of poly-crystalline deformation by Taylor and subsequent workers it was assumed that grain boundary compatability was maintained by each grain undergoing the same shape change as the polycrystalline aggregate in which it is imbedded. According to this assumption, when simple tension or compression is applied to a random polycrystal or to one with a fiber texture, each grain ought to deform with axially symmetric flow. Initially equiaxed grains should become cigar-shaped during wire drawing and pancake-shaped during compression. While microstructural observations of deformed metals are generally in accord with such a picture, certain striking exceptions may be noted. Peck and Thomas5'8 found that grains in heavily drawn tungsten, iron, and niobium (columbium) wires become shaped like ribbons curled about the wire axis, Fig. 1. At a suggestion from the author, they rationalized the development of these micro-structures by considering the orientation of the slip systems in the [011] texture formed by the wire drawing. It is shown in this paper that marked departure from axially symmetric flow of grains is also observed when polycrystalline aluminum is severely compressed. Again the explanation must lie in the orientation of the slip system in the [011] texture, which is formed in fcc metals by compression.' THEORY A simple quantitative argument will be presented to show that the development of these microstructures is a result of flow on the combination of slip systems for which the minimum amount of mechanical work is expended in producing a unit tensile (or compressive) strain. First it must be realized that the macroscopic strains of a crystal resulting from slip are given by: where d dy, and dc, are normal strain increments parallel to the x, y, and z reference axes; are crystallographic shear-strain increments on slip systems

Jan 1, 1964

By G Anders

Underground tests of slusher cables at first might seem to be quite simple and inexpensive. They do, however, take a long time and give results that may be ambiguous and unreliable. Also, because underground test conditions are not exactly duplicable, tests carried out at different times or in different mines could not be compared. An attempt was made to develop a laboratory test method that would provide for all factors affecting slusher cable performance underground in such a way as to make it possible to achieve comparable results from different series of tests by exactly duplicating test conditions. Such a method should also make it possible to vary individual factors systematically in order to give a proper assessment of the effect of changing conditions on cable performance. A set of tests, comparing the same two types of cable both underground and in the laboratory, is described. AN assignment at the Algom Nordic mine called for the comparison of two types of %-in. slusher

Jan 1, 1964

By L. Frost

The establishment of a retreat system of longwall mining in this submarine coal field has been under study for many years and, although in special cases there have been limited local applications of this method of mining, there has been no attempt until quite recently to establish a uniform system of longwall retreating' in this area (see Figure 1) Where retreat walls were established, it was strictly as a result of physical, rather than economic conditions. In some of the operations- of the Corporation, where the coal was liable to spontaneous combustion- or the area subject to bumps as in No. 2 Mine of the Cumberland Railway and Coal Company in Springhills the recovery of the coal on a retreat system was more or less a necessity.

Jan 1, 1964

Wire rope, when used for hoisting on a mine is the weak- est and most vulnerable unit in the most expensive'-group of installations or! the mine. With the introduction' of hoisting on the S1Koepe"' sheave, a new technique was-established. This innovation brought with it the certain- advantages which long had been recognised and which are being developed further. For many years, drum winders of many types had been the sole means by which ore had been hauled from mines. This type of winder, with its capacity for rope storage on the drum, permitted mine operating personnel to cut short lengths from

Jan 1, 1964

By W. W. Vaughn

In the technique described and evaluated, detection of mercury is based on the principle of atomic absorption. An analog signal, produced when mercury vapor absorbs ultraviolet light, is converted to digital form and calibrated to mercury concentration. Interferences are eliminated by selectively trapping the mercury on gold. The lower limit of sensitivity, using a 1-gram sample, is 5 parts per billion. A model of the instrument mounted in a station wagon has been tested successfully in the field.

Jan 1, 1964

By Robert L. Bates

In this paper I use the term "industrial minerals" in its broad general sense, and I distinguish two main groups. The first consists of the bulk materials, characterized by low unit price, nearness of deposits to markets, relatively simple methods of extraction and processing, and a tendency to be closely related to the construction industries. The second group includes those materials valued for exceptional purity, or for some special property such as hardness, immunity to acids, or dielectric strength. These materials are produced in smaller amounts, at high unit values, from deposits notably restricted in. distribution; and they require more or less sophisticated methods of production and beneficiation. The applications of this second group are not closely tied to any particular part of the economy. From the way in which the commodity committees of the Industrial Minerals Division are set up, I take it that the chief interest of most members is with the first group of materials mentioned above. Hence this paper will deal mainly, though not exclusively, with such bulk commodities as sand and gravel, clay, and stone. The first word in the title of the paper also requires brief explanation. It is here given a threefold interpretation. First is the role of the industrial minerals themselves in industry; this would probably be taken as the conventional meaning of the title* The second is the role of the industrial-mineral producers as citizens of the community. The third is what may be called the scientific role of these producers.

Jan 1, 1964

By J. J. Scott

This investigation utilizes three dimensional photo-elastic techniques to determine the stress distributions in the pillars and the roof of a room and pillar mine model. Castolite plastic was used for the construction of the model in which a stress pattern was developed by the stress freezing process. Analysis of the stress pattern was accomplished by observation of points in slices from the model with a polariscope and solving the data thus obtained by the shear-difference method. Slices through the centerline, edge of pillar and centerline of span were investigated. The results of this work provide information on the overall stress distribution in points of stress concentration in compression, shear and tension, show relative magnitude of stress throughout the model and indicate directions of the most important stress values. A generalized roof bolt pattern is developed for room and pillar mines based on the stress distribution. A digital computer was used in the reduction of data and proved to be extremely useful for investigation of this type. Underground excavations disturb the equilibrium of the earth's crust and a core of fracture, or altered stress distributions exists around the openings. This fact is well known by mining operators and investigators in the rock mechanics field. Analysis of the stress distribution in the areas around mine workings is a most difficult problem and one which has no simple and direct solution. Some of the approaches used by investigators in attempts to study stress distribution around mine openings involve mathematical analysis, photoelastic techniques, statistical analysis, model studies on brittle materials and observation of fracture patterns. Models involving imbedded strain gauges, gelatin models using imbedded strings to show internal movement, and many other unique laboratory techniques are employed. Work is also being done in mining operations where load cells, strain gauges, photostress material, convergence plugs, dynamic plugs, etc., are used to measure strain which can in turn be used to obtain stress. Some of these devices measure strain from which stress may be derived. All approaches to the solution of stress distribution are hampered by the fact that the earth is not a homogeneous, isotropic and elastic media. Geologic faults, fractures, bedding planes, vugs, variations in material composition, variations in grain size and structure, etc., make it extremely difficult to obtain results which can be universally applied to mining operations. The purpose of this investigation will be to demonstrate the use of three-dimensional photoelastic techniques to obtain the stress distribution in the pillars and roof of a room and pillar mining operation. This method utilizes full analysis of interior points, and thus it may be that small tensile or shear stresses found in the investigation will prove to be of greater significance than the more obvious points of stress concentration found by two-dimensional techniques. A digital computer was employed to simplify and to shorten the time necessary to obtain final results. Application of the computer to problems of this type may enable future investigators to attempt more elaborate analyses than have been previously considered feasible. THEORY Three Dimensional Stress Analysis-Shear Difference Solution:' Photoelastic studies are based on the fact that an optically isotropic transparent solid becomes optically anisotropic when subjected to forced deformation; the degree of optical anisotropy being proportional to the deformation of the material. There are two fundamental laws which govern photoelasticity: 1) Light is polarized in the directions of the principal stress axes, and is transmitted only on planes of principal stress. 2) The difference in principal stresses is proportional to the difference in the indices of refraction along the planes of principal stress. One method used in three-dimensional photoelastic work is to examine a slice of the object by normal incidence and oblique incidence. In normal incidence,

Jan 1, 1964

Although Canadian bentonite is competitive in quality for most uses, it has not been accepted for the pelletizing of iron ore concentrates. In 1962, Canada consumed about 10,000 tons of imported bentonite for this use. By the end of 1965, the planned domestic consumption for this purpose alone will probably be more than 100,000 tons a year, valued at about $3 million. Consequently, a challenge exists for the establishment of a Canadian source of high-quality bentonite for pelletizing. Such a bentonite would also be suitable for the two other major applications -well drilling and foundry use. Brief mention is made of such topics as the identification, 1noperties, occurrences, exploration, applications, technology and laboratory testing of this clay. In particular, the type of bentonite in demand, the geological horizons warranting exploration, and simple preliminary test methods are discussed.

Jan 1, 1964

By Myles E. Robinson

Significant changes in the markets for coal have taken place since World War II, As used in this study the term ?coal? will refer to bituminous coal, The anthracite industry in size, characteristics, and problems differs materially from the bituminous coal industry, These changes have both influenced and been influenced by the mechanization of mines, and by decreased distribution costs, especially in transportation. It is the purpose of this paper to examine these post-war changes, to assess their impact upon the production and distribution of coal, and to explore future market developments in the light of past and present trends and relationships. The layman lacks adequate informatian on the production, demand, and distribution of coal. There are two reasons for this. First, there is a relative lack of statistics coveting the industry, Coal operators and distributors are not required to file with any government agency the type of much more complete statistics filed by the railroads and public utilities with national and State agencies. The Bureau of Mines assembles much useful information on the coal industry, but several areas, including that of investment and finance, have no central depository which can be used to keep the public informed of the nature and extent of the industry and its problems.

Jan 1, 1964

By Alvin Kaufman

Geothermal plants are competitive with conventional units. A geothermal plant can produce electric energy for 6.70 mills per kwhr, compared with 6.96 mills for coal, 6.74 mills for oil, and 7.04 mills for gas. These costs include fixed and variable charges. Potential for geothermal power exists in the Western United States, Alaska, and possibly Hawaii. Assuming that the current downward trend in cost per kilowatt of coal will cease and that the relative cost of gas and oil, already trending upward, may rise considerably more, geothermal energy will be utilized where available, in producing electric energy. It will be used in California first because it is directly competitive with gas-and oil-fired installations there. A long-term appraisal is difficult because little is known about the sources of geothermal power and the electric generating capacity which the steam fields will support. However, a market for geothermal steam-generated electricity exists within the Western States.

Jan 1, 1964

By D. W. Frommer

In continuing its long range studies of methods of treating low-grade iron ores, the Bureau of Mines has developed a new selective flocculation, desliming, and flotation procedure that enables effective beneficiation of the finely disseminated ferruginous jaspers of the Marquette range, Mich. The process, developed on a bench scale and later confirmed in the 800-lb/hr pilot plant, comprises dispersion, selective flocculation, desliming to reject fine silica and clay, and flotation of silica from the remainder of minus 400-mesh pulps. Pilot plant flotation of two Marquette range ores, using the selective flocculation procedure on feeds containing 36 percent Fe, yielded iron recoveries of about 84 percent in concentrates containing 65 to 66 percent Fe and 4 to 5 percent silica. These results were metallurgically superior to those obtained when selective flocculation was not used. Also operating characteristics were better, and reagent costs were lower.

Jan 1, 1964

By Danforth R. Hale

The pressure of military use of quartz resonators led to efforts to Grow high, grade quartz crystals in Germany and in Great Britain during 19)3-25, and was responsible for a series of U.S.A. Signal Corps contracts beginning in 1946 with the Clevite Corporation (as the former Brush Development Company), Bell Telephone Laboratories, Antich College, and others. The technique of growing crystals from the melt, such as KI, NaBr, was already commercially inuse Quartz could not be so grown, since its utility depends on the form stable below 573°C, and, even if it could be grown from an extraordinarily viscous melt, the higher form passing through this transition becomes twinned. Again, several crystals were being grown commercially from water solutions; quartz, however, is listed in the common literature as being insoluble in water. Fused quartz, or vitreous silica, was chosen as raw mater¬ial by the European experimenters because of its thermodynamically lesser stability than quartz, and various alkaline solutions were tried for the purpose of enhancing the solubility.

Jan 1, 1964

By John Bley

White Pine Copper Company operates a mine in the Upper Peninsula of Michigan using a modified room-and-pillar system for extracting ore.1 Mine production averages 15, 500 tons per day. The terrain is predominantly level and the depth of cover varies from 500 to 800 feet over the present workings with depth increasing as mining progresses down the dip. The deposit is situated on a low angle plunging, anticlinal structure composed of sedimentary beds. Local terminology for the stratigraphic units which contain the ore horizons, named in ascending order, is as follows: lower sandstone, parting shale, upper sandstone and upper shale. The ore zones of copper enrichment are, contained in the parting and upper shales. The parting shale will vary; from 6. 5 to 9.0 feet thick; the upper sandstone from 2 to 10 feet; and the upper shale from 1. 5 to 6. 5 feet. Two variation of the room-and-pillar system are used to extract the ore depending on grade and local ground conditions. One system is called the parting shale method and recovers the parting shale only. This system requires a mining height of 8 1/2 feet to accommodate large-scale, high-capacity equipment and this working height is obtained by removing approximately 1 to 2 feet of the barren lower sandstone with the ore. Under the second system, locally termed full column, the mining height is about 14-1/2 feet and this system removes the parting shale, the upper sandstone and the lower mineralized zone, approximately 1-1/2 feet, of the upper shale at which point it is possible to maintain a competent back (Fig. 1).1

Jan 1, 1964

By Martin Weinstein

A technique is described for preparing finegrained lead telluride by ultrasonic agitation of a solidifying melt. Material prepared by this technique is dense and chemically homogeneous. N-type PbTe, containing 0.03 mole pct PbIz, has been made and its thermoelecCric Properties have been measured as a function of temperature. For comparison, the properties of similarly doped PbTe made by cold pressing and sintering, and by extrusion, have also been measured. The ultrasonically prepared material compares favorably with the others in its thermoelectric-efficiency factor. Comparison of compressive-flow curves for the three kinds of PbTe show that the ulhasonically prepared material has much superior ductility. The cleavage strength of the ultrasonic material is related to the grain size, D, by the Petch relation:Extrapolation to infinite grain diameter yields a fracture strength of 5000 psi for single-crystal PbTe. WHEN metals and semiconductors solidify in a mold they normally assume one of three cast structures illustrated in Fig. 1.' Solidification in a casting starts at the mold walls where a large number of fine crystals of random orientation can be nucleated to form the chill zone. Because of the anisot-ropy of the growth rate, those crystals whose direction of maximum linear growth is parallel to that of the heat flow grow faster and crowd out the crystals of less favorable orientation. A second zone, having a preferred orientation, called the columnar zone, thus forms adjacent to the chill zone. The speed of growth of the columnar grains will depend, in the case of limited undercooling of the melt, on the rate at which heat can be abstracted. The columnar zone can extend to the center of the casting, Fig. l(a), but it is frequently followed, in solid-solution alloys, by another zone of equiaxed randomly oriented grains in the central portion of the casting, Fig. l(b). The equiaxed structure in Fig. l(c) represents the completely grain-refined case where the equiaxed grain size is small. The third type of structure is the most desirable because it imparts a somewhat higher strength for all except high-temperature applications, it reduces segregation of the doping constituent, and it reduces the possibility of hot tearing (the separation of grains due to the melting of a low-melting point constituent in the grain boundaries). In order to obtain fine-grained castings, the nu-cleation frequency must be increased and grain growth must be restricted. Various techniques have been employed for obtaining this end, namely: rapid cooling, vibration, and inoculation of the melt. The success of these techniques depends upon the characteristics of the metal species and on factors controlled by heat transfer through the crucible walls. Recent studies2" have shown that the application of ultrasonic energy to the solidifying ingot is an extremely powerful tool in the improvement of the crystalline structure of metallic castings. Both the mechanical properties and homogeneity of the ingots are improved. Ultrasonic oscillations may affect the crystallization process by 1) permitting subcritical nuclei to agglomerate and thus form nuclei of sufficient size to cause crystallization, 2) changing the state of surface adsorption of various catalysts found in the liquid melt, 3) breaking pieces of solid from the solidified surface near the supercooled region thereby increasing the number of possible nuclei, 4) causing temperature fluctuations to occur in certain parts of the melt thereby increasing the supercooling at specific points in the liquid, and 5) decreasing the critical nucleus size by increasing the pressure at specific points in the melt.' Various investigators have concluded that the effectiveness of the ultrasonic oscillations results from cavitation which disrupts the growing solid-liquid interface The present paper describes the application of ultrasonic oscillations to the crystallization of the semiconductor N-type PbTe. The purpose of this study is to prepare crystalline

Jan 1, 1964

By H. M. Thorne

Oil shale, a potential source of products presently obtained from petroleum, is found in many countries. The most extensive known deposits from the standpoint of potential shale oil in place are those in Brazil and the United States of America. Mining methods used for oil shale range from open-pit operations for shallow deposits to room-and-pillar and longwall techniques for deposits with thick overburdens. Oil shales from different sources vary greatly in the amounts and types of organic and inorganic constituents. By retorting, the organic material is converted to oil, gas, and coke. The largest percentages of oil are obtained from materials having the highest hydrogen content. Over 2,000 retorting systems have been patented, but only a few have been used industrially, and no single process seems best for all types of shales or economic conditions. Shale oils have different characteristics, depending on the source rock and method of retorting. They contain large quantities of olefinic hydrocarbons and more oxygen, nitrogen, and sulfur derivatives of hydrocarbons than most petroleums. Consequently, petroleum refining methods usually must be modified for shale oil. This is particularly true in catalytic processing. Hydrogenation, even under mild conditions, improves shale-oil refinability. Several byproducts may be obtained from both the retorting and refining steps.

Jan 1, 1964

By M. J. Marcinkowski, A. Szirmae, R. M. Fisher

Room -temperature hardness measurements obtained from single and polycrystalline samples of a 47.8 at, pet Cr-Fe alloy which were aged for various times al 500°C show a two-fold increase over that of the unaged alloy after annealing for 1000 hr. A detailed examination of the deformation markings in the neighborhood of the hardness imbressions reveals that twinning becomes an increasingly more important mode of deformation as aging proceeds. this observation is shown to be inconsistent with the Proposals that the transformation is eve of order-disorder On the other hand, the results are in agreement with previous observations of Fisher et al. of a coherent chromium-rich precipitate which forms in an iron-rich matrix as a result of a miscibility gap in this alloy system as proposed by Williams . Using the coherent precipitate hypotlzesis as a model, a detailed analysis of the various possible strengthening contributions to both the slip mid twinning stresses is made. In the case of' slip, lattice friction within the chromium-rich phase and the chemical energy associated with the interface between the two phases contribute about 60pet to the total strength. The contributions from coherency strains and modulus differences are thought to contribute the remaining 40 pet of the strength but are difficult to evaluate because of uncertainties regarding the flexibility of the dislocation line. All of the factors have nearly the same or else a smaller effect on the twinning stress in the aged alloy. Twinning is never observed in the unaged alloy because the twinning stress is much higher- than that for slip. With increased aging times, the various contributions to the total stress for both twinning and slip increase, but most of those for slip increase much more rapidly, so that, in the fully aged alloy, it surpasses the stress for twin propagation. When a twin is nucleated by the chance occurrence of an internal stress concentration during a test, the subsequent twin burst results in a low hardness reading. FeRNTIC Fe-Cr alloys from about 15 to 80 at. pet Cr content show considerable change in properties such as hardness, electrical resistivity, saturation magnetization, and so forth, after aging in the vicinity of 500°C.* The most marked change is a large increase in hardness accompanied by a sharp decrease in ductility, so the phenomenon has often been referred to as the 475°C (885°F) em-brittlement problem. Changes in microstructure are rather subtle and most investigators have not been able to observe any X-ray diffraction or metal-lographic changes during aging. There is little doubt that the phenomenon is inherent to the Fe-Cr binary system and is not directly related to the formation of a phase. Two distinct schools of thought have developed during the past decade concerning this problem. Masumoto, Saito, and sugiharal have concluded, from their own specific-heat measurements, that atomic ordering occurs in this temperature range. Pomey and Bastien2 have also attributed the changes in physical properties with aging in the neighborhood of 500°C to atomic ordering. In addition, Takeda and Nagai3 claimed to have found X-ray verification for superlattices corresponding to the compositions FesCr, FeCr, and FeCr3. However, all known attempts to observe superlattices in Fe-Cr alloys using neutron diffraction, which should be much more sensitive, have been unsuccessful. These have been reported by Shull et al.4 for 25 at. pet Cr, williams5 for 75 at. pet Cr, and Tisinai and samans6 for a 28.5 at. pet Cr. steel. The second and more prevalent opinion ascribes the 475°C embrittlement phenomenon to the formation of a coherent precipitate due to the occurrence of a miscibility gap in the Fe-Cr system below about 550°C. This latter concept was first indicated by the results of Fisher, Dulis, and Carroll,7 who were able to extract fine particles about 200Å in diameter from samples of 28.5 at. pet Cr steels aged from 1 to 3 years at 475°C. The extracted material was found to be nonmagnetic, to have a bee structure with a lattice parameter between that of iron and chromium, and to contain about 80 at. pet Cr. Williams and paxton8 and williams5 confirmed these results and first explicitly proposed the existence of a miscibility gap below the a region in the equilibrium diagram. Alloys aged within this gap

Jan 1, 1964