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By David W. James, Howard Jones, George M. Leak

Conditions are described for producing, by primary recrystallization, a matrix suitable for the growth of large grains near (110)[001] orientation in silicon iron strip by secondary recrystallizaliun in a steep temperature gradient. The orientation distribution of these large grains is expressed in terms of rotational deviations about the cross-rolling direction, the rolling direction, and the normal to the sheet, the deviational spread increasing in that order. With the aid of cowplenientary published data on the orientation dependence of growth rate, it is shown that this observation is consistent with the oriented-growth theory of recrystallization lextures. It is conclutled that growth-rate and orientation-distribution data obtained in a steep thermal gradient should be used with caution to account for isothermally Produced recrystallization textures. SEVERAL authors have reported methods of growing large grains by re crystallization of a small-grained matrix in silicon iron 1- B and pure a cr The present study was a preliminary in the growth of single crystals and bicrystals for surface relaxation," grain boundary mobility, and grain boundary diffusion studies. The method was to control the growth of a seed crystal into a suitable primary re crystallized matrix by feeding through a steep temperature gradient. The driving energy for growth derived from the grain boundary energy released as the seed crystals grew into the matrix. Thus, stability of the matrix against normal grain growth was considered to be essential for success. It was known that the manganese sulfide dispersion present in commercial silicon iron performs this function during secondary recrystallization to the (110)[001.] texture.12 Hence commercial, rather than high-purity, material was used throughout. The paper describes the growth conditions for grains large enough to be used as seed crystals for further growth into single crystals. The orientation distribution of the seed crystals is analyzed and its significance for the theory of recrystallization textures is discussed. EXPERIMENTAL PROCEDURE Strip material was supplied by the Steel Co. of Wales, Ltd. The chemical analysis in weight percent was Si, 2.90; C, 0.015; Mn, 0.059; P, 0.011; S, 0.027; Ni, 0.032; 0, 0.009; Fe, balance. A gradient furnace of similar design to one described previously4 was loaned from B.I.S.R.A. It consisted essentially of a vertical water-cooled copper slot projecting downwards into the hot zone of a molybdenum furnace. Hydrogen was passed through the furnace to protect both heating element and specimen from oxidation. Strip specimens up to 8 cm wide and 0.2 cm thick were sealed into the furnace at the mouth of the copper slot. A coating of light oil on the strip surface maintained the seal during translation of a specimen. The maximum temperature gradient in the region just below the copper slot was 500°C per cm over 1 cm, with the hottest point controlled at 1175°C. Several large grains would usually grow by secondary recrystallization from the primary matrix when a specimen was immersed in the hot zone for about 30 min. A back-reflection X-ray camera was constructed to facilitate rapid and accurate orientation determinations of the large grains produced. It was possible to reproduce a standard geometry, with regard to strip and camera, without the tedium of careful alignment on each occasion. Specimens, typically 4 cm wide and 75 cm long, were cut with the longitudinal axis parallel to the rolling direction of the original strip. The surfaces were cleaned by immersion alternately in a hot aqueous solution containing 2 pct hydrofluoric acid plus 10 pct sulfuric acid and in cold 10 pct nitric acid. The nitric acid etch was just sufficient to reveal the grain structure. Rolling and annealing treatments to prepare the matrix (discussed below) were followed by growth of seed crystals in the gradient furnace. The matrix was transformed to a single crystal by growth of a selected seed crystal connected to the matrix by a thin neck. 4,5 Growth was promoted by controlled feeding into the gradient furnace. Several single crystals of controlled orientation were grown successfully from seed crystals by twisting the interconnecting neck in a reorien-tation jig.4 EXPERIMENTAL RESULTS AND DISCUSSION Growth Conditions. A suitable matrix for growth of large grains was prepared starting from primary re-crystallized strip 1.9 mm thick. This was cold-rolled in two stages each being followed by a recrystallization anneal at 800°C for a few minutes. Such treatment gave the required growth matrix only if the two cold-reduction stages were each performed in several passes and in the following ranges: the first, 30 to 70 pct; the second, 10 to 50 pct. Immersion in the temperature gradient otherwise resulted in an equiaxed

Jan 1, 1967

By C. F. Seaman, R. G. Clay

The mines of The Tennessee Copper Co. are in the Ducktown Basin, in southeastern Tennessee. The ore is a heavy sulphide consisting principally of chalcopyrite, pyrite and pyrrhotite and in places running as high as 95 per cent sulphur and iron. Operating mines are the Burra Burra and Eureka. Development ' of the Boyd ore body was started in 1940. Late in 1939 the decision was made to change from fuse and cap to all electric blasting and at the same time electric cap lamps were installed to replace carbide. These changes were made to improve the safety and working conditions in the mines. Both the Bureau of Mines and explosives manufacturers recommended electric blasting as a safety measure. Until that rime, electric blasting had been used only for shaft sinking and in places where it was absolutely essential for safety. Very few men had had experience in this type of blasting, as the places where it was required were those that also required direct supervision. It was necessary for the mining staff to work out methods, procedure, and equipment to be used. In this they were ably assisted by representatives of the explosives manufacturers. Many mistakes were made and it is the purpose of this paper to describe the original plan and installation, show the major difficulties encountered. the remedies applied, and present the practices now being followed. Comparison of costs of the two methods will also be discussed. About six months were required to make the change and eliminate fuse and cap blasting entirely. The first electric blasting stations were installed in November 1939 and the last fuse was taken underground in May 1940. A very unusual condition forced the use of fuse for a short time in one heading after May, but that will be discussed later. Original Equipment and Installation A power line is generally recommended as a source of current where permanent blasting stations are used. The plan worked out for electric blasting was to tap 220-volt alternating-current lines when they were available and use 250-volt direct current from the trolley wire at all other places. A blasting machine would be available at each shaft for places where there were no regular blasting stations and could be used if a regular station should fail. The equipment decided on was No. 16 duplex reinforced lamp cord for lines to within about 50 ft. of the working place and No. 20 lead wire from that point to the shots. An open double-pole, double-throw switch with slate base was put in the circuit, so connected that the down position would close the line to the shots 2nd the up position would connect it to the Iine from the power contactor. This switch was located in the circuit as close to the blast as was safe (should the shots explode when it was placed in the shooting

Jan 1, 1943

By R. G. Clay, C. F. Seaman

The mines of The Tennessee Copper Co. are in the Ducktown Basin, in southeastern Tennessee. The ore is a heavy sulphide consisting principally of chalcopyrite, pyrite and pyrrhotite and in places running as high as 95 per cent sulphur and iron. Operating mines are the Burra Burra and Eureka. Development ' of the Boyd ore body was started in 1940. Late in 1939 the decision was made to change from fuse and cap to all electric blasting and at the same time electric cap lamps were installed to replace carbide. These changes were made to improve the safety and working conditions in the mines. Both the Bureau of Mines and explosives manufacturers recommended electric blasting as a safety measure. Until that rime, electric blasting had been used only for shaft sinking and in places where it was absolutely essential for safety. Very few men had had experience in this type of blasting, as the places where it was required were those that also required direct supervision. It was necessary for the mining staff to work out methods, procedure, and equipment to be used. In this they were ably assisted by representatives of the explosives manufacturers. Many mistakes were made and it is the purpose of this paper to describe the original plan and installation, show the major difficulties encountered. the remedies applied, and present the practices now being followed. Comparison of costs of the two methods will also be discussed. About six months were required to make the change and eliminate fuse and cap blasting entirely. The first electric blasting stations were installed in November 1939 and the last fuse was taken underground in May 1940. A very unusual condition forced the use of fuse for a short time in one heading after May, but that will be discussed later. Original Equipment and Installation A power line is generally recommended as a source of current where permanent blasting stations are used. The plan worked out for electric blasting was to tap 220-volt alternating-current lines when they were available and use 250-volt direct current from the trolley wire at all other places. A blasting machine would be available at each shaft for places where there were no regular blasting stations and could be used if a regular station should fail. The equipment decided on was No. 16 duplex reinforced lamp cord for lines to within about 50 ft. of the working place and No. 20 lead wire from that point to the shots. An open double-pole, double-throw switch with slate base was put in the circuit, so connected that the down position would close the line to the shots 2nd the up position would connect it to the Iine from the power contactor. This switch was located in the circuit as close to the blast as was safe (should the shots explode when it was placed in the shooting

Jan 1, 1943

By Leo J. Vogel, E. D. Hummer

INTRODUCTION by E. D. HUMMER An efficient refuse-disposal system is a necessary part of the modem cleaning plant. The large-scale refuse system and disposal area, engineered for the lifetime of the plant, has become more important due to the greater tonnages of refuse produced from increased quantities of mechanically mined and prepared coal. Laws and increased government regulations have affected the design and operation of disposal systems. THE EFFECT OF MINE AND PLANT OPERATION Refuse disposal starts at the mining face. The mining system, the type of roof support, the machinery used, and the degree of discipline at the face contributes to the amount and type of refuse that must be removed through the disposal system. Economies gained through modification of the mining system or mining machinery may be partially offset by increased dilution of the mined coal with impurities from associated rock formations. In some cases the change in the mining system and equipment has reduced the dilution. In all cases the ratio of impurities that must be removed from the raw-coal feed to the plant not only affects the maintenance and operating costs of the plant, but greatly affects the design of the refuse disposal system. The design of a mine and plant should include the location and the estimated capacity of the disposal areas for the life of the property or plant. Complete evaluation of the disposal system and an estimate of its annual cost of operation over the life of the property or plant should be incorporated in the plant and mine evaluation. Plant design should be as simple as possible, consistent with the efficient production of clean coal. Material transfer points, crushing, screening and pumping operations should be kept to a minimum to reduce degradation and the subsequent increased difficulty and cost of refuse removal. The maintenance of good process control by operating management will result in a minimum of misplaced material in both refuse and clean coal. Reduction of misplaced float material in the plant refuse is an important factor in preventing combustion in the refuse storage pile. THE REFUSE DISPOSAL AREA Combustion in refuse piles occurs when air enters the pile in sufficient quantity to support oxidation. At certain rates of air in-filtration, the heat produced by the oxidation process is not dissipated and temperature rises.

Jan 1, 1968

By R. H. Olds, B. H. Sage

The formation volume and volume of the liquid phase of oil and gas obtained from four fields in the San Joaquin Valley have been investigated at pressures, temperature, and gas-oil ratios comparable to those encountered in underground reservoirs. All the fields covered in this investigation yielded a product of a gas-oil ratio in excess of 5000 cu ft per barrel and the gravity of the tank oil for the four fields in question varied between 52° and 63' API. The results of the investigation, together with analytical data concerning the composition of the oil and gas, are submitted in tabular form. Rough correlations of the formation volume as a function of pressure, temperature, and gas-oil ratio and of the retrograde dew-point pressure as a function of gas-oil ratio, temperature, and gravity of tank oil are presented. It was not found feasible to correlate simply the formation volume of the liquid phase as a function of the applicable variable. It is desired to emphasize that these correlations are considered applicable only to the range of conditions covered in this investigation and for systems of similar nature and composition. Introduction Information concerning the physical properties of mixtures of oil and gas from particular fields have often been employed in predicting the situations obtaining in underground reservoirs. One of the earlier studies of this nature was the work of Beecher and Parkhurst,1 while a more recent study of the Dominguez Field2 presented detailed volumetric data in the two-phase as well as in the single-phase regions. Although these studies were confined to individual fields, their results proved of value in application to other fields. It has recently been shown 3,4 that it is possible in the region of low gas-oil ratios* to correlate the volumetric behavior of naturally occurring hydrocarbon mixtures from a single geographical area with sufficient accuracy to be of industrial value. For this reason it is considered of interest to submit information concerning the volumetric behavior of oil and gas mixtures from four different fields in the San Joaquin Valley and, in combination with similar published data5 concerning mixtures of oil and gas from the Paloma field in the same area, to show rough correlations between the composition and the behavior of materials from these fields. This effort seems particularly worth while since all of the

Jan 1, 1947

By R. H. Olds, B. H. Sage

The formation volume and volume of the liquid phase of oil and gas obtained from four fields in the San Joaquin Valley have been investigated at pressures, temperature, and gas-oil ratios comparable to those encountered in underground reservoirs. All the fields covered in this investigation yielded a product of a gas-oil ratio in excess of 5000 cu ft per barrel and the gravity of the tank oil for the four fields in question varied between 52° and 63' API. The results of the investigation, together with analytical data concerning the composition of the oil and gas, are submitted in tabular form. Rough correlations of the formation volume as a function of pressure, temperature, and gas-oil ratio and of the retrograde dew-point pressure as a function of gas-oil ratio, temperature, and gravity of tank oil are presented. It was not found feasible to correlate simply the formation volume of the liquid phase as a function of the applicable variable. It is desired to emphasize that these correlations are considered applicable only to the range of conditions covered in this investigation and for systems of similar nature and composition. Introduction Information concerning the physical properties of mixtures of oil and gas from particular fields have often been employed in predicting the situations obtaining in underground reservoirs. One of the earlier studies of this nature was the work of Beecher and Parkhurst,1 while a more recent study of the Dominguez Field2 presented detailed volumetric data in the two-phase as well as in the single-phase regions. Although these studies were confined to individual fields, their results proved of value in application to other fields. It has recently been shown 3,4 that it is possible in the region of low gas-oil ratios* to correlate the volumetric behavior of naturally occurring hydrocarbon mixtures from a single geographical area with sufficient accuracy to be of industrial value. For this reason it is considered of interest to submit information concerning the volumetric behavior of oil and gas mixtures from four different fields in the San Joaquin Valley and, in combination with similar published data5 concerning mixtures of oil and gas from the Paloma field in the same area, to show rough correlations between the composition and the behavior of materials from these fields. This effort seems particularly worth while since all of the

Jan 1, 1947

By D. A. Elgillani, S. Atak, D. A. Rice, M. C. Fuerstenau, R. B. Bhappu

Quartz and feldspar cannot be floated with sulfonate at any pH; spodumene floats over a narrow acid pH range, while beryl responds moderately over a broad pH range. After wet-grinding in a steel mill, beryl, quartz, and spodumene float well with sulfonate below about pH 7, whereas the improvement in the response of feldspar is not so marked. A mechanism by which iron can be adsorbed on these minerals is presented. Also, the responses of leached, natural, and wet-ground beryl to amine, sulfonate, and oleate flotation are shown and related to the measured zero-points-of-charge of these materials. Earlier work with leached beryl showed that good flotation could be obtained with alkyl aryl sulfonate over a rather wide pH range using a Fagergren flotation cell.' When a similar response was observed with leached quartz, it was decided that unintentional activation was being obtained from the metallic components of the Fagergren cell. To obviate this difficulty, a microflotation cell was designed, and an experimental technique was devised. These have been described elsewhere. Experiments conducted with the small cell showed that leached quartz could not be floated at any pH with any sulfonate addition,3 which is in agreement with the observations of Kraeber and Boppel.4 Similarly, it was also found that leached beryl responded to sulfonate flotation only over a narrow pH range rather than the broad range reported earlier.1 This early work,1 however, revealed the important effect that wet-grinding in a steel mill has on the flotation response of certain silicates. That is, it was found that quartz and especially beryl floated well over an unusually wide pH range after wet-grinding in a steel mill. Microcline, however, floated poorly below pH 4, even though wet-ground under the same conditions. The work of Eigeles6 on adsorption of oleic acid on leached quartz and iron-contaminated quartz at constant pH is in agreement with these flotation data. Other research has shown that ferric iron, added as a salt to the system, functions as an activator in the narrow pH range in which Fe +++ iron hydrolyzes to its hydroxy complexes.3,5 These phenomena indicate that iron functions differently in flotation systems depending on its method of introduction. The object of this paper is to determine the mechanism by which iron is adsorbed on certain minerals, the mechanism of collector adsorption after iron abstraction, and the role that Fe++ and Fe+++ assume in the selective separation of these minerals. EXPERIMENTAL MATERIALS AND METHODS Sodium alkyl aryl sulfonate, mol wt 450,7 pure potassium oleate, and pure dodecylamine were used as collectors. All other chemicals were reagent grade in quality, i.e., n-amyl alcohol as frother; HC1, H2SO4, and KOH for pH adjustment; and ferric chloride as activator. Conductivity water, made by passing distilled water through an ion exchange column, was used in the experimental work. All minerals used in the investigation were hand-picked specimens. Sample Preparation: Each of the minerals was crushed through 8 mesh, and the product was divided into two groups, one to be ground dry and the other wet. Dry grinding was accomplished with an alumina mortar and pestle. The product was dry-screened to 48 x 150 mesh, cleaned magnetically, deslimed in conductivity water, and dried. Preparation of the samples by wet-grinding involved grinding a 200-g charge of the mineral (-8 mesh) at 60% solids with natural water in a mild steel rod mill for four minutes. This charge was then wet-screened immediately with natural water to 48 x 150 mesh, dried, and cleaned magnetically. Some experiments were also conducted with leached beryl and quartz. These products were prepared by leaching the sized sample (48 x 150 mesh) with concentrated HC1 with a percolation technique until no iron could be detected in the leach liquor. Following this step, the sample was rinsed with conductivity

Jan 1, 1967

By F. Bahnemann

IN discussing the problem of abnormal magnetic polarization, C. A. Heiland1? emphasized the unfortunate fact that our knowledge of the geological and physical conditions relating to such occurrences is very limited and that a more detailed insight into their physical causes would be extremely valuable for interpreting measured anomalies. He also pointed out that to arrive at quantitative physical formulas that would express the conditions that cause abnormal polarization many more occurrences of the kind would have to be recorded. The first part of this paper is a contribution to such descriptions.

Jan 1, 1935

By L. A. Geoffrion, R. H. Perkins, J. C. Biery

Densities of cerium metal and several lour-melting binary cerium alloys were measured over the range 25° to 800°C. A rolumeter, using NaK as working fluid, was used to obtain the data. The cerium, Ce-Co, Ce-Ni, and Ce-Cu alloys all exhibited an increase in density on melting, while a Ce-Mn alloy expanded on melting. FOR the proper design of a nuclear reactor, the change in density of the fuel with temperature must be known. This is especially important in a system utilizing molten fuel, such as LAMPRE (Los Alamos Molten Plutonium Reactor Experiment), since a relatively large change in density usually occurs during the solid-liquid transition. The fuel for LAMPRE is a Pu-2.5 wt pct Fe alloy with a melting temperature of 410°C. However, limitations in reactor design with this fuel have led to consideration of other plutonium-containing alloys for use in future generations of this type of reactor. Several ternary alloys containing plutonium and cerium as two components have satisfactorily low melting points. The system that at the present time appears to be most acceptable is Pu-Ce-Co; it exhibits little change in melting temperature with wide variation in plutonium concentration. Other alloys that have received some consideration contain nickel, copper, and manganese as the third constituent. The proposed fuel alloys are difficult to handle experimentally in the 25" to 800°C temperature range since they oxidize readily, react with many solvents, and contain a poisonous fissionable material. In addition, in this temperature range the alloys pass through the solid-liquid transition. Several techniques are available for measuring the densities and volume coefficients of expansion of solids or liquids. However, the only apparatus that appears suitable for measuring expansion coefficients over this temperature range and through the phase transition is a volumeter. In a volumeter, the indicating medium must be essentially inert to and insoluble in the material being studied. It must also possess a low vapor pressure over the operating temperature range, and its coefficient of expansion must be accurately known. One material that is satisfactory in nearly all of these respects is the alloy Na-78 wt pct K, which melts at -10°C and has a vapor pressure of 860 mm Hg at 800°C. This relatively high vapor pressure at 800°C requires an overpressure of an inert gas to prevent boiling. While a volumeter is capable of determining accurately the volume coefficients of expansion of materials, it cannot be used for absolute density measurements. Therefore, a density determination at a known temperature must be coupled with the volumeter measurements to give all the desired data. The weight-loss technique using immersion in bromobenzene at room temperature proved to be satisfactory. The preliminary work that was done on this experimental program involved developing and calibrating the equipment, and measuring the densities and volume coefficients of expansion of cerium and some low-melting binary cerium alloys. The complications that are caused with the introduction of plutonium into the system were avoided until the equipment was proved to be satisfactory and until experience was gained in its operation. It is this first phase of the experimental work that is described in this report. DESCRIPTION OF EQUIPMENT AND OPERATING PROCEDURE The NaK volumeter is shown schematically in Fig. 1. Basically, the equipment consists of two weld-sealed stainless-steel containers of nearly identical volume. One container holds a tantalum crucible and the specimen being measured; the other contains a tantalum crucible and a tantalum specimen used as a control reference material. To avoid temperature gradients, the bombs are located in a copper block inside the furnace. Stainless-steel capillaries of equal length and volume connect each stainless-steel container to a glass viewing capillary. The stainless-steel containers, stainless-steel capillaries, and a portion of the glass capillaries are filled with NaK (22 wt pct Na-78 wt pct K). The NaK/gas interface in the glass capillary is viewed with a cathetometer which is accurate to *0.5 mm. The cathetometer readings are used to calculate the volume changes of the samples during a run. This volumeter is basically the same as that described by F. Knight in Plutonium 1960. 2 However, changes in equipment design and operating procedure were made to eliminate some major operating difficulties. These changes are summarized below. 1) In filling the manometer with NaK, gas was frequently entrained in the system. Evacuation of the system before filling failed to eliminate the en-

Jan 1, 1965

By W. Rostoker

Single isothermal sections were constructed for the titonium-rich corners of the systems Ti-Fe-O, Ti-Cr-O, and Ti-Ni-0 with a view to locating the shape and disposition of the ternary intermediate-phase fields for the compounds isomorphous with Fe3W3C. IN a previous note,' it was reported that a group of ternary intermediate phases existed which occurred in the general composition range Ti,X,O-Ti&O where X was one of the following elements: copper, nickel, cobalt, iron, or manganese. In two instances, binary intermediate phases occurred (Ti²Cu and Ti²Ni) which appeared to be isomorphous. The X-ray diffraction patterns of the phases could be indexed on a cubic lattice whose cell edge was of the order of 11 kX. Karlsson2 stated that the line extinctions and line intensities indicated that these phases were isomorphous with Fe³W³C and therefore belonged to the space group Oh. This author also noted that no unique phase of this type occurred at the composition Ti,Cr,O. This latter statement was accepted as true at the time the previous technical note was written.' However, work continued along these lines and that reported here has shown that a phase isomorphous with Fe³W³C does exist in the vicinity of the composition Ti³Cr³O but not at or near Ti4 Cr²O. The lattice parameter of this phase was found to be 13.01 kX. Metallographic examination of both as-cast and annealed specimens of these supposed ternary oxide phases disclosed structures which were far from single phase in many instances. It was considered a point of some interest to locate more positively the composition coordinates of the single-phase fields. To this end, single isothermal sections for the systems Ti-Fe-O (1000°C), Ti-Cr-0 (1000°C), and Ti-Ni-0 (900"C) were constructed. Phase relationships were studied by both X-ray diffraction and metallotrra~hic methods. Allovs were prepared as 10 g buttons by melting in a noncon-sumable electrode, water-cooled copper crucible arc-melting furnace using a helium atmosphere. Oxygen was introduced quantitatively by the use of weighed amounts of TiO² or TiO. Iodide titanium and the purest available alloying metals were used. All results are discussed in terms of the nominal composition of the melts. Previous experience with making oxygen-rich alloys had shown that oxygen losses were not significant if a homogeneous melt was produced. Weight-loss measurements were used to check loss in metallics during melting. Anneals were conducted in evacuated Vycor bulbs, and annealing times ranged from 24 hr at 1000 °C to 48 hr at 900°C. To achieve equilibrium in certain sluggish alloys, seven-day anneals were used. Debye-Scherrer powder patterns were taken in a 14 cm diam camera using filtered CuK radiation (K² = 1.541232 kX; K., = 1.53739 kX). Specimens were prepared by crushing and screening previously annealed buttons. In general, the X-ray diffraction results were used to identify the major phases, while the metallographic examinations were more useful in indicating the number of phases present. By the use of the combined results and general fundamental rules governing ternary equilibrium, it was possible to construct isothermal sections in good detail. In some instances where auxiliary lattice-parameter data were available, it was possible to lay down tie lines and to locate more positively corners of three-phase fields. Isothermal Section of the System Ti-Fe-O at 1000°C The binary systems Ti-O³ and Ti-Fe4 have been published. Binary phases, TiO, TiFe, and TiFe2, are likely to be encountered in the titanium-rich corner of the system. The structures are NaCl (Bl), CsCl (B2), and MgZn, (C14) types, respectively. Although preliminary X-ray diffraction studies indicated the presence of a ternary phase in the composition range Ti,Fe,O-TiJ?e,O, metallographic examination of two specimens at these compositions revealed the presence of other phases. Thirty-eight alloys were used to delineate the phase boundaries of the isothermal section illustrated in Fig. 1. The five almost single-phase ter-

Jan 1, 1956

By Joseph W. Leonard

Evidence is presented to show that certain coals can be super-cleaned, using present coal preparation processes, to reduce sulfur below levels that are commonly believed to be possible. The evidence points to the need to develop continuous sorting methods by which coal coming from a mine can be segregated so that different raw coal types can be processed separately to produce a super-clean coal in addition to coals cleaned to more common levels of sulfur. Evidence is presented and techniques discussed that may be applicable for making the method feasible.

Jan 1, 1976

By J. B. Newkirk, R. W. Hendricks, R. Baro

STUDIES of the kinetics of precipitation in binary alkali halide systems are of interest from a theoretical point of view, because of the possibility of controlling diffusion rates by additions of aliovalent impurities. This note reports some preliminary results of a study of the kinetics of precipitation of AgCl from supersaturated solid solutions of AgCl in NaCl containing trace amounts of divalent cation impurities. In their study of the system NaC1- AgC1, Stokes and Li1 derived the phase diagram containing a mis-cibility gap with a broad maximum at approximately 170°C. They found that single crystals quenched from above the miscibility gap and aged at various temperatures within the two-phase region gradually turned light blue, then cloudy white, and finally opaque. The rate of transformation depended markedly on the aging temperature. The light-blue color in the early stages of aging was interpreted to be the result of Rayleigh scattering from precipitated particles less than 0.1 µ in diameter. These qualitative observations have been confirmed by us. However, a more precise tool was needed in order to quantitatively follow the growth kinetics of the precipitate particles. Because of the suspected small size of the precipitate particles and for other reasons, small-angle X-ray scattering was thought to be a suitable technique for this study. Small-angle X-ray intensities scattered from powder specimens were recorded on a General Electric XRD-5 diffractometer using the four-slit geometry described by Neynaber, Brammer, and Beeman.2 The slits were 0.08 mm wide by 10.00 mm high. It was found that, with very careful alignment, meaningful data could be obtained to within 3 min from the middle of the direct beam. Chromium radiation (?Ka = 2.29Å) was used in order to spread the scattered intensity to a relatively high angle, as indicated by Eq. [1]. A specimen containing 21.0 at. pet AgCl was prepared by melting analytic reagent-grade AgCl and NaCl under a chlorine atmosphere in a vycor cap-

Jan 1, 1964

By W. M. Robertson

The rate of crack Propagation thvough a solid meta1 in the presence of a liquid metal has been calculated. The crack is assumed to propagate by solution of the solid in the liquid under the influence of an applied stress, with volume diffusion of the dissolved solute through the liquid controlling the propagation. The calculated velocities can be tens of centimeters per second or higher. THE embrittlement of normally ductile solid metals by liquid metals has been the subject of extensive study, as summarized in the book by Rostoker, McCaughey, and arkuus.' In experimental studies of liquid-metal embrittlement it is usually concluded that the observed crack-propagation rates are too high to be accounted for by diffusion processes. Diffusion is considered to be an unimportant factor and various other mechanisms are invoked to account for the experimental observations. The similarities of liquid-metal embrittlement to stress-corrosion cracking, to hydrogen embrittlement of steel, and to low-temperature embrittlement of bcc metals are frequently used as analogies for these mechanisms.1"3 The present paper assesses how rapidly a crack could propagate by a mechanism of volume diffusion through the liquid metal. We assume that the crack propagates by solution of the solid in the liquid at the crack tip under the influence of the applied stress and diffusion of the dissolved solute away from the crack tip. The model uses only macroscopic thermodynamic, kinetic, and elastic concepts. The calculations indicate that this dissolution-diffusion mechanism can give high crack velocities. In some previous treatments4'' of crack propagation in a liquid-metal environment the fundamental step has been the breaking of atomic bonds at the crack tip. The liquid greatly decreases the energy necessary to break these bonds. The present model assumes the crack is filled with liquid metal; the presence of the liquid is essential because diffusion through the liquid is assumed to control the rate of propagation. With proper modification this model could also apply to stress corrosion in a liquid environment. THEORY Consider a crack in a homogeneous elastic continuum, ignoring all the structural details of the solid. This neglects a host of metallurgical details which can be significant in the problem of liquid-metal embrittlement;' but this simple assumption is a useful approach in evaluating the role of diffusion through the liquid. The stress distribution around the crack tip establishes a gradient in the chemical potential at the tip, which causes a diffusion flux through the liquid away from the tip. The solid-liquid interfacial tension works against crack propagation, since propagation requires creation of interfacial area. From these two considerations we derive the diffusion flux, which then yields an expression for the velocity of the crack tip. The concentration of the solute in the liquid, C, is equal to the equilibrium concentration in the presence of an unstressed, flat surface, Co, plus the excess concentration due to the stress, AC(a), plus the excess concentration due to capillarity, AC(y): We calculate AC(o) and AC(y) and then obtain the diffusion flux. Consider (Fig. 1) a long flat crack of length 2L, thickness 2r, and tip radius r, where r remains constant as the crack propagates in the positive x direction. There is no stress ay in the y direction across the flat surfaces of the crack. The magnitude of the stress at the crack tip due to the applied stress, a,, is given by the relation6 ^=^[l-2^] 12] which, for long narrow cracks, becomes The stress increases the chemical potential in proportion to the strain energy.? The excess chemical potential due to the stress, Ap(a), is given by where 52 is the atomic volume of the solid and E the Young's modulus. Inserting Eq. [3] gives Now consider the crack to be filled with a liquid metal. The excess solubility due to stress, hC(a), is given by the excess chemical potential due to capillarity, Ap(y), is given by8 where y is the solid-liquid interfacial energy, and v1 and YZ are the two principal radii of curvature of any surface point. At the crack tip, r1 = -r and vz = m, so TRANSACTIONS OF THE METALLURGICAL SOCIETY OF AIME

Jan 1, 1967

By Donald P. Bellum, Lee Nugent

Southwestern Utah is well known for its scenic attractions. The beauties of Bryce Canyon, Zion Canyon and the Grand Canyon are of world renown. Thusly, Cedar City is known, at least by the local Chamber of Commerce, as the Gateway to the Utah Parks. However, of the thousands of tourists flocking to Utah's many points of interest by way of Cedar City, few realize that any mining takes place in the vicinity, in spite of the fact that iron mines have been in continuous operation for 40 years. The Pinto-Iron Springs Mining District is only 15 miles west of Cedar City, and is the largest iron ore producing district in the West. In recent years, the shipments have ranged from 2% to 4 million tons per year making Utah the fifth-ranking state in iron ore production.

Jan 11, 1963

By L. A. Willey

Although the interierometric method for the determination of length changes was devised by Fizeau more than three quarters of a century ago, it has not achieved the widespread use in the metallurgical field that its precision and simplicity would seem to warrant. The interferometer and the basic principle are both very simple. When optically plane surfaces held at a very slight angle to each other are illuminated by monochromatic light, rectilinear, equally spaced interference fringes arc formed. Each fringe corresponds to a defiuitc thikness of the wedge formed by the optical flat.;. The difference in wedge thickness between two consecutive fringes is cqual to one half the wave length of the illuminating light. Instruments for vicwing the intertero~ncter have passed through a number of modifications. Outstanding among the improvements were those Abbe. in 1884. His improved instrument permitted micrometric mcasurements to the order of one-hundredth of the width of an interference fringe (i.e., lengths were measured to the order of one two-hulldredth of the mave length of light ). It also permitted the consecutive use of light of several wave lengths. which made possible the determination of the order number of any fringe and therefore the absolute thickness of the wedge at any point. The Abbe dilatometer and methods of measuretment, including corrections to he applied for the change of index of refraction with change in tempcrature and barometric pressure in an air wedge, have been thoroughly described by Pulfrich.' Pulfrich2 made further improvements in the interference measuring apparatus. His instrument embodied all the features of the Abbe dilatometer but was made more versatile by its complete mechanical separation from the interferorneter. The introduction of an Amici prism in the piece permitted the simultaneous observ tion of the whole set of fringe systems developed in the interferometer from the visible light of a geisler tulle. .Also, the introduction of a direct-vision, reflecting prism made it possible to set the fringes parallel to the two vertical fiducial line. of the instrument without the necessity of rotating the interierometcr. Interferometric methods employed ill this country have been developed and dcscribed by Priest, Pelers and Cragoe," Austin,5 Merritt,= Saunders,? and Nix and MaNair. Since none of these authors used the type of instrument that was employed in the present investigation, they Will not be discussed here. This paper will be limited to the description of the interfernmetric apparatus and method used at the Aluminum Research Laboratories and to the presentation of data so obtained. Apparatus and Procedure A general view of the dilatometer, not including equipment for controlling and

Jan 1, 1945

By D. L. Feucht, R. L. Longini

The semiconductor heterojunction is considered in terms of simple models which may lead to an understanding of move complex heterojunctions. Metallurgical and electrical properties of hetero-junctions aye discussed including the interface structure, energy -band diagram, and carrier transbovt across the interface. It is found that in a heterojunction all mechanisms such as injection, tunneling, and junction recombination found in simple junctions play modified voles. INTERFACES between materials (grain boundaries, the electrical junction between two differently doped materials in a single crystal, the oxide-metal interface, or metal-metal junctions) are of considerable importance in many situations. These various interfaces all have one very fundamental thing in common. Quantum mechanically speaking, the wave functions of the electrons in one material may penetrate the other material but, in general, only to the extent of angstroms. From an electrical point of view the conduction mechanism changes as a current passes through such junctions. In some cases the change is tremendous, in others almost negligible. The interface, then, is the locus of a change of conduction mechanisms. Some of these, particularly in semiconductors, are well-understood. The ordinary p-n junction in a single crystal can be the locus of an injection mechanism or a tunneling process, depending on conditions. The mechanisms are probably best understood in semiconductors because of the possible simplified view of particlelike conduction. The bands are either nearly filled or nearly empty and band overlap is seldom involved. The same fundamentals are probably important in other situations too but they are very difficult to look at naively. Although the simple look at the semiconductor case only gives us a relatively rough picture which must then be refined, the other systems, which involve a more complex situation, immediately are in many ways too difficult. There are too many initial choices of complex systems and therefore it is not possible to be even reasonably certain of any one model. Because of the relative simplicity of semiconductors, their good and controllable structure, and because of the ability to make many measurements on them not normally available to either metals or insulators! they are probably the best understood materials. It is therefore desirable to use them as a tool to further the understanding of interfaces in general. Semiconductor-heterojunction concepts were first proposed by kroemer1 in 1957. This was followed several years later by reports on the fabrication and experimental characteristics of heterojunction structures by Anderson2 and Diedrich and jotten.3 I) THE HETEROJUNCTION STRUCTURE To get down to hardware, when we refer to a semiconductor heterojunction we imply that there exists an intimate contact between different semiconductor materials. We could put two pieces of material together, complete with oxide layers, we could remove the oxides, or we could even melt the interface and hopefully get wetting and a good "bond" on solidifying. In fact we could by some means grow a crystal of one material using the other as a seed. Essentially we are interested only in the last two because they are the simplest to look at analytically. The degree of perfection of fit varies greatly and is reflected somewhat in the arc welder's joint strength. The lattice match of the two materials, their orientation, and so forth. is obviously necessary for a good bond but so is the continuity of any polar bonds which are involved such as in the III-V semiconductors. The mechanical misfit between two similar lattices can be described in terms of edge dislocations. The edge-type dislocations must be very close together for the usual misfit and there must be dislocations for each of several different Burger's vectors in order to produce a lattice match. The .'dangling bonds'' resulting will be involved in producing interface charge. Order of magnitude estimates of the charge density extrapolated from low densities of dislocations in homogeneous materials give 5 x 1013 cm-2 Ge-Si and 1 X 1012 cm-2 Ge-GaAs electronic charges. Edge dislocations also act as very active recombination centers between holes and electrons. One lattice "matching" difficulty usually exists even if two structures have essentially the same lattice constants as they will have different coefficients of therma1 expansion. Thus, on cooling from the usually high temperature of fabrication to room temperature, dislocations are produced, a good fit not existing at both temperatures. In brittle materials this shrinkage may even result in cracking. For the Ge-Si interface the mismatch is about 2 x 10 -6 per degree whereas it is less than 10"7 per degree between germanium and GaAs. The exact effect of the misfit is dependent on the thickness of the materials involved. For a very

Jan 1, 1965

By C. B. Post, D. G. Schoffstall

A determinatioil of the hydrogen content of molten steel by means of the Vacuum-extraction method, as reported here, consists in first casting a sample of the bath in a bomb, so that the gases evolved during solidification are trapped for analysis. A portion of the cast steel sample is then prepared and heated at a temperature of 600" to 800°C. under high vacuum, and the gaser given off during this vacuum extraction (which are shown to be hydrogen), are collected and measured. Analysis of the gases evolved on solidification and the gases in the solid sample enables an accurate determination of hydrogen in the molten steel. Fig. I shows the bomb and accessories that have been found suitable for trapping the gases evolved on solidification. The bomb is made of scamless steel pipe, approximately 7 in. long by 136 in. i.d., and welded at the bottom. An ordinary pipe cap has a vacuuni-type metal stopcock threaded and brazed in its upper end. This pipe cap fits onto the bomb by means of machined threads. A flange is brazed to the pipe at the point where the cap starts to tighten up, and a rubber gasket is placed between the flange and cap. Heavy vacuum grease is used between the flange and gasket and the gasket and cap. The weight of the complete bomb and it? interval volume is known before the sample is cast. In practice, a sample of about 400 grams of steel is poured into the bomb, the funnel quickly swung out of the way, the bomb cap spun down the threads and tightened against the gasket, and the bomb set in a pail of water to keep the gasket and vacuum grease cool. It is estimated that at least 80 per cent 01 the gases evolved from the liquid sample during solidification are trapped in the bomb."

Jan 1, 1945

By H. L. Hartman

The drop tester has proved an invaluable tool for the investigation of percussion drilling in the laboratory in "slow motion". It has allowed the process of rock penetration by impact to be studied a single blow at a time. In the present work, the relation of cratering to indexing has been determined under conditions simulating those in the bottom of the hole at atmospheric pressure. Indexed blows form craters which are influenced by others adjacent to them. Two unique effects are involved: (1) the provision of additional free faces in proximity to the point of impact and (2) the creation of subsurface damage by the previous blow(s). Both have a pronounced influence on the volume of rock removed per blow, which governs the rate of penetration in actual drilling. The emphasis in this study was placed on determining effects of index distance and impact energy on crater volume when blows were struck on a previorusly "drilled" or damaged surface, a situation most representative of down-hole conditions. The results indicated that (I) the optimum index distance on a damaged surface is greater than on a fresh, undamaged rock surface; (2) the volume of rock broken at optimum index distance is about the same for both surface conditions with die-shaped chisels but tends to be greater on a cratered surface with wedges; (3) the optimum index distance and maximum crater volume are proportional to the energy level; (4) at a given energy level, the volume of rock broken by dies generally exceeds that by wedges; and (5) maximum crater volume varies, approximately, inversely with width of die but is nearly independent of included angle of wedge. INTRODUCTION This is the third of a series l,2 of papers reporting on one phase of a continuing program of drilling research being conducted in the Rock Mechanics Laboratory at The Pennsylvania State U. The phase under consideration is crater geometry — blow energy relations in percussion drilling. While the previous papers have discussed mainly craters produced by single blows, indexed-blow studies are the subject of this paper. The basic mechanism of drilling under study here — that of penetration of a chisel-shaped bit subjected to impact — is the one employed in probably 90 per cent of all rock drilling in mining, percussion drilling. It also forms the fundamental action in nearly all oil well drilling with the so-called rotary (roller-bit) method. Here, the action is more complex, however, and may in actuality comprise rotary-percussion drilling. Certainly, the down-hole air and mud hammer drills, which superimpose percussion on rotation, belong in this latter category. In any event, impact blows constitute one of the principal mechanisms in the vast majority of drilling, mining or petroleum, and it is essential in drilling research to study percussion in all its basic aspects. Percussion drilling can be simulated in the laboratory by means of an impact drop tester. Striking one blow at a time with chisel-shaped bits, the drop tester permits study of most of the parameters in the drilling process except blow frequency and the interrelationship of certain variables. Single-blow craters, the simplest to produce, allow the determination of basic relationships, such as volume vs blow energy; while indexed craters most closely resemble the action in real drilling and provide data for the establishment of optimum operating criteria. Indexed-blow craters are those which are influenced by others in proximity. The simplest case to visualize, and the one studied in detail here, is that in which a given crater is formed adjacent and parallel to a previous crater, such that the second crater breaks into the first. A more complex situation usually exists downhole, where indexing is achieved by rotation of a radial-winged or rolling-cutter bit. But, admittedly, the phenomenon of indexing is more likely to be understood eventually if it is first studied in its simplest form, that related to parallel craters. Limited research has been conducted on indexed blows. The most complete study was that by Simon, 3,4 who proposed universal indexing curves to relate the important variables. His work, however, was conducted entirely with rows of craters formed on a

By Henry Rogatz

Oil.—During the year 1938, there were 434 oil wells drilled in the Texas Panhandle, increasing the daily initial production by 192,706 bbl. —that is, 229 fewer oil wells drilled than in the previous year, with a decrease in total daily initial production of 129,626 bbl. The total daily potential of the field on Dec. 1, 1938, as determined by the Texas Railroad Commission, was 1,250,645 bbl., an increase of 210,663 bbl. over the previous year. On Dec. 1, 1938, the daily allowable of 82,466 bbl. was assigned to the field to be produced from 3931 wells. The total amount of oil produced for the year was 23,227,170 bbl. The total proven productive area includes 148,298 acres. This is 30,248 acres more than for last year, and represents a more accurate calculation of the areas and not new discoveries. Gas.—There were 103 gas wells drilled during 1938, having a combined open flow of 3,166,300,000 cu. ft.; that is, 65 less than the number of wells drilled in 1937, with a decrease in the open flow of 3,144,488 cu. ft. per day. Pipe-line Gas.—The pipe-line companies withdrew 230,307,854,000 cu. ft. of gas (a daily average of 630,980,000 cu. ft.). The total withdrawals by pipe line decreased 5,624,481,000 ft. from that of 1937. Natural Gaso1ine.—Throughout the greater part of the year, 46 gasoline-extraction plants processed 1,376,186,000 cu. ft. per day, a total of 502,308,010,000 cu. ft. for the year. This gas yielded about 275,875,000 gal. of natural gasoline. The total daily capacity of all the plants is 2,519,500,000 cu. ft. During the latter part of 1938, one of these plants was shut down, leaving 45 plants operating at the close of the year. Carbon Black.—Thirty carbon-black plants operated during 1938, burning 266,881,000,000 cu. ft., or a daily amount of 731,180,000 cu. ft. This produced approximately 400,000,000 lb. of carbon black. During the year one plant was dismantled and two plants were shut down.

Jan 1, 1939

By Henry Rogatz

Oil.—During the year 1938, there were 434 oil wells drilled in the Texas Panhandle, increasing the daily initial production by 192,706 bbl. —that is, 229 fewer oil wells drilled than in the previous year, with a decrease in total daily initial production of 129,626 bbl. The total daily potential of the field on Dec. 1, 1938, as determined by the Texas Railroad Commission, was 1,250,645 bbl., an increase of 210,663 bbl. over the previous year. On Dec. 1, 1938, the daily allowable of 82,466 bbl. was assigned to the field to be produced from 3931 wells. The total amount of oil produced for the year was 23,227,170 bbl. The total proven productive area includes 148,298 acres. This is 30,248 acres more than for last year, and represents a more accurate calculation of the areas and not new discoveries. Gas.—There were 103 gas wells drilled during 1938, having a combined open flow of 3,166,300,000 cu. ft.; that is, 65 less than the number of wells drilled in 1937, with a decrease in the open flow of 3,144,488 cu. ft. per day. Pipe-line Gas.—The pipe-line companies withdrew 230,307,854,000 cu. ft. of gas (a daily average of 630,980,000 cu. ft.). The total withdrawals by pipe line decreased 5,624,481,000 ft. from that of 1937. Natural Gaso1ine.—Throughout the greater part of the year, 46 gasoline-extraction plants processed 1,376,186,000 cu. ft. per day, a total of 502,308,010,000 cu. ft. for the year. This gas yielded about 275,875,000 gal. of natural gasoline. The total daily capacity of all the plants is 2,519,500,000 cu. ft. During the latter part of 1938, one of these plants was shut down, leaving 45 plants operating at the close of the year. Carbon Black.—Thirty carbon-black plants operated during 1938, burning 266,881,000,000 cu. ft., or a daily amount of 731,180,000 cu. ft. This produced approximately 400,000,000 lb. of carbon black. During the year one plant was dismantled and two plants were shut down.

Jan 1, 1939