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By Wheeler P. Davey

When metals are subjected to mechanical working, such as rolling, one of the phenomena that take place is a movement of the crystals of the metal into a system or systems of orientation which bear an angular relation to the direction of working. In rolled metal the crystals may orient themselves with respect to the rolling plane or the rolling direction, or both. Direct evidence of the existence of preferred orientations in rolled metal has been obtained by numerous investigators from X-ray patterns of the rolled metal. Most of these workers used a monochromatic pinhole method. Where the degree of preference for a single orientation is high the monochromatic pinhole pattern may be interpreted by a geometrical calculation based on the angular relationships of the planes in the crystal and the diffraction arcs on the X-ray pattern. This process may be aided by the geometrical construction of the locus sphere (Lagenkugel), and reflection circles of Polanyi,l Polanyi and Weissenberg,2 and Mark and Weissenberg,3 and of the plane polar figures (flachenpolfigur) of Franz Wever.4 R. M. Bozorth5 solves X-ray patterns from metals having a single preferred orientation by means of a series of charts which when placed over the X-ray pattern give directly certain angular relationships, between the crystal planes and the surface of the specimen.

Jan 1, 1930

By H. S. Rankin, F. A. W. Davis, R. A. Laurence, L. L. McMurray, E. C. Houston

This paper is coodensed from several reports by members of the staff of the Minerals Testing Laboratory of the Tennessee Valley Authority, on a series of experimental tests in the beneficiation of barite of the Valley area. These experiments were conducted upon a large number of samples taken from several mines in three different districts. The area contains numerous producing deposits, nearly all of which are hampered by the high iron and silica content of the ores. Because of the small difference in specific gravity between the iron oxide and the barite, a gravity separation is generally poor. The removal of the iron thus offers a special problem. Some of the operators have turned to magnetic separation to meet the shipping requirements for less than one per cent iron. The present experiments were conducted to determine the application of decrepitation or flotation in simplifying the concentration of the barite by removing the iron oxide and silica in one operation. Practically all the barite marketed in the area has been as "off-color" crude. The bleaching studies were made to determine the bleach-ability of the ores to alleviate this inferior grading, placing them on the market as bleached barite. Geology Barite has been produced at many places in the Tennessee Valley area, and prospects and minor deposits are known at many other places, but practically all the production of barite in the Valley has been from the Sweetwater district of East Tennessee. Other leading areas of former production are the Tazewell-Russell counties areas of southwest Virginia, the Del Rio-Stackhouse district of East Tennessee and western North Carolina, and the Fall Branch district of upper East Tennessee. The areas described in this paper are those from which samples used in the concentration tests were obtained.

Jan 1, 1942

By Harold W. Aldrich, Frederick Laist

After a series of experiments covering a period of about three years, extending from the spring of 1912 to the spring of 1915, a 2,000-ton leaching plant for the treatment of the accumulated copper concentrator tailing was built and put into operation. During the experimental period, the first step was that of laboratory experiments or beaker leaches. The results on this small scale were so satisfactory that a small operating plant, capable of handling 5 tons of roasted tailing per day, was installed. Again, the results proved satisfactory and an 80-ton plant was built and operated continuously from August until February, 1913. In this plant, full-sized roasting and leaching units were

Jan 1, 1917

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 H. W. Hitzrot

SEPARATING a mixture of particle sizes of material suspended in a liquid medium is by no means an exact science. Selecting machines for individual classifying operations is even more difficult. The plant operator's own background is of course invaluable, and considerable help may be obtained from technical articles, talks with sales engineers, and handbooks on ore dressing. These several sources of information, however, are difficult to marshal in proper perspective for the major decision on classification units that an operator may be called upon to make. To the present writer's knowledge this assembly of facts is not available in handbooks, and technical papers are scarce on classification equipment developed in the past five or six years. It is believed that this paper will be helpful to users of classification equipment at this particular period in the development of hydro-classification. For easy reference the following classification units now available and in use in metallurgical and industrial operations are listed below, with a brief description of each. Unit-type classifiers, bowl classifiers, and bowl desiltors are all rectangular tanks, slightly tilted, with reciprocating rakes or screws to remove settled sands. The unit-type classifier, Figs. 1 and 2, is available in widths from 14 in. to 20 ft and lengths up to 40 ft. The shallow bowl of the bowl classifier, Fig. 3, equipped with rotating rakes, is superimposed on the lower end of the tank. Reciprocating rake compartments for this design range from 18 in. to 20 ft wide. Bowl diameters vary from 4 to 28 ft. The flat-bottomed bowl of the desiltor, Fig. 4, of relatively large diameter, is equipped with rakes rotating outward and partly over a pit, which is created by extension of the rectangular tank into and under the bowl section. Bowl desiltors are available with reciprocating rake sections 4 to 20 ft wide and bowls from 20 to 50 ft in diam. The bowl desiltor is used for applications beyond the range of the bowl classifier. The hydroseparator, Figs. 5 and 6, is a circular tank equipped with slowly rotating rake arms, set on a slope, with interrupted rake or spiral blades to move the settled solids to a central discharge cone. Tank diameters vary from 4 to 250 ft. Tank depths at center are 2 to 3 ft for small units and up to 25 ft for larger units. Hydraulic classifiers of the sizer and super-sorter types, Figs. 7 and 8, are narrow, deep, rectangular tanks divided by vertical baffles into a series of pockets. Hydraulic water is added near the bottom of each pocket. Perforated constriction plates, spiral flow arrangements, or jets are used to disseminate the water under pressure (hydraulic water) throughout the bed of material in the pocket. Discharge valves on each pocket are operated automatically by a pneumatic mechanism, a pincer-type mechanism, or a pressure control and motor combination actuated by a hydrostatic tube within the pocket. Hydraulic classifiers are available in 4, 5, 6, and 8-pocket units of varying constriction plate areas to suit conditions. There is now a jet sizer of unit pocket design that can be made up in 1 to 25 sections or more to accommodate sizing requirements. The hydroscillator, Fig. 9, is a rectangular tank set on a slope of 3 to 4 in. per ft. A bowl is superimposed on the lower end. The bowl bottom is an oscillating rubber-covered disk, perforated to allow hydraulic water introduced beneath the disk to set up a teeter bed and thus produce an oversize or rake product exceptionally free of slimes, and material minus the mesh of separation. A shallow dam at the periphery of the bowl allows the coarse or oversize fraction to spill over and drop down into the tank compartment, where it is moved up the deck by reciprocating rakes. The material, minus the mesh of separation, overflows a circular and stationary weir which is several inches higher than the dam on the oscillating disk. It is carried off in a circular launder in the usual manner. These units are available in bowl diameters from 4 to 14 ft and with reciprocating rake compartment widths to suit the tons per hour to be handled. Centrifugal classifiers include the solid bowl centrifuge and the cyclone classifier. The solid bowl centrifuge, Fig. 10, consists of a truncated cone fixed to a horizontal shaft and rotating at high speed. An internal spiral rotating at slightly less speed continuously removes solids deposited on the inner surface of the cone, or bowl. Feed enters the cone by means of the hollow center shaft. Overflow leaves through ports at the large end of the cone, and oversize solids, moved by the spiral, exit through ports at the small end. Centrifugal classifiers of this type are available in cone diameters from 18 to 54 in. The cyclone classifier, Fig. 11, is a stationary cone having a cylindrical upper section and a lower cone section. Feed is introduced tangentially into the upper cylindrical section under pressure from a hydrostatic head or by means of a pump. Centrifugal force thus induced effects a classification within the cone, the fine sizes being carried off in the overflow through an opening at the top of the cylindrical section. Coarse solids at relatively high pulp density exit through a control valve at the apex of the lower cone section. Cyclone classifiers are available in 3, 6, 12, 14, 24, and 30-in. diam. The cone classifier, Fig. 12, is a steel-plate cone with sides usually about 60" from horizontal. It contains no rotating mechanism. Feed enters a feed-well at center and classification is effected by gravity and pulp density. Fines are carried off in the flow over a peripheral weir at the top of the cone. Settled solids exit through an opening at the apex. An apex valve actuated through levers and rods by the pulp density in the lower cone section is usually supplied. Diameters are usually maximum at 8 ft.

Jan 1, 1955

By H. F. Yancey, M. R. Geer

The importance of the size composition of coal is reflected in the difference in price of the various sizes of the same coal and in the large number of primary sizes and mixtures of sizes produced by the modern preparation plant to meet the demands of a market that in late years has grown increasingly conscious of coal size. The importance of size in the industrial and domestic uses of coal has its counterpart in the role played by size composition in the laboratory examination of coal. Investigation of many of the physical properties of coal in their relation to its uses requires an evaluation of size composition. In fact, the Standards on Coal and Coke issued by the American Socaiety for Testing Materials in 1936 contains 12 standard methods of testing that involve some use of size composition. The screen analysis is, of course, the standard method of determining size composition, whether the material is coarse run-of-mine coal or fine pulverized fuel. Custorriarily, the analysis is reported as the weight percentages retained on or passing each of a series of testing screens, the number of which may range from only two or three to as many as 20. When more than two or three sieves are used, which is usual, the number of weight percentages obtained is so great as to make the analysis difficult to comprehend. Direct comparison of analyses made 011 the same sieves is hard, and comparison of analyses covering the same range of sizes but made on different sieves is next to impossible. Consequently, a frequent purpose of sizing tests-—-correlation of size with properties and charactcristics related to size-—is rendered difficult. Less cumbersome means of expressing size composition have been attempted with various degrees of success. An average particle size, calculated by any of several formulas, is useful for some purposes, also the weight percentage retained on a single sieve finds some application as a

Jan 1, 1938

By M. R. Geer, H. F. Yancey

The importance of the size composition of coal is reflected in the difference in price of the various sizes of the same coal and in the large number of primary sizes and mixtures of sizes produced by the modern preparation plant to meet the demands of a market that in late years has grown increasingly conscious of coal size. The importance of size in the industrial and domestic uses of coal has its counterpart in the role played by size composition in the laboratory examination of coal. Investigation of many of the physical properties of coal in their relation to its uses requires an evaluation of size composition. In fact, the Standards on Coal and Coke issued by the American Socaiety for Testing Materials in 1936 contains 12 standard methods of testing that involve some use of size composition. The screen analysis is, of course, the standard method of determining size composition, whether the material is coarse run-of-mine coal or fine pulverized fuel. Custorriarily, the analysis is reported as the weight percentages retained on or passing each of a series of testing screens, the number of which may range from only two or three to as many as 20. When more than two or three sieves are used, which is usual, the number of weight percentages obtained is so great as to make the analysis difficult to comprehend. Direct comparison of analyses made 011 the same sieves is hard, and comparison of analyses covering the same range of sizes but made on different sieves is next to impossible. Consequently, a frequent purpose of sizing tests-—-correlation of size with properties and charactcristics related to size-—is rendered difficult. Less cumbersome means of expressing size composition have been attempted with various degrees of success. An average particle size, calculated by any of several formulas, is useful for some purposes, also the weight percentage retained on a single sieve finds some application as a

Jan 1, 1938

By J. D. Pennock

About a year and a half ago, Mr. Morris, an engineer of the Solvay Process Company, was sent to Belgium and France to study the manufacture of coke in the Semet-Solvay ovens, which were in operation at Havre. With complete plans of construction and a good understanding of the methods of running the ovens, he returned to Syracuse. Work on twelve Semet-Solvay ovens was immediately begun. These ovens, with plant for crushing and washing coal, and the necessary condensers, scrubbers, and concentrator for the recovery of the byproducts are nearly finished, and will soon be in operation. As the work approached completion it became necessary to determine what coal should be used. Accordingly, a chemical investigation of the various bituminous coals was made. I. Investigation of Coals. The samples of coal taken for analysis were: I. A sample of Reynoldsville coal that had been exposed to the weather for a year; 11. Reynoldsville coal taken from a car direct from the mine; 111. Morris Run lump coal; IV. Morris Run fine coal; V. Coal from the Fairmount Coal and Coke Company; VI. A special enginecoal from Pardee colliery, Phillipsburg, Pa.; VII. South Fork, Pa., coal; VIII. Coal from Laceyville, Ill.; IX. Pittsburgh bituminous coal from Ocean mines (gas-coal); X. Steubenville, Ohio, coal; XI. Evansville, Indiana, coal; XII. Coal from the Ohio Coal Company. Proximate Analysis. I. 11, 111. IV. V. VI. Water at 90° C.,* ..................................... Volatile,. .. 31.14 33.00 17.73 18.12 37.20 23.86 Fixed Carbon,. . 64.49 58.07 71.92 71.89 56.68 73.00 Ash,. .. 4.37 8.93 10.35 9.99 6.12 3.14 Coke,. .. 68.86 67.00 82.27 81.88 61.88 76.80

Jan 1, 1893

By L. M. Pidgeon

The reactive metals are above manganese on the electromotive series. Their compounds are characterized by large heats of formation and they cannot be reduced from their ores by classical methods. Three general production methods have been used: a) Fused salt electrolysis, b) reduction of a halide by another metal, and c) reduction of the oxide by another metal. Method (a) is highly developed, as in the case of aluminum, (b) in the case of titanium, and (c) has been successful in the case of volatile metals such as magnesium and calcium. It is suggested that future improvements will take place in (a), and particularly in (c), but are rather less likely in the case of (b). THIS year of 1963 is the centennial of the birth of both Charles Hall and of Heroult, the founders of the aluminum industry. Aluminum is the one reactive metal which has reached massive stature in modern industry and perhaps the only such metal to have been produced in any quantity before the turn of the century. It has been joined by others, some on a very modest scale, but all of importance and all of fascinating interest. When invited to give the Fifth Extractive Metallurgy lecture, it seemed appropriate to look back upon the short history of this group to trace the developments which brought extraction methods to their present state and, at great risk, offer opinions as to future trends.

Jan 1, 1963

By E. Goldin, H. J. Juretschke

THE electrical properties of porous conductors have been studied ever since such materials, usually prepared by pressing and sintering of metallic powders, obtained practical importance. In most cases, however, the results have not been easy to interpret because of the great number of independent variables such as powder size, pressure, pressing rate and temperature, subsequent thermal history, porosity, and so on, which enter into the fabrication of industrially desirable materials. In recent years an interpretation of these properties has become of interest because the electrical properties of many new substances, prepared as fine powders by crystallization from the vapor phase or by reactions in the solid state at high temperatures, have to be determined on porous samples formed from the powder. Since theoretically significant information must refer to the fully dense state of the material, it is important to relate the electrical properties measured on such porous samples to those expected for a sample of 100 per cent density. A simple theory for the porosity dependence of the electrical conductivity and the Hall effect was recently proposed by Juretschke, Landauer, and Swanson.' Their model, assuming a distribution of pores of equal size and shape, sufficiently far apart so that each pore is embedded in a region of uni-

Jan 1, 1959

Jan 3, 1950

By C. C. Miller, C. A. Hutchinson, A. B. Dyes

This paper presents a simple and practical method for the estimation of effective permeability and reservoir pressures from the rise in bottom hole pressure when a well is shut in. The equations on which the method is based consider a stabilized well producing from a uniform formation when flow is shut off at the sand face followed by the unsteady state flow of a compressible liquid from regions far from a well to points closer in during the build-up period. An approximation for extending the method for two-phase flow in the reservoir is also presented. In order to compare the effects of extremes in the conditions existing at the external boundary of the reservoir, two general equations defining the build-up characteristics of the reservoir are shown: first, for a reservoir with constant pressure maintained at the radius of drainage, and second, for a reservoir with no influx over the radius of drainage. These equations define the build-up characteristics for the shut-in well as functions of time, the permeability and porosity of the drainage area, the viscosity and compressibility of the fluid flowing, the production rate prior to shut-in, and the radius of drainage of the well. When a well is shut in at the surface, rather than at the sand face, flow will continue into the well bore after shut-in due to the compressibility of the fluids in the bore. The effect upon the build-up characteristics of this flow into the well after shut-in has been studied by means of the electrical analyzer. From the basic relationships and consideration of the limitations due to continued flow after shut-in, methods have been developed for the estimation of the effective permeability of an area from the plot of the build-up characteristics of the well producing that area. Likewise, equations are presented for the estimation of the reservoir pressure from an early portion of the build-up curve. By means of the electrical analyzer, studies have been made concerning the variations in the build-up characteristics resulting from damaged or improved permeability in the immediate vicinity of the well bore. These studies show that the permeability estimated from the build-up curves represents the average effective permeability of the majority of the drainage area and that the permeability in the immediate vicinity of the well does not affect this estimate. Since the major portion of the drawdown is in the immediate vicinity of the well, variations in the permeability of this area greatly affect the productivity of the well as expressed by the productivity index. From pressure build-up and productivity index tests the ratio of the permeability of some arbitrarily specified area immediately surrounding the well and the effective permeability in the majority of the drainage area can be computed. This ratio is a measure of any damage to the well incurred in drilling or reworking and likewise any benefits as a result of remedial measures. In build-up tests and many other tests that are made on a producing well it is at least desirable, if not absolutely necessary, that the well be stabilized prior to testing. A method is presented here for relating the time required to stabilize a well and the reservoir and fluid properties. An equation is also presented for approximation of the length of shut-in time required to obtain sufficient build-up data for the estimation of permeability and reservoir pressure.

Jan 1, 1950

By D. R. Wieland, H. T. Kennedy

The object of the work reported here was to determine the content of elemental sulfur in gaseous methane, carbon dioxide, hydrogen sulfide, and in mixtures of these gases, at pressures and temperatwes encountered in natural gas reservoirs. Sulfur content at equilibrium is reported for pure methane, carbon dioxide, hydrogen sulfide, and on three binary mixtures of each of the three pairs of gases at pressures of 1,000, 2,000, 3,000, 4,000, 5,000 and 6,000 psia and at temperatures of 150°, 200° and 250°F. In addition, the sulfur content of three ternary mixtures at the same temperatures and pressures are reported. The results indicate that the sulfur content is higher in the gases at higher temperatures and pressures. The content is highest in hydrogen sulfide, intermediate in carbon dioxide and lowest in methane. INTRODUCTION At ordinary pressures and temperatures, the concentration of a nonvolatile material, such as sulfur in a gas at equilibrium, is a function of the vapor pressure of the material and is independent of the nature of the gas. As the pressure and temperature increase, the gas assumes some of the properties of liquids, including the power to dissolve other liquids and solids, to an extent dependent on the nature of both the gas and the material dissolved. At equilibrium, the content of sulfur in the several gases considered here may thus be considered as solubilities which are fixed for a given composition of gas, temperature and pressure. The study of the solubility of elemental sulfur in gases is of interest because sulfur is sometimes present in reservoirs producing natural gas and must be present in the vapor phase. Upon reduction of pressure and temperature, the sulfur precipitates from solution in the reservoir and in the tubing and fittings. Due to the fact that the greatest pressure drop in the reservoir is around the wellbore, the volume of sulfur precipitated will be greatest in this locality and can cause a substantial reduction in the permeability of the formation in this area. As the natural gas flows up the tubing string, the pressure and temperature are further decreased, causing further sulfur precipitation. If the volume of free sulfur is large and remedial measures are not taken, complete plugging of the tubing can occur. Knowledge of the content of sulfur as a function of composition, temperature and pressure will enable the operator to determine what changes in pressure and/or temperature are necessary to keep the sulfur in solution. If the sulfur solubility is large and can be controlled, the operator may desire to produce the well at a high wellhead pressure and temperature and reclaim the sulfur at the surface. The high solubility of sulfur in hydrogen sulfide (5.6 per cent by weight at 5,000 psi and 200°F) suggests the feasibility of recovering sulfur by injecting this gas into sulfur-bearing reservoirs and expanding the produced gas to precipitate out the sulfur. The present project was designed to measure the solubility of sulfur in carbon dioxide, methane, hydrogen sulfide and mixtures of these three gases at various temperatures and pressures. These gases were the major constituents of the gas well where plugging by sulfur was encountered. A study of the published literature shows no data on the solubility of sulfur in any gas, although Hannay and Hogarth,' in 1880 reported that it was soluble in carbon disdlide above the critical temperature of carbon disulfide. EQUIPMENT AND PROCEDURE Fig. 1 shows the layout of equipment employed to bring gases to equilibrium with sulfur and to isolate the quantity of sulfur contained in a known volume of gas. Pure gases were measured in the charging bomb at known temperatures and pressures and displaced into the reservoir bomb to make up the desired mixtures. When equilibrium was achieved

By C. G. Dunn, F. W. Daniels, M. J. Bolton

IN recent papers on interface energies in metals¹,² the concept of an equilibrium of forces has been used in the measurement of interfacial tensions. Mathematically the equilibrium of three forces is given by the relations: where the 2's are the interfacial tensions (interface energies per unit area of interface) of three phases or grains meeting at angles 21 22 and 23 (212 relates to the 1-2 boundary formed by grains 1 and 2;223 to the 2-3 boundary, etc.). If these relationships are valid, one can calculate relative values of the interface energies from measured boundary angles on specimens which have been brought to equilibrium. Since Eq 1 may be derived through a mathematical process of minimizing the grain boundary energy under the restriction that the ?'s be independent of boundary orientation: the concepts of surface tensions and equilibrium of forces are not particularly essential. To deal with the general case involving dependence of boundary energy on boundary orientation, it becomes desirable to drop certain concepts formerly held (namely that energy per unit area is identical with force per unit length or surface tension) and to use the energy concept alone. It is appropriate, therefore, to use E in place of ? in deriving and using the more general equations that express the anisotropic nature of the grain boundary energy. Herring3# ' recently has derived the required general equations using the principle of minimization of energy. Specifying the boundary orientations in terms of angles (4) measured with reference to crystal axes within the grains, Herring's equations take the form E23 + E21 cos?8 + E12 cos?2 — sin ?12 + sin?2-?E12/?12 =O [2] where the partial derivatives are measured in the direction of counterclockwise rotation of the boundaries. Eq 2 implies that an infinitesimal displacement of the triple point along the 2-3 boundary produces no change in the boundary energy. Similar equations apply for infinitesimal displacements along each of the other two boundaries. From such equations Herring obtains the following general relationship (1 + E1 E2) sin?8 + (E2 — E1) cos?3 ________ E38______________ = (1+ E2 E8) sin ?1+ (E3— E2) cos ?1 __________^5____________[3] (1 + E sin ?2, + (E1 — E8,) COS ?2 1 E28 where E1 = 1/E23- E25 and PC and c8 have similar expressions. It is apparent that Eq 3 reduces to Eq 1 when the c's vanish. Eq 3 also reduces to Eq 1 when the E'S are all equal. Shockley and Read' have pointed out one limitation to these equations. When E plotted versus 4 appears as an energy cusp, as their theory requires, for example, for the energy near a twin boundary position, then Eq 3 (and therefore Eq 1 also) no longer applies if one boundary is in the minimum energy position. One of the equations of form Eq 2, however, applies if the infinitesimal displacement is along the boundary associated with the energy cusp. From the foregoing treatment it will be apparent that equilibrium angles alone are not sufficient in general for calculating relative interface energies.

Jan 1, 1951

By P. Ramachandrarao, T. R. Anantharaman

EVER since the technique of quenching metals and alloys from the melt (splat cooling) was perfected a decade ago, it has been recognized that the grain size of products solidified by this technique may be extremely small.' The further observation that fcc metals quenched from the liquid state contain very few dislocations has led to the inference2 that metals are subjected to negligible or no stresses during the rapid solidification characteristic of the "gun" or "piston-and-anvil" technique. Evidence for the incidence of appreciable densities of stacking faults has, however, been obtained in case of some splat-cooled fcc and hcp alloys,3 although not for pure metals. In the light of these earlier observations it was considered desirable to study X-ray line-broadening effects, if any, in fcc metals rapidly cooled from the melt. In the present work pure silver (>99.99 pct), aluminum (>99.99 pct) and lead (>99.9 pct) were quenched from the liquid state from temperatures about 50°C above the melting point by the "gun technique" and the resulting foils were subjected to X-ray examination in a Philips Diffractometer. The quenched foils (up to -10 u thick) did not generally stick to the substrate surface and could be easily transferred to the Diffractometer without introducing any plastic deformation. The profiles of the first five reflections from the foils were recorded in each case with Cu Ka, radiation at the slowest available scanning speed of 1/8 deg per min. To correct for instrumental broadening, profiles were also recorded from the metals annealed in vacuo at suitable temperatures. The integral breadths of the X-ray reflections were arrived at by a procedure described earlier.' There was a distinct suggestion of preferred orientation in the recorded intensities of reflections from aluminum and lead foils. Such an effect was not observed in case of silver. In addition, the integral breadths of X-ray reflections from splat-cooled aluminum and lead were not significantly different from those recorded for the annealed metals. The analysis was therefore continued only for silver where the X-ray line broadening was appreciable. The pure diffraction broadening, B, was evaluated for each X-ray reflection (hkl) from silver from the observed, B, and instrumental, b, breadths with the aid of each of the three equations due to Scherrer,5 Anantharaman and Christian,6 and Warren and Biscoe,7 respectively: Bs= B-b BAC=B- b2/B Table I gives the values of particle size, 71, the lattice strain, E, arrived at by the use of the following well-known relations and on the assumption that all observed diffraction broadening could be attributed to lattice strain or particle size, respectively: E = 1/4 cos ? n= B cos ? where A is the wavelength of X-radiation and 0 is the Bragg angle. As no significant peak shifts or asymmetry could be detected in the profiles from the foils, the possibility of any significant contribution due to twins or stacking faults was ruled out. The absence of faults is by no means surprising since pure silver is known to develop stacking faults only on severe deformation and the stacking fault densities recorded so far for even silver filings have been extremely low.' The very low values for percentage mean deviation from the mean value for the particle size in Table I strongly suggest that all observed broadening in splat-cooled silver can be attributed only to small particle size. This conclusion receives further support from the lowest mean deviation recorded for data computed from the Scherrer equation based on Cauchy profiles that are considered characteristic of particle size broadening. Further analysis for separation of particle size and lattice strain effects was considered unnecessary in view of the very large mean deviations obtained for strain values and also the earlier results suggesting absence of even detectable strain in metals and alloys quenched from the melt. It is to be stressed in this connection that the particles are actually grains and not cells formed by walls of high dislocation density usually encountered in deformed samples. As such, the absence of strains is not surprising. The present results are probably the first to record X-ray line broadening due only to small particle

Jan 1, 1970

By R. Maddin, N. Ujiiye

ALTHOUGH the cold-rolled texture for body-centered-cubic metals and alloys is well known (see, e.g., Barrett'), the pole figure representing the texture may be interpreted in two ways. It may be regarded as consisting of several ideal preferred orientations with an associated spread (a view which is shared among several investigators2), or it may be regarded as consisting of two sets of continuous preferred orientation also with an associated spread."." Recently, Chen and Maddin7 noted a stable (001) [loo] end orientation for molybdenum single crystals rolled at low rates of reduction provided the initial rolling. orientation" was close to the cube ori-

Jan 1, 1957

By Joseph Jensen

California's outstanding contribution to unit operation is the plan of development now established for the North dome of the Kettleman Hills. Beginning April 1, 1931, the Kettleman North Dome Assn. will control the unified operation and development of 10,800 acres of proven and semiproven oil land, and at the same time the Standard Oil CO. of California will operate as another unit its fee land of 9460 acres of similar character. The holdings of the two companies are in a checkerboard mile-square pattern. In addition to this, 410 acres of land may yet be included in the Kettleman North Dome Assn. unit and 530 acres of land are definitely out of both units. The owners of some of this land have expressed their intention of cooperating in a reasonable way with these two units. Cooperative agreements are now in force as to most of this field. Under the definitions of a unit pool and a near-unit pool,' the operation at Kettleman Hills will be a near-unit operation, but because of the size of the structure and its proven highly productive character, the arrangement. concluded on Jan. 31, 1931, in the approval of the Kettleman North Dome Assn. Agreement by Secretary of the Interior Ray Lyman Wilbur and by California State Oil and Gas Supervisor R. D. Bush is of outstanding importance to the entire oil industry. No other major unit operation plans are under way in California at the present time. There has been some little discussion of a plan in the North Belridge field and a feeling that the discovery of oil in the Lost Hills field and also in the South Belridge field would necessitate consideration of unit plans. So few data are available for these areas, as to the land that should be included in such unit plans, that little constructive action is now possible. The beginning of drilling on the Middle dome of the Kettleman Hills also makes it an area deserving consideration for unit operation. All four of the above-named areas lie on the west side of the San Joaquin Valley, in Kings and Kern counties, to the south of the

Jan 1, 1931

By G. S. Cole, G. F. Bolling

Recent experitnents on crystal growth have indicated that thermal convection in the liquid influences the conditions of solidification and subsequent crystal characteristics. However, the important columnar-equiaxed transition in castings has not been examined as a function of this free convection. An experiment is presented here to demonstrate a change in the transition as convection is suppressed. Lead- and tin-based alloys were cast in stainless-steel molds either without special procedures or with thin grids placed horizontally across the tnold diameter in portions of the castings. While the grids allowed some diffusion of heat and mass transport to occur during solidification, massive fluid flow was hindered in the vegiotz of the grids. A larger percentage of columnar grains appeared in the grid region than in other parts of the special castings or than in all regions of normal castings. This structural difference can be explained in terms of thermal convection. THERE is little information about the possible effects of natural convection which may occur during the solidification of a casting. Ruddlel-3 has stated that the movement of liquid metal produced by convection might assist in the transfer of heat, but in the absence of confirmatory evidence he suggested that this idea be treated with caution. chalmers4 considers, but does not assess, the importance of fluid motion in casting, while Tiller5 suggests that, in liquid metals which have extremely high thermal diffusivities, the effects of thermal convection may be negligible. In addition, throughout the literature, there are statements indicating the possible presence of thermal convection but without proofs or evaluations of its influence. Natural convection may be divided into two categories: thermal convection, where liquid flow is due to density differences caused by temperature gradients in the liquid (e.g., liquid near a cold wall falling with respect to hotter liquid further away from the wall); and solute convection, where flow is due to density differences as a result of concentration gradients, see Wagner.6 In most instances thermal convection predominates over solute convection. Nevertheless, even thermal convection has not been studied in any detail and is difficult to handle, since it can vary quantitatively from one experiment to another depending upon the exact positions of heat sources and sinks or the attitude of the container with respect to gravity. In spite of these difficulties it is possible to realize that a higher rate of heat transfer must result with convection than in any situation where conduction acts alone. Thus, the degree of increased heat transfer is the important undecided question in considerations of casting. It will be demonstrated here that a reduction in convective flow leads to a suppression of the columnar-equiaxed transition in a casting and that this suppression is related to a decrease in the degree of heat transfer. Fortunately it is possible to do this by comparative rather than quantitative measures. The insertion of horizontal plates or grids into a simple mold does not appreciably influence heat transfer per se, but in reducing the allowable height through which colder liquid may fall freely it reduces natural thermal convection. This leads to a reduced fluid velocity, a different flow pattern, and an altered heat transfer which can be measured. EXPERIMENTS The alloys were prepared from elements of 99.9 pct nominal purity and cast into an uncoated 2-in.-diameter stainless-steel mold insulated at the bottom with a suitable refractory so as to ensure predominantly radial heat flow during freezing. Casting was performed either in empty molds or in molds containing grids or plates in various configurations . The grids were constructed of aluminum screen (1/32 in. thick) which was cut to the desired shape, cleaned in aqua regia, and coated with a mixture of 2 parts aqua dag graphite -1 part Sauereisen cement mixture, thus supplying a hard, protective, and insulating layer approximately 0.006 in. thick. The

Jan 1, 1965

By Richard G. Warren, Michael M. Minor, Gayle J. Thomas

INTRODUCTION Los Alamos Scientific Laboratory (LASL) initiated its effort in the Hydrogeochemical and Stream Sediment Reconnaissance (HSSR), a part of the Department of Energy (DOE) National Uranium Resource Evaluation (NURE) program, in late 1975. Since that time, LASL has completed sampling of the Rocky Mountain states of New Mexico, Colorado, Wyoming, and Montana at a density of about one water or waterborne sediment sample per 10 km2 and has sampled about 85% of Alaska at a density of at least one per 25 km2. Analytical results for these samples are reported by National Topographic Map Series (NTMS) quadrangle. All collection and analytical procedures have been standardized from the outset (Sharp, 1977; Sharp and Aamodt, 1978). Until early 1979, only uranium results were reported for these samples; thereafter, results include analyses for at least 42 additional elements in the sediment samples. Each LASL HSSR report also includes a discussion of the relationship of these analytical data to known or possible uranium resources; more recently, these data have been re- examined for their relationship to resources for other metals (Beyth et al., 1980; 1980a). Analytical results for LASL HSSR sediment samples are both comprehensive, including 43 elements, and precise, allowing close inter-comparison of data between quadrangles. A recent HSSR study shows that elemental concentrations in sediment samples from the Dixon Entrance quadrangle in Alaska are insensitive to the choice of sieve size fraction and do not vary significantly between stream locations a few meters apart, except for extremely high elemental concentrations (Warren, et al., 1980). Elements that are particularly reproducible include thorium, hafnium, and the .ram earth elements. Fortunately, sensitivities for these elements, which are often associated with uranium, are excellent by the nondestructive analytical technique of neutron activation analysis that LASL employs. Wet chemical techniques may not always give reliable results for these elements in sediment samples due to the difficulty of dissolving the resistate mineral phases that normally contain these elements. LASL has recently open-filed results for a large number of NTK3 quadrangles; to date analyses have been reported for about 605 of the quadrangles within the states of the Rocky Mountain region. As a result, uranium analyses am now complete for all sediment samples collected from the state of Wyoming. We have chosen to sumnarize the analytical results for Wyoming and portions of adjoining states hereafter termed "the ~ Wyoming regionn (Fig. 1 ) ; nearly 24 000 uranium analyses and nearly 17 000 analyses for 42 additional elements are available for sediment samples collected from this area. The DOE open-file report numbers are shown in Fig. 1 for reports open filed before September 1, 1980. The Wyoming region provides an ideal area for an examination of regional geochemical patterns ex- hibited by sediment samples. It is endowed with a variety of exposed geologic units and with widely distributed uranium districts associated with host units of several ages. However, discussion will focus on rock units of Eocene and Precambrian ages because they are widely exposed and host the majority of the uranium resources within the region (Fig. 2). Miocene units are also widespread and host mineralization in the Brown's Park Formation (Fig. 2). Epigenetic uranium mineralization occurs in sand- stones of lower Eocene age such as the Wasatch, Battle Springs, and Wind River Formations whereas vein type mineralization occurs in Precambrian crystalline rocks. Precambrian rocks within the region consist of a variety of granitic and meta- morphic rocks with l .4-2.8 billion year ages, except within the Uinta Arch, where they consist of a sequence of very low grade metamorphosed or unmetamorphosed 1.0 billion year old sedimentary rocks. Precambrian rocks have served as sources for much of the clastic material comprising the lower Eocene units, and may also have provided the source for the uranium in mineralized Eocene or Miocene sandstones (Stuckless, 1979). The remainder of this paper describes the relationship of elemental concentrations in HSSR sediment samples to exposures of Eocene and Precambrian rocks. The results are used primarily to determine where these Precambrian rocks might provide the most suitable uranium source areas and to infer the direction of transport toward adjacent depositional basins during the Eocene.

Jan 1, 1980

By J. L. Walter

Extra-low carbon iron sheet, when deformed and annealed, undergoes exaggerated or abnormal grain growth in the critically deformed regions of the sheet. This exaggerated pmth occurs, for low strains (3 to 6 pct), only in sheet which has a fine dispersion of precipitates in the subsurface region of the sheet and fewer and coarser precipitates in the sheet interior. These particles have been identified as manganese sulfides. Wing the anneal, grains near the surface are gvowth-inhibited by the fine particles but the grains in the interior are free to grow normally. With the additional driving force provided by the strain energy, the interior grains first grow into the small subsurface pains. Eventually, these growing grains grow completely through the sheet. Calculations of limiting grain sizes at various values of strain indicate that a volume fraction of precipitates in excess of 10-' would be required to eliminate exaggerated growth in material strained to 10 pct. OPEN-COIL annealing has made decarburization of sheet steel both efficient and economically practical. Use of such material for porcelain-enameling stock is one of many possible applications of low-carbon iron since carbon in steel is deleterious to porcelain-enameling properties.' However, the extra-low carbon iron presently available presents another problem, that of exaggerated grain growth in regions where the sheet has been deformed as by bending or stretching. In exaggerated grain growth a few grains start to absorb their neighbors and these may become very much larger than the average grains of the sheet. Other names for exaggerated grain growth are coarsening, critical grain growth, secondary recrystallization, abnormal grain growth, or discontinuous grain growth. While this grain growth does not affect the enameling qualities of the low-carbon iron sheet, their presence results in a marked reduction of tensile-yield strength in the region of the sheet containing the large grains. The loss of tensile yield strength may render the material unsuitable for many applications . This report describes the results of a study undertaken to determine the cause of the exaggerated grab growth in extra-1ow carbon iron and, if possi- ble, to prescribe practical procedures for its prevention. GENERAL THEORY The driving force for exaggerated grain growth is the grain boundary free energy. This driving force is proportional to (l/rl + l/r2) where rl and r2 are the mutually perpendicular radii of curvature of the boundary between the growing grain and the grain being consumed. Thus, the greater the difference in size between the growing grain and the matrix grains, the higher the driving force for grain growth. If, however, the matrix grains are free to grow simultaneously, the driving force for exaggerated growth will be diminished. Stability toward growth of the matrix grains may be caused by a) a strong single orientation texture (texture inhibition),' b) a dispersed second phase,3"5 c) the thickness effect,' or d) intergranular segregation.7"9 As exaggerated growth occurs when growth of the matrix grains has been slowed by the stabilizing processes mentioned above, there must be an additional factor acting to promote growth of a few of the grains to the point where they are enough larger than the matrix grains that boundary energy driving forces are sufficient to cause continued growth. For instance, at the annealing temperature, growth-inhibiting inclusions may slowly dissolve and coalesce. Eventually, a grain boundary becomes unlocked and migration occurs at the expense of neighboring grains. Or, an additional driving force may be supplied to some of the grains if the material is strained. Then, since some grains will be strained less than others, the difference in strain energy between adjacent grains may be sufficient to overcome boundary locking and allow growth of the grains with lower strain energies. In the present study, therefore, such factors as the presence or absence of dispersed phases, the nature of the exaggerated growth, and the effect of strain have been considered. EXPERIMENTAL PROCEDURE I) Material and Processing. Three types of low-carbon iron were used in this study; types A and B were commercial grades, each from a different supplier.* The precise details of the processing of

Jan 1, 1963