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By C. C. Nitchie, G. S. Brooks

With the gradual depletion of the natural-gas pools of the Kansas district, together with the uncertainty of further cheap fuel developments, some of the western zinc companies turned to the coal fields, attracted by their permanency and the success of the Matthiessen & Hegeler Co. and the lllinois Zinc Co. Being then confronted with the problem of using a relatively high-priced fuel, although the ultimate supply was very great, the fuel economies of the kilns and furnaces became of far more importance, and the more modern equipments, as a result, embodied distinct gaias in this phase of the business. In addition, there have been some pronounced advances in the actual making of gas from these coals. Increased efficiency in gas making has contributed its hare to lowering costs and those plants located in the higher priced fuel districts have probably been obliged to study these economies somewhat more closely. Naturally, many beneficial changes have resulted in both practice and apparatus in these sections. On certain western coals, for instance, the actual saving in fuel consumption has been 50 per cent. By this is meant that, where about 1.75 tons were burned to smelt 1 ton of oxidized ore, 0.7 to 0.9 ton is now required. While comparisons by T. R. Ingalls1 of fuel economies in smelting in this country and Germany before the war may, in general, be correct, they do not appear to do justice to the more progressive American practice. It is doubtful whether German plants were substantially bettering these fuel ratios. Data furnished by Bender and Frams do not afford records averaging less than 0.9 ton coal per ton ore on materials from 40 per cent. to 50 per cent. zinc. Fuels As producer fuel, Illinois, Indiana, and Kansas coah offer a wide range of material, although varying much in their amenability to gasscation. The proper fuel for each plant can only be determined after com-

Jan 1, 1920

By D. L. Ritter, N. J. Grant, B. C. Giessen

Forty-six alloys covering the complete concentration range of the Nb-Rh system were examined by metallographic and X-ray methods; solubility limits of terminal ad intermediate phases and transformation and solidus temperatures were determined. There are nine intermediate phases; two eutectic, five peritectic, two eutectoid, and three peritectnid reactions were encountered. The experimental methods and the constitution diagram are described in Part I. Part 11 deals with the crys -tallography and relation of the intermediate phases. The Nb-Rh system was selected for study for three reasons: first, it was hoped that the anticipated similarity of the Nb-Rh phase diagram to the Ta-Rh1 and Ta-Ir2 diagrams treated earlier (see also Ref. 3) and to the Nb-1r4 diagram treated simultaneously would allow a crystallographic and comparative evaluation of the intermediate phases in these related systems; second, it was likely that the previous experimental methods could be carried over without significant change; and third, it was expected that the interesting mechanical properties of the a1 phase of the Ta-Rh and Ta-Ir systems would also be encountered in similar phases of the new systems, and that these phases could be investigated more closely. The phase diagram had not been treated fully in the literature; only brief surveys of some intermediate phases were found.5-7 It was attempted to cover the details of the phase boundaries, Part I, as well as to present the crystallography of the intermediate phases, Part 11. EXPERIMENTAL METHODS Specimen Preparation and Treatment. The following high-purity starting materials were used. 1) Niobium powder, 99.8 pct pure, mesh size -60 +200, from Wah Chang Corp., Albany, Ore. The analysis furnished by the supplier showed the following major impurities: Ta, <500 ppm; Zr, <500 ppm; 0, 300 ppm; Fe, 280 ppm; Ti, <I50 ppm; W, Si, <100 ppm; C, N, 30 ppm; all other impurities, <30 ppm. 2) Rhodium powder, ground sponge, 99.9+ pct pure, mesh size -80, from J. Bishop Co., Malvern,

Jan 1, 1964

By J. H. Nead

The experiments herein described were undertaken with a view to investigating thoroughly the influence of carbon on the tensile and impact physical properties of carbon steel. The original comprehensive plan included investigation of a series of steels with varying carbon contents over a wide range of heat treatments. These were to be studied as to their static tensile qualities, and also their resistance to shock as measured by the Charpy impact bending test. A thorough metallographic examination was likewise included in the schedule. The Charpy tests and the metallographic examination have not been completed to date, and are accordingly withheld for another report. All heat treatments, however, have been made, and the static tensile tests have been completed. A description of the procedure of the experiment and the results thus far obtained are therefore reported herein. Conclusions No attempt is made to draw general conclusions from these experiments, but the curves and the data are submitted as being of general importance and wide applicability. Composition of Materials An attempt was made to secure steels increasing in carbon by increments of 0.1 per cent. from 0.1 per cent. up to 0.8 per cent., and from that composition to 1.6 per cent. by increments of 0.2 per cent. Actually, however, steels of the composition given in Table I were procured, and as the carbon contents were arranged sufficiently well so that satisfactory curves could be drawn showing the relation between carbon content and other properties, these steels were used in the experiments.

Jan 1, 1916

By Emmanuel P. Papadakis

Ultrasonic velocity measurements have been made to study the preferred orientation in cube-textured copper. Methods applicable to thin specimens were employed since the specimens were necessarily of sheet material. The measured velocities in various directions in the sheet differed from the corresponding values in single-crystal copper by 1 to 6 pet. The distribution of the deviations indicated that the align-ment of the (001) planes with the rolling plane was better than the alignment of the [100]and [010] directions with the rolling and transverse directions. Ultrasonic pole figures (velocity us orientation) are shown to be useful in the study of preferred orientation. THIS paper describes one set of experiments in a continuing study of preferred orientation in worked metals. This study has been undertaken to investigate the fundamental properties of metals when used as propagation media for ultrasonic waves. Many such materials are of current or potential use in ultrasonic delay lines. Fundamental studies on ultrasonic propagation parameters such as velocity, attenuation, and diffraction (beam spreading) are of importance in the design of delay lines, in the development of nondestructive testing methods, and in the study of materials themselves. Preferred orientation in worked poly-crystalline metals influences all three above-mentioned parameters, and hence is of particular importance. When polycrystalline metals are subjected to mechanical working, they develop textures dependent upon their crystal structure and the symmetry of the working operation.&apos; The texture consists in the alignment of the crystallographic axes of the grains in preferred directions with respect to the symmetry axes of the working operation. Since the grains are elastically anisotropic, the elastic moduli of worked metals are anisotropic. Hence the velocities of elastic waves in worked metals depend on the directions of propagation and polarization. The worked metal may be thought of as taking on the elastic symmetry of a single crystal: so it possesses the same number of independent elastic moduli as the crystal class it simulates. In general, a worked metal does not adopt the crystalline symmetry of its own grains. For instance, most rolled sheet becomes effectively orthorhombic while all bar stock and wire develop hexagonal symmetry. However, certain metals with cubic crystal structure develop a cube texture upon rolling and annealing.= Nearly perfect alignment of [100]-type directions with the rolling direction, transverse direction, and rolling-plane norma1 can be achieved in certain fcc metals and alloys. These cube-textured rolled metals provide an excellent opportunity to test preferred orientation by means of elastic waves, since a worked metal with 100 pct cube texture would have elastic moduli identical to the moduli of its constituent metal. It is the purpose of this paper to present the results of an investigation upon cube-textured copper. Ultrasonic waves were used. The methods of measurement and the experimental results on the effective moduli will be given. The ultrasonic measurements will be shown to complement X-ray pole figures for the determination of preferred orientation in worked metals. EXPERIMENT To study cube - textured material, it was necessary to use thin-sheet material since a severe reduction in gage (95 to 99 pct) is necessary to produce cube texture. Special ultrasonic methods were needed to investigate the thin material at megacycle frequencies. A) Materials. The cube-textured material tested was a copper alloy containing 1 pct Zn. Specimens already measured for Young&apos;s modulus4 by Alers were kindly supplied by him. The specimens were slabs 3.00 by 0.25 in. cut from sheet 0.047 in. thick. The orientations of the long axes of the specimens with respect to the rolling direction were taken in 15-deg steps from 0 to 90 deg. B) Measurements. Two distinct experiments were performed to measure the phase velocity in these specimens. One measured the shear wave velocity for propagation in the 0.25-in. direction and polarization in the 3.00-in. direction. The other measured the velocity of both shear and longitudinal waves propagating in the thickness direction in the sheet. 1) Plate-Mode Measurements. The velocity of the zeroth-order shear mode5 was measured in the 0.25-in. direction in each strip. The specimens were ground thinner over half their length to assure that the first-order shear mode would be cut off below 6 Mc per sec, leaving the zeroth-order nondispersive shear mode as the only propagating mode. Piezoelectric ceramic transducers of 5 Mc per sec resonant frequency poled in their long direction were solder-bonded to the edges of the thin part of the slabs as in Fig. 1 after these edges had been made flat and parallel by fine grinding. These transducers produced waves polarized in the 3.00-in. direction and propa-

Jan 1, 1967

By K. M. Kolobova, E. Z. Kurmayev, A. Z. Menshikov, S. A. Nemnonov, V. A. Trapeznikov

The present work represents a review of our intestigations into the X-ray spectra of solids, which have been carried out by us along two lines of upproach: 1) St@ of the electronic structure of high -rnelting compounds of transition metals; 2) stzddy of the interatomic binding forces by the fine structure of absorption spectra under varying temperature and concentration conditions. With this in mind, int>estigations hare been made into the emission and absorption spectra of the K-series of atoms of transition elements in alloys and compounds. In the problem concerned with the electronic structure of high-melting compounds of transition metals, considerable importance is attached to the question of ascertaining the role played by 3d4sp electrons of metal and 2p electrons of metalloid in the formation of chemical bonds and of giving, on the strength of this data, an explanation of the properties which seem to be contradictory at first sight: good conductivity inherent in metals and high brittleness and high-melting characteristics typical of covalent compounds. Over the last few decades this question has attracted the attention of many investigators whose studies were devoted to this type of compound. Many works, both of theoretical1-3 and experimental4- l5 nature , have contributed much to the elucidation of the physical character of the phenomenon referred to. Alongside the investigations in the field of electric resistance, Hall effect, paramagnetic susceptibility, electronic heat capacity, and the temperature of transformation into a superconducting state, we should particularly emphasize the studies on X-ray spectra, which have played a significant role in the development of the zonal theory for high-melting compounds. This fact has become highly evident after the theoretical calculation of the energy spectrum has been made and the density of states curve in Tic, TiN, and Ti0 has been plotted by Ern and Switendick3 who used the method of augmented plane waves. Correlation of the results of the theoretical calculation of the band structure in the compounds listed above with the data obtained by X-ray spectroscopy studies showed that X-ray spectra can be a source of valuable information on the electronic structure of high-melting compounds within a wide range of ener- gies. It is well known that X-ray emission spectra basically give a direct picture of the occupied excited states above the Fermi level of a solid (valence band, conduction band) and that the absorption spectra (region of initial absorption) give a similar picture of states corresponding to the unoccupied levels near the Fermi surface. Full information on the density distribution of electronic states by energies can be obtained by combining the emission and absorption spectra. Such an opportunity arises from investigation

Jan 1, 1970

By H. I. Aaronson, C. Laird

The kinetics of thickening and of lengthening of ?&apos; plates in an Al-3.93 pct Cu alloy in the temperature range 203" to 300" C were determined by means of transmission electron microscopy. The rate of thickening was found to be less than that allowed by volume diffusion control at all temperatures, by amounts which increased with decreasing temperature, in agreement with the predictions of a general theory of precipitate morphology.1 Thickening was treated on the basis of the ledge mechanism. Ledges were deduced to spread across the broad faces of ?&apos; plates at volume dzjrfusion-controlled rates, as anticipated from the disordered structure of their edges. Lengthening of 8&apos; plates, on the other hand, took Place more rapidly than allowed by volume dzjrfusion. This occurred despite clear morPhological evidence of a bmrier to growth at the edges of these plates. It was concluded that the misfit dislocation structure comprising the barrier requires that lengthening take place by a jog mechanism. The tnisfit dislocations, however, also serve as diffusion short circuits, and allow high overall lengthening rates to be achieved. In Part I&apos; it was shown that, within the range of aging temperatures and times studied, the broad faces of 8&apos; plates formed in Al-4 pct Cu are fully coherent with the a, matrix. Virtually .all of the dislocations present in these faces were found to have developed as a result of plastic deformation in the a phase. Such dislocations are thus "intruders", rather than the more usual misfit-compensating variety. The edges of 8&apos; plates were confirmed, by extension of the earlier studies of Mat-suura and Koda,3 to be made up of edge-type misfit dislocations, in sessile orientation with respect to lengthening of the plates. These interfacial structures should cause 8&apos; plates to thicken and to lengthen at rates less than those allowed under the condition of volume diffusion control, such as would be expected if the interphase boundaries had disordered structures.&apos; The narrow width of 8&apos; plates, the reproducible crystallography of their broad faces, and the appearance of these plates in cross section as octagons rather than as circular discs2 provide qualitative support for these deductions. The present study of the rate of thickening and the rate of lengthening of 8&apos; plates was undertaken in order to examine them on a quantitative basis. I) THICKENING KINETICS OF THE BROAD FACES OF?&apos; PLATES A) Literature Review. The measurements now available on the thickening kinetics of single-phase precipitate plates consist of one plot of the thickening of a proeutectoid ferrite plate in an Fe-C alloy,&apos; showing (as predicted) thickening rates less than those allowed by volume diffusion control. B) Experimental Procedure. Details of the preparation of the 4-3.93 pct Cu alloy used in this study have been previously reported.4 As in Part 1,&apos; transmission electron microscopy was the observational tool employed. A general description of the apparatus and procedures of the electron microscopy studies is given in Section I of Part I. In thin foils, 0&apos; plates tend to form at and parallel to the foil surface.&apos; A direct investigation of the thickening process by means of hot-stage transmission electron microscopy was therefore not feasible. It was thus necessary to use the conventional method of aging individual bulk specimens for a wide range of different times at the various temperatures studied. In each specimen, the thicknesses of a number of plates were measured. Since thin foils prepared from "bulk-aged" material contain a large proportion of grains with orientations near (001) , it was relatively easy to find, near the edges of the foils, the characteristic multifold patterns of intersecting extinction contours which indicate regions where the foil is exactly at an (001) orientation. The thicknesses of large numbers of plates were measured along the (200) branches of the "stars" so that the 8&apos; plates were precisely parallel to the optical axis of the microscope. Wherever possible, intersecting extinction contours were adjusted with the parameter s > 0 to improve the visibility of the plates in bright-field illumination. These precautions, in combination with taking the measurements at the thinnest parts of the foils, minimized the errors in the measurement of the thickness of the plates resulting from inexact parallelism to the electron beam. Since the plates were very thin, it was not easy to measure their thickness on the photographs. The techniques of enlargement and of microdensitometry were employed to minimize errors from this part of the measurement. A further source of possible error, that the plates can appear thicker because of contrast associated with mismatch normal to the plane of the plate, was also considered. The images of the plates were usually thinner than those of dislocations, however, and no anomalous changes in apparent plate thickness were observed when regions of foil containing plates were tilted through various diffracting conditions. Any error from this cause must therefore be small. Other sources contributing errors were: a) the microdensitometer traces per se and the subjective estimates of their peak limits, and b) slight fluctuations in magnification associated with small changes in the current of the objective lens of the electron microscope. The overall error probably amounted to no more than 5 to 10 pct. In order to obtain readily interpretable data on thickening kinetics, it is essential that the diffusion fields of adjacent ?&apos; plates not be allowed to overlap. Calculations&apos;-&apos; showed that this condition is definitely not ful-

Jan 1, 1969

By E. P. Pfleider, W. G. Pariseau

This paper reports the theoretical and experimental results of an analysis of ore pass drawdown as a problem in soil plasticity. The method of analysis developed appears to be a promising technique of investigating the mechanics of fragmented materials. A reconstructed plasticity theory brings experiment and theory into reasonable agreement, and hence may provide the foundation needed for rational ore pass design. The gravity-induced movement of broken rock through ore passes is an economical method of transporting fragmented materials through large vertical distances in underground mines, provided the ore pass is well designed. Unfortunately, the design procedures now followed do not very often result in ore passes that function properly. On the one hand, the huge accumulation of empirical data pertaining to the movement of materials in gravel bunkers, storage bins, deep grain silos and other structures that have features in common with ore passes remains uncorrelated. On the other hand, there is a dearth of experimental data substantiating theoretical models of material behavior. Consequently, reliable generalizations encompassing the broad spectrum of problems involved have not been forthcoming. AS an initial step towards improving the situation, a detailed case study of two-dimensional ore pass drawdown was made. The mechanics of the process were analyzed theoretically as a problem in soil plasticity and tested experimentally through observations of a laboratory ore pass model. THEORY Taylor1 defines a soil as a "mass commonly considered to consist of a network or skeleton of solid particles, enclosing voids of varying size." Broken rock in an ore pass is such a material. In plasticity theory this material is replaced by an idealized substance that deforms elastically up to some state of stress at which slip or yield occurs,2 For com-pressive states of stress, the Mohr-Coulomb criterion is a satisfactory yield condition. After the yield point is reached, the ideal soil deforms in accordance with the concept of plastic potential.4 Under plane strain conditions the governing equations separate into a system of stress equations and a system of velocity equations.&apos; Only stress variables appear in the stress system. The velocity system, however, contains a stress variable. The two systems are, therefore, coupled. Both systems are hyperbolic, and each has two real, distinct families of characteristic curves that coincide according to the classical theory of ideal soil plasticity. The

Jan 1, 1969

By James M. Barker

Sulfur is a nonmetallic element of great physical and economic importance to the world. It is widely but sparingly distributed throughout the hydrosphere, lithosphere, and biosphere. Sulfur is the tenth most abundant element in the universe and eighth most abundant in the sun. In the earth&apos;s crust, which is mainly igneous, it ranks 14th, but is eighth or ninth in sediments (Kaplan, 1972; Stanton, 1972). It apparently is very abundant in the core of the earth, because it is a strong chalcophile, and it is fifth in abundance in stony and iron meteorites (Field, 1972) where it occurs as trolite (FeS). In ancient times sulfur was called brimstone, literally "burning stone." Today the term brimstone is used interchangeably with the term elemental sulfur. Shelton (1979) summarized most of the common definitions of terms, grades, and specifications for the sulfur industry as follows (with minor additions): Sources of Sulfur: Combined sulfur-Sulfur that occurs in nature combined with other elements. Cupriferous pyrites-Pyrite containing relatively minor amounts of copper sulfide minerals. Hydrogen sulfide-A toxic gas (H2S) occurring in natural gas and petroleum. Involuntary sulfur-Sulfur produced primarily as a result of legislative or process mandates. Native sulfur-Sulfur that occurs in nature in the elemental (uncombined) form. Nonferrous metal sulfides-Copper, lead, zinc, nickel, and molybdenum sulfides that are processed for their metal content. Organic sulfurs-Complex organic sulfur compounds occurring in petroleum, coal, oil shale, and tar sands. Pyrites-Iron sulfide minerals that include pyrite, marcasite, and pyrrhotite. Sulfate sulfurs-Sulfur in anhydrite and gypsum. Voluntary sulfur-Sulfur produced in response to market forces. Basic Sulfur Products Produced and Marketed: Acid sludge-Contaminated sulfuric acid usually returned to acid plants for reconstitution. Brimstone-Synonymous with crude sulfur. Bright sulfur-Crude sulfur free of discoloring impurities and bright yellow in color. Broken sulfur-Solid crude sulfur crushed to -8 in. Byproduct sulfuric acid--Sulfuric acid produced as a byproduct of a metallurgical or industrial process, generally relating to combined sulfur sources. Crude sulfur-Commercial nomenclature for elemental sulfur. Dark sulfur-Crude sulfur discolored by minor quantities of hydrocarbons ranging up to 0.3 % carbon content. Elemental sulfur-Processed sulfur in the elemental form produced from native sulfur or combined sulfur sources, generally with a minimum sulfur content of 99.5%. Formed sulfur-Elemental sulfur cast or pressed into particular shapes to enhance handling and to suppress dust generation and moisture retention. Frasch sulfur-Elemental sulfur produced from native sulfur sources by the Frasch mining process. Hydrogen sulfide-Associated with natural gas or petroleum and produced at refineries and coke oven plants; used to make sulfuric acid or recovered sulfur. Liquid sulfur-Synonymous with molten sulfur. Liquid sulfur dioxide-Purified sulfur dioxide compressed to the liquid phase. Molten sulfur-Crude sulfur in the molten phase.

Jan 1, 1983

By E. Miller, K. L. Komarek

Equatiorzs have been derived which related maximum solid solubilities in semicondcting compounds having retvograde solidus curves with 1iqllidus data. Liquidus curves in Lke Pb-Te, Pb-Se, ard PB-S systetris have been defermined by thertrzal aralyses. Fvotrz expevimental maximum solibilities ia CdTe, PbTe, uxd PbS vetvograde tetrperatures hale beep1 calculated. TIze resllts support the concept that under certaiz conditiots pronounced itjlections in the liquidis curves arc indzcatiz:e of retropade solidus curves and that the tenlperatltre of the lmaximum solid solubility will be close to the temperature of the point of inflection in the liquidus curve. The maximum solid solihility within a gvoup of homologous cottrpoods SeetlLs to increase with increasing flatness ol the liquidus curvres. The phenomenon of retrograde solubility in metals, i.e., maximum solubility in a solid terminal phase in equilibrium with a liquid phase, has been theoretically predicted by Van aar&apos; in his calculations of hypothetical binary phase diagrams. It was not until 1926, however, that retrograde solubility was experimentally verified in the Zn-Cd system.&apos; Since then many sys- tems with retrograde solubility have been found, so that at present approximately fifty binary diagrams with a retrograde solidus curve are known.3 Meijering4 has critically appraised the accumulated data and has presented calculations which alloy predictions as to whether or not a solidus line will be retrograde. Interest in retrograde solubility increased when it was found that the solidus curves of germanium and silicon alloyed with a great many doping elements are retrrade. The problem was treated thermody-namically by odkinson,% d all available data on solid solutions in germanium and silicon were summarized by Trumbore.7 Although it is to be expected that intermetallic compounds will also exhibit retrograde solubility, experimental evidence is much more limited. Until now retrograde solidus curves have been reported for the compounds de,&apos; be, Ps:" ne," SnSe," and SnS.13 All these compounds are semiconductors, and the solidus curves were usually obtained by determining the carrier concentration at room temperature of samples equilibrated at elevated temperatures and then quenched. It has been hown,&apos;&apos; however, that it is not always possible to quench in the equilibrium compositions from above a certain temperature. Theoretical discussions have either explicitly excluded intermetallic compounds4 or not treated them with respect to retrograde slubilit.j In the following a thermodynamic treatment of retrograde solu-

Jan 1, 1967

By J. G. Morlet, A. R. Troiano, H. H. Johnson

Delayed failure in steel occurs by controlled initiation and growth of a crack. The incubation period for crack initiation was measured. Crack initiation and Propagation are controlled by interaction between hydrogen concentration and triaxial stress state. The incubation period results from stress-induced diffusion of hydrogen to the point of crack initiation. THIS paper describes the phenomenon of delayed failureland the kinetics of crack initiation and propagation in uniformly hydrogenated steel. The investigation was prompted by service failures of high-strength-steel components at applied stresses far below the conventional yield strength, after the part had successfully sustained equal or higher stresses for an extended time interval. This delayed failure phenomenon, often termed static fatigue, is associated1 with the presence of hydrogen. This is not surprising, since the voluminous literature on flaking and hydrogen embrit-tlement demonstrates that hydrogen may exert a potent embrittling influence. Flakes, or internal hairline cracks in alloy-steel forgings, are related to the presence of hydrogen retained from the steel-making process.2 On the other hand, embrit-tlement arises from hydrogen introduced during surface treatments such as acid pickling or electroplating. Laboratory delayed failures have been induced in notch specimens of 4340 steel by electrolytic charging of the specimen surface with hydrogen and subsequent static stressing.l,4,5 Static fatigue was observed over a wide range of applied stresses; however, failure did not occur below a critical applied stress, designated as the static fatigue limit. In this instance the extended time for failure resulted primarily from the macroscopic redistribution of hydrogen. A crack formed to the depth of the hydrogen enriched "case* upon loading; further crack growth naturally awaited diffusion of hydrogen into the material ahead of the crack. The crack-propagation rate was therefore controlled primarily by the macroscopic diffusion of hydrogen into the specimen interior during the test. Thus, in this instance static fatigue was associated with the movement of a gross concentration gradient. However, delayed failure in steel of uniform hydrogen concentration is of greater fundamental interest, as well as commercial significance. With a homogeneous hydrogen distribution a different mode of delayed failure might be expected. As the heterogeneous hydrogen distribution became more uniform,4,5 the initial crack-propagation rate decreased markedly and, in fact, what appeared to be an incubation period for crack initiation was observed. However, the macroscopic concentration gradient precluded an accurate evaluation of these observations. Although the existence of an incubation period, up to this time, has not been established definitely, it is not amiss to point out some implications of the concept. It is of interest in all hydrogen-induced embrittlement phenomena, such as flaking, delayed failure, and hydrogen embrittlement. Much discussion has centered around the possibility of an

Jan 1, 1959

By G. H. Gronhovd, W. H. Oppelt

Complete gasification to produce synthesis gas for manufacture of synthetic chemicals and fuels offers possibilities for utilization of the vast lignite fuel deposits in the U.S. The design of a slugging, fixed-bed, pressure gasification pilot Plant is described. Results are presented for initial operation of the plant at moderate pressure and using low-temperature char as fuel. Gasification of solid fuels is becoming increasingly important in the future overall energy picture, both in this country and abroad. Snythesis gas from gasification of coal consists chiefly of carbon monoxide and hydrogen, and after suitable purification and modification this gas can be used in the production of synthetic ammonia, methanol, higher alcohols, and synthetic liquid fuels, or as a reducing gas in the metallurgical field.&apos; Most synthesis gas used in this country is made from natural gas, petroleum oils, and refining tail-gases, but the direct gasification of coal will become more attractive as costs of petroleum oils and natural gas increase.&apos; A gasification process designed for use with brown coal and lignite was developed by the German Lurgi Co. prior to World War 11. In this process a fixed bed of lump-sized fuel is gasified with steam and oxygen at pressures ranging from 370 to 440 psi. Effective heat exchange between the ascending high-temperature gases and the descending solid fuel results in low gas outlet temperatures, high thermal efficiency, and favorable oxygen consumption. Lurgi gasifiers are used commercially for the production of synthesis gas or as a substitute for coal gas in many countries, including Germany, Czechslovakia, Great Britain, South Africa, Australia and Pakistan.3-6 The chief disadvantage of the conventional Lurgi gasifier which operates under nonclinkering conditions is that large quantities of excess steam must be supplied with the oxygen-steam mixture to reduce the temperature in the fuel bed below fusion temperature of the ash. Most of the steam leaves the gasifier undecomposed with the product gas and, after cooling, produces large amounts of dilute liquor. Evaluation of fixed-bed gasification experiments using dry-ash removal indicated that by increasing the oxygen concentration in the oxygen-steam blast the temperature in the combustion zone could be raised high enough to operate under slagging conditions. 7-8 Operation of a fixed-bed pressure gasifier under slagging conditions would reduce the steam requirements and the volume of waste liquor and would increase the steam decomposition, the overall thermal efficiency of the process, and the rate of gas production per unit cross sectional area of the gasifier. Because the Lurgi gasification process, modified for slagging operation, offered possibilities for efficient gasification of American lignite, the Bureau of Mines decided to investigate the process on a pilot-plant scale at the Grand Forks, N. D., Lignite Research Laboratory. DESIGN Description of Pilot Plant: A flowsheet of the Grand Forks slagging gasification pilot plant is presented in Fig. 1. The gasifier unit consits of the coal lock, the gas generator, and the slag lock. The fuel, which is periodically charged to the coal lock, moves by gravity flow into the generator and is continuously gasified by an oxygen-steam mixture introduced at the bottom of the gasifier. Molten slag is formed at the hearth and flows through a central taphole into a water quench bath. The slag-water slurry is periodically discharged from the slag lock. Process steam is generated and superheated in separately-fired, oil-burning units. Oxygen is supplied to the gasifier from a gas storage bank located some distance from the pilot plant. The capacity of the oxygen storage bank is about 130,000 standard cu ft at 2200 psig. Liquid oxygen is delivered by truck and is converted to gas during the filling operation. The superheated steam and oxygen are metered separately, then mixed and fed to the gasifier tuyeres. The gas generator is surrounded by a water jacket. The steam formed is separated in the steam drum and then discharged to the gas offtake, thus equaliz-

Jan 1, 1961

By F. Weinberg

It has been suggested, for some time, that the behavior of metals under high-temperature creep conditions is strongly influenced by the behavior of the grain boundaries present in the material. This has led to a number of investigations1-6 in which attempts were made to measure the properties of the grain boundaries themselves, both to determine their contribution to the creep process and to obtain further knowledge of their intrinsic structure and properties. The present investigation was undertaken to extend the observed data under more closely controlled experimental conditions and to attempt to clarify sonie of the discrepancies in the literature. A brief report of the preliminary results has been published.7 EXPERIMENTAL PROCEDURE For the present investigation, controlled orientation specimens were used having plane boundaries which terminated at the specimen surface. Trierys-tal specimens were used instead of the bicrystal type of Puttick and King,&apos; in order to simplify the gripping technique required to apply a shear stress along the boundary. The aluminum used was obtained from the Aluminum Francaise and was of 99.994 pct purity, containing 0.002 pct each of Cu, Fe, and Si. The aluminum tricrystals were grown horizontally from the melt, in graphite boats, and in an argon atmosphere, following the technique developed by Chalmers.&apos; The orientation of the tricrystals was controlled by using seed crystals separated by mica inserts. Thermal conditions were adjusted to produce tricrystals having boundaries which were macroscopically straight, parallel to the growth direction, and perpendicular to the top surface. Following growth, the tricrystals were carefully cut with a jeweller&apos;s saw to the test specimen shapes shown in Fig. l(a) and l(b). In Fig. 1(a), the boundaries subjected to shear stresses are indicated AB and CD: Points A and C are the ends of the mica inserts separating the seed crystals; points B and D are at lateral cuts made in the specimen. It was found that the slots left by the mica inserts at A and C had to be enlarged slightly, by cutting, to ensure that the boundary terminated freely at these points. A shear stress was applied to the boundarks by gripping the upper two legs in file-faced Inconel grips and suspending a weight from the lower part of the specimen held in similar grips, as shown schematically in the diagram. The test specimens shown in Fig. 1(b) were cut from long

Jan 1, 1959

By Leonard Grimshaw

DIFFUSION Of carbon from gases into iron has been the object of much research, because of its long recognized importance in carburizing processes, but the direct diffusion of carbon from steel into iron has received relatively little attention. Because of the increasing use of clad metals in industry, direct diffusion from steel into iron is becoming of practical importance. Therefore, the object of this investigation was to study the diffusion of carbon from several different kinds of steel directly into relatively pure iron, realizing that elements in the steels other than carbon might influence the rate of carbon diffusion. The previous work on diffusion of carbon into iron has been consider-able, and includes many reports in foreign languages. This work has recently been well reviewed by Mehl1 and Krynitsky,2 and the reader is referred to their excellent bibliographies.

Jan 1, 1937

By J. Spotts McDowell

INTRODUCTION The magnitude of the thermal expansion of silica brick, and its inability to withstand rapid temperature changes, present problems of considerable importance in the manufacture of siliceous refractories. In the study represented by the experimental data herein described, these problems are considered from the point of view afforded by the results of recent investigators: Fenner and his associates of the "Geophysical Laboratory, Washington, D. C., who have established the stability relations of the silica minerals, and Endell and co-workers in Berlin, who have studied the changes brought about in the constitution of siliceous refractory materials upon the application of heat. In the process of manufacture, the quartzite from which the brick is made changes in part into cristobalite and tridymite. The attempt is herein made to determine by microscopic methods the degree of transformation in various specimens of test bricks manufactured at slightly varying temperatures of burning, with varying coarseness of grain, and to determine the effect of repeated burning. The effect of variations

Jan 10, 1916

By H. M. Ziesemer

PRIOR to 1909 that mountain of porphyry, known as. Sacramento Hill, had remained hardly touched but had always aroused suspicions as to the presence of ore within.. During that year, exploratory work was started by underground methods; drifting and raising continued until 1913. It was proved that a mineralized zone existed, the limits of which had not been determined; so, because of the lower costs of exploratory work and the greater desirability of vertical sections, it was decided to prove the extent of the ore zone by churn drills. Drilling continued until the year 1917, when it seemed almost certain that the horizontal limits of the orebodies had been determined. Ore continued in depth in one direction beyond a point where it was economical to explore by churn drilling; this extension is still being developed by underground methods. The irregularities of the boundaries of the ore zones, together with the variable grades of ore encountered, made it necessary to drill on the corners of 100-ft. squares. Two ore zones were proved, known as the East and West Orebodies. The Sacramento Hill porphyry stock intruded into the Dividend fault. The fault ran roughly east and west with a dip to the south, having pre-Cambrian schists on the north against Paleozoic limestone on, the south. This intrusion was accompanied by a silica breccia on the south periphery, along the limestone contact side. The ore lay in the silica breccia and in the porphyry, some distance from the breccia. No ore was found in the heart of the porphyry mass on the north side, along the schist contact. The West Orebody is elliptic in shape, having a major axis of 1200 ft. (366 m.) and a minor axis of 800 ft. (244 m.); these diminish with depth until, at 300. ft., the axes are 500 ft. and 300 ft., respectively. The ore consists of chalcocite, some bornite, chalcopyrite, and considerable pyrite in a silicious gangue. About 30 per cent. of the copper is caused by

Jan 2, 1922

By R. Wiesenthal

A method is developed for improving the low recovery efficiency which results when viscous oils are flooded by water. Viscous oil has been diluted with a lighter liquid miscible in it in any ratio which produces a mixture possessing a reduced viscosity and which is then displaced by water. Light gasoline was used in these tests to reduce the viscosity of the oil in place. Oils possessing viscosities in the range of 1.28 to 324 cp at the test temperature of 30C were displaced from a cylindrical unconsolidated sand core, with a length of 2 m (6.6 ft) and a diameter of 10 cm (3.9 in.) at a flood of 6.27 cc/sq cm/hr. In two test series up to I PV of light gasoline was injected into the core before water flooding. In the first series the recovery of a low-viscosity oil (1.28 cp) increased as the volume of light gasoline was increased. However, only the oil which could not be recovered by water flooding alone could be replaced by the light gasoline. In the other series, the recovery of a more viscous oil (13.5 cp) was not increased even if large quantities of light gasoline were injected. An oil bank built up ahead of the water front so that the flood water met with equivalent saturation conditions, as would be the case in flooding solely with water. However, the recovery of more viscous oils could be increased substantially when the core was first flooded with water, followed by a slug of light gasoline, and then flooded with water again. Furthermore, an oil bank ,built up ahead of the second water front. The formation of this oil bank is particularly favorable for the displacement process; the greater part of the light gasoline injected was pushed out of the core ahead of the oil and recovered. Using a light oil of low viscosity, it was possible to replace only the residual oil that could not be recovered by water flooding by the light gasoline. As the basic study had shown that highly viscous oils could be recovered by flooding first with water, then with light gasoline, followed by a second injection of water, the study was extended by tests made with reservoir fluids and cores taken from the low-gravity oil reservoir of the Wietze field, Germany. A great increase in recovery over flooding with water alone was obtained in these tests. The results may show a way to recover high-viscosity oils by a comparatively simple flooding procedure. INTRODUCTION In fields where oil recovery has not benefited from natural water drive, increased recovery may be obtained by the injection of water into the reservoir, especially in the case of fields which produce high-gravity, low-viscosity oil. There is a rather close relation between the viscosity of the reservoir fluid and the recovery that can be obtained by water flooding. As the viscosity increases the oil recovery decreases proportionately, so that an oil viscosity about 30 times that of water is generally considered to be the upper limit for an economically successful water flood.&apos; This limitation has been recognized theoretically by Buckley and Leverett,&apos; and has been verified by numerous laboratory flooding tests, such as by Croes and Schwarz,V n the viscosity ratio range of oil to water from 1 to 500. The reason for the inferior recovery of viscous oils by water flooding can best be understood by considering the mechanism of flood tests. In such tests water is introduced into one end of a sand-packed tube which is saturated with oil of the viscosity to be tested, and oil is produced from, the other end. Oil, with a viscosity lower than that of water, is pushed ahead of the advancing water with considerable uniformity, and irregularities in the displacement process tend to be eliminated as the oil saturation decreases and the water saturation increases. However, oil recovery is not complete, for the water forms interfaces with the oil and traps residual oil droplets in certain of the pore spaces. These residual oil droplets are distributed rather uniformly through the sand, and they are not susceptible to recovery regardless of the amount of water passed through the test cylinder. In the case of an oil possessing a viscosity greater than that of water, the injected water tends to move irregularly through the sand in the test cylinder. At the place in the sand where initial water movement takes place, resistance to the movement of water is lowered and the water finger so formed will grow perceptibly; it will extend to the outlet end of the test cylinder so that a breakthrough of water takes place long before much of the oil-saturated volume of the sand has come in contact with water. Once the breakthrough of water takes place, the water-oil ratio is gradually approaching the economic limit, even though much of the oil in the test cylinder remains unaffected by water. Disconnected drops of oil are trapped in the portion of the sand that has been invaded by water, just as when an oil of low viscosity is flooded. The poor recovery of the more viscous oils, therefore, is due to the irregularity of water movement through the test cylinder, and the rate of water movement through restricted sections of the oil-saturated sand increases with the more viscous oils. There are three ways whereby the recovery of viscous oils by water flooding can be improved:&apos; (1) adding materials which will increase the vis-

Jan 1, 1965

By J. H. Bucher

The effect oj strengthening by the precipitation of CbC on the toughness offerrilic steel (0.11 pct C, 0.74 pct Mn, 0.02 pct Cb) was stlrdierl. A g-veater degree of pvecij~itatiotz strengthning is ohtaznable by aging the so11ution-treated steel rtt velaticely Low temperature was (1050" to 1l0O3F) than at higher temperatures (I150" to 1200°F). Tlzis ),eslrlts because a finer dispersion of CbC is obtained. However, the ductile-brittle transition te~ripertltlo.e is raised approximately tlzjeee tirues as IFLIIC~ perv a given yield stress increase) by aging in the lower tempareture range, as opposer1 to the Irigher temperaturee range. This is proposed to result pl-iir~avily because different precipitation distributions ar-e associated with the different aging -treaments. For tile steel aged at 1050" and 1100 F, heavy: precipitation on disloccctions occurs resulting in a high degree of rlislocution pinningh tl~us lowevirzg- the toilguiess. in tll c(.rise of the steel aged at 1150 &apos;a?zd 1300"F, Pvecipitatiol~ is irzove g-enerally distributed throughout the matrix rather limn preferentially on dislocations.; and Ike detlsitj, oj mobile dislocations is not sttyong-ly affected. THE most effective means of strengthening hot-rolled ferritic steels are grain refinement and precipitation hardening. It is well-known that grain refinement increases both the strength and the toughness. However, the upper limit of yield strength obtainable by grain refinement alone is about 60,000 psi,&apos;12 i.e., without the formation of acicular structures of lower toughness. The most economical means of obtaining higher strengths is the addition of small amounts of elements such as columbium, vanadium, and titanium which form carbonitrides. These precipitates are very effective in increasing the strength, but the ductile-brittle transition temperature is is Although it is agreed upon that precipitation decreases the toughness, there has been little effort to isolate the causative aspects of embrittlement. The purposes of this research are to assess quantitatively the embrittlement associated with different precipitate distributions and morphologies, and to correlate the degree of the embrittlement with the microstruc-ture. In this manner, a more fundamental insight into the mechanism of embrittlement may be gained. The steel selected for this purpose was a low-carbon, columbium-bearing steel which, after solution treatment, was aged in various time-temperature cycles while attempting to hold all other microstructural variables constant. MATERIALS AND PROCEDURE The composition of the steel used in this investigation is given in Table I. Starting with commercially hot-rolled material 0.074 and 0.280 in. thick, tensile blanks were cut from the thinner material and sub-size Charpy blanks from the thicker stock. The steel had been rolled using a low finishing temperature and rapid cooling after hot rolling to produce grain refinement. Also, chemical-extraction analysis and electron-microscopic examination revealed that the cooling was rapid enough to suppress any significant precipitation of CbC. Therefore, the as-rolled steel is essentially in the solution-treated condition in terms of the precipitation reaction, and it was used as the base material in this investigation. The room-temperature tensile properties of the as-rolled steel aged at 1100", 1150", and 1200°F for various time intervals were determined, see Table 11. The ductile-brittle transition behavior was studied for smooth and notched tensile specimens, and longitudinal half-size (0.200 in. thick) Charpy V notch specimens aged at 1100" and 1150°F for various times, also Table 11. In addition, tensile specimens aged for single times at 1050" and 1200°F were evaluated with respect to their ductile-brittle transition. Only one 1050°F treatment was used because of the extremely slow kinetics of precipitation at this temperature and because no significant difference between 1100°F aging was observed. Only one treatment at 1200°F was used because aging at this temperature alters the shape of the grain boundary cementite particles present in this steel and complicates analysis. The design of the tensile specimens is given in Fig.1.

Jan 1, 1968

By Ashok K. Sinha

The quasi-binary systems "VFe3"—VCo,—VNi,— "VCu3"and "TiFe3"—TiCo3,—TiNi3-"TiCu3"have been studied by a combination of microscopic and X-ray methods. Of the Phases encountered, eleven had close-packed ordered layer structures. Within each system, there is an approximately linear variation of the degree of hexagonality of the stacking arrangement with electron concentration, e/a. A study of eighty -four known examples of AB3 structures in transition metal alloys indicates that at e/a = 8.65 the ordered structure of the close -packed layers changes from "triangular" (AuCu3 type) to "rectangular" (SbCu3 type). At e/a < 8.65, the slope of hexagonality us e/a line increases with the group number of the A component. An interesting series of close-packed ordered structures is known to exist at the composition AB3; however, their alloy chemistry has not yet been fully understood. Dwight and Beck1 observed a correlation between position of the components in the periodic table and the type of crystal structure of the binary AB2 structures formed by transition metals. No consistent effect due to atomic size was noted and they proposed that electron concentration* predominates in In the present paper, the AB3 structures are characterized by a symbol describing the stacking and a symbol specifying the ordered layer. The stacking symbol used was introduced by Zhdanov,7 and later used in the International Tables,8 and by Beck9 in his survey of possible layer stacking structures. Alternating positive and negative integers are used to represent the number of positive (e.g., in abcabc...) and negative (e.g., in cbacba...) stacking sequences. T denotes the triangular ordering found in close-packed planes of the AuCu3 structure and R the rectangular ordering found in close-packed planes of the SbCu3 structure, Figs. 3(a) and (b). The present structure symbols are listed in Table I alongside the prototypes, where known, and other structural characteristics of AB3 phases found in the present investigation. EXPERIMENTAL The starting materials were metals of 99.9+ purity. The alloys were prepared by arc melting under argon atmosphere using a nonconsumable tungsten electrode and water-cooled copper hearth. The total weight loss upon melting and subsequent annealing was always less than 0.5 pct and hence the alloys will be referred to by their intended (unanalyzed) compositions. The alloys were homogenized and annealed at suitable temperatures in the range 750" to 1200°C, the annealing periods varying from 3 days at 1200°C to 10 days at 750°C. The heat treatments were carried out in sealed silica capsules under argon atmosphere and with a molybdenum foil cover between the alloy and the walls of the capsule. The quenched alloys were microscopically examined and reduced to powder by crushing or filing. The powders were, whenever necessary, given a stress-relieving anneal at the original annealing temperature. X-ray powder patterns were obtained with an asymmetrical focusing camera, a Guinier-deWolff focusing camera, or a Debye-Scherrer camera. Cr, Co, or Cu radiations were used. In some cases, to ensure the minimum degree of contamination, the deeply etched specimens were mounted in the asymmetrical focusing camera to obtain an X-ray pattern. Internal silicon standards were employed for lattice parameter determinations. The intensity calculations were made by using a Fortran IV program

Jan 1, 1970

By J. H. Yang, K. E. Gray

Results of single-blow bit-tooth impact tests on saturated rocks under elevated confining pressures and zero pore pressure were reported in a previous publication.1 This paper presents an extension of the earlier work to include a study of crater formation during tooth impact on both gas- and liquid-saturated Berea and Bandera sandstones at elevated confining and pore pressures. The basic data obtained were force-time, displacement-time, velocity-time and force-displacement curves during crater formation. Crater volume was also measured and the mode of crater formation determined. Bit tooth geometry, depth of penetration and velocity of impact were held constant. Results indicate that, with pore fluid present in the rock, failure trends from brittle to ductile as pore pressure is increased at constant confining pressure (pore pressure and borehole pressure were equal) For a given rock type, the mode of crater formation was dependent not only upon the nominal effective stress, but also upon the fluid which saturated the rock pore space. When confining pressure and pore pressure were equal (zero nominal effective stress), bit-tooth impact resulted in brittle failure for nitrogen-saturated Berea, and brittle to transitional failure for nitrogen-saturated Bandera; when saturated with liquid both rocks failed in a ductile manner at zero nominal effective stress. INTRODUCTION Dynamic wedge penetration tests have been conducted by investigators in several fields, but the failure mechanism of rock under dynamic stresses is not understood completely. The complex action of drilling bits, even considering the action of a single tooth, may be considered as a combination of drag bit and rolling cutter action. Thus, as a first step in understanding rock breakage in oil well drilling, single chisel impact and rock planing are of fundamental importance. For example, Gray 2 and Crisp3 studied drag bit cutting action at brittle stress states. Simon4 and Hartman5 studied the reaction of rocks to vertical impact by means of drop tests. The depth of penetration, crater volume and force-vs-time curves during crater formation were observed. The significance of indexing single-bit impacts has been noted.4,6-8 Gamer et al,9 reported impact tests on impermeable Leuders limestone at atmospheric and elevated confining pressures. In all cases the tests were accomplished on dry rock and pore pressure was considered to be zero. The importance of both confining pressure and pore pressure on the failure characteristics of rock was described. 10-12 It was found that the yield strength and ductility of porous rock depend on the state of stress under which the sample is tested. The importance of pore pressure on drilling rate in microbit experiments was noted by Cumingham and Eenink. l3 Robinson 12 also pointed out that in drilling the most important parameter in rock failure is the effective stress, where effective suess is defined as confining pressure pc minus pore pressure pp. The effect of pore pressure and confining pressure on rock strength was also noted by Serdengecti and Boozer 14 in strain rate tests, and by Gardner, Wyllie and Droschackl5 in elastic wave studies. Until recently all reported wedge impact studies under simulated wellbore stress states have been conducted on dry rock. Maurer 16 reported impact tests on samples saturated with deaerated water. Borehole and formation fluid pressures were equal in these tests except when mud was used in the borehole. With mud in the borehole and a high borehole-to-formation fluid pressure differential. Maurer observed "pseudoplastic" crater formation. Podio and Grayl reported impact tests on Berea and Bandera sandstone saturated with pore fluids having wide ranges in viscosities. In Podio and Gray&apos;s tests, confining pressure was elevated, but pore pressure and borehole pressure were held fixed at atmospheric pressure. The presence of

By N. A. Stockett

SOUTHEAST Missouri is the largest and oldest lead-producing district in the United States. For the year 1941, the statistical picture of pig-lead production, stated in short tons (partly estimated by the Engineering and Mining Journal) is as follows. [Tons World production 2,000,000 United States production 460.000 Southeast Missouri production 242,000] The consumption of primary lead in the United States in 1941 was approximately 900,000 tons, or almost double the country&apos;s production. The largest previous year&apos;s consumption in the United States was 718,000 tons, in 1926. The largest quantities of lead are used for cable sheathing, storage batteries and white lead. During 1941 tetraethyl lead for auto and aviation gasoline consumed 50,000 tons of lead. The entire lead production of Southeast Missouri is now mined by the St. Joseph Lead Co., whose dominant position as the largest producer in the United States of lead directly from ores is best shown by the fact that in 1941 it produced approximately 31 per cent of the lead production of the United States from its mines in southeast Missouri, where 22,000 tons of ore, averag¬ing over 3.00 per cent lead, is mined per working day. It is known that lead was mined at Mine La Motte, Madison County, Missouri, by Renault in 1723. Other white men and Indians probably did some mining prior to that time. Since 1865, the recorded production to Jan. 1, 1942, shows that the St. Joseph Lead Co. and the various other companies that have operated in St. Francois County mined lead ore, which, after milling and smelting losses produced 5,00,000 short tons of pig lead. About 95 per cent of the present lead production of Southeast Missouri is mined in St. Francois County. The northern part of this area is 60 miles south of St. Louis. The remainder of the lead is obtained at Mine La Motte, about 25 miles southeast from the center of the producing area in St. Francois County. PROSPECTING In this district, most of the ore is discovered by surface and underground diamond drills and by prospect drilling underground with rock drills. Each 2-ft. length of the cuttings from these Jackhamer prospect holes is assayed for lead. These holes are marked and the records are entered on maps. It has been found that close drilling--100-ft. centers of holes, and sometimes less-is necessary in order to locate most of the smaller commercial ore bodies, many of which previously had been missed by drilling the areas with holes spaced 200-ft. centers or more.

Jan 1, 1943