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By A. K. Mukherjee, J. E. Dorn, J. D. Mole

Investigations were carried out on the effect of polyslip on the strain hardening of aluminum single crystals. The orientations investigated were those lor which the tensile axis was in the [001], [111], [112], and [012] directions plus another for which the Schmid angles for {111}(110) slip were 1 deg. The experimental data were analyzed on a model based on the intersection of dislocations with particular emphasis on the effect of polyslip on the activation volume for inter-section. It is shown that the rate of strain hardening inreases for those orientations wherein attractive dislocation intersections occur and that those orientations which produce the greater number of such intersections exhibit the greater strain hardening. Good correlation of the data is obtained with the concept that attractive junctions, as proposed by Saada, Play an important role in accounting for the rate of strain hardening. EXISTING concepts on the nature and cause of strain hardening in fcc metals have been deduced principally from experiments on the deformation of single crystals under single slip. The effect of crystal orientation on the shapes of the stress-strain curves for single slip have been summarized by seegerl and more recently by Clarebrough and Hargreaves.2 Tensile specimens whose axes fall near the center of the [001]-[011] line of the standard triangle of the stereographic projection exhibit the longest range of easy glide (Stage I) and the lowest rates of linear hardening (Stage 11) whereas specimens whose axes lie near fie [001]-[111] line of the standard triangle have limited or no easy-glide range and exhibit somewhat higher linear strain-hardening rates. Specimens whose axes lie near the [001] or the [ill] poles do not exhibit easy glide and have the highest rates of linear hardening. Kocks3 has shown that the highest rates of linear hardening Occur under Polyslip when the tensile axis coincides with the [111] or the [ 001] pole. Since the rate of strain hardening is sensitive to specimen orientation and the incidence of polyslip, these relationships might help to discriminate between various dislocation models for strain hardening in fcc metals. Previous attempts to analyze the effect of orientation on strain hardening,1"3 however, did not provide a unique answer to this problem. Consequently the present investigation was undertaken wherein additional data, particularly that for the effect of polyslip on the activation volume for intersection, was also determined in order to provide more complete information on the details of strain hardening. Whereas analyses of these data reveal that several recommended models for strain hardening are at variance with the facts, good correlation of the data is obtained with the concept that attractive junctions4 play an important role in accounting for the rate of strain hardening. I) EXPERIMENTAL APPROACH seegerl demonstrated that slip in fcc crystals at low temperatures is dependent on thermally activated intersection of glide dislocations with forest dislocations. This has been confirmed by tests on single crystals of aluminum by Mitra, Osborne and Dorn5 and on polycrystalline aluminum by Mitra and Darn.' Thus in accord with Seeger's theory, the shear strain rate, ?, below a critical temperature, T, is where .V is the number of points of contact per unit volume between forest dislocations and glide dislocations, A is the area swept out per successful intersection, b is the Burgers vector, v is the frequency of vibration of the segment of the glide dislocation undertaking intersection, U is the activation energy for intersection, k is Boltzmann's constant, and T is the absolute temperature. For aluminum, which has an extremely high staeking-fault energy, the constriction energy is negligibly small and therefore the activation energy decreases practically linearly with the stress according to as will be recomfirmed later, where Uo is jog energy at the absolute zero, G and Go are the shear moduli at the test temperature T and O°K, respectively, L is the spacing of the forest dislocations, t is the applied shear stress for slip, and tGo is the stress field that must be surmounted athermally.

Jan 1, 1965

By Harmon F. Fisher

In the course of a comprehensive investigation for the development of the electrical process for the dehydration of oil-field emulsions, the writer has had an unusual opportunity to direct and execute a number of related, parallel studies concerning crude oil emulsions and extending over a period of nearly six years. Among these was an investigation utilizing the microscope for studying both the general characteristics of crude oil emulsions, the nature of their electrical charge and the action of an alternating current field in causing coalescence of the finely dispersed, more or less permanently suspended, emulsion particles into larger droplets of such mass that subsequent dehydration would follow by the ordinary process of settling, further agglomeration of the water droplets and, finally, separation into commercially dry, pipe line oil and a clean water discharge. It is not the purpose of this paper to enter into a detailed discussion of the highly specialized subject of microscope technique, nor into a theoretical discussion concerning the origin of the electrical charge on the emulsion particle or concerning the mechanism of the electrical phenomena occurring during the electrical treatment of oil-field emulsions. In a short paper of this character one can hope to touch on only a very limited discussion of the theoretical aspects of crude oil emulsions. The subject of emulsions and colloids is comprised in a comparatively young science in which, however, very rapid progress is being made and consequently it is undergoing many changes; a tentative conclusion valid today may be overthrown tomorrow. Nor would it be a simple science even if it were no longer undergoing this rapid progress; a thorough study of emulsions is based upon a knowledge of such fundamental subjects as molecular structure, ionization and other electrical phenomena, surface chemistry, surface and interfacial tension phenomena, viscosity and other factors too numerous to discuss here and the fundamental theories of which are still undergoing more or less change. Therefore this paper will confine itself largely to a generally descriptive discussion, a sufficiently detailed outline of the microscope technique and a brief comment on

Jan 1, 1931

By Howard C. Pyle, John E Sherborne

Core analysis is a recent development in the field of petroleum technology. The earliest work on this subject was done in connection with evaluating and planning secondary oil recovery by water-flooding. Present-day analysis of sands of flush fields requires new and independent interpretations of the data provided by cored material. Particular attention is being paid to the development of rapid, routine methods for measuring physical characteristics of sandstone, such as permeability, porosity and grain size, as well as the sand's fluid content. Permeability may be defined as the fluid-passing capacity of a rock. For a sandstone to be permeable it must be possible to pass a measurable quantity of fluid through the material in a finite period of time. The common unit of permeability is the darcy, which may be defined as the rate of viscous flow, in milliliters per second, of a fluid of one centipoise viscosity through a porous medium having a cross section of one square centimeter, under a pressure gradient of one atmosphere (76.0 cm. Hg) per centimeter.' For convenience the subunit millidarcy, or one-thousandth darcy, is often used. Porosity is defined as the fluid-containing capacity of a rock and is usually expressed as a percentage ratio of the total pore volume to the rock or bulk volume. Since measurement of only the effective or communicating pore volume is often made, porosities are distinguished as total or effective.2,3 Net effective porosity is defined as the net pore volume available for oil and gas. Oil and water content of sand is measured and expressed either as the percentage saturation of the total pores or of the bulk rock. The oil content may also be expressed as the percentage saturation of the net effective pores. In connection with water-flooding, methods of core analysis were developed to furnish data that could be used in determining the quantity of recoverable oil14-6 and the probable rates at which various sands or divisions of a sand open to the wells would take water or produce oil. In flush fields, the analytical data are used to predict the productivity of a cored interval. They indicate the presence of oil, gas and water and may

Jan 1, 1939

By Howard C. Pyle, John E. Sherborne

Core analysis is a recent development in the field of petroleum technology. The earliest work on this subject was done in connection with evaluating and planning secondary oil recovery by water-flooding. Present-day analysis of sands of flush fields requires new and independent interpretations of the data provided by cored material. Particular attention is being paid to the development of rapid, routine methods for measuring physical characteristics of sandstone, such as permeability, porosity and grain size, as well as the sand's fluid content. Permeability may be defined as the fluid-passing capacity of a rock. For a sandstone to be permeable it must be possible to pass a measurable quantity of fluid through the material in a finite period of time. The common unit of permeability is the darcy, which may be defined as the rate of viscous flow, in milliliters per second, of a fluid of one centipoise viscosity through a porous medium having a cross section of one square centimeter, under a pressure gradient of one atmosphere (76.0 cm. Hg) per centimeter.' For convenience the subunit millidarcy, or one-thousandth darcy, is often used. Porosity is defined as the fluid-containing capacity of a rock and is usually expressed as a percentage ratio of the total pore volume to the rock or bulk volume. Since measurement of only the effective or communicating pore volume is often made, porosities are distinguished as total or effective.2,3 Net effective porosity is defined as the net pore volume available for oil and gas. Oil and water content of sand is measured and expressed either as the percentage saturation of the total pores or of the bulk rock. The oil content may also be expressed as the percentage saturation of the net effective pores. In connection with water-flooding, methods of core analysis were developed to furnish data that could be used in determining the quantity of recoverable oil14-6 and the probable rates at which various sands or divisions of a sand open to the wells would take water or produce oil. In flush fields, the analytical data are used to predict the productivity of a cored interval. They indicate the presence of oil, gas and water and may

Jan 1, 1939

By Y. C. Liu, R. H. Richman

Deformation and recrystallization textures of the a solid solutions of Cu-P, Cu-As, and Cu-Sb alloys are examined as a function of composition. It is found that the deformation texture of copper is unckanged up to a composition of 0.43, 0.41, and 0.24 at. pct of phosphorus, arsenic, and antimony, respectzvely, and then the transition to the 70 : 30 brass type of deformation texture proceeds linearly as the logarithm of the solute content. Recrystallization textures consist of strong, new components that do not all bear the usual<111> rotational relation to the deformation components. The dependence of the deformation texture transitions and the recrystallization orientations upon composition and solute-element type is discussed. A systematic evolution of individual recrystallization components in the annealing texture of copper was portrayed as a function of germanium or tin content in a previous study.&apos; Similar patterns of tex-tural change have been observed with copper-zinc alloys,2 and in less detailed studies of other systems.3,4 In fact, most of the literature dealing with preferred orientations in copper alloys indicates that the influence of solute elements upon textures in copper is of one general type. As the alloy content of copper is increased, the deformation texture changes from the copper type to the 70:30 brass type, and the annealing texture undergoes a comparable change from the (001) [ loo] orientation of unalloyed copper to the {113} <211> type of 70:30 brass, with the notable exception of copper alloyed with Periodic Subgroup V-B elements.4-8 In almost every case it is possible to describe the reorientations after annealing as 30 to 40 deg rotations about <1ll> poles of the deformation components. Since there is apparently not much difference in the final textures of the copper binary systems already investigated, only a limited variety of preferred orientations has served as the basis for current theories of the origin of annealing textures. In order to test the validity of the proposed theories, and the possibility that the <111> rotations are not unique, it would be most desirable to study the reorientation relationships of additional, and heretofore unanalyzed, recrystallization components if such components exist. Examination of the literature reveals a good deal of uncertainty concerning preferred orientations in copper alloyed with elements in Subgroup V-B of the Periodic Table. Phosphorus is known to inhibit the cube texture in copper when present in amounts as low as 0.01 wt pct,8 but the recrystallized matrix that occurs instead of the cube orientation was reported as either random or weakly textured, with orientations not observed in Cu-Zn, Cu-Ge, or Cu-Sn alloys.4-9 A Cu-0.75 at. pct As alloy apparently contained, along with the (001)[100] and (113) <211> type of recrystallization components, {110} <112> and (110) <001> components, whereas an almost random distribution of orientations was found in alloys of higher arsenic content.4 A {110} <001> component also appeared in rolledand annealed Cu-Sb alloys, but otherwise the recrystallization textures of Cu-Sb alloys seem to con-

Jan 1, 1962

By D. W. Levinson, L. F. Mondolfo, N. A. Gjostein

MANY investigations are reported in the literature on the age hardening of Al-Mg-Zn alloys but most of them are concerned mainly with mechanical property changes. The present investigation was started to determine the structural changes in an AlMgZn alloy. The alloy composition was chosen in the existing phase diagram" so as to lie on the quasi-binary section Al-(AlZn)Mg Actually, it was found that the diagram as published was inexact at the lower temperatures and that the phase in equilibrium with aluminum at the lower temperatures is not the ternary compound. Technique The alloy used for the investigation was prepared from high purity materials and the resulting composition as determined by chemical and spectro-graphic analysis was: Zn, 6.17 pct; Mg, 2.13 pct; CU, 0.03 pct; Si, 0.009 pct; Fe, 0.005 pct; and the remainder, aluminum. An ingot -in. thick was cast, homogenized, hot and cold-rolled to strip 0.064-in. thick for dilato-metric and powder work, and to foil 0.005-in. thick for single crystal work. Solution treatment temperature for all specimens was 475°±5°C for periods of at least 1 hr, either in air furnaces or lead baths. Aging was done in oil or Pb-Bi baths controlled to within ±3°C. The aging was investigated at the following temperatures: room (30°), 130°, ZOO0, 260°, and 300°C. For the dilatometric study, the length changes were measured continuously, at temperature, using strips of alloy 10 in. long, shaped as channels to eliminate undesirable deflection due to bending. To compensate for thermal expansion and contraction due to the variations in the temperature of the aging baths, the dilatometers were built of the same alloy as the one being tested, with the same shape and size, but with material fully annealed. Gages on which 0.0005 in. could be read and 0.0001 in. estimated were used to measure the dilation. Length changes were also measured at room temperature. Strips approximately 10 in. long were solution-treated, quenched, and measured in a supermicrome-ter in which 0.0001 in. could be read and 0.00001 in. estimated. The specimens were immediately aged for a given time, remeasured, and then the cycle was repeated, including the solution treatment. The error of measurement with this technique was somewhat larger, but the results confirmed those obtained by continuous measurements. The sheet used for the dilatometric work was checked to determine grain orientation. Both X-rays and etching methods revealed a rather coarse grain size but only a negligible amount of preferred orientation. Thus, volume changes calculated from length changes are not invalidated by preferential orientation effects. Pieces of the sheet used for the dilatometric work were also used for the metal -lographic work. Filings for the powder X-ray study were produced from a homogenized piece of sheet. These filings were magnetically purged of iron, screened to 200 mesh, sealed in a Pyrex tube containing an argon atmosphere, and solution-treated. When quenching, the glass tube was broken, so that the powder dropped directly into cold water. After drying with alcohol, the powder was sealed into capillary tubes containing an argon atmosphere and then aged for the required times. In spite of all these precautions the three strongest lines of a( Al2o) appeared in all patterns, and were used as internal standards. By the use of these standards, accurate corrections for film shrinkage were obtained. For the back reflection patterns, annealed nickel powder was mixed with the specimen to act as internal standard. A preliminary investigation was made in small (57.3 mm diam) powder cameras. From these patterns the changes which took place in the solid-

Jan 1, 1957

By Joachim J. Hauser

Experiments on latent hardening were peyformed by compressing single crystals along a direction perpendicular to the tension axis. The slope and length of easy glide in the tension test were found to depend only on prior deformation in the same slip plane. Prior deformation on a different slip plane changes the stress level of the resulting stress-strain curve. The yield points appearing upon reloading after prior extension and unloading were related to the end of easy glide. SEVERAL researchers have studied the latent hardening due to deformation of a crystal by slip on a slip System after prior deformation. These experiments can be divided into those in which the prior deformation was on the same plane as the subsequent and those in which the two deformation processes were in different planes. In the former category are the experiments of Buckley and Entwistle,1 Parker and washburn,2 and Haasen and Kelly.3 The latter case has not been studied systematically; it was the main purpose of this investigation to produce this type of latent hardening and explain the results in terms of the existing theories of work hardening. In general, tension producing slip on a certain slip system can be preceded by tension, transverse compression or longitudinal compression, each with predictable dislocation movement and intersection. The intersection of dislocations can lead to glissile or sessile jogs, Cottrell-Lomer locks and other sessile dislocations. The effect on the stress-strain curve could depend on which combination of the former mechanisms is operating. Haasen and Kelly3 have studied the yield points which occur in aluminum and nickel single crystals upon reloading after prior unloading in a tension experiment. They attributed this effect to the anchoring of dislocations occurring during unloading. As Cottrell and stokes4 have shown that dislocations cutting through the "forest" could only lead to reversible changes, they attributed the anchoring to the formation of sessile dislocations during unloading. However, different kinds of sessile dislocations could be formed during unloading, and it was the purpose of this experiment to determine whether Cottrell-Lomer locks are responsible for the yield effect and for the end of easy glide. The case where a longitudinal compression is followed by tension along the same axis is commonly referred to as a Bauschinger test. This type of effect was studied by Buckley and Entwistle1 on aluminum single crystals and by Parker and washburn2 on zinc single crystals. In such a test, the tension and the compression activate the same slip plane with opposite slip directions. The use of sideways compression in the present experiments permits the activation of different types of slip systems and the study of their effect on the easy glide region and on the transition between the elastic and easy glide region. The theory of seeger5 for the flow stress in fee materials is applied to explain the latent hardening. EXPERTMENTAL PROCEDURE All the single crystals used in this investigation had an axial orientation close to <210>, called the "0.5" orientation. This is the orientation for which the tensile axis is 45 deg from both the slip plane and the slip direction. The single crystals were grown from the melt under a helium atmosphere using milled graphite boats,=at a rate of 8.6 mm per min. The silver used in the experiment was 99.98 pct pure. The single crystals had a square cross section about 0.9 by 0.9 cm and a length of 14 cm. The orientation of the specimen was determined within ±2 deg by the Laue back-reflection method. The specimens were annealed at 940&apos; ± 2°C in a helium atmosphere for 24 hr and then furnace cooled over a period of 7 hr. The specimens were electropolished in a solution of 9 pct KCN in water. The specimens were tested in a soft-type tensile machine (the load is prescribed) up to 3 pct strain. The stress was increased continuously at approximately 30 g per mm2 per min. The strain was measured over a 5 cm gage length with a mechanical extensometer employing an optical lever. The strain and stress were measured with accuracies of i 2 X 10-5 and ± 2 g per mm2, respectively. The remainder of the stress-strain curve up to 20 pct strain was obtained in a hard-type tensile machine (the strain rate is prescribed). The strain and the stress were measured in that machine with an accuracy of ±2 pct. The compression tests were performed in the hard-type machine using accurately machined steel blocks without lubrication. The blocks were used so as to apply a uniform compression over a length of 13 cm. The strains were measured on the hard-type machine and with a micrometer.

Jan 1, 1962

By Ralph Smith

DEVELOPMENT of the lime industry in Ste, Genevieve County began in a crude way in 1840. According to information furnished by the Missouri Bureau of Geology, in the early days small vertical kilns built of stone were used, and wood was the fuel. Modern development began in 1904 when one company introduced steel shells lined with firebrick. Within a few years two more companies erected similar plants, and in 1925 a fourth company began operations. Thus there are today four lime companies at Ste. Genevieve, all operating at high capacity and with a gradually increasing production. GEOLOGY The limestone of Ste. Genevieve County, which has the chemical composition and purity required for lime burning, is the upper 80 or 90 ft. of Spergen formation. The Missouri Bureau of Geology, in its geological map of Ste. Genevieve County, gives the Spergen formation a total thickness of 160 ft., but only the upper portion is pure enough for lime burning, with an average raw-stone analysis of 98.7 per cent CaCO3; 0,35 Si02; 0,3 R203; 0.35 MgCO3; 0.3 SO3. The Spergen, one member of the Meramac group, Iowa series, of the Mississippian system, underlies an area approximately 12 miles long north and south, by 5 miles wide east and west (Fig. 1) in Ste. Genevieve County. The entire eastern two-thirds of Ste. Genevieve County is sedimentary, the formations dipping gently toward the east on an average grade of about 4 per cent, or 2 ½ °. Thus the outcrops of the various sedimentaries run approxi-mately north and south. A line running west from Ste. Genevieve crosses the outcrops of the sedimentaries, ranging from the top of the Mississippian to the Ozarkian geological system in a space of 12 miles. Thus with the gentle dip of 2 1/2° the 160-ft. thickness of the Spergen formation stretches out in its outcrop so that it is approximately one mile

Jan 1, 1938

By John Chipman, Raymond L. Orr

Recently reported high -temperatlnre thermal data have been incorporated in a reuieu&apos; of the therinody-r~ar,zic propesties of iron. The recent data permit mot corlsisterlt and reliuble choices to be made for many of the pvoperties, resnlling in bettev eslablished tabrtlations of the thermodynamic functions. Values of Cp, h°t- - H°298. s°t - S2sa, and (G°T -H298/T are tabulated for -the solid and liquid phases of iron in both stable and melastable regions. Consistency of the tabulations has been maintained to the precision necessr~vg to yield the Gibbs energy change belween the bcc (a, 8) and fcc (y) phases of iron at temperatures pertinenl to alloy studies. THE importance of the metal iron has stimulated many investigations of its thermodynamic properties at elevated temperatures. Reviews and summaries of the data have appeared from time to time. Among these the 1951 paper of Darken and smith&apos; deserves highest recognition for the quality of its criticism and for the precision and thermodynamic consistency of its tabulations. These and the more recent table of Kaufman, Clougherty, and weiss2 reproduce the Gibbs energy of the (a, 6)--Y transformation with sufficient sensitivity for alloy studies. Other recent compilations of equal validity3-&apos; make no attempt to do this. Since this Gibbs energy change is not greater than 22 cal per g-atom over the temperature range 1100° to 1800°K, it is obviously desirable to tabulate values of (G°t - H298)/T to four places of decimals even though the absolute accuracy would not warrant such precision. The necessity for reconsideration of the problem is emphasized by the recent publication of several important researches on the enthalpy and heat capacity of iron. The older work is well-covered in the reviews cited and will be mentioned here only when actually employed in the tabulations. GAMMA IRON Transition temperatures are taken from the selec -tions of Elliott and Gleiser,5 based on the work of Boulanger7 and earlier workers. For the a-y (A3) transition at 1184°K we retain the value 215 cal per g-atom adopted by Darken and smith.&apos; It has received confirmation in the recent work of Dench and Kubaschewski,&apos; and of Braun8 using adiabatic calori-metry, and of Wallace, Sidles, and Danielson10 using a pulse heating technique. The enthalpy data of Olette and ferrier" and of Anderson and Hultgren12 at higher and lower temperatures may be extended to 1184°K to give the following values which are adjusted to the required value of ? 1184 Ha,1184 Ha 298 = 8030 cal per g-atom [11 hr,1184-ha298 = 8245 cal per g-atom [2]

Jan 1, 1968

By Nicholas J. Grant, A. W. Mullendore, Paul Predecki

The Duwez technique of splat cooling in which a molten droplet of metal is accelerated and made to impact on a cold, highly conducting substrate was investigated.- An apparatus for producing "splat" was constructed employing an explosive powder charge to accelerate the molten metal. Transport of the molten metal just prior to impact with the substrate was studied by means of high-speed photography. The molten particles are small spherical droplets from about 1 to 50 µ diameter. The average cooling rates for aluminum, silver, and a gold alloy splatted on nickel substrates at room temperature were determined experimentally and were found to vary from 18 to 5 x 10&apos; C per sec. The heat-transfer coeficients for pure aluminum and pure silver splats cooled on nickel substrates at room temperature were found to be 2.7 to 6.8 and 13.6 to 54.2 cal per sec sq cm &apos;C (2 to 5 x 104 and 1 to 4 x 18 Btu per hr sq ft OF), respectively. Solidification rates in pure aluminum and silver splats were calculated. "SPLAT cooling" is a term describing a technique for extremely rapid freezing and cooling of molten metals and alloys to room temperature or below. The technique was developed by Duwez et al.&apos; in 1960, and after refinement2 consisted in transferring a few tenths of a gram of molten metal to near sonic velocity to strike a suitably placed cold copper surface. Upon impact, the metal spread into a thin nonuniform film called a splat, about 10-4 cm thick. The splat particles produced in this manner were thin enough in some areas to be suitable for transmission electron microscopy, without further treatment, and, together with X-ray data, yielded a variety of structures which would be classified as follows: 1) supersaturated solid solutions (increase in solubility limit), 2) metastable crystalline stoichiometric and non-stoichiometric intermediate phases ( in Au-20.5 at. pct Si and in Au-14 at. pct Sb, respectively), 3) amorphous alloys, 4) retained high-temperature phases, 5) alloys having equilibrium phases present, but with unusual, markedly altered structures. The crystalline phases present in splats were usually extremely fine-grained and had low dislocation densities. Present interest in splat cooling centers around a study of the unusual structures produced by the technique, their contribution to alloy theory, and the possibility of the development of new or unusual properties. In addition, the technique is being examined for the production of bulk quantities of new high-strength alloys for low- and high-temperature use. Although a number of alloy systems have already been investigated by the technique, relatively little is known about the mechanism of splat formation and the physical conditions encountered by the metal during solidification and cooling. The purpose of this work was: 1) to determine the velocity, shape, and size of the molten metal droplets just prior to impact with the cold substrate; 2) to try to estimate or measure solidification rates, heat-transfer coefficients, and cooling rates in splats. EXPERIMENTAL TECHNIQUE Splatting Apparatus and Procedure. An apparatus similar to the type originated by Duwez et a1.,2 but employing an explosive charge to accelerate the molten metal, was used. A "Ramset" fastening tool (a gun normally used for driving studs into concrete, steel, and so forth) was mounted vertically above a resistance-heated graphite crucible as shown schematically in Fig. 1. A splat product was produced by melting a few tenths of a gram of metal at the position shown in Fig. 1, and then exploding a powder charge in the breach. The shock wave thus generated traveled down the barrel into the furnace, ejecting the molten metal through the 0.06-in.-diameter hole at the bottom of the crucible. The ejected metal was impacted on a high-conductivity metallic substrate where it formed a splat. High-Speed silhouette Photography. In order to investigate the size and shape of the ejected, molten metal just prior to impact with the cold substrate, high-speed silhouette photographs were taken, and are shown in Figs. 2 and 3. These photographs were obtained with the aid of an Edger-ton, Germeshausen, and Grier microflash unit and a submicrosecond flash drive equipped with a variable time delay. Two types of triggers were

Jan 1, 1965

By R. S. Wagner, R. G. Treuting, W. C. Ellis

Use of the Weisseizbevg goniometer for the study of the morphology of whisker crystals and transfer of the results to a stereograplzic projection are described. While in almost all instances a complete and rapid solution is obtained with a purely gaphical treatment, an absolute analytical treatment applicable to difficult cases is given. Examples are given for determination of growth direction and external features of a crystal, for detection of &apos;twintzittg, and for establislting the orientation relntionships in a kinked whisker crystal. We give here a method for the use of the Weissen-berg goniometerl" in the study of orientation relationships in "whisker" (micro) crystals3-8 and direct transference of the data to the stereographic projection. The operations are straightforward and require no involved calculations: in almost all cases solely graphical treatment is adequate. In a few complex instances, a more exact analytic method may be required. In the method, not only are equatorial reflections of an oscillation photograph used, but also those on higher layer lines, or those not occurring on a recognized layer line. Such reflections off the zero level are often essentialy to detect the presence of twinning. The method is particularly suitable for examination of whisker crystals since the axial or growth direction is almost always one of high symmetry, permitting a more restricted oscillation range to obtain the necessary reflections and an accordingly shorter exposure time. The method is also applicable when there is no lattice-related external symmetry, and is as well able to identify external crystal surfaces, when such exist, with the aid of an optical beam. Thus growth direction, identification of lateral faces, twinning, and orientation relationships in a kinked crystal can be established. A test for the Eshelby twist6-8 can readily be made. The method can be used for orientation, for structure analysis, and as an aid in the identification of an unknown crystal. Moving-film techniques have previously been employed variously for crystal-orientation studies.1,2,9-13 In particular, use of the Weissenberg method for orientation determination has been reported by Wooster and wooster.14 While their method derives the same data as here described, it differs in depending on the tracing of constant p streaks, a less than dependable phenomenon with small specimens, a few microns or less in cross section. The Laue method can and has been used for orientation studies of microcrystals,15 e.g., 2 p in cross section, but requires the extreme intensity and concentration from a microfocus tube to obtain reasonable exposure time. PRINCIPLES OF THE PRESENT METHOD Consider a crystal of random orientation with respect to the oscillation axis in a Weissenberg goniometer. Its diffraction pattern need not necessarily result in recognizable layer lines. In Fig. 1, a stereo-graphic projection of the reference sphere is given with the equatorial plane XZ normal to the oscillation axis Y, and the X-ray beam directed from X towards 2. The great circle ZZ is then normal to the beam, and the axes are right-handed. Thus the reflected X-ray beam lies at the intersection R of small circle ARB of radius 28 from 2, and of small circle RE of radius a from the rotation axis Y. a is the conventional semiapex angle of a cone of diffracted rays from the atoms aligned in the direction

Jan 1, 1967

By N. F. Schulz, H. A. Lex

Representative samples of typical manganiferous iron ores from the Cuyuna Range, Minn., were reduced to the metallic iron state at temperatures just short of fusion with an excess of coke in the manner prescribed by the R-N Direct Reduction Process. The magnetic separation characteristics of the reduced ores were determined at several grinds by means of the Davis magnetic tube concentrator. The efficiency of metallic iron concentration by magnetic separation was a direct function of the degree of metallization of the ore sample and of the degree of liberation at-tained in grinding. Some improvement of liberation characteristics was observed if a small amount of sodium chloride was present in the ore during reduction. Despite the extremely fine-grained structure of the crude ores, iron concentrates containing more than 90% Fe at iron unit recoveries of 90% or more were obtained from well-metallized samples of three of the four ores tested. The rejection of manganese to the tailings corresponding to such separations varied from 80% to 95%. The manganiferous iron ores of the Cuyuna Range in Minnesota constitute a major potential source of manganese in the United States provided that a technically and economically feasible process can be devised for its recovery. The iron and manganese of these ores occur chiefly as oxides or carbonates in the form of very small, irregular, discrete grains embedded in a matrix of quartz or other siliceous gangue. The present investigation was undertaken as a sequel to an earlier one conducted jointly by the U.S. Bureau of Mines and the R-N Corp. Those results indicated that the R-N Direct Reduction Process might be a means for recovering both a metallic iron concentrate and a marketable manganese by-product from Cuyuna manganiferous iron ores.&apos; The R-N Process is one of many proposed schemes for the treatment of crude iron ores involving the di- rect reduction of the iron content to metallic iron followed by physical extraction of the iron. In general, it consists of the following stepsz2 1) Iron oxide in crushed natural ores or iron concentrates is about 95% reduced to metallic iron at elevated temperatures but without fusion in a rotary kiln in the presence of a solid carbonaceous fuel (usually coke), limestone, and combustible gases. 2) The kiln product, consisting of metallized ore, excess coke, lime, and coke ash is cooled. The excess coke is recovered and recycled to the kiln feed. 3) The metallized ore is ground for liberation and magnetically separated to yield a metallic iron concentrate. 4) The metallic iron concentrate is agglomerated by a briquetting process. The reduction kiln temperatures must be high enough for the desirable chemical reactions to proceed at practical rates without causing fusion of any of the ore constituents. The time of exposure of the ore to the reducing conditions must be ample for 90% to 95% metallization of the iron oxides present. If more than 95% of the iron is metallized, however, difficulties may arise in the briquetting step, presumably because of accompanying higher carbon content of the metallic iron. Although not always necessary, powdered limestone or dolomite may be added at some time during reduction to aid in eliminating sulfur and phosphorus from the final product.3,4 Other additives, notably sodium chloride, when present during reduction, result in improved liberation characteristics of the metallic iron from certain reduced ores.&apos;v6 Under the reducing conditions normally employed, P(co + H2)= 1 atmosphere, and 1830&apos; to 2150°F (1000° to 1170°C), the R-N Process is claimed to be adaptable to a wide variety of low, medium, and high grade iron and manganiferous iron ores. The manganese oxides and carbonates are reduced mostly to nonmagnetic MnO which is rejected to the nonmagnetic tailings. Manganese-bearing pyroxenes of the original ore, however, may be rejected poorly, if at all, apparently because these minerals occur within the iron lattice or are entrapped in the metal particles.7 The investigation was limited to studies of the Cuyuna ores listed in Table I, which were reduced to the metallic iron state under various conditions

Jan 1, 1969

By W. L. Martin, J. N. Dew, H. B. Steves, M. L. Powers

This paper presents and discusses the results obtained during a pilot test in the Loco field in southern Okla homa. The test was conducted in a 2%-acre pattern that was part of a 20-acre conventional waterflood pilot area. The conventional flood was well past its economic limit when the hot waterflood was initiated to obtain technical information and operating experience. Temperature data from nine observation wells showed that about 75 percent of the pattern was affected by heat, and that heat losses were severe in the pilot pattern. About 60 percent of the injected heat was lost to overburden and underburden zones during hot-water injection. Wellbore heat losses were held at tolerable levels at the shallow depth of the test by providing a low-pressure air annulus between the injection tubing and well casing. Hot water provided water injectivity increases of 200 to 400 percent. The hot water channeled across the lower portion of the oil sand in three directions through zones of relatively high water saturation. There was no conclusive evidence that natural fractures or pressure partings aflected the flow of fluids in the pilot pattern; however response undoubtedly was aflected by localized pressure gradients and by injection-production rate ratios. The results showed that hot waterflooding increased oil recovery in a reservoir containing 600 cp oil. The total tertiary oil production from the pilot pattern area was 3,896 bbl or about 156 bbl/acre-ft swept by heat. The corre.sponding WOR was about 34:I. Description of the Hot Waterflood Process To hot waterflood an oil reservoir, water is injected that has been heated to a temperature substantially higher than the original reservoir temperature, but lower than the vaporization temperature of water at the prevailing pressures. In the reservoir the hot water flows continuously into cooler sand and rapidly loses heat to the sand until it has been cooled to the original reservoir temperature. Thus, a heated zone and a region or "bank" of cooled water begins to accumulate immediately after hot water injection is started. This bank of cooled water continues to grow ahead of the heated zone, which also grows, but at a slower rate. This occurs because heat transfer is almost instantaneous, and the ratio of heat capacities of water to rock is such that two or three unit PV of hot water must be injected to heat a given unit bulk volume of the reservoir. The primary displacement mechanism is the same for both hot and conventional cold waterfloods; i.e., "piston" displacement occurs at the original reservoir temperature. The incremental benefits of hot waterflooding usually occur long after the breakthrough of cold water at producing wells, and the increased oil recovery necessarily is accomplished with high WOR&apos;s (water-oil ratios). Heat decreases the viscosity and density of oil and water. These effects result in more rapid and increased recovery of secondary or tertiary oil. If the cost of the required heat is low enough, the ultimate oil recovery of a hot waterflood should be increased substantially over what would be expected at the economic limit of a conventional cold waterflood. The economic benefits of any hot-fluid injection project depend primarily upon the cost of the heat required to produce more oil at an increased rate. This cost depends in part upon the amount of heat lost to surrounding formations. Heat loss depends upon reservoir thickness, water injection rate and temperature, the depth of the formation, well spacing, and the characteristics of the reservoir rock and surrounding formations. In general, percentage heat losses decrease as injection rate and reservoir thickness increase. Although it is an old idea, hot-water injection has not received widespread field application in the oil industry as a drive process. Much of the original field work with hot water was done in Pennsylvania fields where water permeabilities and injection rates are low. In these cases, hot-water injection was used primarily as a means of increasing in-jectivities — not as a recovery process. Ramey&apos; recently has published an excellent review of the development of hot fluid injection processes. Recent publications"&apos; and our own experiences now indicate that hot water or steam injection also can effectively increase the oil recovery from reservoirs containing viscous crudes. However, the economics of these methods as displacement processes have not been established. Several theoretical predictive techniques have been published (for a review see Ramey&apos;), but simplifying assumptions make

Jan 1, 1969

By H. A. Bedworth

ALLOYS of copper and silicon have been known for one hundred years or more but the commercial development of this type of alloy has taken place during the past few years. In 1905, Sperry1 proposed the use of copper-silicon alloys for springs and other purposes for which copper-tin bronzes were used. Some attention was given to this proposal at the time but no one succeeded in producing a practical alloy containing more than a fraction of a per cent. of silicon. The equilibrium relations of the copper-silicon system were studied first by Rudolfi2 and later by Sanfourche3 and Corson.4 The constitution of the system has also been recently investigated by Matuyama,5 and in the laboratories of the American Brass Co. by Smith.6 Some of the physical properties of the copper-silicon alloys have been investigated by Norbury7 and by Geiss and Van Liempt.8 Summarizing the results of various investigators of, the constitution of copper-silicon alloys, the solubility reaches its maximum value, 6.7 per cent. silicon, between 721° and 782° C. At 852° C. the solubility is 5.25 per cent., while at 400° C. it is only 4.1 percent. silicon. The copper-silicon alloy begins to get so hard at about 3 per cent. silicon that it is difficult to manage. It was found by Jacobs that the addition of manganese to this alloy considerably improved the working

Jan 1, 1929

By N. P. Goss

ASTERISM appearing in X-ray Laue dia-grams is an extremely sensitive index of changes in the internal structures of indi-vidual grains of polycrystalline metals. It indicates the existence of various forms of subboundary structure or subdivision within the grain. The present viewpoint is that the grain is made up of lattice blocks having substantially the same size and shape.1-4 When these blocks all assume exactly the same orientation, the crystal is perfect and asterism is absent. Cleaves and Thompson5 observed that the hardness of iron is virtually constant over a range of grain sizes. It is quite possible that the subboundary structure caused this, and that the latter is just as important as grain size itself. While the experiments reported here are not con-clusive, they do support this viewpoint. Metals can, under certain conditions, be prepared entirely free from asterism, but this preparation does not necessarily require long heating or slow cooling, as will be shown here. In this paper a distinction is made be-tween mosaic and distorted grain struc-tures but the difference is only a matter of degree. In a previous paper9 it was shown that the grains can become distorted even during heat-treatment. The block structure exists inherently, even in a perfect crystal; the size and shape of these crystallites, or lattice blocks, varies, depending upon a number of factors. Goetz, for example,7 has shown that a metal before crystallizing from the molten state must go through a paracrystalline phase with oriented groups of atoms about 10-14 to 10-15 c.c., or 10-5 cm. in size.

Jan 1, 1940

By Ellis Clark

The mining town of Pribram is situated in Central Bohemia, on the western slope of the Heiliger Berg. 30 miles southwest from Prague. Birkenberg, the village ill which most of the shafts and ore-dressing establishments are situated, is built on a mountain of the same name. It is about a mile from Pribram, is 1700 feet above the sea, and is surrounded by graywacke rocks of Silurian origin, which arc intersectd by greenstone dikes, and in the southerly, southeasterly, arid southwesterly direction are bounded by granite. The graywacke formations consist on one side of graywacke sandstone and quartzite, and on the other of graywacke slate. These last are separated from the first in the immediate vicinity of the mines by a graywacke seam converted into clay. For many years this so-called clay seam (lettenkluft) was considered as a boundary of the ore deposits in both zones of graywacke. The graywacke formation L divided according to its harduess, structure, texture, and color, into fine, coarse, compact, slaty, whitish-gray, reddish-gray, and black graywacke. The miner divides the formation into four divisions. The first or lowest division, which is in contact with the granite, consists of a fine-grained dirty gray slate; the -second is a very fine to a very coarse schist, white to reddish-gray in color, and rich in quartz, but containing little mica; the third consists of a slate with a confused cleavage, which has a dirty gray, dark gray, and very often black color and is often graphitic in its composition; the fourth consists of a fine to coarse-grained graywacke schist, of a grayish-white or reddish-gray color, and rich in quartz. The cleavage in all four divisions strikes from northeast to southwest, and the dip is sometimes northwesterly, sometimes southerly, and often vertical. All four zones are cut through by a great number of diorite arid greenstone dikes and chimneys. The thickness of these dikes, which are of

Jan 1, 1881

By John H. Schemel

Large Zircaloy-2 hammer or press forged bars did not exhibit the uniform excellent corrosion resistance to steam normally expected of the alloy in wrought form. Weight gains of coupons cut from forged bars were 40 to 60 mg per sq dm compared to the 28 mg per sq dm obtained on hot rolled sheet and strip. The mechanism of this corrosion and its relation to microstructure is discussed. After these observations, a solution heat treatment followed by rapid cooling was tried on coupons from eight heats of forged bars. The basket-weave structure resulting from the quench did not show agglomeration of intermetallic compounds. These coupons showed uniformly good corrosion resistance with weight gains very close to the 28 mg per sq dm expected of Zircaloy-2 after the 14-day steam test. A large forging was solution heat-treated and tested for structure, mechanical properties, and corrosion resistance. Corrosion resistance was excellent and uniform throughout the section. The normally anisotropic mechanical properties were changed to completely iso-tropic. Strength levels were raised while there was a small loss in ductility at the service temperature. Tempering of the quenched structure below the ß transus did not improve the ductility at the test temperature of 600°F. ZIRCALOY-2 end caps for nuclear fuel elements Zircaloy-2 is an alloy of 1.5 pct Sn, 0.1 pct Fe, 0.1 pct Cr, and 0.05 pct Ni, balance hafnium-free zirconium patented by Westing-house Electric Co. used in pressurized water reactors are machined from large hammer-finished forged bars. The bars forged for this application range from 3 1/2 in. to 7 1/2 in. squares. One of the tests used to evaluate Zircaloy-2 for this service is a 14-day exposure to very high-purity steam at 75oF and 1500 psi pressure. Normally wrought products will exhibit a black lustrous film of zirconium oxide after the test and show a weight gain of approximately 28 mg per sq dm. Coupons representing the forged bars exhibited a wide variety of corrosion results ranging from acceptable black coupons to some covered with white crystals of zirconium oxide that had weight gains of nearly 100 mg per sq dm. One of the most common effects was a white corrosion product that looked like a stain to some observers and the outline of massive metal grains to others. Very careful specimen preparation prior to the corrosion test did not affect the result and metallographic examination did not reveal a structural feature of a size and shape that would correlate with the corrosion product. In addition to the relatively poor corrosion resistance, the forged product was not as ductile as desired. The problem of obtaining uniform and more acceptable properties in these heavy-forged sections seemed to be a function of the microstructure of the metal and, in particular, the distribution of the intermetallic compounds. None of the four alloying elements however are appreciably soluble in a zirconium and are present as compounds which usually appear scattered randomly throughout the structure. Moudryl showed that the distribution of these intermetallic compounds in Zircaloy could be related to a ostringero corrosion failure. Grozier et al. discussed another structural defect that causes a similar corrosion effect. In this case, an elongated gas-void was determined to be the cause. M. L. Picklesimer held in his discussion of the Grozier paper that at least a part of the observed =stringersn were caused by the distribution of the intermetallic compounds. He proposed a

Jan 1, 1962

By Glenn Allen

SAN FRANCISCO Mines of Mexico, Ltd. owns and operates an extensive group of claims in the San Francisco del Oro-Santa Barbara district, about 15 miles southwest of Parral, Chihuahua. The property comprises the mines, aerial tramways, flotation mill, power plant, shops, offices, assay and testing laboratories, modern hospital, water and sanitary system, quarters for miners, mechanics and operators, a well housed colony for Mexican staff employees and residences for foreigners. Each colony has a club house and mess and tennis courts. The employees have constructed a nine-hole golf course. In other words, the property is self-contained and completely integrated for production of lead and zinc concentrates from complex sulfide ores.

Jan 1, 1930

By H. L. Lovell, L. H. E. Weyher

Cyclones have been used successfully in the mineral industries to solve solid-liquid as well as solid-solid separation problems in the processing of fine particles. Substantial information is available about the operation of cyclones as thickeners, classifiers, and concentrators using a dense medium. However, very little is known about the operation of the cyclone as a fine coal concentrator not using dense medium. This application of the cyclone, namely to wash fine coal in water, requires that classification phenomena be minimized in order to arrive at an effective separation of the high density ash and sulfur-bearing mineral particles from the low density coal particles over a wide particle size range. The authors have investigated the role of feed pressure, orifice diameters, and vortex-finder length in the cyclone washing of fine coal (--1/4 in.) in water. The results of this investigation show that cyclone washing of fine coal in water is an effective unit operation particularly capable of reducing the inorganic pyritic sulfur content. The combination of hydrocyclones with complimentary equipment such as Sieve bends, shaking tables, and flotation units appears to be especially promising and may ultimately yield fine coal processing systems that could approximate the high recovery efficiencies of today&apos;s coarse coal cleaning circuits. In the future, fine coal beneficiation can be expected to receive even greater research emphasis as a result of increasing sulfur restrictions on all major coal markets. In a previous paper, work, conducted at the Pennsylvania State University, on the hydrocyclone washing of fine coal was discussed.&apos; The initial evaluation based on that wo-rk demonstrated the feasibility of hydrocyclones as fine-coal cleaning devices, and in that previous paper selected test data were presented that showed in principle how product yield and assay respond to variations of the major cyclone operating variables. The present paper reports in greater detail on the findings and presents a comprehensive evaluation of the data as follows: (1) Hydrocyclone throughput rates were related to feed pressure and other variables by regression equations. These equations are compared with other capacity-vs.-pressure drop expressions taken from the literature on classification cyclones. (2) The flow ratio was found to be the most important variable for the separation of the solids. Control of this ratio through various cyclone operating parameters is discussed. (3) The data on the product yield as well as the ash and sulfur assays from the tests were evaluated by means of correlation and multiple regression analyses. Because size-classification phenomena cannot be suppressed completely in hydrocyclone washers, product yield and assay data are regressed against cyclone operating variables separately for different size classes. These equations then reveal how the interactions of the cyclone operating variables vary in terms of the separation for different size classes. (4) Density partitions from additional tests were analyzed by supplementing product-size analyses with sink-float analyses of the separated product size classes. The evaluation of these data show how classification phenomena affect separation by density. The results demonstrate in particular the feasibility of the hydrocyclone washer for removing pyritic sulfur from fine coal. In addition to these specific findings, the investigation points up the value, in general, of using hydrocyclone washers in combination with unit operations such as screening, table concentration, and flotation. In order to make optimum use of the hydrocyclone washers and work out the most effective combination of unit operations, it is important to have careful flowsheet analyses corresponding to the given feed and product requirements. Analyses of this kind are now possible by means of computer simulation of flowsheets and other operation research tools. INTRODUCTION Before proceeding with the detailed treatment and evaluation of our results, it will be useful to review the fundamental aspects of cyclone separators and also restate the experimental procedures and data handling employed in these studies. Review of Cyclone Fundamentals: AS shown in Fig. 1, the basic components of cyclones commonly used

Jan 1, 1970

By Charles H. Jacoby, Stanley J. LeFond

Salt, or halite, has a long and most varied history. While we know the Chinese were producing salt as early as 3000 B.C., the first written reference to salt appears in the book of Job recorded about 2250 B.C., which reads: "Can nothing which is unsavory be eaten without salt?" We do not know when man first used or realized that he needed salt. Perhaps one of our early Eolithic ancestors noted a piece of salt shining along the shore of a salt lake or a bay. He may have been attracted by its shining luster and tasted it. He found that it had a tart, zesty, distinctive flavor and perhaps chewing a large piece, became ill. However, by experimentation he soon learned that taken in the proper proportions salt was a very pleasant additive to his food. He may have noticed, too, that it increased his feeling of well-being. Thus, when the curtain of recorded history rises, we find man using salt for his health&apos;s sake, seasoning his food with it, feeding it to his animals, and using it in many superstitious and religious ceremonies. These uses, however, are a far cry from the uses for salt today. The first attempts of white man to make salt in continental United States were reported in the year 1614, while the first commercial production was in 1753 from the Kanawha licks. Practically all this salt was for human consumption, preserving food, and curing hides. Prior to the coming of the white man, Indians are known to have made salt from salt springs such as those that existed at Avery Island, LA, Charleston, WV, Saltville, VA, and Onondaga, NY. In 1862 the first rock salt was mined in the US from the Avery Island salt dome. Almost immediately thereafter, rock salt was mined at Saltville, VA and then at Retsof, NY in 1885. Of the more than 39 million tons produced annually in the United States, about 58% or 23 million tons are consumed by the chemical industry in the production of chlorine, caustic soda, hydrochloric acid, sodium metal, and some 30 other basic chemicals. These basic chemicals, in turn, are used in the preparation of approximately 14,000 chemicals which range from soap and detergents, to such chlorinated hydrocarbons as DDT, BHC, carbon tetrachloride, etc. Utilization of cavities created in salt beds and domes has grown rapidly since 1947 until now the waste salt is creating an ecological problem. The uses for both dry- and solution-mined cavities range from the storage of liquid hydrocarbons to containerized storage of toxic wastes, from compressed air for the peak shaving of power to storage of nuclear wastes. Geology Mineralogy Properties: Because of its simple structure, halite, the mineralogical name for salt, was the first structure to be analyzed by X-rays. It has the following properties: Formula: NaCl (Na-39.34%. Cl2-60.66% ) Crystallography: isometric, hexoctahedral, 4/m 32/m Space group: Fm3m A0: 5.627 kX Cell contents: Na4CI4 Habit: usually cubic, rarely octahedral, massive, granular to compact Physical properties: Refractive index: 1.554 Twinning: observed on {111} Cleavage: {001} perfect Fracture: conchoidal, brittle

Jan 1, 1983