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By S. Feuerstein, L. Rice

The effect of low pressures on the flow and fracture behavior of molybdenum is described. For poly crystalline samples, room-temperature tensile tests indicate greater ductility under 10 Torr than under intermediate pressures up to and including atmospheric pressure (760 Torr). In addition, tests conducted at 760 Torr under atmospheres of air, dry nitrogen, and purified argon exhibited no apparent difference in mechanical properties. Critical tests involving baking in situ as well as those involving single-crystal deformation further imply that the ductility effect is a pressure-dependent phenomenon related only to the fracture process. This dependency is discussed in terms of adsorption and diffusion contributions. THE effect of very low pressures on material properties has heretofore been presumed to be important only for substances possessing relatively high vapor pressures at ambient temperatures. Research has therefore been concentrated primarily on organic solids and liquids, and in some instances on metals such as zinc and cadmium. Most vacuum-effect studies' on the mechanical behavior of metals have been performed under conditions of either cyclic loading or creep rupture at elevated temperatures, i.e., over extended time periods. These studies were not restricted to high vapor pressure materials but also encompassed such metals as gold, copper, and nickel. Very little concern, however, was placed upon the importance of a vacuum environment on the mechanical behavior of metals subjected to a simple unidirectional deformation at ambient temperatures. A tension test is generally of short duration as compared to a creep test, and at room temperature vacuum effects if any would be expected to be surface-limited. In early 1963, Kramer and podlaseck2 reported a change in the bulk flow behavior of aluminum single crystals during room-temperature tension tests. The deformations were performed under pressure conditions of 760 to 3.4 X 10-8 Torr and indicated for the first time a vacuum surface effect contributing to the bulk tensile behavior of metal specimens. As a consequence, an experimental program was initiated in this Laboratory to study the effects of ultrahigh-vacuum conditions on the mechanical behavior of metals. The results of a preliminary study on poly-crystalline molybdenum3 revealed, unlike Kramer's observations of changes in the stress-strain behavior, only an increased ductility under ultrahigh vacuum. Flow behaviors were nearly identical for all tests re- gardless of pressure. This paper presents comprehensive results obtained in this area of research. 1) EXPERIMENTAL PROCEDURE Three material categories were used in this study: sintered and are-cast polycrystalline molybdenum of nominal purity 99.93+ pct and single-pass electron-beam zone-refined molybdenum single crystals having a nominal purity level of 99.99+ pct. The interstitial levels (weight percent) as determined by the Materials Testing Laboratories, Division of Magnaflux Corp., were as follows: sintered molybdenum (C— 0.005, H—0.0004, O—0.015, N—0.008); and arc-cast molybdenum (C-0.0038, H-0.0003, O-0.015, N-0.023). Single-crystal molybdenum obtained from Materials Research Corp. had a typical interstitial analysis of C-0.0015, H-0.00007, O—0.00045, and N-0.0001. Tensile specimens having a 5 mm diam by 50.8 mm length were prepared from these materials. An average grain diameter of 0.059 mm was obtained for the sintered specimens following a 4-hr, 1600°C heat treatment. Grain sizes from 0.019 to 0.149 mm were obtained in the arc-cast specimens following heat treatments from 1100° to 1600°C for 1 hr. This series of specimens was used exclusively for the grain-size effect studies. All samples were electrolytically polished in 97 pct sulfuric acid solution prior to testing. Experiments were performed at room temperature in an ion-pumped ultrahigh-vacuum system positioned in an Instron tensile machine, Fig. 1. A constant strain rate of 4.2 x 10-4 sec-1 as derived from crosshead displacement was assumed for the deformations. Starting vacuums ranged from 2 to 0.5 X 10-10 Torr. These pressure measurements were made using corrected values4 of an NRC Redhead gage. Comparative readings were also made against a G.E. triggered dis-

Jan 1, 1967

By N. H. van Lingen

A laboratory stud], has been made to determine what factors affect the penetration rate of roller bits, diamond bits and drag bits in rock drilling with clay /water muds. The rather simple relations that exist when pressures in and around the borehole are equal become more conzplicated when under down-hole conditions the penetration rate is hampered by the existence of a pressure differential between the mud at the hole bottom and the pore liquid at cutting depth. Expressions that have been derived for both the penetration rate and the magnitude of the pressure differential in permeable rock together fully account for operating, rock, mud and bit variables. In impermeable rock a similar pressure differential is caused by the bit action itself. In all cases, the pressure difierential and the reduction in penetration rate increase with the effectiveness of the plastering at the bottom of the hole by mud particles. Where bits are employed whose action is largely that of crushing, however, the plastering may become even more effective owing to the addition of rock particles rubbed into the pores of the rock. With roller bits, a plastically hehaving layer may be formed, which causes a further reduction in penetration. In the case of bits whose action is chiefly scraping, moreover, penetration may be arrested by the bit's becoming balled-up. The various adverse effects are reduced by thorough scavenging of the hole bottom. This paper shows how with jet bits the efficiency of such scavenging may he improved by suitable choice of the position of the nozzles. INTRODUCTION The reduction in a bit's penetration rate with increasing depth of hole has been the subject of many investigations. Various investigators ',' have independently reached the conclusion that this reduction occurs not so much because the rock-breaking process becomes more difficult as it does because the lifting of the rock fragments is impaired by a fluid pressure differential holding the fragments down. When such a pressure differential can be avoided, as in air drilling and to a smaller extent in water drilling, penetration rates remain high. Although the range of applicability of these techniques is being extended, most oil wells still have to be drilled with mud. In this paper we present the results of laboratory experiments carried out to determine what factors govern the hold down effect encountered in mud drilling. In the course of this investigation, the well known importance of bottom scavenging came more and more into prominence. Not only may it reduce the magnitude of the hold-down forces, but also it appeared to be a means of preventing the accumulation of a plastic mass of cuttings and mud on the hole bottom and bit which may cause penetration to cease almost completely. So that the effects of fluid pressures may be more readily understood, the factors that govern penetration rate in the absence of these pressures will first be discussed. The effect of down-hole pressures will then be assessed for the case of permeable rock where fluid pressures are well defined, and it will be demonstrated how rock strengthening due to confining can be accounted for. Subsequently, fluid pressures in less-permeable rock will be examined; we will show that in impermeable rock it is the bit action that governs fluid-pressure distribution and hold-down. In the case of poor scavenging and/or high bit load. cutting cake manifests itself. The effect, like various others. appears to depend on the type of bit used. From the very beginning, therefore, we shall base our discussion on the three main types of bits used in rotary oil-well drilling— roller bits, diamond bits and drag bits. Since space is limited, it will be impossible to make more than a passing reference to many aspects of the problem. Moreover. certain relations that are not of primary irnportance to our argument will unavoidably have to be stated in a somewhat dogmatic fashion, and the experimental data on which these are based necessarily must be omitted. EQUIPMENT The drilling experiments were performed on three machines, of which one has been designed for the realistic simulation of down-hole pressure conditions. HIGH-PRESSURES MACHINE In this machine (diagramed in Fig. 1) the mud, pore and confining pressures can all be adjusted independently. The foil-covered rock sample contained in the inner pressure vessel is confined by oil that is pressurized by means of a hand pump. The pore space of the watersaturated sample is connected to an arrangement which keeps the pressure in the pore space constant regardless of the rate of filtrate flow through the sample.

By G. H. Wilson

INTRODUCED in 1946 to serve a need in power-plant operation, closed-circuit TV has been used by well over 200 organizations in approximately 25 different industries. Known as industrial television, or simply ITV, it can be described as a private system wherein the television signal is restricted in distribution, usually by confinement within coaxial cable that directly connects the TV camera to one or several monitors, Figs. 1, 2. The picture is continuous and transmission is instantaneous, permitting an observer to see an operation that may be too distant, too inaccessible, or too dangerous to be viewed directly. Destructive testing or the machining of high explosives can now be conducted hundreds of feet away by personnel who still have close control through the eyes of the TV camera. It is also possible for one man to control operations formerly requiring the co-ordinated efforts of several workers. For example, at a large midwestern cement plant conveyance of limestone from primary crusher to raw mill and loading into five storage bins once necessitated the work of two men, one having little to do but prevent spilling of material by manually moving the tripper on the belt conveyor as occasion required. TV cameras mounted on the tripper now provide bin level indication to the conveyor operator at the crusher position so he is able to control the entire loading operation remotely, Fig. 3. By means of a switch, the picture from either camera is alternately available on a single viewer, or monitor, Fig. 4. Each camera is mounted on the tripper by means of a simple adjustable support and looks down into the bin, which is identified by the number of cross members on the vertical rod. Each associated power unit is located on a platform above the camera, Fig. 5. This centralized control by means of TV often has produced superior results, and in many instances saving in operating costs has been sufficient to write off equipment costs within six months to a year. Where a key portion of a process may be enclosed or otherwise inaccessible, TV again reduces the likelihood of mistakes and permits closer control by making available to the operator valuable information he might otherwise never possess. An example of this can be found at a strip mine where the coal seam lies 50 ft or more below the overburden, which is removed by a large wheel shovel. From his centrally located position the shove1 operator was unable to judge accurately to what extent the wheel buckets engaged the earth. His chief indication of efficiency was the amount of overburden on the belt conveyor as it passed his control point 75 ft from the wheel. Now, two television cameras mounted on the tip of the boom permit the operator to view the wheel from each side and provide him with a close-up view of the buckets so that he can take immediate and continuous advantage of their capacity, quickly compensating for ground irregularities and avoiding obstructions, Fig. 6. While the word television conjures up visions of highly complex and intricate apparatus such as that employed in modern TV studios and transmitting stations, the term industrial television should indicate compact, straightforward equipment. Most present-day ITV systems contain fewer than 25 tubes including camera and picture tubes. The average home television receiver alone requires at least that many tubes. Equipment like that illustrated in Fig. 1 contains only 17 tubes, of which 3 are in the camera. It can operate continuously and dependably, without protection, in any temperature from 0" to 150°F. It consumes less current than a toaster and weighs under 140 lb. Camera and monitor may be separated by 1500 to 2000 ft and by greater distance with additional amplification. This equipment is designed to withstand vibrations up to 21/16 in. and will operate successfully under more severe conditions of vibration and heat when suitable enclosures are provided. Any number of cameras may be switched to a single monitor, and any number of monitors, within reason, used simultaneously. Two types of applications in the mining industry have already been described. A third under serious consideration by several organizations will make use of ITV for remote observation of conveyor transfer points at copper concentrating plants so that evidence of belt breakdown and plugging of transfer chutes can be spotted immediately and costly overflow of material avoided. A television camera will soon be installed to view a trough conveyor near the exit of an iron-ore crusher to indicate clogging of the crusher as evidenced by reduction or absence of material on the

Jan 1, 1955

By G. N. Goldberg, Robert A. Rapp

The steady-state kinetics and microstructures of simultaneous internal oxidation and external scale formation were investigated for the oxidation of Cb-Zr and Ch-Zr-Re alloys in pure oxygen at 1000°C. For each binary alloy, a constant rate of scale formation was observed at steady state; the internal oxidatton zone reached a steady-state, time-independent thickness. The dependence of the scaling rate on zirconium content exhibited a maximum at a low zirconium colttent; more concentrated alloys oxidized at a slower rate than pure columbium. This composition dependence of the scaling rate may be partially attributed to the effect of the internal oxidation process as an intenla1 sink for oxygen, with the formation of voluminous, and relatively impermeable ZrO2 precipitates. However, the morphologies of the ZrO2 internal oxide precipitates also affected the scaling rate. The internal oxide precipitates were distributed uniformly in the external scale. The steady-state thicknesses of the internal oxidation zones were not in agreement with those predicted theoretically from an idealized simple model. However, in this particular alloy systen1 the ideal model is not satisfied experitmentally. For ternary Cb- Zr - Re alloys with Nr10e = 0.02 or 0.05, the steady-state thicknesses of the internal oxidation zones were less than those for the corresponding binary Cb-Zr alloys. For ternary alloys with NRe(0) - 0.05, a more adherent and much less porous external scale was formed, and a reduction in the kinetics of scale formation was observed. A number of authors'-7 have reported linear oxidation kinetics for the reaction of pure columbium at 1000°C in air or in oxygen of about 1 atm pressure. A thin and tightly adherent oxide layer is found at the metal/oxide interface beneath a porous external layer of scale. Although the suboxides CbO and CbO2 represent thermodynamically stable phases at 100O°C, generally only Cb2O5* is identified as a reaction product in quenched specimens. Studies at 1000°C at lower oxygen pressures8,10 (Po2 - 10-4 Torr) show that both CbO and CbO2 do form and that CbO2 is a protective oxide. The growth of CbO2 results in parabolic kinetics until Cb2O5 is nucleated and grows. Apparently because of the large volume change associated with its formation, Cb2O5 is porous and does not serve as a diffusion barrier; linear kinetics prevail after the surface is covered with Cb2o5. On the basis of these observations, several authors5,9,10 have suggested that the linear oxidation of pure columbium at 1000°C in air or oxygen of 1 atm is limited by a Loriers-type mechanism,11 whereby the total rate or reaction is controlled by ionic diffusion through a thin layer of CbO2 which is maintained at a constant thickness throughout the linear oxidation. However, the concept of a Loriers model for a three-phase CbOlCbO2 Cb2O5 scale, with the only oxygen activity gradient across the NbO2 phase, is not self-consistent. Further, the suboxides CbO and CbO2 were not observed in the high-temperature X-ray diffraction study of columbium oxidation by Goldschmidt.8 From investigations in which the large PO2, dependence of the linear scaling rate was demonstrated, the importance of an oxygen adsorption or dissolution step has been suggested.4,5,7,10,12 Thus the mechanism for the linear oxidation of pure columbium remains quite controversial. Since further insight into the oxidation mechanism of pure columbium is not provided by this investigation, the authors wish to emphasize at the outset that their experimental results are not interpreted in terms of a particular rate controlling step for the oxidation of pure columbium. Previous investigations13-18 of the oxidation of Cb-Zr solid-solution alloys in air or oxygen at 1000°C suggest a remarkable dependence upon zirconium content. For an alloy of bulk zirconium mole fraction, N2r(0) equal to 0.05 or 0.10, the oxygen uptake is reported to be as high as four times greater than that for pure columbium;13,14 for alloys with NZr(0) 0.05 or 0.10 the oxygen uptake is reported to decrease with increasing NZr(0); to a minimum uptake of about one quarter that for pure columbium at NZr(0): = 0.50.13-15Since zirconium forms a more stable oxide (ZrO2) than the lowest columbium oxide (CbO), and since columbium exhibits a high solubility19,20 and diffusivity21,23 for oxygen, the internal oxidation of the zirconium component to ZrO2 is expected at a reaction front ahead of the advancing metal/scale interface. The external scale is then formed at the metal/scale interface by the inward migration of oxygen through the scale, probably through a series combination of molecular and ionic diffusion. Internal oxidation in conjunction with external scale formation has been investigated by Maak24 for the oxidation of dilute Cu-Be alloys in pure oxygen at 850°C. For cu-Be and many other binary alloys,24-27 very small, essentially uniaxial internal oxide particles are formed in the most dilute compositions; for somewhat more concentrated alloys. the internal oxide particles precipitate as platelets or needles. From pertinent solutions to the diffusion equation, Maak28

Jan 1, 1967

By R. F. Mehl, M. Gensamer

Creep investigators have made extensive studies to determine the interrelation of stress, temperature and the tensile creep rates of metals. It has been suggested that at small stresses the secondary or constant creep rates obey a simple viscous law. Building upon this suggestion, departure from pure viscosity as stress increases may be expressed mathematically as a consequence of reversibly altered viscosity or "flowability" in the same sense that temperature change reversibly alters viscosity. From the index to alteration of viscosity, a value for the energy of secondary creep may be derived having the magnitude of the free energy of vaporized metal. The suggestion is made that application of stress alters the energy of secondary creep. Strain energy is argued to be but a minor factor in the energetics of secondary creep. A deformation mechanism involving the large energy associated with secondary creep implies a sort of solid self-diffusion process. Evidence indicates that creep strain above the recrystallization temperature takes place by crystallographically directed self-diffusion at grain boundaries and points of crystal defects. A self-diffusion theory of secondary creep is proposed, embracing the principles of the Dushman-Langmuir theory of solid diffusion. An equation is suggested whereby the rate of tensile creep may be related directly to the physical and structural character of the solid metal. Basis of Investigation Much of the investigation that has been given to the creep characteristics of metals and alloys has been directed toward studying the dependence of creep rate upon stress. Great interest has centered upon the approximately uniform rate of flow that has been demonstrated for numerous metals and alloys. At temperatures above the strain-hardening ranges of materials, this uniform rate frequently is attained after a relatively short period of initial rapid flow, and the period during which it persists determines for most practical purposes the useful life of the

Jan 1, 1938

By R. F. Mehl, M. Gensamer

Creep investigators have made extensive studies to determine the interrelation of stress, temperature and the tensile creep rates of metals. It has been suggested that at small stresses the secondary or constant creep rates obey a simple viscous law. Building upon this suggestion, departure from pure viscosity as stress increases may be expressed mathematically as a consequence of reversibly altered viscosity or "flowability" in the same sense that temperature change reversibly alters viscosity. From the index to alteration of viscosity, a value for the energy of secondary creep may be derived having the magnitude of the free energy of vaporized metal. The suggestion is made that application of stress alters the energy of secondary creep. Strain energy is argued to be but a minor factor in the energetics of secondary creep. A deformation mechanism involving the large energy associated with secondary creep implies a sort of solid self-diffusion process. Evidence indicates that creep strain above the recrystallization temperature takes place by crystallographically directed self-diffusion at grain boundaries and points of crystal defects. A self-diffusion theory of secondary creep is proposed, embracing the principles of the Dushman-Langmuir theory of solid diffusion. An equation is suggested whereby the rate of tensile creep may be related directly to the physical and structural character of the solid metal. Basis of Investigation Much of the investigation that has been given to the creep characteristics of metals and alloys has been directed toward studying the dependence of creep rate upon stress. Great interest has centered upon the approximately uniform rate of flow that has been demonstrated for numerous metals and alloys. At temperatures above the strain-hardening ranges of materials, this uniform rate frequently is attained after a relatively short period of initial rapid flow, and the period during which it persists determines for most practical purposes the useful life of the

Jan 1, 1938

By D. A. Stevenson, R. A. Burmeister

Single-phase silver antimony telluride has been prepared by zone-melting techniques using initial compositions of A new phase appears upon prolonged annealing of this material, but the reaction does not appear to be a simple eutectoid decomposition. A complete analysis of the phase equilibria is complicated by the slow kinetics involved. The Hall coefficient, magneto -resistance, electrical resistivity, and Seebeck coefficient are all sensitive to the presence of second phases. The low Hall mobilities measured for single-phase material indicate that the usual band theory is inadequate to explain the observed transport properties in the system. Density anomalies of up to 2.5 pet between measured and theoretical density were observed but are not conclusive evidence for a defect structure. COMPOSITIONS in the Ag-Sb-Te system have been studied previously by several investigators.1"18 The interest in this system arises from potential thermoelectric applications of alloys on the Ag2Te-Sb2Tes vertical section. Although the composition corresponding to the formula AgSbTe, has received most attention, it has been found to consist of more than one phase.7'8 A thorough understanding of the properties of this heterogeneous material has been impeded by both lack of knowledge of the properties of the homogeneous phases comprising it and the problem of analysis of transport properties in an inhomogeneous system. The present work describes the preparation of the homogeneous ternary phase and the corresponding electrical properties of both homogeneous and heterogeneous material. MATERIAL PREPARATION Most specimens for this investigation were prepared by encapsulating the elements in evacuated quartz tubes after which they were melted and homogenized in the liquid state. The ambient temperature was then dropped to 500°C and the resulting ingot zone melted. The growth rate, width of zone, stoichiometry, and number of passes have an effect on the resultant microstructure. Grains several centimeters in length were easily produced by this method. Other solidification techniques were also used, including uniform slow cooling of the entire specimen and rapid freezing. The microstructures of specimens produced by these techniques frequently differed appreciably from similar compositions prepared by zoning. A variety of nonequilibrium microstructures characterized by long needlelike particles resulted from the rapid-freeze method. PHASE EQUILIBRIA The lack of information on phase equilibria is a major difficulty associated with a comprehensive study of the Ag-Sb-Te system. Considerable confusion has resulted from the use of the formula AgSbTe, to identify the cubic ternary intermediate phase even though it has been established that material of this stoichiometry normally contains AgzTe as a second phase.798 In this paper, silver antimony telluride will denote the cubic ternary intermediate phase comprising the major portion of AgSbTe,. The term "single phase" will denote material which consists of only the cubic phase (as evidenced by metallographic examination and X-ray diffraction) and the term heterogeneous will describe multiphase material containing AgzTe, SbzTe3, or other phases in addition to the cubic phase. The single-phase material may actually contain a variety of inhomogeneities—gradual changes in composition on a macroscopic scale, localized fluctuations in composition, clusters or other products of early stages of the precipitation process, and a variety of point and line defects—all of which will not be detected by the present techniques for determining homogeneity. Single-phase material has been prepared from compositions close to 59 mole pct SbzTe3 21 (this notation refers to the location on the Ag,Te-Sb2TeS vertical section). Zone widths of =2 cm and growth rates 51.2 cm per hr were used. The single-phase region at elevated temperatures extends off the vertical section to a composition which can be expressed approximately as Ag,,SbzgTes,.9 The latter two compositions as well as AgSbTe, are represented in the conventional Gibbs triangle in Fig. 1. It is not presently possible to ascribe exact values to the limits of the single-phase region on a given isotherm or vertical section due to the extremely

Jan 1, 1964

By H. H. Keller, E. J. Couch

Damage to production wells subjected to the high temperatures associated with in-situ combustion projects has been a problem since the advent of this thermal recovery technique. Injection of water down the annulus of hot wells has been successfully utilized for cooling and prolonging the life of such wells. A mathematical model that is suitable for predicting the effectiveness of cooling water in a particular application is developed. Typical results for practical ranges of the various parameters involved are presented. INTRODUCTION In the normal course of in-situ combustion operations, highly damaging conditions develop in the production wells as the combustion zone approaches, and these wells are subjected to high temperatures (up to 1500F). The resulting well damage is recognized as one of the more serious operating problems unique to the in-situ combustion process. Even in operations where well completions have been specifically designed to cope with this problem, the question arises as to how this destructively high temperature can be kept within tolerable limits. A simple and economical approach to this problem is to circulate cooling water down-hole. This method has been used with some success in shallow reservoirs. At greater depths, however, the heat exchange with the overburden surrounding the well and between the fluids in the tubing and the annulus tends to equalize the temperatures of the two fluid streams so that the cooling capacity delivered to the bottom of the hole decreases with well depth. This method would provide no appreciable control over the bottom-hole temperature at great depths. In order to delimit the condition under which cooling by water circulation is effective, the wellbore temperature must be related to the water inlet rate and temperature; to the reservoir depth, production rate, and initial temperature; and to the combustion at at bot tom-hole depth. A model that meets these requirements and that will offer an approach for developing engineering solutions to practical design and operating problems is described in this paper. MATHEMATICAL MODEL Previous studies of temperature distributions include those for flowing wells1p2 and those for hot fluid injection. Adams and Haddenhorst 6 presented solutions for the down-hole circulation of hot oil in the treatment of paraffin-deposition problems. In this paper the thermal model presented by Ramey 4 is adapted to the flow system shown schematically in Fig. 1. Water at temperature Ti is injected at a rate wi and flows down the annulus outside the tubing. It mixes at bottom-hole depth D with the fluids produced at race w from the hot reservoir at temperature T. This mlxtureJ. of injected water and reservoir fluids flows up the tubing and is produced at the surface at TI,. In order to describe the temperature response in this system, we make use of the usual conservation of

Jan 1, 1969

By George A. Moore, Donald P. Smith

In spite of many investigations of the occlusion of hydrogen in iron, the nature of the process and the reasons for the accompanying effects upon the metal are still open questions. This is in large part due to three causes: (1) the difficulty of obtaining iron of adequate purity as starting material; (2) the occurrence of allotropic transformations, which complicate the effects; and (3) the fact that the body-centered cubic modification does not lend itself readily to crystallographic investigation. The present paper attempts a critical review and correlation of the somewhat scattered and disconnected existing observations, and an experimental determination of the extent to which the conclusions that appear to follow from these are applicable to iron of really high purity, studied under well-defined conditions. Review Although only a comparatively few investigations have so far been made on the pure system iron-hydrogen, there is a much larger volume of literature which throws some light on the problem but falls short of a place in the systematic investigations, either because no attempt was made to measure equilibrium conditions or because the metal used was not iron or the gas not pure hydrogen. Such results have been variously dismissed in the past as of no importance, or as too complicated to try to explain; or they have been explained in terms of any of a dozen or more pictures, each of which is contradicted by data from other sources. The present importance of these data thus arises from their very mass and diversity, which present a picture of occlusion as a phenomenon whose variability cannot be ignored. We have attempted to organize the literature into groups comprising similar experiments or data leading to similar conclusions, thus of necessity sacrificing accuracy of historical order. Lattice Occlusion.—Throughout this discussion, the term "lattice occlusion" will be used to denote the formation of a simple solid solution of a gas in a metal lattice, usually of interstitial distribution. The word

Jan 1, 1939

By George A. Moore, Donald P. Smith

In spite of many investigations of the occlusion of hydrogen in iron, the nature of the process and the reasons for the accompanying effects upon the metal are still open questions. This is in large part due to three causes: (1) the difficulty of obtaining iron of adequate purity as starting material; (2) the occurrence of allotropic transformations, which complicate the effects; and (3) the fact that the body-centered cubic modification does not lend itself readily to crystallographic investigation. The present paper attempts a critical review and correlation of the somewhat scattered and disconnected existing observations, and an experimental determination of the extent to which the conclusions that appear to follow from these are applicable to iron of really high purity, studied under well-defined conditions. Review Although only a comparatively few investigations have so far been made on the pure system iron-hydrogen, there is a much larger volume of literature which throws some light on the problem but falls short of a place in the systematic investigations, either because no attempt was made to measure equilibrium conditions or because the metal used was not iron or the gas not pure hydrogen. Such results have been variously dismissed in the past as of no importance, or as too complicated to try to explain; or they have been explained in terms of any of a dozen or more pictures, each of which is contradicted by data from other sources. The present importance of these data thus arises from their very mass and diversity, which present a picture of occlusion as a phenomenon whose variability cannot be ignored. We have attempted to organize the literature into groups comprising similar experiments or data leading to similar conclusions, thus of necessity sacrificing accuracy of historical order. Lattice Occlusion.—Throughout this discussion, the term "lattice occlusion" will be used to denote the formation of a simple solid solution of a gas in a metal lattice, usually of interstitial distribution. The word

Jan 1, 1939

By B. M. Larsen, T. E. Brower

IN an earlier paper1 we discussed a simple, rapid method of taking samples of liquid steel and analyzing them for oxygen, which, though possibly not absolutely accurate (as is likewise true of all other methods), certainly yields results that are satisfactorily consistent. Accordingly, samples from hundreds of heats in different shops were analyzed for oxygen, with results sufficient in number to be handled statistically and permit estimation of some general trends. Measurements were made in acid as well as in basic open hearths, throughout the refining period, to learn how stirring, blocking, adding ore or lime or sand, affects the oxygen content of the bath; we also followed the changes brought about by tapping, teeming, and deoxidizing. Some of these results, discussed in an earlier paper.2 bring out the dominant role of the carbon-oxygen reaction in regulating degree of oxidation both of metal and of slag, also the marked variability of concentration of dissolved oxygen [0] in excess of that which would be in equilibrium with carbon and with carbon monoxide at a partial pressure of one atmosphere. As a logical beginning on this complex problem, we take up in the present paper the variability of this excess oxygen, ?[O], when other factors are as constant as they ever are in open-hearth operation; namely, toward the end of the refining period, when the bath may be regarded as in the comparatively steady state it approaches in absence of disturbing factors. This condition was chosen because by that time the significant reactions, except carbon oxidation, between slag and metal have come to substantial equilibrium; this facilitates interpretation of the complex situation and thus permits more definite conclusions to be drawn. This excess concentration of oxygen, ?[0], in the metal is needed, of course, to make the steelmaking process go at a reasonable rate; alternatively it may be regarded as a measure of the virtual pressure increment above one atmosphere, or of the degree of supersaturation, of carbon monoxide in the metal. According to our measurements, the excess concentration ?[O] in liquid steel varies from about 0.009 to 0.035 per cent oxygen by weight. It is quite sensitive to change of conditions, being altered temporarily by operations such as stirring with green poles, additions of ore, lime, or sand; but as the disturbance works itself out, it resumes a level within the intermediate range characteristic of the steady state. The conditions most common in average furnace practice are covered by the following : [ ] as in a reasonably steady state-that is, when it is boiling normally, is at proper temperature with a well-shaped slag, and has been free from disturbing effects during the preceding half hour-?[O] returns from

Jan 1, 1946

By L. S. Castleman, H. A. Froot

A study was made of the growth kinetics of B-brass layers in a-brass us y-brass diffusion couples in which both phases were saturated in the 6 phase. It was found that useful estimates can be made of the difhsion coefficients at the ß-phase interfaces from interface displacement data, which are relatively easy to measure experimentally; also, a useful estimate can be made of the mean heat of activation for diffusion from layer growth data. The effects of pressure on layer growth kinetics were explored and found to be consistent with a vacancy model for diffusion in 6 brass in both the disordered and ordered temperature range. 1 HE study of multiphase diffusion receives relatively little attention in comparison with that devoted to diffusion in homogeneous materials. Of the hundred or so papers on diffusion written each year,' only a few are devoted to the subject, and it is the rare review article2,3 that devotes any space to multiphase diffusional phenomena. This is unfortunate, since the metallurgist frequently encounters practical situations involving cementation processes such as cladding, protective coating of metals, and so forth in which he needs guidance of a fundamental nature. The investigation of multiphase diffusion phenomena is complicated by the fact that one must consider reactions at phase interfaces as well as the migration of atoms within the individual phases; these reactions cause the interfaces to be displaced within the diffusion zone. The relative displacement of two adjacent interfaces corresponds to the growth of an intermetallic layer, and it is not difficult to determine experimentally the kinetics of layer growth. In the past few years it has been pointed out4,5 that valuable fundamental information may be gained about diffusion coefficients and the concentrations at interfaces through a study of their motion. Accordingly, it is the purpose of this paper to report the results of an investigation of interface motion in a simple multiphase binary system. In the work reported herein, attention was focussed on the growth of a 6 -brass layer in a diffusion couple prepared from a- and y-brass compositions saturated with respect to the 6 phase. This particular system was chosen for a number of reasons. First, the bcc ß-brass phase is disordered for all compositions at temperatures above 468°C and becomes increasingly long-range ordered for all compositions at temperatures below 454° C;6,7 thus, the effects of a variation in order on interface displacement could be determined. Second, diffusion coefficients have already been obtained as a function of temperature in the ß phase both in the ordered and disordered Re- and a theoretical picture of the mechanism of diffusion in this and other ordered solutions is emerging.11'12 Third, some thermodynamic data are available for the a-, ß-, and ?-brass phases,13,4 and these data could be used to gain insight into questions of phase equilibria and concentrations at phase interfaces.

Jan 1, 1963

By K. E. J. Rapperport, C. S. Hartley

The only slip system observed in zirconium crystals deformed at 77", 575", and 1075OK was (1010) [1210] with a critical resolved shear stress in tension of 1.0 kg per sq mm at 77°K; 0.2 kg per sq mm at 575 °K; and 0.02 kg per sq mm at 1075 OK. The active twin planes were {1012}, (1121}, (11221, and (11233) with varying temperature dependence. A detailed analysis for the slip direction using Laue spot asterism is appended. NeARLY all metals of the hexagonal close-packed structure exhibit basal slip, i. e.,(0002)<1120>- type slip. This is true of magnesium,&apos; zinc,&apos; cadmium,3 beryllium,4 titanium,= yttrium,6 and rhenium.Many of these such as titanium 5&apos;8-&apos;0beryllium,4&apos;" magnesium, and zinc13&apos;14 display other slip modes even at room temperature, and nearly all have been reported to slip on other systems under particular loading or temperature conditions of testing. As is shown in this paper, basal slip was not found at any of four test temperatures from 77" to 1075°K in hexagonal close-packed zirconium under the simple loading conditions of tension and compression, even though in one case the resolved shear stress on the inactive (0002) <llgO> system was twenty-five times higher than the critical resolved shear stress on the active (1010) [1210] system. This result is consistent with prior studies on the active deformation processes in zirconium deformed at room temperature. &apos;&apos;-I7 SPECIMEN PREPARATION A) Material—The zirconium used in this work was of two types: 1) as-deposited reactor grade crystal-bar, and 2) arc-melted and forged reactor grade crystal-bar. Typical chemical and spectrographic analyses of these materials as received, and after hydrogen removal and crystal growth are given in Ref. 17. Crystals of type 1) above have the letter prefix (A) and those of type 2) have the prefix (B) throughout this paper. B) Crystal Growth— he zirconium was machined into rectangular parallelepipeds about 0.2-in. scl in cross section and 2 in. iong. These were hand polished through 4/0 abrasive paper, electropolished, given a hydrogen removal anneal, and subjected to long-time anneals at 840 °C in vacuo to produce usable crystals.&apos;7 A second technique used to obtain large crystals was to cycle the samples two or three times between 1200" and 840°C, allowing them to remain at the higher temperature for about 4 hr and at the lower temperature for 5 days.17 These techniques yielded some grains which occupied the entire cross section of the bar and were as long as 3/4 in. C) Orientation Determination—After the growth of large crystals by thermal cycling, the samples were repolished with extreme care through 4/0 abrasive paper and electropolished. Metallographic examination after polishing showed the surfaces to be free of visible deformation traces. Standard Laue back-reflection X-ray techniques were used to find the crystallographic orientations of selected large grains with respect to a specimen face and edge. Fig. 1 shows the stereographic projections of the stress axes for the crystals used. The sharpness of the spots on the Laue photographs indicated that the crystals were of good quality. EXPERIMENTAL METHODS Nine crystals were deformed in tension at 77"K, nine in tension and five in compression at 300°K in previous tests,17 fifteen in tension at 575"K, and eleven in tension at 1075°K. All specimens were stressed by load increments. After a predetermined load was applied, the specimen was removed from the loading appratus and metallographically examined for deformation traces. An attempt was made to initially stress each bar so that some crystals slipped a small amount and others not at all. This was done to bracket the critical resolved shear stress. One bar of special orientation (B-11) was repolished and annealed at 1075°K for 1 hr after lower temperature deformation, before final deformation at 1075°K. In the other bars the loading by increments, followed by metallographic examination, was continued until the surface distortion would interfere with analysis, or until fracture. One example of a crystal pulled to fracture is shown in Fig. 2. This photograph shows a crystal (B-14C) which was pulled at 1075°K and failed by slip on two (10i0) planes. The approximate orientation of this crystal is illustrated in the figure. Specimens were deformed at 77°K in liquid nitrogen on a tensile machine using an insulated bucket with an internal hook to accept a clamped specimen.

Jan 1, 1961

Jan 1, 1892

By Arvid Anderson

THE weathering of copper-bearing ores with the formation of a water-soluble salt and the recovery of the metal by leaching and evaporation or precipitation, are processes long known, which have at various times been utilized with more or less commercial success. It is commonly assumed that the technical principles involved are quite simple and their application to a particular case easy. If these assumptions were true, we should anticipate a long list of uniformly successful leaching operations, which is not the case, and one would be justified only in calling attention to either unique or peculiar features of any particular enterprise; whereas, in studying the problems of the recovery of copper from the old workings of the Ohio Copper Co. in the light of available descriptions of other leaching projects, we have not found the assistance hoped for to guide us to the best realization of our own opportunities. It appears desirable, therefore, to call attention to these guiding principles, together with a description of the facts of accomplishment. Justification lies in the fact that the leaching and precipitation of copper at the Ohio Copper Co. mine in Bingham Canyon, Utah, is successful. This success is measured by an average monthly production of 600,000 lb. of copper at an average operating cost, to date, of 3.85 cents per pound at the company&apos;s workings, or 6.32 cents per pound after paying shipping and smelter charges on the finished copper. A total of 17,076,099 lb. of copper had been shipped to the smelter from the beginning of operations, August, 1922, to April 1, 1925. Probably these results can be bettered with further study and realization of the factors involved and the devising of methods of meeting them. It is now an assured fact that the enterprise will have a relatively long and continuously profitable life and that its reserves will not, nor cannot, be suddenly and permanently depleted.

Jan 9, 1925

By Robert S. Baker

It has been demonstrated in the laboratory by A. J. Phillips1 that a transformation or conversion from beta directly to alpha may take place in a brass of 61 to 62.5 per cent copper content. The completion of the transformiation is dependent on a rapid rate of cooling from the all-beta field through the alpha + beta range to the alpha field. Phillips states that in a slowly cooled alloy containing 62 per cent copper and 38 per cent zinc the copper content of the beta is progressively decreased from 62 to 56 per cent by precipitation of alpha. Rapid cooling tends to prevent the separation of alpha with a copper content of more than 62 per cent by reducing to a minimum the time required for passing through the alpha + beta range. Upon crossing beyond the (alpha + beta) (alpha) boundary to the all-alpha region below, the material is transformed from beta to alpha. It, is essential that there be no change in composition. Phillips obtained his results by quenching a 62:38 copper-zinc alloy from 850" C. in iced brine at -8" C. No reference to the occurrence of this transformation in a manufacturing process has been found in the literature. An investigation of the microstructures of a number of hot forgings made from leaded brass rods yielded one forging in which this striking conversion from beta to alpha had occurred. The purpose of this paper is to describe the transformation and certain conditions under which it may occur during the hot pressing of brass. The conversion was noted in a shape forged from a leaded brass rod, the composition of which was: Cu, 60.26 per cent; Zn, 37.86; Pb, 1.88. In this study the lead content was disregarded and the alloy was considered to be equivalent to an alloy of 61.40 per cent copper and 35.60 per cent zinc (9812 parts = 100 parts). The possibility that the lead might obstruct or accelerate the precipitation of alpha was not studied. The lead appears as black globules in the photomicrographs and has a negligible solubility in the alloy.

Jan 1, 1932

By David R. Mitchell

The mineral pyrite (or marcasite) occurs in coal beds as balls, lenses, veinlets and bands. Several million tons are wasted annually on the refuse dumps from coal mining and coal-preparation activities. Sporadic attempts have been made in the United States to recover this pyrite for manufacture of sulphuric acid but only a few plants have succeeded in recovering it on a commercial scale. Several chemical companies in the East became concerned about supplies of pyrite early in 1943, but by late summer of that year the situation had eased. If for no other reason than national security and self-sufficiency during wartime, methods of recovering pyrite from coal-mine refuse should be worked out and made available to coal-mine operators who are potential producers of pyrite. Eastern sulphuric-acid plants are particularly likely to have their sources of raw material blocked by war conditions, so that special studies to determine where supplies of pyrite can be obtained for these plants from inland sources are desirable. Davis&apos;s1 summarization of conditions during World War I gives the following facts: During those years, the shortage of pyrite became acute. Shipments of hand-picked pyrite were made from a number of coal mines in Illinois, Indiana, western Kentucky, Ohio and Pennsylvania. A mechanical concentrating plant for sepa- rating pyrite from picking-table refuse was built at Danville, Ill., and operated for several years, and a small pyrite-concen-trating plant treating washery refuse near Gillespie, Ill., operated for several months in 1918. The Consolidation Coal Co. of Fairmont, W. Va., constructed and operated a sulphuric-acid plant using pyrite recovered from coal-mine refuse. The U. S. Bureau of Mines during 1917-1919 made a comprehensive survey of pyrite-production possibilities from coal mines and estimated that there was a potential yearly production of 435.000 tons from Ohio and Pennsylvania and 928,000 tons from Kansas, Missouri, Iowa, Illinois, and Indiana mines. This estimate included only mines that could produce one per cent or more of their coal production as pyrite containing a minimum of 40 per cent sulphur. PyRite Production According to the Minerals Yearbook,2 approximately 660,000 long tons of pyrite was produced in the United States in 1941, with an average sulphur content of 42 per cent. The average value f.o.b. mines was $3.09 per long ton. Spanish pyrite, 48 per cent sulphur minimum, was quoted at 12 cents a unit c.i.f. U. S. ports, equal to $5.76 a ton for shipments of minimum sulphur content. Most of the pyrite produced in the United States is obtained as a by-product in the dressing of copper and zinc ores. Metal mines in the East making pyrite concentrate for the market or use in company-operated sulphuric-acid plants

Jan 1, 1944

By David R. Mitchell

The mineral pyrite (or marcasite) occurs in coal beds as balls, lenses, veinlets and bands. Several million tons are wasted annually on the refuse dumps from coal mining and coal-preparation activities. Sporadic attempts have been made in the United States to recover this pyrite for manufacture of sulphuric acid but only a few plants have succeeded in recovering it on a commercial scale. Several chemical companies in the East became concerned about supplies of pyrite early in 1943, but by late summer of that year the situation had eased. If for no other reason than national security and self-sufficiency during wartime, methods of recovering pyrite from coal-mine refuse should be worked out and made available to coal-mine operators who are potential producers of pyrite. Eastern sulphuric-acid plants are particularly likely to have their sources of raw material blocked by war conditions, so that special studies to determine where supplies of pyrite can be obtained for these plants from inland sources are desirable. Davis&apos;s1 summarization of conditions during World War I gives the following facts: During those years, the shortage of pyrite became acute. Shipments of hand-picked pyrite were made from a number of coal mines in Illinois, Indiana, western Kentucky, Ohio and Pennsylvania. A mechanical concentrating plant for sepa- rating pyrite from picking-table refuse was built at Danville, Ill., and operated for several years, and a small pyrite-concen-trating plant treating washery refuse near Gillespie, Ill., operated for several months in 1918. The Consolidation Coal Co. of Fairmont, W. Va., constructed and operated a sulphuric-acid plant using pyrite recovered from coal-mine refuse. The U. S. Bureau of Mines during 1917-1919 made a comprehensive survey of pyrite-production possibilities from coal mines and estimated that there was a potential yearly production of 435.000 tons from Ohio and Pennsylvania and 928,000 tons from Kansas, Missouri, Iowa, Illinois, and Indiana mines. This estimate included only mines that could produce one per cent or more of their coal production as pyrite containing a minimum of 40 per cent sulphur. PyRite Production According to the Minerals Yearbook,2 approximately 660,000 long tons of pyrite was produced in the United States in 1941, with an average sulphur content of 42 per cent. The average value f.o.b. mines was $3.09 per long ton. Spanish pyrite, 48 per cent sulphur minimum, was quoted at 12 cents a unit c.i.f. U. S. ports, equal to $5.76 a ton for shipments of minimum sulphur content. Most of the pyrite produced in the United States is obtained as a by-product in the dressing of copper and zinc ores. Metal mines in the East making pyrite concentrate for the market or use in company-operated sulphuric-acid plants

Jan 1, 1944

PRIOR to the World War most of the barite used in the United States for manufacturing lithopone and barium chemicals was imported. Germany, by virtue of an abundance of high-grade ore and low labor costs, was in a position to dominate the world market. With the cessa-tion of imports and with the war demand for barium chemicals, the barium chemical industry and the mining of barite became well; estab-lished in the United States. This industry has continued to expand because of the increasing use of lithopone. In 1914 the sales of domestic crude barite was 52,919 tons and in 1934 it was 209,850 tons. Barite deposits of economic importance occur in at least 20 states, but the principal producers in 1934 were Missouri, Georgia, Tennessee, South Carolina, Virginia, California and Arizona. The main mining centers are located near the crude barite markets of the three principal marketing districts-the Pacific Coast, the Midwestern area, and the Eastern area. The Pacific Coast is supplied entirely by California, Nevada, and Arizona. The Midwestern area uses most of the Missouri crude and a small amount from the southern states. The eastern market is the chief competitive area. Practically all of the imported crude is marketed there; also the bulk of the southern crude and ground barite. In addition, this area absorbs a small part of the Missouri crude and 80 per cent of the ground barite. Besides the advantage of low delivered costs and purity of product, the imported barite has commanded a price differential because it is soft rather than hard, like many of the domestic ores. The inherent physical properties of the southern ores remain, but the purity can be controlled to a great extent by beneficiation. Simple washing or gravity concentra-tion has sufficed in the past, but in many cases a more efficient process now becomes imperative to remove impurities not amenable to these methods. Certain deposits now being opened are of lower, grade and require more precise milling conditions. In some ores, the kind of impurities has changed as the mining advanced.

Jan 1, 1936

By G. D. Just

INTRODUCTION Large scale underground mining involves the bulk handling of fragmented material. The cost and efficiency of the mining systems is there- fore significantly influenced by material flow characteristics. Flow problems may occur in the form of ore pass blockages which interrupt the free flow at extraction openings. The costs of such delays can be readily assessed and compared to the costs incurred in reducing blockages by improved fragmentation or larger ore passes. In practice the problem is more complex than this statement suggests because it is generally un- economic to design for zero ore blockages. Another major flow problem occurs in the form of relative movement of ore and waste as the fragmented material is extracted. This produces waste dilution in the recovered ore and influences total ore recovery. This flow problem is much more complex than the ore block- age phenomena. Many questions concerning the precise flow characteristics remain unanswered because of the variability of size distributions, particle shapes, material properties and the total extraction layout and design. Model studies can provide a visual and quantitative illustration of probable flow characteristics but full scale data collection is necessary to evaluate the precision of such information. The methods and types of data obtained must be carefully selected to recover the maximum volume of useful information for operational control and future design. It is essential that honest precision levels are assigned to the data and any subsequent analyses. Grade control data may give misleading short term information on flow characteristics because of the difficulty in knowing the true grade of the mass of material before extraction commences. However, in the long term control of extraction grades is vital to the profitable operation of the mining system. The most efficient extraction design and operational schedule can only be determined after all of the facts and variables are known. This is usually only possible after the orebody has been completely extracted. However, if design and operational personnel have a full appreciation of the nature and variability of material flow under different conditions the best possible results should be achieved. The most significant features of material flow are out- lined in this paper in order to provide mine planning and mine management personnel with some of the necessary information relating to material flow. Available facts and reliable figures from selected publications are noted in association with unbiased and hopefully accurate opinions of the relevance of the data to mine design and mine system control. Possible future developments and profitable areas for research into material flow problems are also detailed. MATERIAL FLOW AND MINING METHODS The effects of material flow on the design and operation of an integrated underground ore handling system is one factor which is common to most mining methods. Analysis of the system as detailed by Just, 1980, permits the identification of unit process objectives. For example, a typical underground ore handling system as illustrated in Figure 1, involves the following unit operations:- (i) Gravity flow of ore in stope (ii) Ore extraction at base of stope (iii) Ore haulage on the production level (iv) Dumping of ore into ore pass system (v) Gravity flow of ore in the ore pass (vi) Underground crushing of ore (vii) Haulage of crushed ore to shaft (viii) Hoisting of ore to the surface. Average flow rates in each of these unit operations can be misleading due to variability in incremental capacity caused by flow blockages and machine delays. Thus to effectively analyse the probable performance of the system, it is necessary to have a measure of the flow loading and haulage rate variability. Mechanical equipment performance specifications can be used to provide such information for loading, haulage and crushing; however, in the case of the gravity flow of material field measurements are required to relate the probability of "hang-ups" to the degree of fragmentation. Factors affecting the frequency of flow stoppages are, size, distribution and cohesiveness of broken material and the geometry and size of the flow channel. Ore pass channel design is relatively simple since regular cross-sectional shapes are used

Jan 1, 1981