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By C. Elbaum

Specimens consisting of several crystals, each with a prescribed geometry and a controlled orientation with respect to both the extermally intposed stress and the highboring crystals, werer deformed in tension at room temperature. It is shown that the influence of a grain boundary on the plastic defolrmation of a mullicrystal depends on the extent to which the presence of the grain boundary, contributes to the necessity 01. multiple slip in the component crystals. MANY investigations were carried out in the past on the plastic deformation of aluminum single crystals, bicrystals, and polycrystals. The various studies of bicrystals aimed primarily at elucidating the influence of grain boundaries on the mechanisms of plastic deformation. In the earlier studies the emphasis was placed primarily on finding the "strength" contributed by a grain boundary. In more recent investigations it became apparent that the grain boundary does not contribute any strength per se but rather acts by influencing the mechanism of plastic deformation in the adjoining grains. The concept thus emerged of the plastic properties of a bi-crystal, and by extension of a polycrystal. depending solely on the mechanism of deformation prevailing in each grain. The contribution of the grain boundaries thus becomes limited to the type of restrictions imposed on each grain by its neighbors. The present investigation of the behavior of specimens consisting of more than two crystals was designed for the purpose of studying the influence of the grain boundary in simple aggregates. The findings of this study further support the concept that the restriction imposed on a deforming crystal by its neighbor constitutes the predominant factor in the plastic deformation of polycrystals. The term "multicrystal", in contrast with single and polycrystals, is used to describe specimens consisting of several crystals. Each one of the component crystals has a prescribed geometry and a controlled orientation with respect to both the externally imposed stress and the neighboring crystals. Two groups of multicrystals were prepared. All the component crystals of both groups of multicrystals had the axial orientation (isoaxial multicrystals) shown in Fig. 2, with the primary slip plane and slip direction both at 45 deg to the specimen axis. In the first group (hereafter referred to as group I) the component crystals were symmetrically oriented with respect to the plane of the grain boundary; the primary slip plane and slip direction were respectively at an angle of 60 and 30 deg to this plane. For the second group (group 11) the axial orientation remained the same and the relative positions of the primary slip plane and slip direction are shown in Fig. 3. EXPERIMENTAL METHODS The material used was aluminum 99.993 pct pure, according to the manufacturer. The specimens were produced by growth from the melt in a horizontal graphite container. In order to maintain the prescribed geometry of the individual crystals of a multicrystal, a technique described elsewhere was used.' The specimens were grown under a small, positive pressure of helium at a rate of approximately 1 mm per min. annealed in air for 24 hr at 640°C and cooled over a period of several hours to room temperature. All the multi-crystals were rectangular in cross-section, 6 by 18 mm (see Fig. 1) and from 150 to 170 mm long. In each group bicrystals, tricrystals and quadru-crystals were prepared as shown in Figs. 1 and 4.

Jan 1, 1961

By Dean Goodermote, Carla S. Stone

I Introduction Coal fuels China. Roughly 70 percent of all commercial energy demand is supplied by domestic coal production and with the recent Chinese opening to the West, the Chinese Coal Industry may figure prominently in the export market as well. Because of the importance of China's coal industry to the future of China and the Pacific Rim energy balance, this paper reviews the industry and offers some cautious projections for its outlook. II Energy's Position in the Current Political and Economic Climate Traditionally, Chinese society has been dominated by the policies of its most important government leaders. Deng Xiaoping, Vice Chairman of the Communist Party is the current leader of China. Deng and his proteges are pragmatists. Although China's government structure is based on Marxist/Leninist tradition, Deng and his followers are promoting experiments with market economics and expanded relationships with Western Countries, which have encouraged foreign investment in China. Energy companies represent just one type of industry that is interested in helping the Chinese to develop their abundant natural resources. Although China's leadership is committed to a program of economic modernization, that program currently is experiencing what the Chinese government terms "readjustment". Readjustment cuts back in imports due to deficient foreign exchange and deemphasizes heavy industry, while it encourages agricultural and consumer goods output and, most imporant, energy production. Increased Chinese coal and oil production is essential both to fuel industry and, equally important, to provide foreign exchange. If sufficient energy production is not forthcoming, then economic growth will be severely retarded. China's 1979 per capita GNP of $260 is only slightly better than the weighted average achieved by low income countries of $230. (1) Delays in growth could lead to social unrest, threatening the position of the current leadership. Since there is no institutionalized mechanism for leadership succession and policy continuation, it is reasonable to assume that leadership changes could result in energy policy changes. III Energy Consumption Energy production is important to China's future economic health as highlighted by the World Bank. If China's economy grows rapidly, 5 percent to 6 percent during this decade, the Bank noted, a significant energy shortfall could occur as early as 1985. This state of affairs contrasts sharply with China's current position as a net hydrocarbon exporter. (2) To assure a healthy economic future, China's leadership is attempting to reduce its rate of increase in energy demand through conservation as well as to boost energy output. A massive conservation promotion program has been underway since 1979 and there is much room for improvement. China's industrial sector is only about half as energy efficient as is U.S. industry. (3) During the last two decades, each percent of increase in GNP has been accompanied by a 1.8 percent of increase in energy consumption. (4) This compares rather poorly with the United States where a less than one-to-one relationship exists. IV Energy Supply The short term prospects for oil production are uncertain. Production increases were rapid in the 1960's and early 1970's, averaging 20 percent annually, but most of this increase came from one field, Daquing. Now that Daquing's production has peaked and the offshore potential has yet to be developed, petroleum production has maintained a plateau of 2.1 million b/d, at least temporarily, of which approximately 15 percent is exported. (5) Output

Jan 1, 1982

By D. R. Parrish, W. E. Lamoreaux, W. W. Owens

Several methods are now being used by the industry for determining the gas-oil flow characteristics of reservoir rock samples. Most of the laboratory experirnerltal rlzethods can be classified either as steady-state, unsteady-state, or Hassler-type tests. Although the validity of the results obtained by any specific method is not questiorzed, in general, the complexity of these methods leaves much to be desired. This investigation dealt primarily with the development of a simplified unsteady-state (gas drive) laboratory test method for measuring kg/ko re1ationships of small core samples. A procedure for selecting uniform and representative sandstone rock samples was developetl since it was observed that the reliability of the test resu1ts was dependent upon having a sample which was uniform in porosity and permeability. The importance of factors known to influence the results of this type test, such as oil viscosity, gas expansion, and pressure differential were eva/uated. The method of calculating the test results was found to give valid data over a wide range of gas expansion. The limits of pressure differential and oil viscosity which would insure reliable results were defined. In cornparisorz with other presently used testing methods, the gar drive method requires considerably less apparatus, is less time consuming, and is more readily adaptable to a routine type core test. INTRODUCTION The detcrmination of the gas-oil flow characteristics of reservoir rocks has been given concentrated study by the oil industry for the past decade. Both analytical and experimental methods have been considered. The analytical methods have generally relied on a simplified characterization of porous materials in order that the fundamental laws of fluid flow and capillarity could be utilized. More direct experimental methods have been proposed by numerous production research laboratories with the primary goal being a simple and inexpensive, yet reliable method for measuring the gas-oil flow characteristics of reservoir rock samples. The experimental methods which have been reported in the literature generally can be grouped into one of the following classifications: 1. Steady state1,2,3,4 in which a fixed ratio of flowing fluids is forced through the test sample until equilibrium conditions of saturation and pressure gradient are established. 2. Hassler or stationary liquid method5,6,7 in which a uniform liquid saturation is attained, usually through capillary desaturation, then gas or oil is flowed through the sample at a pressure drop insufficient to disturb the pre-established saturation. :. Non-steady state method1,8,9,10 In which only the gas phase is injected into the sample, causing displacement of the oil phase and resulting in a system of continually changing average saturation and saturation gradient. The steady-state and Hassler methods have been most popular because, no doubt, of the simplicity of the actual relative permeability calculations. The problems involved in these methods were limited to apparatus design and measurement techniques. In the steady-state method, for instance, a constant flowing fluid ratio is established which, at equilibrium, results in an essentially uniform saturation over the entire length of the test sample. Therefore, the basic flow characteristics could be obtained by correlating the average saturation of the test sample with the kg/ko determined at various flowing gas-oil ratios.

Jan 1, 1957

By I. Fatt, D. N. Saraf

A method is described for measuring two- and three-phase relative permeabilities in sandstones or sand packs using a nuclear magnetic resonance (NMR) technique to determine fluid saturations. Two- and three-phase relative permeabilities have been determined on Boise sandstone using the NMR technique of saturation measurement. Three-phase relative permeability to water was found to depend only on the water saturation, whereas three-phase permeability to oil depended on both the water and oil saturations. Relative permeability to gas in three-phase flow was found to depend only on the total liquid saturation. INTRODUCTION Three-phase relative permeabilities are extremely useful in calculating field performance for reservoirs being produced by simultaneous water and gas drives. Three-phase relative permeability data are also needed for analyzing solution gas-drive reservoirs which are partially depleted and are being produced by water drive. Some thermal recovery processes involve three-phase flow which require three-phase relative permeability data for predicting reservoir behavior. Unfortunately, three-phase relative permeability measurements have rarely been made. Also, because of the scarcity of three-phase data, it has not been possible to date to relate other measured rock characteristics to the relative permeabilities with a great certainty. Leverett and Lewis,l Reid2 and Snell3 have reported three-phase relative permeability data on unconsolidated sands. Leverett and Lewis used ring electrodes spaced along the length of the sand sample to measure the resistivity of the sample which was assumed to be monotonically related to brine saturation. Gas saturation was determined from pressure-volume measurements. Oil saturation was obtained by material balance on the cell containing the sand sample. This method is involved and time consuming. Another difficulty arises from the fact that the resistivity of the sand is a function not only of saturation of brine but also of the distribution and saturation history of the brine in the pore spaces. Reid2 used a gamma ray absorption technique for measuring liquid saturation. This method has the disadvantage that total liquid saturation rather than oil or brine saturation is all that can be measured and still another method is required to determine the saturations of individual components. snel13 used a neutron bombardment method which also required a separate determination of the individual component saturations. Caudle et al.4 measured three-phase relative permeability on consolidated sandstones using vacuum distillation for determining fluid saturations. Distillation after each reading makes this technique very lengthy and time consuming. Corey et a1. 5 and Naar and Wygal 6 measured three-phase relative permeability on sandstones by the capillary-pressure method. Semipermeable diaphragm assemblies were used at each end of the core specimen to keep the water phase in the core. Gravimetric methods were used to determine fluid saturations. Sarem7 recently reported an unsteady-state method for measuring three-phase relative permeability on sandstones. This method is an extension of Welge's method8 for measuring two-phase relative permeability. Although Sarem's method is simple and comparatively fast, the assumptions involved may oversimplify the problem. Sarem's assumption, that in all rocks relative permeability to each fluid will depend only on the saturation of that fluid, seems to be rather unrealistic. Neglecting capillary effects at the end of the core is also a weak assumption. Donaldson and dean9 measured three-phase relative permeability using a method similar to Sarem's.

By George P. Chapman

Mica is a platy mineral occurring in a variety of complex hydrous aluminosilicate forms with differing chemical composition and physical properties. Principal minerals in the mica group include: Muscovite-potassium mica (colorless or pale green/ ruby) Phlogopite-magnesium mica (dark brown or amber) Biotite-magnesium-iron mica (black or dark green) Lepidolite-lithium mica (lilac) Selected properties are given in Table 1. Muscovite is most important commercially with phlogopite of lesser use. The laminated structure of mica enables it to be split into very thin films which are transparent and tough as well as having outstanding dielectric and insulating properties. Commercially, mica is used in a number of forms (Chowdbury, 1941; Rajgarhia, 1951; Skow, 1962). Sheet mica consists of flat sheets mined from naturally occurring books of mica, free from defects and capable of being punched or stamped into required shapes. Sheet mica is separately classified into blocks, films, or splittings according to thickness. Built-up mica, or micanite, is made by arranging overlapping splittings in layers , cemented with a binder and pressed together at high temperature. Reconstituted mica, or mica paper, is made by depositing fine flakes of high-quality scrap mica in a continuous film impregnated with binder. Scrap and flake mica are normally unsuitable in quality or size for making sheet mica. Originally the term scrap mica referred to the waste byproduct of mining and fabricating sheet mica, and distinct uses were developed for this material. Subsequently it became economically feasible to mine lower quality mica for these uses, and the term flake mica was introduced. Although the two terms are still used somewhat synonymously, it is considered better, at least in the United States, to use the term flake mica in referring to mica mined for uses other than as sheet mica; and to restrict the term scrap mica to mica mined for or with sheet mica, but which will not meet the specifications. Synthetic mica, such as fluorophlogopite, is produced by slow crystallization of a melted blend of pure raw materials. Mineralogy In the true sense the term mica does not relate to, a particular mineral, but to a group or family of minerals of similar chemical composition and to some extent similar physical properties. These minerals are predominantly potassium aluminum silicates with varying amounts of magnesium, iron, and lithium. The precise formulas and isomorphic relationships of the various group members have been studied, but general agreement has not been reached (Grimshaw, 1971; Hurlbut, 1952; Skow, 1962). The general formula describing the chemical composition of micas is [X2Y4-6Z8020(OH, F)4, where X is mainly K, Na, or Ca; Y is mainly Al, Mg, or Fe; Z is mainly Si or Al (Deer, et al., 1962).] These minerals have an internal structure of the layered lattice type where the silicon atoms are in the center of a tetrahedral grouping of oxygen atoms. The groups are linked together in a single plane by three oxygen atoms that lie within the common plane. Each of these oxygen atoms is shared by two tetrahedra. These linked tetrahedral groups, when continually extended, produce a hexagonal network within the plane. This internal structure of the mica has been used to explain the ex-

Jan 1, 1983

By I. W. Alcorn

THE cost of drilling in the past few years of proration and ever decreasing allowables has received increasing thought and study. It seems to parallel the strides made with respect to pumping problems in 1932 and 1933. Low profit margins stimulate the search for economies. Any discussion of slim-hole drilling involves a multitude of abstract values, and the problem can be attacked only by a study of records and rational thinking. In a measure, traditional methods must be studied with a questioning attitude. The words "slim hole" may be somewhat misleading, as the term is entirely relative. For that reason I wish to define it as used in this discussion. On the Gulf Coast, I would define a normal hole as one in which 10 3/4-in. surface casing has been set and below which a 9 7/8-in. hole is dug. With this as a datum, holes of larger diameter below surface would be called "large holes," with 12 1/4 in. as the "extra large" class and holes of smaller diameter classed in the slim-hole range, 6 1/4 in. representing about the minimum size. The optimum size has not been definitely determined, but the preference is for a program that would call for setting 8 5/8-in. surface casing and digging a 7 3/4-in. hole. Different sections of the country might very properly deviate from this practice because of differences in depth, formations, regulations, or other factors. This paper will be confined to a discussion of the drilling of exploratory wells, as the drilling of this class of wells is quite a different problem from that of drilling a proven field, although many of the same considerations apply in both cases, as will be apparent. Although for many years shallow slim-hole and core-test holes of small diameter had been dug, it was not, I believe, until the fall of 1937 that serious consideration was given to its application in drilling wells 7000 ft., 8000 ft. and 9000 ft. deep on the Gulf Coast. This does not mean that nearly all such wells drilled on the Gulf Coast now are of the slim-hole variety, but only that efforts have been aimed in that direction with very encouraging results and there has been a very definite trend to reduce the size of holes, a trend that probably will continue. As to exploration policy, there appear to be two distinct and opposite views. The one usually followed in the past was more or less designed to "shoot the works" on one well. Generally on the Gulf Coast, the depth at which production might be obtained is limited by the drilling equipment and economics. With this thought in mind, wildcat wells are often planned with the idea of carrying the depth to 10,000 ft., or even 15,000 ft. All of the possible hazards are anticipated and the general drilling and casing programs are so predicated. Such wells contemplate the drilling of large-diameter holes; the setting of at least one protective string of casing and an extensive coring policy, all of which finally adds up to an expensive well. As opposed to this general policy is the slim hole. This, on the Gulf Coast, recognizes that new discoveries represent gam-

Jan 1, 1941

By C. L. Sollenberger, Will Mitchell, Ford F. Miskell

Heat treatment of ore prior to comminution reduces power requirements for grinding, reduces grinding media wear, and improves recovery of iron values from a typical Minnesota magnetic taconite. Test data demonstrating this, as well as an analysis of the economics of commercial application of the technique, are presented. THE taconites in general are hard, tough ores, difficult to grind. Liberation of iron mineral constituents usually is accomplished by grinding the ore through at least 100 mesh, and often it has been found necessary to grind substantially through 325 mesh to achieve satisfactory recovery and grade in the concentration process. Because of the fineness of grind required and the enormous tonnages of material contemplated for treatment in the future, costs resulting from grinding media wear and power consumption, together with capital investment required for comminution, approach astronomical figures. Economy in any one of these elements per ton of material ground could very well reflect a considerable saving to the ferrous industry in yearly costs. With this in mind, the Research Laboratories of Allis-Chalmers Manufacturing Co. have launched a program to discover means of effecting this economy. The initial phase of the work as described here deals with a heat treatment of crushed raw ore, followed by thermal shock in cooling, for the preparation of rod mill feed. Several investigators1-" ave noted an improvement in the grindabilities of ores treated in this manner. One investigator2 subjected low grade iron ores to heat treatment in an electric furnace. Basing his conclusions on screen analyses of crushed products, he observed that treated ore was more easily crushed than the untreated. He reported that observation of the treated and untreated ore through a microscope revealed cracks following the grain boundaries in treated ore, whereas no cracks were present in untreated ore. However, few if any have quantified the improvement in terms of total hp hours saved, reduction of wear of grinding media, or reduction of capital costs of grinding equipment involved. By means of Bond rod mill and ball mill grindabilitiesh nd by comparative wear tests, the conditions maintained during this investigation have been definitely evaluated. Heat treatment experiments have been made on a batch scale in a muffle furnace, followed by continuous scale experiments in a rotary kiln under various conditions of temperature, atmosphere, retention time, and quenching to determine the combination that would give the greatest improvement in the grindability of a taconite without affecting adversely the magnetic susceptibility of the magnetite. From these data, relative costs have been calculated for grinding both untreated and heat- treated ore on a basis of plant capacity of 120 tons per hour. Heat requirements for a rotary kiln, as well as the kiln capacity required for the treatment, have been estimated. For these tests 50 tons of ore were obtained from the Aurora mine of the Erie Mining Co., Hibbing, Minn. The ore was reported7 to have been selected from the magnetic portion of the lower chert horizons. An average chemical analysis of' this portion is shown in Table I and an approximate mineralogi-cal analysis is shown in Table 11. No attempt was made to differentiate between the various silicates because the compositions vary widely on the different horizons and depend on the degree of oxidation. Minnesotite, however, is the predominant silicate. The siderite grains were dispersed throughout the ore but were essentially associated with the rock-forming minerals. In a series of preliminary tests in which batches of —6 mesh ore were heat-treated in a muffle fur-

Jan 1, 1953

By R. J. Towner

Tensile properties of Aluminum Powder Metallurgy (APM) products at 600°, 800°, and 1000°F were lowered by cold reductions of as little as 10 or 20 pct. The detrimental effect of cold work on yield strength at elevated temperatures increased with temperature. Heating cold-worked products at 850° to 1150°F removed the structural effects of cold work through the process of recovery and restored, at least partially, the strength at 600°F to the level of hot-worked material. Material containing 5 pct A1203 was recrystallized by cold reductions of 97 pct or more followed by annealing at 1100°F. Recrystallization lowered sharply the strength at room temperature, but raised the strength at 600°and 800°F relative to that of the cold-worked state The high strength of Aluminum Powder Metallurgy (APM) products at elevated temperatures'-4 is well-known. In this paper, some conditions of processing that can affect this important characteristic are presented. The following nomenclature will be used to identify different alloys: All of the above alloys are of the aluminum-aluminum oxide type made from milled powders of commercially pure aluminum with the exception of M486, which is fabricated from atomized A1-Fe alloy powder. The products made from milled powders are hardened by a dispersion of aluminum oxide par- ticles in the aluminum matrix, while the intermetal-lic compound FeAL is the dispersion hardening agent in M 486.' The process used for making all APM products involves the application of heat and pressure to form a compact from powder which is fabricated into an extrusion, sheet, strip, or wire by standard techniques. Probably the most common cold-worked APM product is sheet. Cremens, Bryan, and rant' determined the room-temperature tensile properties and the 600°F stress-rupture properties of XAPOOl and XAPOO3 sheet and reported that there was little difference between the as-extruded, cold-worked, and annealed at 1200°F conditions. On the other hand, Emmons6" found that the tensile and stress-rupture properties of XAPOOl and XAPOO3 sheet at 600" and 800°F were lower than those of extrusions. The tensile properties of XAPOO3 sheet were also determined at elevated temperatures by Doyle' and ~ayward.' According to Friske" and Kendal et a1.," cold working by swaging, rolling, and tube drawing reduced the tensile and creep-rupture strength of XAP 001 Recrystallized aluminum powder metallurgy products are rare because the dispersion in the aluminum matrix is usually too fine, uniform, and concentrated to permit recrystallization. However, Lenel12 was able to recrystallize wires made from aluminum powders containing about 1.75 and 3.0 pct oxide and found that the tensile properties at room temperature remained higher than those of annealed commercially pure aluminum because of the dispersed oxide particles. Westerman and Lenel13 found the kinetics of recrystallization of the powder products were very different from those of cold-drawn commercially pure aluminum wire. The alloy containing 3.0 pct oxide recrystallized to a very coarse grain size was more creep-resistant at 400" to 600°C (752" to 1112°F) than in the as-extruded, fine-grained condition, according to Ansell and weertman.14 Ansell and aenel" further studied creep at 500" to 620°C (932" to 1148°F) of recrystallized 1.75 pct oxide wire and confirmed the creep model of Ansell and Weertman. The present work is being reported for the fulfillment of the following objectives: 1) to show the effect of cold work on tensile properties at elevated temperatures;

Jan 1, 1964

By Will Mitchell, Ford F. Miskell, C. L. Sollenberger

Heat treatment of ore prior to comminution reduces power requirements for grinding, reduces grinding media wear, and improves recovery of iron values from a typical Minnesota magnetic taconite. Test data demonstrating this, as well as an analysis of the economics of commercial application of the technique, are presented. THE taconites in general are hard, tough ores, difficult to grind. Liberation of iron mineral constituents usually is accomplished by grinding the ore through at least 100 mesh, and often it has been found necessary to grind substantially through 325 mesh to achieve satisfactory recovery and grade in the concentration process. Because of the fineness of grind required and the enormous tonnages of material contemplated for treatment in the future, costs resulting from grinding media wear and power consumption, together with capital investment required for comminution, approach astronomical figures. Economy in any one of these elements per ton of material ground could very well reflect a considerable saving to the ferrous industry in yearly costs. With this in mind, the Research Laboratories of Allis-Chalmers Manufacturing Co. have launched a program to discover means of effecting this economy. The initial phase of the work as described here deals with a heat treatment of crushed raw ore, followed by thermal shock in cooling, for the preparation of rod mill feed. Several investigators1-" ave noted an improvement in the grindabilities of ores treated in this manner. One investigator2 subjected low grade iron ores to heat treatment in an electric furnace. Basing his conclusions on screen analyses of crushed products, he observed that treated ore was more easily crushed than the untreated. He reported that observation of the treated and untreated ore through a microscope revealed cracks following the grain boundaries in treated ore, whereas no cracks were present in untreated ore. However, few if any have quantified the improvement in terms of total hp hours saved, reduction of wear of grinding media, or reduction of capital costs of grinding equipment involved. By means of Bond rod mill and ball mill grindabilitiesh nd by comparative wear tests, the conditions maintained during this investigation have been definitely evaluated. Heat treatment experiments have been made on a batch scale in a muffle furnace, followed by continuous scale experiments in a rotary kiln under various conditions of temperature, atmosphere, retention time, and quenching to determine the combination that would give the greatest improvement in the grindability of a taconite without affecting adversely the magnetic susceptibility of the magnetite. From these data, relative costs have been calculated for grinding both untreated and heat- treated ore on a basis of plant capacity of 120 tons per hour. Heat requirements for a rotary kiln, as well as the kiln capacity required for the treatment, have been estimated. For these tests 50 tons of ore were obtained from the Aurora mine of the Erie Mining Co., Hibbing, Minn. The ore was reported7 to have been selected from the magnetic portion of the lower chert horizons. An average chemical analysis of' this portion is shown in Table I and an approximate mineralogi-cal analysis is shown in Table 11. No attempt was made to differentiate between the various silicates because the compositions vary widely on the different horizons and depend on the degree of oxidation. Minnesotite, however, is the predominant silicate. The siderite grains were dispersed throughout the ore but were essentially associated with the rock-forming minerals. In a series of preliminary tests in which batches of —6 mesh ore were heat-treated in a muffle fur-

Jan 1, 1953

By P. A. Beck, Hsun Hu

As described by means of quantitative pole figures, the annealing texture of highly rolled aluminum consists of the four retained components of the rolling texture near (123) [121], rather more sharply developed, and of a cube texture component. Local reorientation corresponds fairly well to 40 rotation around a [111] axis. In copper strip rolled 96 pct, the annealing texture is mainly the cube texture, with the four twin orientations as minor components. The annealing texture of highly rolled brass strip consists of four components of the (225) [734] type. REVIEWS by Wassermann,' Barrett,' Dunn,3 and Richards' give detailed accounts of the numerous publications dealing with annealing textures in rolled polycrystalline metals. Although a considerable amount of information of an empirical nature has been available for many years, even relatively recently the state of recrystallization-texture theory was considered uncertain. The reviews referred to above deal mainly with the description of experimental results, without developing generally applicable principles, suitable for explaining the observed annealing textures. The investigations of Burgers and Louwerse5 and Barrett6 showed that in deformed single crystals of aluminum the orientation of the recrystallized grains deviates drastically from that of the deformed matrix. According to Barrett and to Beck and Hu,7 the relationship between the two orientations can be best described as a rotation of about 40° around a [111] axis. Recent investigations led to similar orientation relationships for various face-centered cubic metals with a simple texture, regardless of whether the annealing process was recrystallization (strain-free grains growing in a highly deformed large crystal of aluminum' or copper: or in deformed cube texture copper") or coarsening (strain-free grains growing at the expense of an essentially strain-free, fine grained, polycrystalline matrix of single orientation texture copper,'" aluminum,' or nickel-iron). Barrett" pointed out the possibility that this orientation relationship may be a result of the orientation dependence of the rate of grain boundary migration. More recently, considerable evidence became available in favor of this view.12,13 In apparent contradiction to the above results, it has been known for a long time that the recrystallization texture of polycrystalline metals is often similar to the deformation texture. This was found, in particular, for the fiber textures obtained by wire drawing, compression, or compression rolling.' Following a suggestion by Barrett,2 Kronberg and Wilson and Beck and Hu7 described a mechanism by which a [Ill] fiber texture, resulting from plastic deformation, may be retained upon recrystallization, even though the orientation of individual recrystallized grains differs from that of the local area of the matrix in which they grow. This mechanism assumes that the reorientation corresponds to a rotation around the [1ll] axis, which is also the fiber axis. The present investigation was undertaken to examine in detail the orientation relationship between deformation texture and recrystallization texture in rolled face-centered cubic metals, using the quantitative methods of texture determination that have recently become available.", '" Quantitative pole figures for the rolling textures of such metals were reported recently." Quantitative pole figures for annealing textures are given in the present paper. It was planned to investigate whether or not the orientation relationship previously found for the recrystallization of deformed single crystals, and for coarsening of single-orientation texture material, is capable of accounting for the observed, often complex, annealing textures in rolled polycrystalline metals. The question whether local reorientation is predominant, even in the early phases of the annealing process, was to be studied with high purity aluminum. by making use of an oxide film and sensitive tint illum-

Jan 1, 1953

By C. W. Carpenter, P. T. Bail, J. E. Bobek

This paper presents the results of model studies made to demonstrate the validity of applying the "basic" waterflooding scaling relationships of Rapoport1 to water-wet reservoirs composed of communicating strata of different permeability. Results demonstrate that these relationships can be validly applied, and also show the combined effect of variables on recovery. This demonstration was needed to confirm that the sizable effects of communicating strata on waterflood behavior, observed in model studies, were actually representative of field behavior. INTRODUCTION Rapoport1 Collins2 and others have presented scaling laws for modeling water-oil displacements. The validity of these laws has been experimentally demonstrated for homogeneous systems only. Recently, however, several investigators have presented the results of multilayer model studies made to determine the effects of viscous, capillary and gravitational forces on oil recovery in systems composed of communicating layers of different permeability. Dyes and Braun,3 using miscible displacements to simulate water flooding, showed that vertical communication adversely affects recovery at unfavorable viscosity ratios in the absence of capillarity. Ogandzhanyants and Egorova, 4 Gaucher and Lindley,5 and Richardson and Perkins6 modeled water-oil displacements in layered systems using immiscible fluids with capillary forces present. These investigators found more efficient behavior than in the miscible system of Dyes and Braun. However, since the scaling laws had not been verified for heterogeneous systems prior to or during these tests, it was necessary to assume that the results were representative of field behavior. This report presents the results of model studies made at Jersey Production Research Co. to find out if the waterflooding scaling relationships are valid when applied to water-oil displacements in heterogeneous reservoirs with vertical communication. Data obtained in the study show the combined effects of viscous, capillary and gravitational forces on oil-recovery behavior. The studies were performed in strongly water-wet systems where strong imbibition forces were present. For systems of different wettability, the effects of capillary imbibition would be somewhat different than those presented. APPROACH The scaling laws studied were those developed by Rapoport1 and designated by him as "basic" scaling laws. These relationships require that the model be scaled to the geometry of the prototype, and that the model and prototype be operated at the same viscosity ratio and have identical relative permeability curves, contact angles and boundary conditions. It is also necessary that the groups** be identical in the two systems, although any of the parameters making up the groups may be different. Finally, the capillary pressure of one system must be directly proportional to that of the second. Studies were conducted in two four-layer models, representing quadrants of five-spots, which were geometrically similar and which had the same glass-bead packing. The fluids used assured the same wettability in both models. Thus, the contact angles and relative permeabilities of comparative sand layers in the two models were identical and the capillary pressures were directly proportional. However, one model had a characteristic length three times that of the other. To make the scaling groups equal and to check the scaling laws, it was necessary to adjust the rate, water-viscosity level, interfacial tension and water-oil density difference to compensate for the difference in model sizes.

By R. Hastings Keller, Ralph E. Esarey

Oil and gas activities in Indiana during 1943 continued to decline at about the same rate as in 1942. New development, production, and prospecting, all showed the results of Federal regulation, low price for crude oil and shortages of labor and materials. Several local stripper-well operations were shut down, but no large-scale abandonment has occurred as yet. During the year, 277 holes were drilled for oil and/or gas, of which 99 were completed as oil wells, 19 as gas wells and 159 as dry holes. This record was a decline of 21 per cent over last year in the total number of completed tests, 20 per cent in the number of oil wells and 9.5 per cent in the number of gas wells. As in the previous year, most of the drilling (82 per cent) was in the southwestern part of the state, Gibson County ranking first, with 77 completions and 49 oil wells. Posey County was second, with 59 completions and 20 oil wells. The remaining 18 per cent of the drilling was in the old Trenton oil and gas area. The total footage drilled during the year was 482,799 ft., a decline of 18 per cent from the previous year. Of this, 146,559 ft. was wildcat footage. The total initial production of the oil wells completed was 6362 bbl. and of the gas wells was 2,562,000 cu. feet. Three tests in the old Trenton area were drilled into the Cambrian and reported nothing more than tar residue. A Devonian test was to be made in the Griffin field in the Wabash River but owing to the delay caused by Federal restrictions this test did not get started in 1943. It is expected to spud in March 1944. The new discoveries in 1943 were virtually all in the southwestern part of the state, and all, so far, one-well pools, except the North Owensville pool, in Gibson County. The latter was brought in during the month of February and by the end of the year nine wells were producing in the pool, with a reported initial yield of 1260 bbl. per day. By the end of the year it had a daily average production of 401 bbl. and an accumulated production of 39,129 bbl. The average gravity of the oil is reported to be 35.6. On the Ohio-Indiana state line, early in 1943, a new pool was opened up in the old Trenton area. The discovery well was on the Ohio side of the line. An offset well was completed on the Indiana side, with an initial yield of 64 bbl., and settled down to 5 bbl. per day. This well produced 1154 bbl. up to Dec. 31, 1943. There was no further development here, because of the Federal Conservation Order M-68, restricting drilling to one well on 40 acres. The development pattern usually followed in this area is one well to 5 acres. The E. Rogers field was extended by one pool (Table 4). Most of the development in the oil-field pools during the year took place in the Kirksville pool, in Gibson County, and the Caborn pool, in Posey County. The crude-oil production in 1943 was approximately 5,273,000 bbl., a decline of 29 per cent from the previous year. The Griffin field, of Gibson and Posey Counties,

Jan 1, 1944

By R. Hastings Keller, Ralph E. Esarey

Oil and gas activities in Indiana during 1943 continued to decline at about the same rate as in 1942. New development, production, and prospecting, all showed the results of Federal regulation, low price for crude oil and shortages of labor and materials. Several local stripper-well operations were shut down, but no large-scale abandonment has occurred as yet. During the year, 277 holes were drilled for oil and/or gas, of which 99 were completed as oil wells, 19 as gas wells and 159 as dry holes. This record was a decline of 21 per cent over last year in the total number of completed tests, 20 per cent in the number of oil wells and 9.5 per cent in the number of gas wells. As in the previous year, most of the drilling (82 per cent) was in the southwestern part of the state, Gibson County ranking first, with 77 completions and 49 oil wells. Posey County was second, with 59 completions and 20 oil wells. The remaining 18 per cent of the drilling was in the old Trenton oil and gas area. The total footage drilled during the year was 482,799 ft., a decline of 18 per cent from the previous year. Of this, 146,559 ft. was wildcat footage. The total initial production of the oil wells completed was 6362 bbl. and of the gas wells was 2,562,000 cu. feet. Three tests in the old Trenton area were drilled into the Cambrian and reported nothing more than tar residue. A Devonian test was to be made in the Griffin field in the Wabash River but owing to the delay caused by Federal restrictions this test did not get started in 1943. It is expected to spud in March 1944. The new discoveries in 1943 were virtually all in the southwestern part of the state, and all, so far, one-well pools, except the North Owensville pool, in Gibson County. The latter was brought in during the month of February and by the end of the year nine wells were producing in the pool, with a reported initial yield of 1260 bbl. per day. By the end of the year it had a daily average production of 401 bbl. and an accumulated production of 39,129 bbl. The average gravity of the oil is reported to be 35.6. On the Ohio-Indiana state line, early in 1943, a new pool was opened up in the old Trenton area. The discovery well was on the Ohio side of the line. An offset well was completed on the Indiana side, with an initial yield of 64 bbl., and settled down to 5 bbl. per day. This well produced 1154 bbl. up to Dec. 31, 1943. There was no further development here, because of the Federal Conservation Order M-68, restricting drilling to one well on 40 acres. The development pattern usually followed in this area is one well to 5 acres. The E. Rogers field was extended by one pool (Table 4). Most of the development in the oil-field pools during the year took place in the Kirksville pool, in Gibson County, and the Caborn pool, in Posey County. The crude-oil production in 1943 was approximately 5,273,000 bbl., a decline of 29 per cent from the previous year. The Griffin field, of Gibson and Posey Counties,

Jan 1, 1944

By David Cornell, Yusuf K. Sukkar

The fundamental differential equation for fluid flow has been rearranged, integrated numerically for natural gases, and the results presented in tabular and graphical form suitable for the direct calculation of vertical gas flow problems. The integration is rigorous except for the use of a constant average temperature. Both static and flowing bottom-hole pressures may be calculated by (his method without resort to trial and error procedures. INTRODUCTION Bottom-hole pressures can be determined either by direct measurement with a bottom-hole pressure gauge or by calculation. Since measurement with a bottom-hole pressure gauge is costly, calculation of bottom-hole pressures is to be preferred when possible. Calculation involves knowledge of the wellhead pressure, the properties of the gas, the depth of the well, the flow rate, the temperature of the gas, and the size of the flow line. These quantities must be combined in a suitable equation for vertical flow. Several equations have been developed for the purpose of calculating gas flow through both horizontal and vertical pipes1,2,4,5,6,7,8,9 These equations all have the basic differential equation for flow as their starting point. They differ only in the assumptions which are made in order to simplify the integration step. The bottom-hole pressures calculated using any of the better known equations are in good agreement with bottom-hole pressures calculated by a more rigorous but considerably more tedious stepwise integration method. All of these methods, however. require a trial and error solution for the calculation of flowing bottom-hole pressures. The purpose of this paper is to present a method which provides a direct solution of static and flowing bottom-hole pressures without use of a trial and error solution. At the same time the method involves fewer simplifying assumptions than any of the previous methods used, except lor the lengthy stepwise method. The derivation of any practical flow equation begins with the basic differential equation which is rigorous for almost all flow problems. The five terms in Equation 1 represent the potential energy, the potential energy of position, the kinetic energy, the shaft work done, and the energy losses due to motion of the fluid respectively. Equation 1 reduces to Bernoulli's theorem for the case of horizontal flow of an incompressible fluid, no work done, and no energy losses due to friction. In the present case, the term (v) (dv)/(g,.) can be shown to be quite negligible compared to the other terms, and is therefore neglected in the derivation. The term — dws includes work done by a pump or turbine in the system and is zero in this case. The frictional losses in the pipe are included in the term — d(lw) which is expressed in terms of the Moody friction factor as in Equation 2. (f) (v2) (dL) d(lW) = (f)(V2) (dl)/(2) (g) (d) The specific volume of a gas can be expressed in terms of the temperature, pressure, molecular weight, and compressibility factor. The velocity of the gas can be expressed in terms of the weight rate of flow, the specific volume, and the dimensions of the pipe.The reduced pressure Pr is to be used because z can be expressed as a function of Pr and Tr alone for most natural gases:

Jan 1, 1956

By E. D. Gardner, E. M. Sipprelle

The Synthetic Liquid Fuels Act (58 Stat., 190; 30 U.S.C. Sup., Secs. 321-325) was approved by Congress April 5, 1944; it directed the Bureau of Mines to build demonstration plants to produce synthetic liquid fuels from coal, oil shale, and agricultural products. The most important oil-shale deposits in the United States are in the Green River formation of Colorado, Utah, and Wyoming. The oil shale of western Colorado generally is more amenable to exploitation, more persistent, and apparently richer than elsewhere in the Rocky Mountain Region. It occurs at the top of a high plateau surrounded by bold, nearly vertical escarpments 500 to 600 ft in height. The top 400 to 500 ft of these escarpments comprises an oil-shale measure that averages 15 gal of shale oil per ton; the bottom 70 90 100 ft of the measure, called the Mahogany Ledge, averages over 30 gal per ton. The full measure in a 1000-square-mile area is estimated to contain 300 billion barrels of shale oil;' the Mahogany Ledge is estimated to contain 100 billion barrels of oil. These estimates are based on numerous surfac,e samples and on core-drill holes drilled by the Government and by private enterprise. The oil-shale beds are undisturbed and lie nearly horizontal. The name "oil shale" is unfortunate, as the rock is a tough, strong marlstone. Organic matter named "kerogen" is a constituent of the rock. The oil-shale demonstration mine is on Naval Oil-Shale Reserve No. 1; it is about 5 1/2miles by mountain road from the plant site, which, in turn, is 2 miles from U.S. Highway 6 and 10 miles west from Rifle, Colo. The highway parallels the Colorado River, the Denver and Rio Grande Western Railroad, and a 66,000-volt public-utility power line. Early in the program it was realized that an oil-shale enterprise would have to be on a large scale to be commercial, and that unusually low mining costs would be necessary. The physical characteristics of the Mahogany Ledge and an overlying roof stone are unusually favorable both for large-scale operation and low mining costs. Quarry practices largely will be followed underground to mine the Mahogany Ledge. The aim has been toward complete mechanization of all mining operations. A mining unit would comprise a square mile containing 100,000,000 tons of oil shale with allowance for mining losses. An investment of $1,000,000 would be $0.01 a ton; such an expenditure, therefore, could be made to save, say, $0.015 per ton daily operating cost. A goal of a mining cost of $0.50 per ton was set up in 1945. Open-cut mining costs then were about $0.25 per ton of material handled; it was hoped that a cost double this amount could be obtained in mining the Mahogany Ledge. Costs of labor and supplies have increased since 1945 and so has the selling price of petroleum products. To those unacquainted with the character of the Green River deposits, the name "shale" suggested high mining costs. Others assumed that coalmining costs of $2 to $5 per ton would apply. To many, the expected mining costs appeared the principal handicap to the establishment of an oil-shale industry. The purpose of the Bureau of Mines is to demonstrate methods and to establish costs for mining the oil shale on a large scale. It is hoped this work will lead to the establishment of a large-scale, commercial oil-shale enterprise.

Jan 1, 1950

By N. E. Garner

Laboratory experiments were conducted to investigate the cutting of a single diamond on limestone and shale under simulated down-hole conditions. A high-pressure chamber was modified by adding a rock-rotating device so that planing tests could be run. Weight on the diamond, diamond geometry and differential pressure across the face of the rock were varied. It was found that (I) high differential pressure reduced the volume of rock cut by the diamond at a given bit weight by strengthening the rock and changing the mode of failure; (2) a finely powdered rock left in the bottom of the grooves reduced the volume cut by as much as 50 percent; and (3) orientation of a single diamond about the axis of a drill point had considerable influence on diamond cutting efficiency. INTRODUCTION Diamond bits consist of many diamonds held in a matrix provided with water courses for fluid passage to clean, cool and lubricate the diamonds as they drill formation. Each diamond contributes its share to the overall effectiveness of a bit, but a lack of understanding of the performance of a single diamond has hampered efforts to engineer improvements in diamond bits. The need for those improvements prompted this study. This paper describes the findings of a laboratory investigation of the outting action of a single diamond where the differential pressure between the wdlbore and formation, diamond geometry and vertical force on the diamond were independently varied. The tests were conducted in a pressure chamber that provided relative horizontal motion (planing) between a rock and diamond under simulated down-hole pressure conditions. EQUIPMENT HIGH-PRESSURE CHAMBER WITH ROTATING DEVICE The high-pressure chamber used in previous rock mechanics studies' was modified for this study by addition of a rock-rotating device. The modified chamber (Fig. 1) differs from the old chamber in that the rock can be rotated to provide relative horizontal movement between the rock and the penetrator which may be a small element of a diamond or a drag bit. In this study the penetrator was a single diamond. The rock sample holder inside the chamber is mounted on a thrust bearing and is connected to the external drive mechanism by a stem that passes through two seal elements. The seal elements are needed to allow formation pressure to enter the bottom of the rock sample through a small hole in the stem. The Kapseal seal elements (Tefion boots backed by O-rings) provide low friction (hand free) even at differentials of 5,000 psi. The drive mechanism is a variable-speed transmission with a speed range from 0 to 30 rpm and an output torque of 2,800 in.-lb. A right-angle-drive gear box couples the drive to the stem. The new design has two independent pressure systems (formation and borehole) to simulate down-hole rock stress environment. Formation pressure enters from the bottom of the rock through a 6-in. diameter area, and borehole pressure acts over the remaining surface. A 14-in. layer of zero fluid loss oil-base mud poured over the top of the rock and an O-ring seal on bottom allow a differential between the borehole and formation pressures. Bayol 50 was used as the hydraulic fluid in the chamber. The differentials reported here were obtained by elevating the borehole pressure while keeping the formation pressure at zero.

By Charles C. Templeton

Any explanation of the nature of multiphase fluid flow through porous media must ultimately involve a knowledge of the mechanism of such flow through the individual pores of the medium. To provide quantitative information of the latter type, a study was made of gas-liquid and liquid-liquid displacements in single uniform Pyrex capillaries with diameters as small as 4 microns. Quantitative observation of air-liquid displacements with zero contact. angle indicates the adequacy of a model based on Poiseuille's Law and the independence of capillary pressure and interfacial velocity. Consequently, this work discounts previous claims that flow is abnormally retarded in very small capillaries. For the displacement of a very viscous oil by water in a capillary initially filled with water, flow is faster than predicted by the above model. This behavior is probably due to the existence of a thin annular film of water between the oil column and the capi1lary wall as postulated by Yuster. INTRODUCTION The need for experimental observation of the microscopic nature of multiphase fluid flow, to further the understanding of the results of macroscopic flow investigations, has been previously recognized. Chatenever and Calhoun1 in connection with the API Project 47B have extensively studied the flow of fluids through layers of glass or lucite spheres between glass or lucite plates. Lowman2 prepared an interesting film concerning flow in a single capillary, using an apparatus which made a moving interface appear stationary in the field of a microscope. The purpose of the present investigation was to deter- mine what contribution might be made to this field by comprehensive quantitative observation of gas-liquid and liquid-liquid displacements in single capillaries of uniform, very small diameter. The techniques used are similar to those of Lowman but incorporate improvements necessary for quantitative work. Quantitative observations must begin with fluids of simple chemical composition to provide a basis for analyzing the more complex behavior that may be expected with natural reservoir fluids. However, some qualitative observations on systems involving crude oils are presented. Experiments of this sort involve the observation of the velocity of the interface separating two fluids, and have been performed in horizontal or vertical capillaries by several investigators.3,4,5,6,7,8 The most general treatment of their mechanics, by Brittin,9 involves forces due to capillarity, viscous resistance, gravity, an "end-drag" effect, and the rate of change of momentum of the capillary contents. Since the range of pore diameters of interest in petroleum reservoirs is about 0.1 to 100 microns, it was desired to perform these experiments in the smallest capillaries possible, to ascertain whether capillary diameter had any effect on the existing theory based on data from larger capillaries.* It was also important to be able more systematically to vary the direction and rate of displacement than was done by previous investigators. Finally, to concentrate attention on viscous and capillary forces by eliminating gravity as a parameter, this study involves only horizontal capillaries. The work of Eley and Pepper' with a "large" (0.766-mm diameter) horizontal capillary is the previous investigation which is most similar to the present method of quantitative observation. Here capillaries with diameters as small as 4 microns will be studied.

Jan 1, 1955

By C. M. Wayman, G. R. Srinivasan

A metallographic study of the isothermal products formed between 750° and 285°C was made in an Fe-7.9 wt pct Cr-1.11 wt pct C alloy, and a time-temperature-transformation diagram was determined. The study shows that the austenite decomposes into three different products: pearlite above 540°C, ferrite and carbide between 540° and 300°C, and lenticular bainite below 300°C. No upper bainite forms in this alloy. The results are discussed in terms of carbon diffusion models for upper bainite formation. AUSTENITE transforms into several products depending on the temperature, composition, and rate of cooling, and the various transformation products have been a source of controversy for a long time. Since the classical study of Davenport and ~ain' extensive work has been carried out. The present study concerns the isothermal transformations in an alloy which was used for a detailed investigation of bainite crystallography and provides information supplementary to the work of Lyman and Troiano who studied austenite decomposition in steels containing 1 pct C and varying amounts of chromium. Their work showed that increasing the amount of chromium in high-carbon steels had the effect of depressing the B, temperature and of shifting the TTT curves to longer times and lower temperatures. They further found that if the chromium content is increased in a 1 pct steel to about 9 pct no bainite would form even after a period of 100 days. However, a preliminary investigation by the present authors showed that bainite plates do form in steels containing about 8 pct Cr and 1 pct C. In view of this and some results from a thin-foil electron microscope investigation of the bainite formed in the present alloy: it was considered desirable to investigate the other isothermal products as well. EXPERIMENTAL PROCEDURE The alloy used in the present investigation was obtained from a triply vacuum-melted ingot prepared from high-purity materials. Chemical analysis for the alloy verified the composition to be Fe-7.9 wt pct Cr-1.11 wt pct C. Metallographic observations were made on i by i by « in. specimens which were aus-tenitized at 12 50°C for 50 to 60 hr in evacuated quartz capsules and then water-quenched. Since the M, temperature for this alloy is below room temperature, the homogenizing treatment produced a completely austenitic structure consisting of very coarse austenite grains (ASTM #0-1). Several samples of the austenitized specimens were metallographically prepared and observed for any proeutectoid carbide separation. It was found that all the carbon was in solution. The water-quenched specimens were upquenched and given isothermal treatments at temperatures between 285" and 750°C for varying periods in molten salt or lead baths. The specimens were then water-quenched, and those showing less than 5 pct transformation were used for plotting the beginning of the austenite decomposition. To ensure the removal of the disturbed layer, the mechanically prepared specimens were electropolished in a 1:6 HzS04, CHSOH solution for 10 to 15 sec at 20 v. Final polishing was done with a vibratory polisher using 0.05-p alumina. Various etchants including nital, ferric chloride, and hot ferricyanide (Murakami's reagent) were used to bring out details in the different transformation products. The ferricyanide etch was used whenever the preferential etching of carbides was desired.

Jan 1, 1969

By A. S. Appleton, M. B. Bever

The stored and expended energies of an Au-Ag alloy deformed in torsion were investigated as functions of strain, strain rate, and temperature. At room temperature, the stored energy, measured by tin solution calorimetry, increased linearly up to an intermediate strain, above which it was nearly constant; at 78 °K the relation was linear up to fracture. Approximate values of the energy stored at 4 OK indicate a rapid increase below 78 OK. The energy stored by specimens deformed successively at 4o and 78oK changed slowly with increasing second strain from the curve for energy stored at 4 OK (measured after annealing at 78oK) to that for deformation at 78°K. The ratios of the stored to the expended energy at room temperature and 78 oK were unusually large. The additional amount of energy stored at the lower temperature is attributed mainly to an increase in the number and energy of dislocations. The stored energy as a function of strain rate at 4oK (measured after annealing at 78oK) increased to a sharp maximum over a narrow range of strain rates, whereas the expended energy changed only slightly. These effects are explained by the generation of point defects resulting from the enforced nonconservative movement of jogs in fast moving screw dislocations. The effect of straining successively at two strain rates at 4oK was also investigated. Stress-strain curves for 4o, 78oK, and room temperature and the results of micro examination of specimens deformed at these temperatures are also reported. THIS investigation is a continuation of a research program primarily concerned with the effects of variables on the energy relations involved in the deformation of metals. The variables investigated in earlier work have included strain, strain rate, temperature of deformation (room temperature and 78oK), and the type of deformation process. Most of this work has been carried out with Au-Ag alloys. In the investigation reported here, the deformation process was torsion, which had not been used previously in the program. The stored and expended energies involved in the deformation process were measured as functions of strain, strain rate and the temperature of deformation in the range 4" to 373" K. The microhardness and microstructure of deformed specimens were also investigated. The relation between stored energy and strain differs for different deformation processes.1,2 In general, the stored energy increases with strain and may attain a nearly constant value at large strains. This value and the rate at which it is reached, however, depend on the process of deformation. This dependence has been attributed, at least in part, to differences in the effective strain rate and rise in temperature of the specimen during deformation. The effects of the temperature of deformation on both the stored energy and the energy expended in the working process have been the subject of only a few investigations.3-6 Values of these quantities at low temperatures are of special interest as they yield information on point defects which, for many metals, is not obtainable at higher temperatures. The effect of the strain rate on the stored and expended energies has received little attention The strain rate has usually been measured only in relative terms, and hence the interpretation of its effect on the stored energy has been mainly comparative.

Jan 1, 1963

By R. D. Reiswig, J. M. Dickinson

The 0s-Ir equilibrium diagram was determined. The diagram is of the simple peritectic type, with a peritectic temperature of about 2660°C. The solid miscibility gap is narrower than previously reported, the nearly vertical solvus lines occurring at about 42 and 63 wt pct 0s. Widmanstaetten figures resembling martensite in some of the two-phase alloys account for a previously suspected transformation. In view of the long history of use of such alloys, it is surprising that the 0s-Ir equilibrium diagram has not yet been completely determined. The boundaries of the miscibility gap in this system have been estimated to be between 24 and 39 wt pct 0s and 79 and 100 wt pct OS. It has been predicted3 that alloys of ruthenium, osmium, and rhenium with the fcc platinum metals should solidify peritectically in their two-phase regions. The metallographic examination of natural osmiridium alloys has been said4 to indicate, by the presence of a martensitic structure, the existence of a transformation or a phase separation. On the basis of superconducting transition temperature measurements, a 70 at. pct 0s alloy was found5 to be two-phase prior to annealing. EXPERIMENTAL The elemental components used in this work were obtained from several suppliers as sponge. The purities, stated by each supplier to be in excess of 99.8 pct, were confirmed in each case by a semiquantitative spectrographic analysis. The pure components were premelted in an inert-gas tungsten arc furnace with the evolution of some fume, crushed, and pickled for use as alloy melting stock. Upon arc melting to the final compositions, no fume evolution was observed. Because weight losses of the order of 15 mg or less were observed in preparing alloy buttons weighing 15 g, "synthetic analyses" were used in determining the compositions of the alloys. Alloys used in this investigation contained 15, 20, 33, 40, 42, 43, 45, 50, 55, 60, 63, 64, 66, 70, 79, and 80 wt pct 0s. Heat treatments of the alloy buttons and pieces thereof were performed in a previously described6 tungsten tube furnace under pressures of 105 torr or less. It was found that homogenization treatments on the specimens were essential to remove the severe coring which was present, a 3-hr treatment above 2300°C removing all the metallographi-cally visible evidence of coring. Following the various heat treatments, the specimens were "vacuum-quenched" by melting a tungsten fuse wire and allowing them to drop onto a water-cooled copper plate. In a few instances, specimens were quenched into molten tin for comparison, but no difference was apparent. Vacuum-quenched specimens cooled from 2400°C to below a red heat in less than 60 sec. Typical equilibration times varied from 3 hr above 2300°C to 88 hr near 1100°C. The utilization of successively longer equilibration times and the approach to equilibrium from both directions indicated that the times used were sufficient to give a close approach to true equilibrium. Heat-treatment temperatures were measured with a calibrated Leeds and Northrup optical pyrometer through a 0.120-in. lateral sight hole in the tungsten heater tube. It was known that the assumption of black-body conditions inside the 1-in.-diam by 10-in.-long tube was unwarranted. The empirical results of work with thermocouples and melting

Jan 1, 1964