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By R. Grierson, R. N. Parkins

The m.echanica1 properties, at high lzomologous temperatures, of the intermetallic compounds InzBi and Mg17A112 were measured as a .function of temperature, applied strain rate, previous thermal and mechanical history, and composition. Mgl,Al12 was investigated ilz compression, whereas Zn,Bi was investigated in tension. A decrease inflow stress with increasing strain was observed jor both alloys. The results obtained are discussed in terms of the dislocation-multiplication processes in these materials. MANY intermetallic compounds are reported to undergo a brittle-ductile transition at high homologous temperatures.' There is evidence in the literature that some of these compounds exhibit a large yield drop when plastically deformed.'j3 Both of these forms of behavior are shown by the covalent elements germanium and silicon4,5 and also by certain ionic compounds.8 The present work is a study of the deformation, at high homologous temperatures (>2/3 Tm), of two intermetallic compounds, In2Bi and Mg17Al12. InzBi has a disordered hexagonal structure7 (c/a = 0.598) and a solubility range of 32.3 — 33.2 at. pct Bi.8 It has a melting range from 72° to 89°C. Mg17Al12 has an ordered bcc (A12 type)7 structure and exists over the range 50 to 60 at. pct Mg8 with a melting range from 437° to 462°C. We have been unable to find any reference to previous investigations of the mechanical properties of BiIn,. Novikovg has reported that cast samples of Mg17A112 show ductility, when bend-tested, at temperatures above 380°C. EXPERIMENTAL Ingots of In2Bi and Mg17Al12 were melted under an argon atmosphere and cast, in situ, in a graphite crucible. The materials used were of 99.99 pct purity. The alloys prepared contained 66.9 at. pct In in the case of In2Bi and 58.4 at. pct Mg in the case of m17A112. The ingots were homogenized and then extruded. Two-in.-diam Mg17Al12 ingots were extruded at 375°C to give 3/8-in.-diam rod. The rate of formation of this rod was 0.25 in. per min. One-in.-diam InzBi ingots were extruded at 20°C, using a rate of 1 in. per min, to give 1/8-in.-diam rod. In both cases the extruded rod had a recrystal- lized, fine-grain, structure. (For Mg17Al12, d = 11.2 µ; for BiIn2, d = 22 µ.) Mechanical-property determinations were made in a hard-beam machine, in tension in the case of In2Bi and in compression with Mgl7Al12. The tensile tests were on specimens having a gage length of 1.1/2 in. and a diameter of 1/8 in. The compression tests on Ml7A112 were on specimens of 3/8 in. diam by 3/8 in. high and the ends were coated with poly-tetrafluorethylene to minimize friction. RESULTS In2Bi. Fig. 1 shows, particularly at the higher applied strain rates, that In2Bi exhibits a marked yield drop as the deformation increases to about 2 pct, after which the material shows neither hardening nor softening up to 15 pct strain. The magnitude of the yield drop, the stress in the region of flow under constant stress (the stress plateau), and the 0.5 pct proof stress were all dependent upon the applied strain rate according to an expression of the form

Jan 1, 1965

By John D. Corrick

The environmental and nutritional characteristics necessary for maximum copper extraction from a low-grade ore by Ferrobacillus ferrooxidans have been explored as have many of the limiting parameters. Criteria considered were oxygen consumption, copper extracted, soluble copper concentration, temperature, pH, particle size, nutrients, and other inorganic salt concentrations. A set of environmental and nutritional conditions were developed for E. ferrooxidans Which supported cell reproduction and maximum microbial oxidation of a low-grade copper sulfide ore. Percolator tests conducted under these optimum conditions resulted in an 18 percent increase in the quantity of copper microbially extracted over that extracted under conditions considered to be standard. Manometric tests determined those extremes of environmental conditions and nutritional factors Which were detrimental to the extraction of copper by E. ferrooxidans.

Jan 1, 1965

By J. G. Eisele

Solvent-extraction characteristics of dodecyl phosphoric acid (DDPA) were investigated to determine its potential as a fractional or selective extract-ant for individual elements in a rare-earth-yttrium mixture. The DDPA is an effective extractant for splitting rare-earth mixtures into light and heavy subgroups. Yttrium normally extracts with the heavy rare-earth elements but may be shifted toward an extraction sequence with the light rare-earth elements by increasing the pH. Elements in the light and heavy ends of the rare-earth series can be separated from middle-group rare-earth elements by using diethylenetriaminepentaacetic acid (DTPA) as an aqueous phase counter-extractant. Hydrogen-ion dependency of the distribution coefficients differs from that reported for similar systems at tracer-level concentration.

Jan 1, 1965

By Ralph H. Whaite

The Bureau of Mines program for microfilming maps of abandoned mines in the Pennsylvania anthracite region is described. A catalog of the maps that have been microfilmed in the Eastern Middle anthracite field--the first area to be covered in the program--is presented. Additional catalogs will be published as significant mining areas are completed.

Jan 1, 1965

By K. N. Weaver

In the early 1950's the cement industry began putting a new emphasis on geology. This article points up some of the industry's raw materials problems that geologists are uniquely qualified to handle. Portland cement can be made from relatively abundant industrial minerals and rocks, and this may explain why cement producers placed little emphasis on geology during the early days of the industry. After World War 11, however, the industry began to recognize the need for geological exploration and some of the larger companies began to build a permanent geological staff. This development has its roots in: 1) The rapid expansion of the industry. After World War II and continuing into the early 1950's the demand for cement far exceeded the production capacity. This placed a great deal of pressure on the producers to enlarge capacity at their plants and to develop new sites. 2) The closing of many cement plants due to inadequate raw materials. Producers feared lack of raw materials due to inadequate exploration and evaluation. 3) An ever increasing pressure for upgrading of the quality of portland cement, necessitated upgrading the quality of raw materials. 4) The increasingly large capital investment needed to build new cement plants required a higher degree of accuracy in reserve calculation. These reasons are more or less self explanatory and will not be elaborated on. They are outlined to illustrate the probable evolution of thought among cement management to justify the development of a geological staff. In the author's personal experience the geologist must continually readjust to changing conditions within the industry. For example, cement production capacity grew so rapidly that today production is only about 70% to 75% of rated capacity (73.8% in 1963). Therefore, whereas the geologist's function during the active expansion of capacity was primarily one of exploration, one of his major functions today is the development of existing reserves. This assumes of course that reserves at existing plants have been proven to be adequate in terms of the company's reserve policy. Through the proper development of raw materials, the geologist can markedly influence quality control, production and long range planning. Examples of several of the operations of Medusa Portland Cement Co. will illustrate how proper attention to geologic detail pays off in the above areas. Because limestone is the major raw material of port-land cement, the examples will be concerned with it. DEVELOPMENT OF GEOLOGIC DETAIL One of the prime objectives of an exploration or development project should be the establishment of the stratigraphy and structure of the deposit. The basic tool for exploration and development is still the core drill, and the geologist must gain a maximum amount of information from a minimum amount of drilling. In order to obtain this objective the following is essential: 1) Adequate detailed geologic logging of cores. The core is first logged and separated into lithologically distinct units. In order to make the lithologic breaks as meaningful as possible, representative pieces of core (not all) are etched in dilute HCI. This removes the "drill polish", brings out the structure of the rock and indicates the proportion of dolomite and argillaceous material because dolomite and argillaceous material etch in relief. In this way the lithologic breaks become clearer and one gains a general idea of the chemical makeup before analysis. This method of logging lessens the probability of including two types of stone, e.g. limestone and dolomite into the same sample for chemical analysis. 2) Representative sampling for chemical analysis. After logging, the lithologic units are sampled for chemical analysis. A representative analysis can be obtained by extracting a 1-in. sample for every foot of core. For example, a lithologic interval of 10 ft to 20 ft would yield ten 1-in. samples taken at 11 ft, 12 ft, 13 ft... and 20 ft. These samples are then crushed, pulverized and split into a sample for chemical analysis. This sampling method represents a significant saving of time over splitting the entire core. 3) Preparing the core as a record. Because of the expense of storage and the difficulty of handling large amounts of core, only representative samples of each lithologic unit are saved for reference. An

Jan 1, 1965

By S. Leber

Pole figures and pole distributions were used for the quantitative detevinination of the preferred orientations in swaged tungsten rods and the effect of subsequent wire drawing on the texture. In the swaged rod, the preferred orientation could best be described as a pseudo (111-112) [110] cylindrical texture. A secondary component was assigned the indices (110) [001]. Further reduction by swaging retained these cylindrical textures. Wire drawing caused lattice rotations about the wire axis, converting the cylindrical texture into a normal fiber texture. The conversion was initiated and proceeded lnost rapidly in the center of the wire. The (110) /001] component was converted into a (110) fiber texture by wire drawing. The effective rotations were about axes contained in the lransverse plane. The preferred orientation associated with tungsten wire usually has been assumed to consist of a (110) fiber texture. This implies rotational randomness around the wire axis. Leber1 has shown that rotation about the wire axis may be restricted resulting in a preferred orientation designated as a cylindrical texture. Specific crystal planes tended to remain aligned parallel to the wire surface. This texture seemed to be the result of the swaging operation used in the intermediate stages of fabrication. Bhandary and cullity2 detected similar textures in swaged iron wires. Peck and Thomas3 suggested that the preferential alignment of crystal planes parallel to the wire surface was the result of tangential flow, characteristic of swaging. Wire drawing, following swaging, twisted the crystals about axes parallel to the wire axis, converting the cylindrical texture into a normal fiber texture.4 In this investigation, quantitative techniques were used to more accurately characterize the cylindrical texture and to study its conversion into a normal fiber texture. PROCEDURE The material investigated was lamp-quality tungsten. Three ingots were rod-rolled and swaged to 112 mils diameter, and were then drawn to 10-mil wire. Samples were obtained after each drawing pass. (110) and (200) pole figures were obtained from samples prepared as shown in Fig. 1. To form the sample shown in Fig. l(a), l-in. lengths of wire were glued side by side to form a l-in. square. The composite was ground and electropolished to form a diametral reference surface. For certain specific tests, samples were prepared as shown in Fig. l(b). This composite was made from 10-mil-thick strips prepared by grinding on parallel longitudinal planes. The polished reference surface in this case was, in essence, the wire surface. The two forms of samples [~igs. l(a) and l(b)] were related by a 90-deg rotation around the wire axis. Because of ease in preparation, most data was obtained from the diametral samples. The X-ray data were obtained using a Siemen's pole-figure goniometer. These data were not corrected for absorption or defocusing effects, since only the angular locations of the intensity maxima were of interest. Regions of the pole figure more than 80 deg from the center were not investigated. Partial monochromatization was achieved by the use of unfiltered copper radiation and a krypton-filled proportional counter. No evidence of spurious white radiation effects5 could be detected. Therefore, more elaborate X-ray techniques were not required. Intensity levels were chosen to show all pertinent details of the orientation distributions. The reference plane for the pole figures was the diametral section. The orthogonal reference directions, shown in Fig. 1, were the wire axis, the radial axis per-

Jan 1, 1965

By F. M. Smith, R. H. Moore, J. R. Morrey

Electrodiffusion in y cerium reported by Henrie has been confirmed and a Preliminary estimate made of the relative rates of electrodiffusion of iron, cobalt, and nickel. These diffuse to the anode at rates decreasing in that order. In addition, copper and manganese exhibit slow, but detectable, diffusion to the anode and molybdenum exhibits detectable diffusion to the cathode. The electrodiffusion of carbon, .zirconium, antimony, magnesium , and silicon in y cerium could not be detected. Iron and cobalt diffuse in y cerium at rates proportional to the current density and with no apparent dependence on temperature. Decreasing polarization of iron and cobalt with increasing temperature, which cancels the expected rate increase, would account for this behavior. The electrodiffusion rate of iron in y uranium and in E plutonium has been measured. Diffusion of iron is anode-directed. Tin was found to diffuse to the cathode, in y uranium, at an appreciable rate. In all of these solvent metals, negative ions diffuse to the anode and positive ions to the cathode. The potential field effect appears to account satisfactorily for these results. FROM early experimental work summarized by Jost1 and Seith,2 the driving force for electrodiffusion was attributed to the potential field acting on ions in a metal. More recently, Heuman,3 Wever,4 and Huntington5 have shown that momentum interchange between conduction electrons and mobile entities in the metal contributes to electrodiffusion. Electron momentum interchange is anodically directed and the direction of diffusion resulting from the field force is dependent upon the charge on the diffusing entity. These two effects may either reinforce or oppose each other. Glinchuk6 has pointed out that momentum transfer in defect conductors should be cathode-directed and this appears to be the case as demonstrated by wever's4 work on iron. Barnett's7 work, on the other hand, indicates that, even in defect conductors, electrons show a negative E/m ratio when accelerated with respect to the lattice and should lead to anode-directed momentum transfer. In discussing this problem, Wever and seith8 suggest that defect electrons interact preferentially with activated ions so as to allow a net movement toward the cathode while still maintaining an electron momentum transfer in the anode direction. Williams and Huffine9 and Henriel0 have demonstrated that electrodiffusion may be useful for purification of yttrium and cerium. In yttrium, Williams and Huffine note that movement of several metallic impurities toward the anode is in keeping with observations in most other metallic systems and indicates that yttrium remains a normal electronic conductor at least to 1230°C. Close inspection of their data shows, however, that oxygen, nitrogen, and the transition elements diffused toward the anode, while nontransition elements diffused toward the cathode. This suggests that potential field effects may have been appreciable. The present work was concerned with the applicability of electrodiffusion as a technique for purification of plutonium, but, because of the obvious hazard inherent in work with this metal, experiments to develop the technique were carried out using cerium and uranium. The results of electrodiffusion measurements on these metals and on plutonium are reported here. EXPERIMENTAL The metal specimens prepared for this work were 6 in. long, 1/4 to 1/2 in. wide, and 1/16 to 3/32 in. thick. The uranium specimens were machined from a bar which analyzed 310 ppm Fe and the electrodiffusion of iron was followed by spectrographic and by chemical analysis. Cerium and plutonium specimens were cut from sheet rolled from ingots obtained from molten salt-metal equilibrations during which radioactive tracers were introduced. The electrodiffusion of the tracers was subsequently determined by counting methods. The specimens were electrolyzed between nickel electrodes containing resistance heaters used to equalize the specimen and electrode temperatures, thereby reducing thermal gradients. The temperature of the electrodes adjacent to the ends of the specimen was measured with chromel-alumel thermocouples which were connected to the heater controls. The surface temperature of the specimen at a point midway between the electrodes was measured with a sapphire rod pyrometer, the output of which controlled the dc power supply. This assembly was enclosed within an evacuable chamber containing a quartz viewing window. The temperature of the specimen over its entire length could be scanned with a portable pyrometer through

Jan 1, 1965

By P. W. Barton, A. A. Johnson, E. J. Hughes

THE only systematic work on the effect of carbon on the recovery and recrystallization kinetics of iron so far reported in the literature is that of Venturello et al.1 These workers found that doping high-purity iron so that it contained up to 86 ppm C caused a marked retardation of recovery but had little or no effect on the recrystallization kinetics. Such evidence for an effect as was obtained was inconclusive. In the course of a study of electron-beam zone-refined iron the authors have recently examined the effect of added carbon on the recrystallization kinetics of this material. The amount of carbon added was about 50 pct more than was used by Venturello et 01. and definite evidence was obtained that carbon at this level retards recrystallization. The starting material was taken from a batch of 0.2-in.-diameter Johnson-Matthey spectroscopically pure iron rods which had been further purified by being given three passes at 4 in. hr-1 in a standard MRC electron-beam zone-refining unit. The purity of this material. which was used in two other investigations of the properties of high-purity iron,2,3 was established by an extensive series of analyses. Four laboratories, the National Research Corp., Newton, Mass., the Naval Research Laboratory, Washington, D.C.. the Battelle Memorial Institute, Columbus, Ohio, and the National Physical Laboratory. Teddington. Middlesex, England. carried out analyses for carbon. oxygen. and nitrogen. and in addition a complete mass-spectrograph analysis was carried out at Battelle. In all, twelve analyses were carried out for carbon, seventeen for oxygen and twelve for nitrogen. The amounts of these elements found to be present were 10 * 7, 8 i 5, and 0.9 i 0.1 ppm, respectively. The limits given are rms deviations. Two results, one of 46 ppm of oxygen and another of 31 ppm of nitrogen, were rejected as anomalous. The mass-spectrograph analysis revealed the major impurity to be 25 ppm of tungsten. All of the other elements detected were present in amounts less than 0.5 ppm. Some of the rods were doped with carbon by being immersed in a suspension of carbon in oil, heated in a vacuum at 400°C, and then zone-leveled to make the distribution of carbon uniform. Carbon analyses carried out on three of the doped rods gave a mean value of 130 ± 45 ppm. Some of the doped and undoped rods were deformed 58 pct by swaging and cut into specimens 1/2 in. in length. Isothermal recrystallization experiments were then carried out on them at 575", 600°, 615", 630°, and 650°C, the volume fraction of each specimen recrystallized being measured by a point-counting method described by Hilliard and Cahn.4 The results for the two types of specimens are shown separately in Figs. 1 and 2. In Fig. 3 the pairs of recrystallization curves for each temper-

Jan 1, 1965

By Stanley L. Lopata, Eric B. Kula

The problem of preferred orientation has been considered in quantitative phase analysis by X-ray diffraction techniques. The average intensity of a diffraction peak can be obtained by integration over the whole pole figure, or by random rotation of the specimen in the X-ray beam, or by a combination of both. For rod or wire, where the pole figure shows rotational symmetry, the intensity is measured along a radius of the pole figure. Where no symmetry is present, rotational symmetry is imparted by rapid rotation of the sheet around its surface normal during measurement. These methods are applied to the determination of aus-tenite in an Fe-31 pct Ni rod and Fe-28 pct Ni sheet. X-RAY diffraction techniques are frequently used for quantitatively determining the relative amounts of two or more phases present in a structure.1,2 Briefly, the method requires a measurement of the intensity of a Bragg reflection for each phase. The method is based on the principle that the intensity of a Bragg reflection, IA, is directly proportional to the volume fraction of the given phase present, CA: T KRACA/2µ [1] where K is a constant independent of the diffracting phase, RA can be calculated and depends on the Bragg angle ? and the particular reflection measured, and µ is the linear absorption coefficient of the mixture.' For a mixture of two phases A and B, IA = RAcA [2] IA/IB=RAcA/Rbcb and CA+ CB = 1 [3] This allows the volume fraction of a phase to be calculated directly from the measured integrated intensities of the two phases present. This method is frequently used for quantitatively determining retained austenite in steels, but can be used for the quantitative determination of in titanium alloys, as well as phases in other alloy systems. The intensities are generally measured by diffracting only from planes whose normals are perpendicular to the specimen surface, with the implicit assumption being made that this intensity is typical of reflections from planes whose normals lie at other angles to the surface. If the specimen contains a texture or preferred orientation of the crys- tallographic planes by virtue of previous mechanical working, however, this measured intensity is correct only if the intensity level fortuitously is one times random. Examination of pole figures for actual rolled sheet shows that the intensity level at the center of the figure is seldom at the random level, and can very easily differ by a factor of five or more, leading to a commensurate error in the calculated amount of the phases. Textures have been commonly found in materials which are cold-rolled or recrystallized after cold rolling. This problem is becoming of greater importance since structural materials in use today, such as the high-strength stainless steels, frequently are further strengthened by cold rolling, and hence contain textures. Although high-strength carbon-containing alloy steels generally do not contain textures, some of the newer thermomechani-cal treatments will impart a texture even in these cases. In the case of hexagonal metals, such as titanium, probably every wrought sample will show some anisotropy. Since the standard X-ray techniques are inapplicable in all these cases, there is a clear need for some method of taking this anisotropy into account. The specific problem is to obtain the integrated intensity of a Bragg reflection for each phase, averaged over all orientations of the sample with respect to the X-ray beam. This can be done either by purely mechanical means or by a mathematical averaging. Mechanically, a small spherical speci-

Jan 1, 1965

By E. R. Helderman, C. Y. Ang, C. C. Nealey

Beryllium-base alloys have been successfully p7.-epared by the liquid-phase sintering technique. Depending orz the composition and amount of the intended liquid please, microstructures either single -phase or duplex in feature with randomly oriented grains have been obtained. Qualitative and semi-qualitative determination of distribution of alloying elements md microsegregations in some experi)uzental alloys haue been made by electron-micro-probe analysis in conjunction with microliardness testing and standard metallography. Tensile tests reoealed that some conzpositions possess attractive elastic properties with Young's mot1uli greater than 40 X 10' psi. In powder metallurgy, liquid-phase sintering is a process or phenomenon that has proven to be of practical value. For example, the heavy metals such as tungsten-copper-nickel, high-strength heavy gyro alloys,' heavy-duty electrical contacts,' and tungsten carbide tool materials are all products of liquid-phase sintering. Mechanisms involved in liquid-phase sintering, however, are not completely understood. Questions regarding the exact roles played by rearrangement of particles, liquid/vapor surface energy, solution and precipitation, and so forth, have not been completely answered. Evidence has been cited3 that at least volume shrinkage in the densification process is diffusion-controlled. It is possible that the predominant mechanisms for the complete densification and grain growth in a liquid-phase sintered system depend primarily on the alloy systems involved, in addition to processing conditions. Despite the lack of sound understanding of the mechanisms of the process, liquid-phase sintering has been and is being used to advantage either to synthesize microstructures for their special properties or to prepare alloys which are difficult to form by fusion process. Liquid-phase sintering of beryllium alloys was first attempted by Jones and Williams.4 They first tried infiltrating beryllium with magnesium, and then succeeded in preparing the alloy by sintering Be-Mg powder compact in molten magnesium bath. This investigation resulted in the identification of some Mg-Be intermediate phases. Crossley et a1.5 also used liquid-phase sintering technique in an attempt to produce ductile beryllium alloys for structural applications. The major liquid-phase components investigated by Crossley et al. were aluminum and silver with minor additives of germanium, calcium, lanthanum, cerium, and yttrium. The lack of wetting and the bleeding out of liquid phase were the difficulties encountered during experimentation. According to Hodge,6 the two compositions investigated by Crossley, which showed some promise based on compression tests, involved large amounts (over 35 wt pct) of silver, thus making them too heavy to be of practical interest to the aerospace industry and military users. The present investigation was prompted by the search for light-weight (density less than aluminum) beryllium alloys exhibiting small anisotropy in physical properties for precision inertial navigation instrument applications. In addition to isotropy, good structural properties such as high elastic modulus or desirable combination of mechanical and physical properties are also objectives of this investigation. The technique of liquid-phase sintering was chosen for its versatility in producing either duplex or homogeneous microstructures. This report is concerned with the use of copper and aluminum, with or without silicon addition, as the intended liquid phase, and the resultant micro-structures and some physical properties of the beryllium alloys. Qualitative and semiquantitative electron-microprobe analyses of some of the alloys are presented to illustrate the usefulness of this microanalytical technique for the identification of microconstituents and their distribution. EXPERIMENTAL PROCEDURES The beryllium powder used was -200 mesh Brush Beryllium Co. QMV NP-50 grade. Typical chemical analysis of the powder is shown in Table I. Commercial high-purity copper, aluminum, and silicon powders all screened to —100 mesh were used as additions. Mixed powder compositions were ball-milled in ceramic jars for 1/2 hr to ensure thorough blending. Milled powder was loaded either in 3/4-in.-diam button die or in Metal Powder Association flat tensile specimen die and compacted under top and bottom pressure. No lubricant or organic binder was used. Sintering was carried out in a quartz tube under a vacuum of 50 to 100 µ pressure. Surface hardness and some microhardness readings were taken on sintered specimens. Sintered density was

Jan 1, 1965

The Industrial Minerals Milling Section of the Mineral Processing Division has been engaged for the past three years in a study of the separation of minerals, by means of electronic sorting equipment, on the basis of their colour. Considerable knowledge of the subject has been built up. Because the object of this study is application as a means of beneficiation, a number of examples of the separations achieved are presented. Introduction T 0 the mineral collector, the colour of a mineral may be pleasing, even fascinating; to the mineralogist, student or professional, it may also be practical. It serves, to some extent, as a distinguishing feature in many minerals, and helps to fix with reasonable accuracy the identity of a few. It may now become a useful tool of the mineral dresser. The idea of using a difference in colour as a means of separation of one mineral from another is not new. Hand sorting dates back to ancient time. However, the means by which this can be done mechanically was developed only during the past decade. As far as the Mineral Processing Division is concerned, interest dates from March, 1960, when the following item was observed in the

Jan 1, 1965

By R. L. Solmer

During 1959-61, the Bureau of Mines investigated the strain and deformation induced in rock and concrete linings around mine openings by retreat panel caving at the Climax Molybdenum mine. Two concrete-lined slusher drifts on the Phillipson level of the mine were instrumented with both electrical strain gages and extensometers. Changes in strain and deformation were recorded over an 18-month period during the undercutting and caving of the mining panel. General agreement was found between the strain and deformation measurements and the hypothesis that the vertical component of the stress field on the openings is almost completely removed by undercutting. This phenomenon is a possible explanation for the structural failures that occur in the slusher drifts during the undercutting cycle.

Jan 1, 1965

By Gilbert M. Farrior

The electrical resistivity the coefficient of electrical resistivity the Hall coefficient, and the absolute thermoelectric power were determined in this Bureau of Mines investigation for nine compositions of the TiB2-CrB2 sub-system. The numerical values of the electrical resistivity and the thermo-electric power were greater for the intermediate compositions than for the end members. The absolute values of the Hall coefficients and the coefficients of electrical resistivity were less for the intermediate compositions than for the end members. The electrical resistivities and Hall coefficients were about the order of magnitude of most metals--from 34 to 202 microhm-cm and from about 0 to -23.3 X 10-4 cuP/coulomb. The thermoelectric power was somewhat greater than that of most metals--up to 15.6 microvolts per 0 C.

Jan 1, 1965

By Harry M. Conger

Kaiser Steel Corporation's Eagle Mountain Mine is located in the Colorado Desert, 60 miles east of Indio, California. Concentrates from the mine are shipped by rail 164 miles to the company's steel mill at Fontana, and also to Longbeach, California for export. Temperatures are typical of the lower desert ranging from a high of 120 degrees in the summer to a low of 25 degrees in the winter. The average annual rainfall of about two inches comes mainly as cloud bursts during the summer months. From its inception, the Eagle Mountain Mine has had the problem of breaking its mine rock. Practices followed from 1949 until 1962 were very costly, did not produce uniformly good fragmentation, and were incapable of sustaining high production. During this period, every conventional type of explosive then in use was tried and found to be unsatisfactory for one reason or another. The first slurry test work at Eagle Mountain was started in 195E and finally by 1962, after having tried all the slurry mixtures then available including some "home made" formulas, a metallized slurry was perfected at the mine which overcame all of the disadvantages of former blasting methods.

Jan 1, 1965

By J. M. Kuchta

Experimental data are presented on the autoignition temperature (AIT) characteristics of the hydrocarbon jet fuel, JP-6, in various oxygen-nitrogen atmospheres under conditions of constant volume and constant pressure. AIT's of this fuel in air varied little with fuel injection pressure but increased greatly with decreasing fuel content at low fuel-air-ratios. They also increased with decreasing oxygen content of the fuel vapor-oxidant atmosphere. Consistent with thermal ignition theory, the ignition temperatures increased with decreasing initial pressure, ignition delay, and vessel radius; expressions are given which define the observed variation of AIT with these variables for JP-6 fuel vapor-air mixtures. The significance of autoignition temperature data obtained using various ignition criteria is discussed to show the usefulness of such data in evaluating fire and explosion hazards. In addition, data are presented on the extent of oxidation that occurs prior to autoignition of this fuel in air at various temperatures.

Jan 1, 1965

By R. E. Ogilvie, H. C. Gatos, R. E. Hanneman

The ejj-ect of high pressures on chemical inter-diffusion in the Fe-V system was determined by analyses of concentration vs distance profiles of atmospheric and high-pressure diffusion couples. Diffusion data were obtained as a function of tern -perature and composition. Activation energies, activation volumes, and frequency factors were determined at 1 atm, 20 kbars, and 40 kbars as a function concentration in the a and y phases. The A great deal of research has been carried out in the measurement and understanding of binary chemical inter diffusion in solids. Studies of the effects of high pressure on interdiffusion in binary systems, however, have been virtually nonexistent until the present work. This paper gives a detailed account of the effect of high pressure on interdiffusion and the Kirkendall effect in the Fe-V system. The present data are compared to existing theo- Kirkendall effects were measured at 1 atm and 40 kbars. At 1 atm Dy > DFe at the marker concentration; however, Dv approaches DFe under pressure, and at 40 kbars the values are approximately equal. The high-pressure and atmospheric diffusion data are evaluated on the basis of theoretical models. Chemical analyses of the diffusion -couple profiles were made using an electron microbeam probe. retical treatments of pressure dependence of diffusion which are based upon self-diffusion studies. THEORY The rates of atomic migration in metals and alloys are regulated by the repulsive forces exerted on an atom during its motion from one equilibrium lattice site to another and by the availability of a jump site. Application of high pressure is expected to decrease diffusion rates because it decreases interatomic distances as well as defect concentrations. A number of theoretical treatments have been focused on the problem of calculating self-diffusion coefficients in solids under atmospheric pressure. In general, the vacancy mechanism of diffusion appears to be dominant at high temperatures in most metallic systems. The migration of an atom by this

Jan 1, 1965

By M. R. Geer

Samples of coal from six beds in the Roslyn-Cle Elum field of Washington were subjected to float-and-sink tests to determine their amenability to the production of high-ash boiler fuel for on-site power generation. Grindability tests and analyses of ash were made. All of the coals would require some degree of cleaning to insure a product of 25 percent ash. With two of the coals the entire size range would have to be washed. With the other four, it would suffice to clean only the coarse coal and bypass the raw fines.

Jan 1, 1965

By P. S. Rudman

Laves phases, AB2, are considered as Izerrzisub-stitutional solutions m1hich are defined by a one-for-truo replacement scheme. Atomic-size tnisfit is considered in terms of deviations of the ratio 2V°b/V°A from unity, where v° = atomic volume. A simple elastic model has been used to calculated deviations from "Vegard&apos;s law of atomic vol-umes". Comparison has been made between calculated and observed atomic-volume deviations fov 222 Laves phases. Agreement is generally very good although there ave some few exceptions which appear to be excusable in terms of electronic changes that ore beyond the scope of the present model. We can consider the formation of a binary sub-stitutional solution A-B from an A solvent as one-for-one replacements of A atoms by B atoms. As the atomic-size ratio deviates from unity, the solution becomes thermodynamically less stable and hence more restricted because of atomic-misfit strain energy. In accordance with our previously presented conclusion1 that the atomic volume, v, is in general the most appropriate measure of atomic size, the ideal size ratio for a binary sub-stitutional solution is vg/vA = 1. The Laves phases have been described by Berry and Raynor2 in terms of various stacking sequences of hexagonal layers of B atoms for the three structures MgZn2(C14), MgCu2(C15), and MgNi2(C36). To form the Laves phase of ideal composition AB, we start with complete hexagonal layers of B atoms in the appropriate stacking sequence and we remove, according to an appropriate scheme for each structure, two out of every four B atoms and replace the two removed atoms by one A atom. We thus might expect to find that the ideal size ratio for the Laves phases is 2v/B/ VA= 1. From this point of view, then, we call Laves phases hemi-substitutional solutions since we employ one-for-two replacements. By analogy with substitutional solutions we can expect for Laves phases that as the ratio 2VB/Va deviates from unity the phase occurrence will be more restricted. Laves3 has plotted the distribution of Laves phases as a function of the radius ratio, ?A/rB, and found that, while the distribution extended from 1.05 < rA/B < 1.50, the

Jan 1, 1965

By A. G. Weber, H. J. Welge

A published calculation method for predicting incompressible, multidimensional fluid displacement has been adapted to the problems of water and gas coning in oil wells. Since depth and radial distance from the wellbore are the two key dimensions affecting the shape of a gas or water cone, coning calculations are well suited to the use of two-dimensional methods. The alternating direction implicit procedure (ADIP) was used for relaxation calculations of two-phase potentials in a two-dimensional grid. From the potentials and the capillary pressure relationship, saturation and pressure distributions were calculated which trace cone growth with time. Predictions have been made for well producing histories both before and after core breakthrough. To check validity of the method, two-dimensional calculations have matched the coning behavior and produced water-oil ratio history of a laboratory sand-packed model. They have also matched the coning behavior of several producing wells, for which the calculations were compared with produced water or gas cuts and logs showing water or gas cone movements. INTRODUCTION The application of two-phase, two-dimensional calculations using ADIP to various reservoir flow problems has been described in the literature.1-3 When adapted for computer solution, this method has proved to be a powerful tool for simulating well and reservoir behavior. This paper discusses the method as applied to well coning calculations. Single-well and coning calculations comprise an especially difficult class of two-dimensional problems which require special techniques for computer calculation and determination of reservoir characteristics. Refs. 4 through 8 describe previous approaches to the coning problem. Several examples of water and gas coning calculations, including studies on both laboratory models and producing wells, are presented here. The two-dimensional method accounts realistically for the most critical parameters affecting coning behavior, including production rate, formation stratification, horizontal and vertical permeabilities, depth of well penetration, gravity and capillary forces. The method considers the different densities and viscosities of the two phases and the relative permeability and capillary pressure characteristics of the rock and fluids. In addition to tracing cone growth in the vicinity of the wellbore, the method calculates the overall movement of the fluid interface throughout the well&apos;s drainage volume. Incompressible fluid flow is assumed to occur between the producing interval and the well&apos;s limit of drainage. Calculations can be made for the producing history both before and after cone breakthrough. A typical two-dimensional grid or array of blocks used to solve a coning problem contains about 400 blocks. The well&apos;s cylindrical drainage volume can be represented by about 20 radial subdivisions and the formation thickness by 20 vertical subdivisions. The grid spacing is normally smaller near the withdrawal interval to define the cone shape accurately. For this work we used an IBM 7074 digital computer having a core memory of 10,000 ten-digit words. A typical study, covering 5 to 10 years of well producing history, required from three to six hours of computing time. MATHEMATICAL SIMULATION OF CONING BEHAVIOR BASIC METHOD In coning calculations, the reservoir volume drained by the producing well is represented by a two-dimensional system of blocks as shown in Fig. 1 for water coning studies. The horizontal dimensions of the blocks increase with radial distance from the well axis in geometric progression, i.e., the block size is small near the wellbore and large near the well&apos;s drainage radius (re). Vertically, the blocks are bounded by horizontal planes located at different depths through the

Jan 1, 1965

By J. E. Harris

By elimination of other possible nucleation processes, it has been demonstrated, for commercially pure magnesium and a Mg-Al alloy, that at stresses less than that necessary for triple-point cracking creep cavities are most probably nucleated heterogeneously at second-phase particles. Evidence for the existence of such particles is presented and the role of grain boundary sliding in the nucleation process is examined quantitatively. DURING creep deformation of polycrystalline magnesium and its dilute alloys in the temperature range 0.45 to 0.7 Tm (Tm = absolute melting temperature) cavities form mainly along grain boundaries oriented normal to the stress axis and failure eventually occurs by their growth and impingement.&apos; The possibility of low-ductility creep failure of magnesium-alloy reactor cans during service has prompted a number of studies of cavity formation in these materials.2-5 In this paper divergent theories of cavity nucleation6-10 are examined critically and conclusions drawn regarding the most probable mechanism of formation of cavities in magnesium. The paper is divided into two parts. The first section consists of the review and quantitative assessment of the possible role of grain boundary sliding in the nucleation process. In the second part an experimental program is described where an electron-microscope technique has been used to determine if second-phase particles exist in as-received commercially pure magnesium and in a magnesium alloy 1) THEORETICAL REVIEW Possible nucleation sites for creep cavities are: a) high-angle grain boundary triple points,11-14 b) subboundary/grain boundary intersections,15-18 c) ledges in the grain boundary, 19-25 d) second-phase particles. 9,26-30 Each of these possibilities is now considered with special reference to deformation of magnesium. 1.1) Triple-Point Cracking. The stroh31 condition to nucleate fracture is: " > vr [1] where ss = applied shear stress, ? = surface energy, C = shear modulus, L = length of sliding interface. This relationship is independent of the nature of the interface and it is possible to calculate the stress concentration at the end of a sliding high-angle grain boundary and thus deduce, approximately,* the minimum applied stress necessary to nucleate triple-point cracking. Such theoretical predictions for Nimonic alloys have been made by McLean13 and found to agree quite closely with the minimum stress determined by experiment. Stresses capable of nucleating triple-point cracking should also be sufficient to nucleate fracture at a grain boundary due to intragranular slip, for the lengths of sliding interface in the two cases are approximately equal. Thus the minimum stress for triple-point cracking should represent a demarcation between failure due to general "cracking" and that due to cavitation. Hauser, Landon, and Dorn32 have demonstrated that for polycrystalline magnesium in the temperature range 78° to 298°K the fracture stress is inversely proportional to the square root of the mean grain diameter. As pointed out by stroh31 this result indicates that Eq. [I] describes the fracture characteristics of magnesium at low temperatures. Heal3 has reported that for rapid deformation (112 pct hr-1) of polycrystalline magnesium the transition from cracking to cavitation occurs in the temperature range 175" to 275°C. He also presented the fracture-stress values for the same material tested under similar conditions. From Eq. [I] taking G = 1.3 x 10" dynes , ? = 600 ergs . cm-2,33 and L = 0.017 cm, a Stroh-McLean13,31 tensile stress of -266 kg. cm-2 is calculated, corresponding to a transition temperature of -190°C; this is in

Jan 1, 1965