Search Documents

By Wilson Blake

The Bureau of Mines used a mathematical model based on the finite element method of stress analysis to calculate stresses and displacements surrounding an open pit mine in a gravity-loaded rock mass. Comparison of the finite element solution for a semicircular notch in a gravity-loaded plate with the theoretical solution for a semicircular notch in a plate under uniform compression parallel to the free boundary demonstrates the inapplicability of the latter method to openings at the free surface of a gravity-loaded medium. High stress concentrations are formed at irregularities along the boundary of an open pit in a gravity-loaded continuous competent rock; however, for this type of rock the magnitudes of the stresses are too low to be considered a major factor in open pit slope stability. High stress magnitudes will occur if, in addition to the gravity stress field, a large horizontal stress field exists.

Jan 1, 1967

By Richard W. Knostman

A study was made of the factors affecting lead and zinc production in the Pacific Northwest. Costs, ore reserves and potential resources, and domestic demand were analyzed. It was concluded that a projected 3.1-percent average annual increase in U.S. demand for zinc through 1975 and a corresponding 2.5-percent rise for lead will be supplied mainly from mines in the Eastern and Central States. Annual Pacific Northwest mine production of lead is estimated to fluctuate around 82,000 tons, while zinc output may average 135,000 tons through 1975. Measured, indicated, and inferred reserves in the Pacific Northwest, containing 1.56 million tons of lead and 2.59 million tons of zinc, are more than sufficient to maintain this level of production. Annual production from Pacific Northwest electrolytic zinc plants is expected to increase to over 300,000 tons of slab zinc by 1975. Lead smelters may experience difficulty in maintaining output at 1964 levels.

Jan 1, 1967

Several of the current concepts of brittle fracture involve consideration of, the existence of defects or flaws. Griffith 1 observed that the tensile strength of brittle materials was several orders of magnitude less than might be expected from the calculated strength of the molecular bonds. He was able to show that the stress concentration at the tip of an elliptical crack is sufficient to raise the local stress level many fold. He therefore proposed that real materials do contain such stress risers in the form of minute cracks and that this accounts for the rather large difference between theoretical and actual strengths of brittle materials. The degree of stress magnification depends to a great extent upon the orientation of the crack with respect to the general stress system, and to the general geometry of the crack. It is but a small step to extend the theory to include flaws and defects of other sorts which, though they may be less tractable mathematically than cracks, may still function as stress risers in a real sense in real materials. Brace 2 proposed that the application of the Griffith theory to rock material could be tested in two ways: "(a) by finding the orientation of cracks from which macroscopic fractures have developed and (b) comparing failure strengths from tests at different conditions of loading." In 1963 the author and coworkers at the Bureau of Mines, Twin Cities Mining Research Center, working on a problem involving relationships between strength, sonic velocity, and microstructure "eveloped an experimental technique to examine several somewhat similar questions; namely. does the frequency of occurrence of actual or potential stress risers dictate the relative strength of the material as proposed by Weibull;4 can actual flaws or defects in the rock structure be identified and related to strength and perhaps other properties in accordance with Griffith's theory; and is the anisotropic strength and elastic behavior of certain rocks related to the preferred orientation of these actual or potential stress risers? The experimental approach developed to answer these questions appears equally applicable to the testing of Griffith's theory as proposed by Brace. Basically the approach consists of a series of point-load tensile tests followed by petrofabric examination of thin sections prepared from the specimens in order to identify and apply a quantitative measure to microstructural defects which may have contributed to the failure process. In the point-load test, tensile stresses are induced by a compressive load applied to the center of a disc-shaped specimen by means of two opposing hemispherical indentors. Failure generally occurs as a single fracture parallel to the axis of loading and bisecting the disc. Because of the geometrical symmetrical the induced tensile stresses are symmetrical about the loading axis

Jan 1, 1967

By B. D. Lichter

In a previous paper, Oelsen, Schuermann, and Hey-nertl pointed out the possibility of obtaining complete thermodynamic functions for alloy systems from calorimetric measurements alone. Specifically, if the heat content of a heterogeneous, multicomponent system is known as a function of temperature and composition, then it is possible to derive the heats, entropies, and free energies of formation of liquid phases and of solid intermediate phases of fixed composition. The authors present equations and graphical techniques applicable to eutectic systems and systems with intermediate phases without solid solubility at lower temperatures. eijering has considered possible extension of the treatment to systems with complete solid-state miscibility at lower temperatures; however, experimental difficulties practically restrict the method to systems with very limited miscibility in the solid state. The purpose of this note is to present an alternative derivation of the heats and entropies of formation of liquid phases and of solid intermediate phases from heat-content measurements alone. Fig. 1 shows three types of phase diagram to which the analysis may be applied. If the heat content is determined as a function of composition x, at temperature T, we have quite generally and the heat of mixing of the liquid is obtained directly from heat-content measurements. If the temperature T lies in a two-phase region (solid-liquid) then

Jan 1, 1967

By T. Estelle Gardner

Heat-capacity measurements were made over the range 8° to 350° K on beryllium sulfate dihydrate and beryllium sulfate tetrahydrate using an adiabatic calorimeter. No anomalies were noted in the curve for either compound. Smooth values of heat capacity, entropy, enthalpy function, and free-energy function were calculated from the heat-capacity data at 10° K intervals and at 273.15° and 298.15° K. The entropy values calculated at 298.15° K were 39.01 ± 0.12 entropy units (eu) for the dihydrate and 55.68 ± 0.17 eu for the tetrahydrate.

Jan 1, 1967

By Gordon W. Hines

This paper, dealing with network planning in an industrial complex, discusses the type and size of project that can be handled on a manual basis. After a review of the fundamentals of network planning, and specifically of the Critical Path Method, the author analyses several different types of projects, each with its own characteristics. Some can be handled in conjunction with a computer, but others can be dealt with equally well without one. Among the projects discussed are a blast furnace reline, the installation of a billet mill flying shear, and routine maintenance-type operations.

Jan 1, 1967

By F. V. Shallcross

Physical properties of thin films of CdS and CdSe formed by vacuum deposition onto glass sibstrates have been studied as a function of deposition and processing conditions. The crystallinity and surface features of CdS films were examined using electron microscopy and electron and X-ray diffraction techniques. The films were poly crystalline; the preferred orientation and crystallite size increased with film thickness, substrate temperature, and deposition time. The CdS films consisted primarily of hexagonal-phase material, in contrast to similarly prepared CdSe films which have previously been observed to contain mixtures of cubic and hexagonal phases. As-deposited CdS films showed no major dependence of Hall mobility on crystallite size or degree of preferred orientation. Hall mobility and carrier concentration in CdS and CdSe .films were measured at various temperatures; both parameters increased with temperature and yielded activation energies which depended on fabrication conditions. Surface-desorption phenomena and overcoating of the semiconductor with SiO affected the observed electrical properties significantly. THIN films of cadmium sulfide1,2 and cadmium sele-nide3,4 have been employed by various workers as semiconductors in the insulated-gate thin-film field-effect transistor, known as the TFT. These devices are most commonly made by vacuum deposition of all materials onto an amorphous substrate such as glass. A knowledge of the microstructure and electrical properties of semiconductor layers used in the thin-film transistor is essential in order to form a realistic model for the device and to improve its performance, reproducibility, and reliability. This paper will describe studies of the physical properties of vacuum-deposited CdS and CdSe films prepared under various conditions. Structural characteristics examined in- cluded phases present, crystallite size, nature of preferred orientation of crystallites, surface roughness, and structural homogeneity throughout the film thickness. Electrical properties measured were Hall mobility and conductivity and their dependence on temperature and ambient. Thin-film properties are affected by many fabrication parameters including purity and physical form of evaporant, deposition rate, film thickness, design and temperature of the evaporation crucible, geometry of the deposition chamber, nature of the residual atmosphere, composition and temperature of the substrate, and details of postdeposition processing. PREPARATION OF FILMS In this work the semiconductor films were deposited in a conventional oil-diffusion-pumped system with pressures in the 10-8 torr range. The CdS evaporant was obtained from the Eagle-Picher Co. as a high-purity coarse-grained crystalline powder; the CdSe was a high-purity sintered powder supplied by the Harshaw Chemical Co. The evaporation crucible was a resistance-heated molybdenum-wire basket coated with aluminum oxide and filled with a quartz wool plug at the top. The source to substrate distance was usually 10 cm. This region was enclosed by a Pyrex inner cylinder. The substrate was heated with an overlying Pyrex plate coated with tin oxide. The substrate temperature was controlled using a thermocouple attached to the lower side of the heater. This thermocouple was calibrated against another thermocouple attached to a dummy substrate and by observation of melting points of various metal films deposited in the system. The substrates were polished borosilicate glass plates and conventional glass microscope slides. Substrate preparation included cleaning with an ultrasonically agitated detergent bath followed by isopropanol-vapor de-greasing. Film thickness was measured interferomet-rically during and after deposition. STRUCTURE OF CdS FILMS Structural studies were performed on CdS films using electron diffraction, electron microscopy, and

Jan 1, 1967

By G. J. Biefer

"Fatigue and corrosion fatigue measurements were carried out on five commercially available metals -four steels and an aluminum alloy -which are used as structural materials in mine shaft conveyances. In the corrosion fatigue measurements, drain waters collected in the shafts of three different Canadian mines were used as corrodents. The mine waters had been selected on the basis of their relatively large differences in acidity and/ or composition.It was found that the corrosion fatigue strengths of the four steels were similar, despite their differences in tensile properties, and that the type of water used in the tests had little effect on the results. Mild steel showed the highest and most consistent values of the damage ratio (ratio between the corrosion fatigue and the plain fatigue strengths at 107 cycles). The corrosion fatigue behaviour of the aluminum alloy (ASTM Type 6061-T6) was found to differ markedly in the three mine waters. A high damage ratio (i.e., superior performance) was shown in a mine water in which the corrosion attack was uniform; much lower damage ratios were shown in waters which produced localized corrosion attack. Corrosion rates were too low to be deter-mined conveniently by conventional weight-loss methods, but calculations from polarization curves provided a rapid demonstration that corrosion rates were distinctly lower in the mine water which produced high damage ratios."

Jan 1, 1967

By A. M. Starfield

The study of strain waves in rock over the past decade has, for the most part, been an investigation related, but not applied, to rock blasting; the design of rock blasts has proceeded on a basis that is independent of strain wave research. This duality is reflected in the paper by Dr. Clark.1 While the greater part of the paper is devoted to a discussion of spherical waves in elastic and visco-elastic media, it is in an entirely unrelated section, the section on scaling and cratering, that the practical approach to rock blasting is found. Work done by the U. S. Bureau of Mines, as described in the paper by Duvall, Atchison, and Fogelson,2 has established a correlation between crater dimensions and the peak compressive strain in the rock. Strain wave measurements have thus been used to compare explosives but have not, as yet, been applied to the planning of a production round once an explosive has been selected. The optimum burden, for instance, is still determined either by experience, empirical formulae (e.g. that of Langefors 3), or a cratering experiment and the theory that has been developed around that proposed by Livingston.4 Even then there is some ambiguity in applying deductions from short, concentrated explosive charges to the long charges often used in practice (although Bauer 5 reports doing this with considerable success) and wave theory has until recently thrown no light on this problem, being confined, with only a few exceptions, to spherical charges. The hesitation in applying strain wave theory has probably been due to two questions that have not been answered satisfactorily: just how important is the strain wave in rock breakage, and if it is important, under what conditions will the wave break rock? This paper is an attempt to answer the first question, to avoid the second question by an admittedly oversimplified assumption, and then to investigate the implications of this assumption for blasting with long cylindrical charges.

Jan 1, 1967

By Rogers F. Davis

This publication has been prepared to supply manufacturers and industrial users a listing of mobile diesel-powered transportation equipment approved or certified by the Bureau of Mines f r use in gassy noncoal mines and tunnels. Testing of diesel-powered equipment is one phase of the Bureau's health and safety program of approval of electrical and diesel equipment designed to prevent explosions, fires, shocks, and toxic hazards in underground mines. In mines such equipment must be used and maintained properly. Manufacturers submit machinery and component parts to the Bureau for study f their design and safety features. Equipment must pass exacting tests and meet strict requirements established through research, development, and experience before the Bureau approves it as permissible for safe use in mines.

Jan 1, 1967

By G. Krauss, J. M. Thompson, H. Y. Kumagai

Boron-doped p-type and arsenic-doped n-type source materials were used to deposit thin silicon films on amorphous fused quartz substrates by cathodic sputtering in argon atmospheres. All as-sputtered films were found to have high electrical resistivities of about 104 ohm-cm, despite controlled variation of the substrate temperature from 50O to 400°C. The high resistivity of the n-type films persisted even after postdeposition heat treatments as high as 1000°C, while p-type films showed a sharp decrease in re-sistivity to values on the order of 1 ohm-cm or lower after heat treatments above 650°C. X-ray and electron diffraction, together with transmission electron microscopy of the p-type films, revealed that the improved electrical properties resulted from two distinct processes. A primary crystallization or recovery within the pains, which were approximately 200Å diam in the as-sputtered films, accompanied the initial sharp drop in resistivity at 650°C. Following this process, a secondary recrystallization or discontinuous grain growth was nucleated in films heated at 1000°C. The resulting significantly increased size of certain grains and the corresponding decrease in grain boundary area accompanied an additional decrease in resistivity after heat treatment at 1000°C. The properties of thin silicon films are of interest because of their possible application in device technology. Although evaporated silicon films on amorphous substrates1-3 and both sputtered and evaporated germanium films4-' have been studied in some detail, sputtered silicon films have not been widely investigated. It has been observed that evaporated silicon films deposited at substrate temperatures below approximately 600°C are amorphous.1,3,9,10 At substrate temperatures higher than this, the films are polycrys-talline, sometimes exhibiting a fiber texture with the fiber axis normal to the substrate surface.' Similar results have been obtained with germanium films, although in this case the substrate temperature for the amorphous to crystalline transformation is reported to be as low as 150OC.5 The mechanism of film deposition by cathodic sputtering differs markedly from that of thermal evaporation. It might be expected, therefore, that the properties of sputtered and evaporated silicon films would also differ. The purpose of our study was to determine the effects of deposition conditions and heat treatments on the electrical resistivity, structure, and composition of thin silicon films sputtered on fused quartz substrates. EXPERIMENTAL DETAILS Apparatus. A schematic diagram of the sputtering apparatus is shown in Fig. 1. The vacuum chamber was enclosed by an 18-in.-diam by 12-in.-high Pyrex bell jar mounted on a stainless-steel base plate. Access holes in the base plate were used to supply argon gas to the chamber, to allow for various electrical feedthroughs, and to provide mechanical motion to the shutter between the source material and substrate. The chamber was evacuated by a pumping system consisting of a 720 liter per sec oil diffusion pump backed by a 13 cu ft per min mechanical pump. Ultimate pressures of less than 1 x 10-6 torr could be achieved. The substrates were securely mounted on the stainless-steel substrate holder by quartz tabs held in place by stainless-steel screws. Temperatures of the substrate holder were measured by a thermocouple inserted within the holder. A quartz lamp was used to heat the holder and temperatures as high as 420°C could be maintained. Deposition Conditions and Procedure. The substrates used were polished fused quartz slides 116 by 1-12 by 3 in. and were outgassed at 200°C for 1 hr at a pressure less than 1 x 10-5 torr before film deposition. This was followed by a presputtering period of 2 hr during which the movable stainless-steel shutter was so positioned that deposition on the substrate was prevented. At a sputtering voltage of 5000 v dc and an argon pressure of 0.03 torr, the cathode cur-

Jan 1, 1967

By W. C. Winegard, J. R. Carruthers, A. Plumtree, L. R. Morris

The unidirectional solidification of dendrites containing central twin planes was studied in A1-Ti alloys. Once nucleated, the twinned dendrites are a Twore ejficient form for solute redistribution and therefore grow in preference to the normal columnar dendvites. Comparison of these twinned dendrites to adjacent colunmar dendrites by means of decanting experinzents and electron-probe rnicvoarmlysis indicates that these special dendrites grow with less undercooling than normal dendrites. These findings are further supported by the effect of forced convection on the dendrite morphologies. COMMERCIAL semicontinuous cast ingots of most aluminum alloys frequently exhibit large grains which appear to be composed of hundreds of parallel, continuous, thin lamellae. This structure has been termed "basaltic",' "fiederkristall", or, commonly, "feathery grain". The lamellae are 'about 100 p thick, several inches long, and each lamella contains a central (111) coherent twin boundary. The feathery grain has been reported to have a (112) direction2 and a (110) direction4 in the twin plane parallel to the casting direction, in contrast with the usual columnar structure where a (100) direction predominates. Aust et uZ.~ proposed that the twin boundaries were growth twins nucleated by stacking faults on the octahedral planes. chalmers6 has suggested that feathery grain may grow by a re-entrant edge mechanism, as proposed by wagner7 for twinned dendritic growth in germanium. Cahn et ~1.~ have concluded that the occurrence of feathery grain is evidence of some form of lateral layer growth rather than the atomically continuous growth normally observed in metals. The postulates by Chalmers and Cahn would seem to be contradicted by the work of Nakao~"' who showed that feathery grain only occurs when growth rates are high and the aluminum contains some solute. Specifically, Nakao found that in order to obtain feathery grain, in small castings solidified unidirec-tionally upward, the rate of growth must be above 2.4 cm per min and a critical solute concentration must be present. Below this solute concentration the grain structure was totally columnar. The critical solute concentration was found to be approximately: 0.04 wt pct Ti, 2 wt pct Cu or Mg, and 8 wt pct Zn. As pointed out by Chalmers it is not obvious why a twin-plane re-entrant edge mechanism would occur in aluminum which is thought to have a diffuse solid-liquid interface. The present experiments were undertaken to determine the growth mechanisms in- volved and to study the solute segregation in more detail. EXPERIMENTAL PROCEDURES Alloys ranging in composition from 0.05 to 0.23 wt pct Ti* were prepared from 99.9 pct pure Ti and 99.993 pct pure Al. Two-hundred-gram samples of A1-Ti binary alloys were solidified unidirectionally and vertically upward from a water-cooled copper base, in a heated insulated mold. The 1-in.-diam, 6-in.-length mold was made of Marinite (manufactured by Johns-Manville Co.). The mold was attached to a 24-in. pivoted arm such that by dropping a weight the mold was rotated 180 deg, throwing the liquid metal from the solid. In this way, the solid-liquid interface was revealed by decanting. A sketch of the decanting mold is shown in Fig. 1. The alloy was poured into the mold at temperatures ranging from 680" to 750°C, partially solidified by water cooling from the base, and decanted after a measured time interval. Growth rates for each metal-pouring temperature were calculated from solidification-time vs length solidified curves. Temperature gradients in the melt were measured using four No. 34 gage thermocouples which protruded into the mold cavity. Grain orientations were determined by X-ray diffraction using Laue back-reflection techniques. Grain substructures were examined metallographically, using polarized light, by applying a thin epitaxial anodic film to polished sections after the method of Hone and pearson." Titanium micro segregation was measured by electron-probe microanalysis using a NORELCO AMR/~ with a mica crystal and proportional-flow counter. Several of the cast samples exhibited feathery and columnar dendrites growing in the same direction and

Jan 1, 1967

By P. G. Shewman, T. L. Wilson

Using published surface-diffusion (D,) data and published sintering equations, it is shouln that surface difusion should dominate the neck-growth stage of intering for all materials in which D, has been measured (six metals and A1as). Also, grain boundary diffusion can be expected to contribute appreciably to shrinkage and possibly to neck growth below some critical temperature of the order of 70 pct 01- the absolute melting temperatuve. In view of the widespread conclusion in previous sintering work that volume diffusion dowzinates neck gvowth, experiments were conducted using spherical copper powders to test this conclusion. Scaling studies on neck growth at 950°and 1020°C clearly demonstrated that suyface diffusion dorninates. Kinetic studies on shrinkage gave more equivocal results that indicated an increasing role of' grain boundary transport at lower temperatures. Five diarszeters from 100 to 300 u were used in the scaling sludy and a temperature range of -650' 10 950 C was covered in the shrinkage studies. All experiments were conducted in dvy hydrogen. In 1949, Kuczynski published his now classic paper on the determination of the transport mechanism in sintering from the time laws of neck growth. In the interim, these laws have been applied to many systems and slightly modified by several authors. Essentially all these authors concluded that, for crystal- line materials, the dominant transport mechanism in neck growth is volume diffusion. This stems from the observation that the neck radius increases about as t"5 and that the activation energy approximates that for lattice diffusion. A related but independent series of studies stems from Mullins' rigorous analysis of the growth of the groove formed where a grain boundary meets a free surface." xperimental work stemming from this analysis has shown that for each crystalline material studied (Au, Ag, Cu, Ni, Fe, Pt, Al2O3) surface diffusion was clearly the dominant transport mechanism for groove widths up to the order 10 to 20 p. The ratio of the quantity of material being carried by lattice diffusion to that carried by surface diffusion increases linearly with the groove width, so surface diffusion is dominant for all widths under 10 to 20 u. The analysis of the relative contributions of surface and volume diffusion to grain boundary grooving, and to neck growth in sintering, shows that they are quite similar. Thus, using the available surface-diffusion data and the approximate equations of Kuczynski, or the more rigorous recent equations of Nichols and Mullins, 3 it can be shown that the small necks between particles must grow almost entirely by surface diffusion. The purpose of this study was to re-examine the basis for the conclusion that the neck-growth stage of sintering proceeds by volume diffusion. Using spherical copper powders, of several different diameters, precise experimental measurements were made of both neck growth and shrinkage. Application of Herring's scaling laws to the neck-growth data clearly indicated that neck growth occurred by surface transport, even though the neck radius increased as or Using the recent analysis of Mullins and Nichols as well as published data on surface diffusion, it is shown that the observed time law, as well as actual rate of neck growth, can be satisfactorily explained by a surface-diffusion mechanism.

Jan 1, 1967

By S. A. LoPilato, J. T. Smith

SEVERAL techniques have been evaluated for cooling the throat area of rocket-nozzle inserts to prevent erosion or fracture of the inserts during exposure to high operating temperatures and pressures. Self-cooled composites, such as infiltrated tungsten, have shown considerable promise for these applications. These composites can be fabricated by infiltrating the refractory matrix with a lower-melting metal or non-metal which is insoluable in tungsten. During firing, the lower-melting substance undergoes a series of continuous endothermic phase changes which absorb sufficient heat to maintain the nozzle matrix material at or below a safe operating temperature. At present, the state-of-the-art has reached a point where the refractory matrix density and microstruc-ture have been established as the critical parameters to be controlled for optimum self-cooled performance.'" Nondestructive testing has been utilized to ensure that porous tungsten billets were of uniform density and free from cracks or other defects prior to fabrication into rocket nozzle inserts. Ultrasonic-velocity techniques have been employed because of their reliability and reproducibility. The purpose of this note is to present and interpret the test data developed for porous tungsten matrices. For evaluation purposes, tungsten powders with Fisher subsieve sizes of approximately 4 and 18 p have been obtained for study from four commercial sources: the General Electric Co., Wah Chang Corp., Fansteel Metallurgical Corp., and Kennametal, Inc. Porous tungsten matrices were fabricated from the powders by hot pressing in induction-heated graphite die assemblies. Typical billets ranged from 3 in. diam, 2 in, high to 5 in. diam, 5 in. high. The ultrasonic-velocity measurement technique employed was through transmission, pulse echo at a frequency of 1.0 mc using matched barium titanate crystal transducers. The testing equipment included a pulsed ultrasonic generator, an amplifier, a specimen holder, and an oscilloscope, as shown in Fig. 1. The porous tungsten thickness was measured to i 0.0005 in, with precision micrometers while the oscilloscope achieved 0.02 psec time measurement accuracy. The time for a sound wave to pass through the billet, the bulk wave velocity, was calculated to 0.5 pct using Eq. [l]: V-} where V = bulk wave velocity, in. per psec, T = specimen thickness, in., and / = time, psec. To develop inspection standards, the bulk density of a porous tungsten billet was determined by the ASTM water-immersion technique.3 The ultrasonic-velocity measurements were completed at seventeen positions for each billet and averaged to develop a characteristic standard velocity for a particular tungsten powder at several density levels. A plot of ultrasonic velocity vs density is presented in Fig. 2 for six different tungsten powders. This graph has been established as

Jan 1, 1967

By E. Hoek

The stability of a rock structure depends primarily upon the extent to which fracture develops within the structure, The prediction of the extent of potential fracture, the first step in the study of fracture development, involves a knowledge of both the stress distribution in the structure and the criterion which governs rock fracture under various stress conditions. While a great deal of research effort has been devoted to the development of techniques for analyzing the stresses in mining and civil engineering structures1-3 and to the investigation of the fracture mechanism of rock 4-6 relatively little attention has been paid to the application of available knowledge to the solution of practical engineering problems. This paper describes a photoelastic technique for the determination of potential fracture zones in certain types of rock structures. A practical example, based upon a problem which might be encountered in designing the layout of deep-level mine excavations, is given as an illustration of the application of this technique. STRESS ANALYSIS AND ROCK FRACTURE In deciding upon the technique to be used for the solution of a problem involving the prediction of rock fracture it is necessary to consider: 1) What type of stress information is required to satisfy the fracture criterion for rock; anti 2) How this information can most conveniently be obtained. It has been established, both theoretically 4,7 and experimentally 5,6,8that the fracture of hard rock depends primarily upon the relationship between the algebraically greatest and the algebraically smallest of the

Jan 1, 1967

By Robert E. Barieau

This report describes a method for treating pressure-volume-temperature (PVT) data obtained with a Burnett compressibility apparatus. The method makes use of a general nonlinear least-squares technique developed at the Bureau of Mines Helium Research Center. It is assumed that an adequate functional form is available for the expression of the compressibility factor as a function of either the molal density or the pressure. The functional form of the compressibility factor can be either linear or nonlinear in the parameters to be evaluated. Formulas are given for calculating variances and covariances of all parameters evaluated and for calculating the variance of calculated quantities of interest.

Jan 1, 1967

By N. Mungan, F. W. Smith, J. L. Thompson

Adsorption of polymers and transport, rheology and oil recovery efficiency of their solutions were studied in the laboratory to evaluate the use of polymers in waterflood-ing. While a tenfold mobility reduction was obtained with polymer concentrations as low as 0.05 per cent by weight, the mobility reduction depended on the type of polymer, molecular weight, salinity and pH of water, crude oil and capillary properties of the porous media. Choice of a suitable polymer and a workable concentration will have to be tailored for each application. Little reduction in the residual oil saturation can be expected from polymer flooding. Improvement in the volumetric sweep efficiency is possible hut the extent of the improvement can best be evaluated by properly designed field testing. Some aspects of the field use of polymer floods are discussed. INTRODUCTION Waterflooding is a simple, inexpensive secondary recovery method and is being used widely. Innumerable laboratory studies have been made to unravel the fundamentals of the displacement of oil by water and to find the ways of most efficient oil recovery. These studies and a great many field case histories have revealed that the prime cause of poor oil recovery is the inefficient and incomplete sweep of reservoir volume by the injected water. Sweep efficiency is affected by many factors of which the mobility ratio is an important one. Mobility ratio M is defined here as the ratio of water to oil mobilities: M = (k»/y,r)/(k,JJJJ........(1) In Eq. I, the permeabilities are the effective permeabilities and depend on fluid saturations and, hence, change during the different depletion stages in a flood. A wide practice is to use the effective water permeability at residual oil saturation and the effective oil permeability at interstitial water saturation in Eq. 1. If the mobility ratio is greater than one, the mobility ratio is unfavorable and water, being more mobile than oil, would finger through the oil zone resulting in poor oil recovery efficiency. If the mobility ratio is favorable (one or less) the displacement of oil by water occurs more or less in a pistonlike fashion. In some waterfloods. the mobility ratio is unfavorable and any additives by which the mobility of water can be decreased would favor more efficient oil recovery. The thing to bear in mind, however, is whether or not the improvement in oil recovery is sufficient to more than pay out the cost of the additives needed. For example, materials like sugars, alcohols and glycerine reduce water mobility by thickening the water, but the cost of material requirement precludes any field application. For an additive to be useful in water-flooding, it must bring about a large reduction in water mobility at low concentrations; it must be adsorbed only negligibly; and it must not completely plug up the formation. Some synthetic organic polymers have shown promise of meeting these requirements and have been used in the field.'-W owever, no in-depth studies of the rheological, adsorption and oil displacement characteristics of polymer solutions have been reported. The present work is a study of these properties. EXPERIMENTAL In this work, concentrations are given on a weight per volume basis; 0.5 per cent concentration means 0.5 gm of polymer is dissolved in enough water (or NaCl solution) to make 100 ml. A bactericide, usually 0.1 to 0.2 per cent by volume of 38 per cent formaldehyde solution, was used in the polymer solutions. The NaCl solution was 30,000 ppm. Some properties of the polymers studied are given in Table I. Physical properties of all cores used are in Table 2. Flow behavior of polymer solutions was studied by three consecutive flow tests in cores. First, water (or brine) was injected at constant rate of about 1 ft/D to obtain the water mobility. Then, filtered polymer solution (prepared in water or brine) was flowed through the core. Since the rate was constant, increase in the pressure drop across the core reflects decrease in the mobility. Finally, the core was flooded with water (or brine) to study recovery of mobility. The Alundum cores which were used in

Jan 1, 1967

By Robert E. Ogilvie, Zvonimir Ban

Oxidation experiments were conducted above 600°C to investigate the oxidation products formed on the surface of MoSi2. Results are presented which indicate that minor iron impurities play a key role in the oxidation behavior of MoSi2 above 600 °C. Based on considerations of the crystal chemistry of the oxidation products, MoSi2 with rhenium and iron additions was found to be resistant to oxidation in the pesting temperature range. AS early as 1914, Honigschmidtl observed that some silicides of molybdenum exhibited high resistance to oxidation at elevated temperatures. This fact did not arouse much interest until 1950, when Kieffer and cerwenka2 examined this property in more detail. They found that Mo-Si alloys with approximately 70 pct Mo (by weight) could be heated to 1600°C in an oxidizing atmosphere without any significant damage. The surface was found to be protected by the formation of an extremely thin silica glass layer which had no tendency to spa11 during subsequent thermal cycling. In 1955, Fitzer3 discovered that even solid bodies made of MoSi2 completely oxidized within a relatively short time when exposed to the air in the temperature range from 300° to 600°C. To describe this phenomenon he proposed the name "molybdenum disilicide 'pest' ", clearly analogous to the previously observed "tin plague" ("tin pest") which, however, arises as the result of a phase transformation. Studies performed by Fitzer and, in particular, one published recently by Berkowitz, Blackburn, and Fel-ten,' comprise the most extensive research to date on the pest phenomenon in MoSi2, as far as the fundamen- tal mechanism of the process is concerned. The first of these studies revealed the existence of a crystalline phase which appeared at the surface at 750°C and dissolved in the glassy silica layer at 1150°C. The logical assumption was that this phase was some reaction product of MOO3 and SiO2. The formation of a reaction product of this type seemed probable since it had been mentioned by Glemser and Lutz6 in a paper describing their studies of molybdenum oxides; however, this assumption was later disproved.8 It is our belief that information concerning the exact nature of this crystalline phase may be important for a better understanding of both pesting and the protection mechanism. Therefore, since the only available general description of the pest phenomenon was that of Fitzer, it was decided to reproduce his experiments. These experiments established that, in addition to the "pest" and "nonpest" temperature range, an intermediate region exists between 600" and approximately 650°C. This region is characterized by the appearance of a variable amount of yellow to orange colored crystals. The electron-beam microanalyzer was used to qualitatively determine their composition. Iron and molybdenum were found to be major constituents. This result can be explained based on the following facts: 1) iron, according to literature data,* is the most common impurity in molybdenum powder, and its content can be as high as 0.25 pct; 2) technical silicon powder usually contains iron; 3) steel ball mills are often used for the crushing and grinding of MoSi2. In order to clarify the exact role of iron, it was deliberately added to a stoichiometric mixture of molybdenum and silicon. The observed results corroborated the previous experiment, proving that iron (probably as some silicide phase) concentrates along the grain boundaries. I) EXPERIMENTAL PROCEDURE A) Oxidation of MoSi2 with Iron Additions. 1) Specimen Preparation. Specimens were prepared by both

Jan 1, 1967

By the use of flotation tests it was confirmed that there are two functions of oxygen in sulphide mineral flotation. Sized samples of galena and chalcopyrite were sulphidized, washed free of excess sulphide ion, and then contacted with air-saturated water for certain lengths of time. The mineral was then transferred to a sealed laboratory flotation cell containing water with a known concentration of dissolved oxygen. Xanthate and frother were added and flotation continued for 1 min.Both the extent of mineral oxidation and the concentration of dissolved oxygen markedly affected the flotation of galena and chalcopyrite. The response to a change in either variable is dependent on the level of the other, but generally best flotation occurs with the maximum degree of air saturation of the pulp. Galena flotation is hindered by oxidation of the mineral beyond a small threshold amount but a similar effect for chalcopyrite was not observed...

Jan 1, 1967

By H. M. Strong, R. A. Oriani

THE technological interest attaching to light, age-hardening alloys for structural uses has been pointed out to one of us.1 A potentially interesting alloy would be titanium-rich Ti-Mg alloy, provided that sufficient solid solubility exists. or could be induced at high pressure. and provided also that age hardening can be induced by proper temperature and/or pressure annealing. It was decided therefore to explore the feasibility of producing a Ti-Mg alloy in the high-pressure apparatus. Experimental. Three high-pressure runs have been carried out. In each case the geometry of the sample was that of a cylinder of titanium of commercial purity, into which a narrow hole had been drilled along the axis; this hole was filled with magnesium wire,

Jan 1, 1967