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By I. B. Cadoff, J. C. Bilello, R. Rosenberg

Diffiusion of magnesium into the surface of LiF crystals to controlled depths and subsequent heat treatments provided a wide range of surface zone harahesses and structure, The bend strength of the LiF crystals was increased by as much as an or-dev of magnitude. Ductility was achieved when dislocation generation occurred in the diffusion zone or when dislocations penetrated to the surface from the intevior. A critical surface hardness of 130 to 140 kg per sq mm was found helozu which generation could take place in the diffusion zone and ahoue which the zone was impenetrable, This hardness was obtainable by several methods, among them the aging of quenched MgF2 -LiF solutions to produce MgF, precipitation. Maximum hardness was ohtained in quenched specimens with no visihle evidence of MgF,. Diffusion-zone formation followed a parabolic rate law and an activation energy of 20.9 kcal per mole was obtained for the process. RECENTLY, the properties of ionic crystals as related to surface condition have been receiving much attention, specifically the transitions between ductile and brittle behavior. Originally Joffe 1 showed that NaCl crystals could be made ductile by immersion in water and related this to the elimination of surface microcracks. Aerts and DeKeyser 2 and Gorur 3' have subsequently shown that ionic crystals are inherently ductile and are embrittled through contact with air. Machlin and Murray4 hypothesized that a layer of NaCIO3 produced by contact of ozone with NaCl induced embrittlement by acting as a barrier to outward dislocation flow. westwood,' Rosenberg and Cadoff,9 and Bilello and cadoff' have reported surface strengthening of LiF crystals by coating with a magnesium compound and then heat treating for adherence. The major effect of the coat was to inhibit dislocation-slip lines from reaching the specimen surface. westwoods showed microcrack formation and fracture to be caused by slip-band interactions at the surface. The material presented in this paper is an extension of the work reported earlier by Bilello, Rosenberg, and cadoff'6,7 and illustrates the wide range of surface properties and bulk behavior obtainable by use of heat-treated magnesium-diffused surface regions in LiF crystals. EXPERIMENTAL PROCEDURE The LiF single crystals were obtained from the Harshaw Chemical Co. Some batch to batch variation was observed; therefore all specimens for a given test series were cleaved from the same crystal. The typical dimension used was 1 by 0.1 by 0.40 in. Surface damage resulting from cleavage was removed by chemically polishing in a 2 pct NH4OH solution. Each group of specimens was given a vacuum anneal at 700°C for 4 hr to provide a base standard for measuring comparative effects of various surface treatments. To produce the reacted surface zone, the annealed specimens were immersed in a boiling suspension of MgF, in doubly distilled HzO, agitated slbwly for 30 sec, removed, and dried at room temperature. Uniform coatings of MgF, were deposited with a thickness of approximately 5 mils. It should be noted that this technique can be modified for use with crystals which are soluble in water by using boiling absolute alcohol as the dissolving medium. This was found effective for the coating of NaCl with MgF2. The diffused surface zone was obtained by annealing the coated samples at elevated temperatures in a vacuum of lob4 mm Hg. Penetration depth was controlled by varying the annealing time from 1/2 to 28 hr. After heat treatment, the samples were tested for bend strength and hardness. Load was applied by four-point bending in a hard-beam testing jig. Four-point rather than three-point bending was used to provide a wide area of constant stress and to minimize the effect of localized inhomogenities in the specimen. The deflection rate was 8 x min-' and the distance between knife edges was 1/4 in. Load-time curves were obtained from a chart recorder coupled to the machine and converted to resolved shear stress on the shear plane vs deflection, as plotted in the figures. The unstressed portions of the sample outside of the two outer knife edges were used for the microhardness studies. Microhardness measurements were made with a Bergsman tester attached to a Reichert metallograph. All hardness impres-

Jan 1, 1964

By R. J. Lutton

Empirical data from 91 rock excavations have been used to construct a family of slope curves on a chart relating excavation height and inclination. The highest and steepest slopes from each excavation are plotted and connected by a line. The 31 1ines appear to establish one or two geometrical slope fields through which the curves are projected. The curves apparently represent a lumped eflect of many factors too complex to be considered individually. Important factors such as geological structure or ground-water conditions can dominate the picture, but where these factors do not overshadow others, the slope chart should be useful for estimating or checking optimum inclination. The U.S. Army Corps of Engineers (USAE) has been engaged since 1962 with the U.S. Atomic Energy Commission in a joint research program to develop nuclear excavation technology. The Corps is responsible for collecting the requisite data on engineering and construction problems associated with nuclear excavation. The ultimate objective is to develop a capability to use nuclear explosives as a construction tool on public works projects such as harbors and canals. The present study on empirical inclination-height curves for conventionally excavated slopes is an outgrowth of an investigation' sponsored by the USAE Nuclear Cratering Group on applicability of data from existing excavations in establishing guides for engineering judgment in crater excavation. Data were generously contributed by over 50 mining companies among other organizations. Inasmuch as several companies preferred that their contribution be anonymous, all data are treated so here. Some Factors Affecting Stability Many factors affect or are suspected of affecting the stability of excavated slopes, e.g., adverse structural orientation, degree of structural ordering, ground water, climatic conditions, mechanics of excavation, and plan-profile configuration. Such factors are lumped together in developing a slope chart. Obviously geological structure and ground water can overshadow all other factors. Where such is the case, the simplification of slope charts may give an erroneous picture (not conservative enough). A further complication results from the fact that the concept of stability may vary according to the use of the excavations. For example, slope adjustments that would be regarded as failure in a powerhouse excavation, might be tolerable in a mining operation. Mine slopes are continually being modified by further excavation, and instability that would develop in a similar permanent excavation slope over a period of years might not have time to develop in a mine. Inclination vs. Height Charts Charts of inclination vs. height for particular formations or conditions have been used in the past as an aid for designing excavation slopes. Some of these have been based upon empirical analyses of collections of data and experience. MacDonald" and Lane have presented slope tables and charts for excavated and natural slopes in relatively weak sandstone and shale. Coates' has shown an inclination-height chart for slopes in incompetent rock. Most organizations have developed slope design criteria which relate bench widths, heights, and inclinations to use in various rocks. Slope data collected in present studies can be similarly used to develop inclination-height charts; however, a plot of all slopes on such a chart shows very little because of the wide spread of the data. Reasons for the dispersion of points are: (1) many slopes are not carried at optimum inclination, particularly in mines where maintaining roadways and following irregularities of ore bodies are more important than achieving steep inclinations; (2) many engineers and geologists with varied backgrounds and viewpoints have been involved in designing these slopes; and (3) each slope is characterized by a unique combination of factors affecting stability and in turn optimum inclination. Significant curves can sometimes be constructed where the points can be grouped into related clusters from the same excavation. The essence of this approach appears when only two slopes from each excavation are considered—the highest slope and the steepest slope, connected by a line segment (Fig. 1). This reduces considerably the usable data because in many cases only one of these two slopes is available. Nevertheless, the concession seems justified. Construction of Slope Curves Ninety-one pairs of points and connecting line segments were assembled in this study. The line segments were assumed to approximate a geometrical slope field (Fig. 2), and a family of curves has been visually projected through to represent the slope field. It should be

Jan 1, 1971

By Allan T. Gwathmey, J. Bruce Wagner, Kenneth R. Lawless

Between 250°and 550°C in oxygen pressures of 10 to 760 mm Hg, the relative oxide thicknesses formed per unit time on the (100), (111), (110), and (320), decreased in this order. The predominant oxide orientation was (001)Fe3O4 and [110] Fe304 A small amount of a-Fe2O3 which exhibited a fiber pattern was observed in all oxides except those formed at 250°c in low oxygen pressures. IN order to understand the properties and behavior of thin films, particularly their role in oxidation reactions, there is needed more experimental information on their structure, composition, and kinetics of formation on clean surfaces of known geometry. The present study was undertaken to obtain such information for thin oxide films formed on single crystals of a body centered cubic metal, iron. Crystals in the form of spheres were used in order to expose all possible crystal planes to the reactant gases simultaneously. Using this procedure the relative rates of oxidation of all planes could be estimated, and those exhibiting, maximum or minimum oxidation rates could be selected for a more intensive study of composition and expitaxy. Since the three types of information were obtained from the same experiment using a single crystal substrate, any differences between rate, composition, and expitaxy on the several planes may be attributed to the influence of the substrate structure. EXPERIMENTAL The starting material for this study was Armco iron rods, 6 in. long and 3/8 or 1/2 in. in diam. The analysis was reported to be 99.8 pct Fe, with major impurities listed as carbon 0.018 pct, manganese 0.027 pct, phosphorous 0.005 pct, sulfur 0.029 pct, silicon 0.005 pct, and copper 0.11 pct. These rods were cleaned with ether and heated in an atmosphere of moist hydrogen at 950°C for three days. The purpose of this treatment was to decarburize the iron and to provide a consistent, uniform grain size for the growth of single crystals. Crystals in the form of rods, up to 1/2 in. in diam and 2 in. long, were prepared by a method similar to that reported by Leidheiser and Buck.2 Spherical crystals, 3/8 and 1/2 in. in diam and having a handle about 1/4 in. in diam by 112 in. long, were machined from the single-crystal rods. After machining, each crystal was etched in aqueous nitric acid to remove the cold-worked metal at the surface. Before each experiment, the crystal was polished mechanically with metallographic papers through number 4/0, and electropolished in a perchloric acid-acetic anhydride mixture by the method of Jacquet and Rocquet.3 The crystal was washed in running distilled water for at least 5 min. The excess water was blotted with a soft paper tissue, and the crystal was placed in an all-glass reaction vessel (See Fig. 1). The crystal was heated at 550°C in hydrogen for at least 8 hr prior to the oxidation in order to reduce any surface oxides and to help relieve any stresses in the metal. For the structure and composition studies, flat faces were cut parallel to (loo), (111), and (110) planes on the iron crystal spheres. The orientation of these faces was checked by a back-reflection X-ray diffraction technique. The faces were within 2 deg of the desired orientation. The flat faces were treated as described above except that prior to electropolishing they were given an additional polish on metallographic felt saturated with twenty-minute levigated alumina. After the crystal was heated in hydrogen for at least 8 hr, the temperature was adjusted to the desired value, and the hydrogen was evacuated. Commercial oxygen which had been purified by successively passing through tubes containing magnesium perchlorate, Ascarite and magnesium perchlorate was admitted to the desired pressure as measured by a mercury manometer. A resistance-wound furnace surrounded the oxidation chamber, and a temperature controller maintained the temperature within ±3°C. The furnace was provided with a small window for observing the crystal. The changes in thickness of the oxide films were followed by observing the interference colors. The oxidation was allowed to proceed until the desired oxide thickness was attained on a given crystal plane. The experiment was terminated by evacuating the oxidation

Jan 1, 1962

By R. C. Himes, K. Zanio, J. B. Wagner, J. W. Moody, J. F. Miller, W. Johnson

The recent research with which this paper deals has been concerned with the preparation of pure PbTe crystals suitable for control of radiative processes and othe.v electronic applications. The research has been directed toward the developrnent of methods for the preparation of puve, homogeneous, loul-ca,wier-density PbTe crystals suitable for use in the fabrication of optically pumped and electrically pumped diode lasers. Steps in the preparation of the crystals include 1) purification of the starting materials, 2) synthesis and purification of the PbTe, 3) growoth of PbTe crystals, and 4) adjustt~zertt of composition of the crystals This Paper describes the general preparation procedure employed and discusses some investigntiotzs of purification processes. THE as-received lead and tellurium are nominally 99.999 to 99.9999 pct pure. Assays furnished by the suppliers, obtained by emission spectrographic analysis, show only the presence of about 2 ppm Mg in the tellurium. Such analyses are not very informative, however, since they give no information on the concentrations of normally gaseous impurity elements such as oxygen. Both the lead and the tellurium in the as-received state usually contain appreciable concentrations of oxygen—primarily in the form of oxides on the surfaces of the material. To reduce the oxygen content, the lead is held in the molten state in hydrogen at -700°C for several hours. For this treatment, the lead is contained in a graphite boat which is rf-heated, and the hydrogen is passed through a liquid-nitrogen trap prior to use. Tellurium is subjected to multiple distillation in hydrogen to remove oxygen and other foreign impurities. If, in conducting the distillation, approximately the last 10 pct of the charge at each "stage" is left as the discard cut, purification of the tellurium proceeds as indicated in Fig. 1.l Tellurium used in this work has been distilled two or three times to reduce carrier concentration to about 10" per cu cm. The PbTe is prepared from the purified elements by reacting them in the molten state in sealed, evacuated, or hydrogen-filled silica ampoules. The charge is usually held above the melting point of PbTe (923°C) at 1000 C for 24 hr to ensure that it has been homogenized. Two methods have been employed for the growth of the required single crystals of PbTe: growth from the melt, which will be discussed first, and growth from the vapor phase. Large single crystals of p-type PbTe can be grown readily from the melt by the Bridgman method. For this method of crystal growth, the PbTe is synthesized in situ from proper proportions of the purified elements. Growth (dropping) rates in the range 1.3 to 6.5 mm per hr are employed. Material near the maximum melting composition (about 50.012 at. pct Te) is utilized to avoid composition change on freezing, and thus to obtain crystals of nearly uniform composition. Crystals prepared by use of procedures described up to this point were sufficiently pure and perfect that they could be used for the preparation of laser crystals in studies at Lincoln Laboratory.2-5 ADJUSTMENT OF COMPOSITION Good n-type crystals of PbTe cannot readily be grown from the melt. Further, growth from the melt of crystals of any compositions (n or p type) other than those near the maximum melting composition is difficult because of the large composition changes that must occur on freezing.'" However, melt-grown crystals can rapidly be brought to other desired compositions by isothermal equilibration through the vapor phase with a two-phase Pb-Te stock material, essentially as described by Brebrick and Allgaier.1 The work to be discussed has been concerned with the preparation of n-type crystals; thus, the two-phase stock which was employed contained excess lead, and all ensuing discussion is of the preparation and properties of n-type crystals. The equilibration was designed to the shift composition to the lead-rich limit of stability at the selected temperature. Initial treatment of the crystals at high temperature was employed to minimize the total time required for the equilibration. Final adjustments of the composition and state of the crystals were made by use of low-temperature heat treatment at temperatures in the range 200" to

Jan 1, 1968

By R. T. DeHoff, F. N. Rhines

The problem of determining the number of particles of a phase distributed randomly in unit volume c an opaque matrix from measurements made on random plane sections is closely investigated. A formalized derivation for the general case is presented. Applications of this formal result are made to specific types of aggregates dispersed in a matrix; circles, particles with flat circular ends, cylinders, and constant shape aggregates of ellipsoids of revolution. Quantitative measurements of the average geometric properties of these aggregates are developed. In 1953 R L. ullman' developed a technique for determining, from measurements made on random plane sections, the number per unit volume, Nv, of particles imbedded in an opaque matrix. Using meas urements previously developed for volume fraction, vV,' and surface area per unit volume, .SV,= he was able to determine average volume, average surface area, and average dimensions of particles, independent of size distribution, for spheres and circular disks,' as well as for uniformly sized cylinders of any axial ratio.4 The technique is mathematically rigorous for the cases studied. Recent studies of this problem have yielded rigorous solutions for the general case of cylinders, permitting evaluation of NV independent of size distribution and with all axial ratios intermixed. Generalization to shapes having flat, circular ends has been deduced. A solution has also been obtained for the ellipsoid of revolution, independent of size distribution, but requiring a constant axial ratio in the generating ellipses. In the following derivations, as in Fullman's work, it is assumed that the problem is purely a combination of geometry and probability theory,that is,eithe the particles to be measured are imbedded randomly in the matrix, or a sufficient number of random plane sections are taken to make the sample representative. A relationship exists between the number of par- ticles of a given size and shape that may be situated in unit volume (Ny) and the number of intersections a random plane can be expected to make with these particles (Na). It is the purpose of the following section to derive this relationship. The probability of Intersecting Convex Bodies. Consider a convex, closed surface, that is, one for which no two surface normals point in the same direction, situated at some arbitrary position and orientation in a cube of material that is one unit long at each edge. It is not necessary to assume that this surface is symmetrical. Let planes be constructed in the cube parallel to the top face and at random distances from it. Those planes which lie between the two planes which are just tangent to the top and bottom of the surface will intersect it. The probability that a plane will intersect the body may be defined as the limit of the fraction of planes that lie between the two tangent planes as the total number of planes constructed becomes infinite. This fraction, in the limit, is equal to the distance between the two tangent planes, DV, divided by the total length over which planes are constructed, which has been taken as unity. If the body is now rotated to a new orientation, applying the same argument, the probability of intersection is again numerically equal to the distance between tangent planes. Let DV ($, 0) be defined as the distance between tangent planes of a convex body as a function of orientation, Fig. 1. The probability, Pr, of intersecting the body with a randomly oriented and randomly positioned plane, is then equal to the average value of DV (0, $) over all possible orientations. It may be easily shown that for a system of spherical coordinates the probability of finding an orientation between Q and Q + de, $ and $ + d$ is (1/4n) sin $ dB d$, so that This relationship may be applied to each body in an aggregate of convex bodies. In particular, if the bodies in an aggregate are classified according to size and shape, and the ithsuch class is considered, Eq. 111 may be applied to this entire class, the probability of intersecting any body in this class being

Jan 1, 1962

By K. -A. Björkstedt

INTRODUCTION Strassa lies in the central part of Bergslagen, a tradi¬tional mining district, on the eastern side of the Stora Valley at an elevation of about 200 m above sea level. A railway siding runs between the mine and the Stora railway station from which there are railway connections to the shipping port and iron and steel works in Oxelosund, about 224 km away. The distance to the provin¬cial capital Orebro is about 60 km. The climate is typi¬cal for this part of central Sweden and is illustrated by the diagram of monthly precipitation and temperatures for the years 1968-1975 (Fig. 1). HISTORY There is no certain information as to when the Strassa mine was first worked, but it is known from sur¬viving accounts of mine inspectors that there were smelt¬ing works in operation in nearby villages in the 12th century. An example is the Gusselhytta ore smelting works, 10 km south of Strassa, which dates from this period. Around the year 1540 there were two smelting works in Strassa, the Upper Karberg and Lower Karberg works. Ore for these smelters was probably taken from Strassa and from the adjacent Blanka mine. In the year 1624 Strassa is mentioned by the painter Jons Nils Krook in an account of the iron mines in the Linde mining district (Linde Bergslags Jarngruvor). Several mines were listed in the area, the deepest being about 30 m. An impressive power installation is mentioned in 1639, including a piston system of lashed poles for transmit¬ting power from the Stora River to the Strassa fields. Its length was 2670 m. Common ground comprising about 20.2 km2 (5000 acres) of forest was allocated in 1689 for the furtherance of mining operations. Until the beginning of this century only the rich cen¬tral parts of the ore body were mined and these yielded, after handpicking, lump ore suitable for smelter feed. An example of the ore grades from these early times is an analysis of ore from the "Big Mine" (Storgruvan) from the year 1873: 48.5% Fe, 0.008% P, and 0.06% S. This same year a total of about 18 000 t was ex¬tracted from the Strassa mine. OWNERSHIP The mine was owned and run until 1874 by a min¬ing association made up of 119 so-called "bergsman," who were homesteaders often engaged in agriculture and timber-cutting as well. In that year the Strossa Grufvebolag (Mining Co.) was founded. In 1906 it was con¬verted into a joint stock company, the Strossa Gruveaktiebolag. This was acquired in 1907 by Metallurgiska AB for the implementation of Gustav Grondal's beneficiating and briquetting methods, for which the Strassa ore was well suited. The same year saw the completion of a new ore dressing plant with an annual production of 46 000 t of ore concentrate. In 1911 the mine passed to new hands, and in 1913 it was purchased by an Austrian company. Extensive new installations were made and in 1915 a new dressing and briquetting plant was completed with twice the capacity of the old one. In 1917 the Strassa mine was acquired by Granges. Be¬cause of unfavorable business trends and technical diffi¬culties, mining operations were brought to a close in 1923. Pumping kept the mine free of water until 1933 but it was completely filled ten years later. Up to 1950 the surface buildings and installations remained intact but the large dressing and briquetting plant burned to the ground in that year. Today only the machine shop re¬mains from this earlier period of operation, now housing parts of the Mineral Processing Laboratory. The decision to take up mining operations again was made in 1955 and construction work began the follow¬ing year. Of the old installation, only the "southern shaft" could be used for some development drifting after it had been completed with a new headframe. Other¬wise, all the buildings and installations required for the operations had to be rebuilt. New installations ready by 1960 were office and personnel facilities, a new shaft and headframe, a sorting and concentrating plant, a macadam plant, settling basins, pump stations, and a railway and yard with transport equipment. The instal¬lation was completed with two plants

Jan 1, 1982

By F. Weinberg

Measurements have been made of solute segregation during dendrilic growth by using radioactive solute elements and ,measuring the activity of den(12-ites cut from decanted specimens. This has been done for both lead awl tin based binary alloys contaitzing the following solute additions: Ag, T1204, was dependet on ko, the equilibrium distribution coefficient in the following way Fay k &apos;c 0.1, C/C 0.6; for k0 >0.1. 0.6 <c,/c,< I. Qualitative obse?-vations were madc of dendritic segregation, by using autoradiographic techniques, for the Sn + Ag110 and Sn + Tlo4 systems. The observation were found to he in general agreement with the measurements ofCA/Co. Autoradiographic were also obtained of scctiolccl delzr11-iie stalks. These indicated that the stalks had a substructure, dclileated by solute corzetlt?atio?zs nlolg the substructure walls. A new dendrite growth direction <JI2> is reported for tila. SOLUTE segregation in dilute binary alloys has been investigated by Pfann,&apos; Smith, Tiller, and Rut-ter,&apos; and others. They considered the case of a slowly advancing plane solid interface, and derived expressions for the distribution of solute in both solid and liquid during solidification. To determine these expressions, they assumed no diffusion in the solid and either complete mixing in the liquid:&apos; or diffusion controlled solute movements in the liquid without any convective mixing.&apos; The present investigation considers solute segregation during dendritic growth, in which case the solid-liquid interface is not plane, and the growth rates are rapid. Segregation under these growth conditions has not been treated mathematically, because of the relative complexity of the system. It has been suggested by Chalmer, on the basis of preliminary results, that an alternative to the diffusion and heat flow controlled conditions during growth is &apos;diffusionless" dendritic growth in which solid is formed with the same composition as the liquid. He suggests this type of growth may depend upon a solvent-solute relationship that permits some solid solubility without excessive increase in internal energy, as is the case for solutions of tin in lead. On the other hand, Montariol,4 and others, have shown experimentally that some segregation does occur during dendritic growth in metals using etching and radioactive tracer techniques to indicate the concentrations of the solute. The present investigation was undertaken to determine, both qualitatively and quantitatively, the extent of solute segregation associated with dendritic growth in a series of binary alloys, as a function of solute concentration. PROCEDURE The solvent materials used were Vulcan Electrolytic tin (99.997 pct purity) and Tadanac lead (99.998 pct purity). The solute materials were Zn, Sn, and Sb (better than 99.998 pct purity), Ag and Co (99.5 pct purity), and T1 (Fisher "purified" metal sticks). Activation of the solute metals was carried out in the reactor at Chalk River, Canada. Master alloys were prepared by induction heating from the radioactive solute metal and the pure solvent, under argon, in graphite crucibles. Pieces of these alloys were then added to the solvent to give the required solute concentration. Dendrites were grown in essentially the same manner as that described by Weinberg and Chalmer, , in which controlled orientation single crystals were grown dendritically in horizontal graphite boats, and the liquid decanted. The crystals were grown and decanted in an atmosphere of tank argon. Before decanting, a sample of the liquid was drawn up in a glass tube and allowed to solidify rapidly. The orientations of the single crystals were such that <loo> was parallel to the growth direction, and (100) in the horizontal plane for lead, and [1101 and (110) respectively for tin. With these orientations long dendrite stalks formed along the bottom of the boat in the dendrite direction (<100> for lead and [I101 for tin) from which secondary branches grew. Only these secondary branches, which grew freely in the liquid from the dendrite stalk to the liquid surface, were used in the measurements. Accordingly, effects due to substrates and oxides on the surface of the liquid need not be considered. In order to measure the solute concentration C, of the dendrites, individual dendrite stalks were cut from the decanted specimens, remelted, and formed

Jan 1, 1962

By W. F. Hower, W. Brown

Large-scale sand consolidation tests were conducted in an effort to determine the reasons for the successes and failures of this method of sand control. Several different consolidating materials were used in treating both clean and bentonitic sands that were packed in a chamber having a capacity of 3.3 cu ft. The results were essentially the same for all of the different consolidating materials, The data show that low-viscosity consolidating materials pumped at a relatively slow rate gave the best results. Where the formation has produced sand, the treating fluids can compress the formation, thus permitting the channeling of fluids to another horizon. Pressure-packing these zones before attempting to consolidate is recommended. Sands containing more than 4 per cent of water-swelling clays are not good candidates for consolidation. It is indicated that loose sand, particularly when it is bentonitic, can be fractured during the placement of the treating fluids. INTRODUCTION Sand production in oil and gas wells has plagued the industry for many years, and numerous cures for this problem have been suggested. Most methods have been successful to a certain degree, but the great variety of well conditions that exist in the different areas has magni- fied the problem and limited the successful use of the various systems. Four review papers1-4 present a wealth of information concerning the degrees of success that have been obtained by the different sand-control methods. The bridging of sand grains by the use of gravel packs and screens has been quite successful. However, these methods do not leave the casing clear for all types of multiple completions, and the cure does not last for the production life of the well in some instance:;. The control of loose sands by sand consolidation with resins has never been as successful as desired. It has always been hoped that such a treatment would eliminate all sand problems for the life of the well, but. initial applications, starting in the middle 1940&apos;s, were only moderately successful. Lott, et a1,3 reported a success ratio of approximately 50 per cent and made the following conclusions. The highest percentage of successes were obtained where: a. Consolidation of a zone was made at the time of initial completion or prior to the production of sand. b. The interval treated was less than 12 ft in length. c. Between 30 and 50 gill plastic/ft of producing interval was displaced through the perforations. REASONS FOR SAND CONSOLIDATION FAILURES Our own experiences in the field of sand consolidation point toward the following conditions as the major reasons for the failure of sand consolidation attempts. 1. Mud-plugged perforations and mud invasion of the formation. 2. Sand in the casing covering all or part of the perforations. This sand could be either formation sand or one of the coarser sands used as propping agents in hydraulic fracturing. 3. Holes in the casing. 4. Channels behind the casing. 5. Attempting to treat too long a perforated section. 6. Too high a percentage of water-swelling clays in the formation. 7. Formations that have produced sand. Recent attempts were made to treat perforated sections ranging from 10 to 30 ft, in wells that have produced sand, by using a straddle packer that was raised and lowered through the perforations as the consolidating material was being pumped. In most instances, the pressure required to pump fluid into the formation varied considerably as the tool was raised and lowered. This suggested the possibility that significant differences in permeability were present or that only part of the formation had produced sand. There were times when a sudden break in pressure indicated that a fracture was being formed. Research conducted several years ago concerning the problem of the control of water in air and gas drilling indicated that shale sections could be fractured quite easily. In addition, it was determined that it was easier to pump fluids into shale bodies by fracturing the shale itself, or the interface between the shale and sand, than to pump into a fluid-saturated formation. Formations that produce sand are usually adjacent to shale bodies and frequently have shale streaks of various thicknesses inter-bedded in the sand. Therefore, where shale is exposed to fluid pressure it

By H. F. Ramstad, F. D. Richardson

The equilibria (a) SiOz +Hz =SiO +H20 and (b) Si + SiO, = 2Si0 have beet1 studied at temperatures of 1425"to 1600°C ad 1310°to 1485°C respectively. The stattdard free energy changes for the tzrro reactions are given by the equatiotts Combination of the results for both equilibria leads to tiotz removes certain anomalies in existing high-terlzperature data for equilibria involving silica and silicon in iron. In many metallurgical processes and in many laboratory investigations silicon monoxide undoubtedly plays an important role. It is unfortunate therefore that wide differences exist between the results obtained by different investigators1-7 in their studies of such equilibria as In an attempt to put our knowledge of SiO on a surer basis, an exhaustive study has been made of equilibria [I] and [2] at temperatures ranging from 1300" to 1600°C. Reaction [I] was studied by measuring the amounts of silica which could be condensed from streams of Hz or Hz + HzO which had previously been brought into equilibrium with silica at temperatures ranging from 1425" to 1600°C. Reaction [2] was studied by measuring the material that could be condensed from streams of Hz or argon which had been brought into equilibrium with mixtures of silicon and silica at temperatures ranging from 1310" to 1485°C. EXPERIMENTAL Materials. The silicon was "superpure" grade and contained less than 0.1 pct impurities. The silica was prepared from pure mineral quartz; this was crushed and treated with concentrated hydrochloric acid to remove particles of iron, washed with water, and finally dried at 120°C. For the hydrogen + silica reaction, the silica was sized to —20+100 mesh. For the silicon + silica reaction, the two materials were ground to a fine powder in an agate mortar. The hydrogen and argon were commercial oxygen-free gases. The gas streams were controlled with capillary flow meters and the volumes were measured by wet gas meters. After passing through the meters, the gases were partially dried by silica gel. The hydrogen for the HZ + SiOz reaction was then passed through palladised asbestos at 300°C and dried with magnesium perchlorate. The efficiency of oxygen removal was checked throughout the experiments by passing the gas over an electrically heated strip of nichrome, used as an indicator as described by Rathman and de itt.&apos; When mixtures of HZ + Hz0 were required, the partial pressures of water vapor (1.8 to 22 mm) were obtained by passing the hydrogen through oxalic acid dihydrateg&apos; lo held at various controlled temperatures, O.l°C, by means of a water bath. The hydrogen for the Si + Si02 reaction was purified by passing it over a mixture of 3 parts of magnesium to 5 of lime heated to 600°."l1 u The argon for this reaction was passed through titanium powder (-3/16 in. + 100 mesh) heated to 900°C. The nitrogen used to prevent the reaction products escaping from the condenser (see later), was deoxidized by copper or iron at 600°C. All these gases were finally dried with magnesium perchlorate. Furnace, Temperature Contr01, and Measurement A molybdenum resistance furnace was used for both sets of experiments. The reactions were conducted inside a high-grade alumina tube, 36 in. long and 1 in. in diam as indicated in Fig. 1. With this arrangement an even temperature zone (2"C) 4 cm long was satisfactorily obtained. The temperatures were kept constant by means of a proportional controller actuated by a Pt-Pt 13 pct Rh thermocouple. This was placed between the two alumina tubes, so that the temperature at the junction was 1400" to 1450°C. Up to 1485"C, the temperatures were measured with Pt-Pt 13 pct Rh thermocouples. For higher temperatures an optical pyrometer was used, this being sighted (through the glass window 1 in Fig. 1) on the end of the alumina tube, that held the SiOz or Si +SiOz mixture, 10 in Fig. 1. The optical pyrometer was recalibrated whenever a change was made in any part of the apparatus situated in the hot zone. Successive readings with the optical pyrometer were reproducible to within 1"C. Equilibrium Apparatus and Procedure. Hydvogen and Silica Reaction. The apparatus is shown in Fig.

Jan 1, 1962

By R. A. Wattenbarger, H. J. Ramey

A systematic study has been made of the application of the real gas pseudo-pressure m(p) to short-time gas well testing. The m(p) function can be used in real gas flow problems to account for the variation of viscosity and z-factor with pressure. A mathematical model was solved numerically to generate solutions of various real gas flow problems. The effects of turbulence, formation damage and wellbore storage were included in the model. The analysis of simulated well tests showed that the interpretation methods normally used for liquid flow are generally accurate when the m(p) is used. For practical rates without turbulence, the solutions are not rate-sensifive, and the flow capacity.. kh and skin effect can be determined accurately from either a buildup or a drawdown test. However, the kh calculated from a drawdown test can be significantly low when turbulence is present. A case was simulated in which this error wa.s 36 percent. Turbulence does not affect the determination of kh from buildup tests. The proper determination of kh from p and pa buildup and drawdown plots is developed by analyzing their relationship to the m(p) method. A simple equation is given that can be used for long-range gas well performance forecasting. This expression is compared with a method pre-sended by Russell et al." Introduction The formation flow capacity and wellbore damage condition can be determined for liquid-producing tests by means of buildup and drawdown tests. These tests make use of short-time pressure transient data rather than stabilized flow tests that are often used for gas well testing. Tracy&apos; presented a method of gas well testing that was based on ideal gas equations and utilized p2 buildup plots. This method was shown to be good for low pressure wells. MatthewsZ suggested plotting p and using an average slope and average gas properties. This method was more successful on high pressure wells. Al-Hussainy, Ramey and Crawfordh howed that variation in gas properties could be simplified by using the real gas pseu do-pressure m(p). Some cases showed that the use of the m(p) function Original manuscript received in Society of Petroleum Engineers office Aug. 8. 1967. Revised manuscript received June 11, 1968. Paper (SPE 1835) was presented at SPE 42nd Annual Fall Meeting held in Houston Tex., Oct. 1-4. 1967, and at SPE 4th Annual Eastern Regional ~eetin$ held in Pittsburgh. Pa., Nov. 2-3. 1967. 0 Copyright 1968 American Institute of Mining, Metallurgical, and Petroleum Engineers, Inc. &apos;References given at end of paper. provided an accurate method of interpreting buildup and drawdown tests. Because the work of Al-Hussainy et al. included only a few actual cases, there was a need to explore the use of the m(p) method for a greater variety of flow conditions. The occurrence of turbulent flow around the wellbore often is an important factor in gas well testing. Swift and Kiel,&apos; and Carter et a1.&apos; treated turbulence in gas well testing, but did not consider the variation of viscosity and z-factor with pressure. This paper presents the results of an investigation of the application of the m(p) method to buildup and drawdown testing. Vhe investigation included the effects of turbulence, formation damage and wellbore storage. Gas Flow Equations To formulate the mathematical model, many of the assumptions usually used in well testing theory are applied. The system has radial geometry with a closed outer boundary and is composed of a horizontal porous formation that has uniform and isotropic rock properties and uniform thickness. Allowance is made, however, for a radial region of reduced permeability near the wellbore. This region represents formation damage. The geometry of the system is shown in Fig. 1. Darcy&apos;s law does not always apply to gas flow. A more general expression is needed for non-Darcy, or "turbulent" REGION OF DAMAGED PERMEABILITY SEALED BOUNDARIES ClRCULAR WELL BORE Fig. 1—Radial flow model. AUGUST, BT7

Jan 1, 1969

By Yang Li

For the study of overburden movement in longwall mining of shallow coal seams, most scholars merely consider the thickness of bedrock and top soils. In this paper, the overburden movement in longwall mining of shallow coal seams with thin top soils and key strata group was studied. By using numerical simulation, the development of fractures in the overburden was analyzed for different ratios of panel width to depth (W/D) and depth to mining height. The results show that the overburden movement changed with the variation of mining height, panel width and depth under the specific geological conditions. It also explain how different overburden disturbance structures, such as ?three zones? (caved, fractured, and continuous deformation zones), ?two zones?(caved and fractured zones) or ?steps-like collapse? are formed under different mining conditions. The results broaden the vision for research on overburden movement in longwall mining of shallow coal seams.

Jan 1, 2014

By Frank Firmstone

IN the early decades of the past century the method of starting iron blast-furnaces by "scaffolding-down" seems to have been in universal use for coke-furnaces and, at least in this country, for charcoal-furnaces also. It was likewise used at some of the early anthracite-furnaces, as is stated in the important "Reminiscences" printed by the late Samuel Thomas. I It had been generally superseded in Great Britain as early as 1850, by some variations of the plan now used, and was rarely used when Percy wrote.&apos; On the Continent it was still followed in the 60&apos;s,3 and was elaborately described by Valerius in 1852. I have never read any statement as to when and by whom &apos;4 scaffolding" was first dispensed with, but the following extracts from journals of my father seem to fix an authentic date for an instance in this country:

Mar 1, 1907

By Richard J. Lewandowski

Corrosion and product contamination have been difficult problems for extractive metallurgy industries in the U.S. because of the highly active chemicals used. During the past twelve years, other industries, particularly the chemical and paper segments, began to combat this problem with some degree of success using newer materials of construction, including reinforced plastics. These materials are made by combining a corrosion resistant thermosetting resin with a glass fiber reinforcing material and are used to con¬struct hoods, stacks, blowers, tanks, towers, pipe, and equipment of the most complex configurations. For service in contact with aggressive chemicals, the equipment is most often fabricated with the bisphenol-A fumarate polyester resins because of their resistance to corrosive attack. Data from both laboratory work and case histories of field applications are presented-for many common chemicals found in extractive processes. Information is also presented concerning design standards and recommended construction procedures

Jan 1, 1970

By McKenzie A. M

The Corridor ore body is so named because it occurs in an east-west zone or corridor of schist bounded on the north by the siliceous conglomerates of Mount Lyell, and on the south by similar conglomerates of the Tharsis ridge (Fig. 1). It was discovered after the geophysical prospecting methods described below had defined a target zone for diamond drilling.Since the proving of copper mineralisation by drilling, the corridor orebody has served the vital function of a convenient known target body for the orientation of more recently developed geophysical methods. Traversing of the orebody by these new methods has provided experience for the evaluation of anomalies elsewhere.Some of the methods applied had not been used in Australia before, and were introduced to the west coast of Tasmania through the undertaking there of modern regional exploration programmes. The authors feel that the information gained could be of assistance to others engaged in geophysical prospecting.HISTORY OF DISCOVERYProspecting in the Mount Lyell district has been more or less continuous since 1881. The first geological report was published by Thureau (1886).In 1934, Blazey and Douglas (1934-38) commenced geophysical surveys at Mt. Lyell using the equipotential method.They obtained anomalous indications in several discrete zones and actually detected the south-east half of the corridor orebody but their work never became the basis for...

Jan 1, 1961

By P. A. Wright

The note describes the steps involved in the combination of results reported by Shiraishi and Bell in 1968 and 1970 and by Mills and Turkdogan in 1964. Shiraishi and Bell derived from their vapour-pressure measurements an expression for the activity coefficient of tin implying that the miscibility gap in the two-liquid region is symmetrical about the N = 0-5 axis. The limits of the miscibility gap were reported by Shiraishi and Bell and measurements were reported graphically by Mills and Turkdogan. Least-square parabolas are fitted to the transformed results of Shiraishi and Bell and of Mills and Turkdogan for the miscibility gap in the liquid tin-iron system. Back-transformation from these curves gives limits at 1438 K and equations are derived that appear to be a fair average of existing data, although a third term for the activity coefficient equation needs to be investigated

Dec 1, 1971

Several years ago, North American mining companies began to realize they needed to expand their spheres to remain viable. This strategy has been successful, according to Robert W. Schafer. Today, companies from other continents have also recognized the need for an international view for long-term growth and viability, he said. Schafer is vice president for exploration with Kinross Gold. He was the program chairman and moderator of the keynote session at the 1997 SME annual meeting, held in Denver, CO, Feb. 23-27. The theme of the meeting was "Minerals - Serving the Global Community." A record attendance of more than 6,000 people participated in the meeting, which featured 415 exhibitors occupying 582 booths. The title of the keynote session was "Corporate Perspectives on a Global Minerals Industry." Each of the three keynote speakers discussed a different perspective of a global minerals industry.

Jan 1, 1997

By Kyung-Ho Park

The smelting leaching process is known as one of the most favorite methods for the processing of deep-sea manganese nodules because of its smaller environmental impact and easiness of manganese recovery. The sulphuric acid pressure leaching of the matte prepared from deep-sea manganese nodules was studied to dissolve the valuable metals. Almost complete dissolution of Cu, Ni, and Co from matte was achieved under the following conditions: leaching temperature 180°C, time 4 hours, PO2 10 kgs/cm2, acid concentration 2.5% (vol/vol), pulp density 5%, ammonium sulphate 40 g/l. Under these conditions the iron concentration of leach liquor was 0.95 g/l. Optimization of leaching parameters was carried out by statistical design of experiments using 23 full factorial matrix. The linear and interaction co-efficients were evaluated for dissolution of metal values and also for iron concentration in leach liquors.

Jan 1, 2003

By R E. Myers, G N. Phillips

Many of the worldÆs larger iron ore deposits are hosted by rock sequences of Archaean to early Proterozoic age. Most models for the genesis of these deposits are influenced, either directly or indirectly, by the nature of the atmosphere at the time of their formation, and more specifically by the presence or absence of oxygen in the early atmosphere. Since the early-1950s, the geological literature suggests that the Archaean atmosphere was æreducingÆ, and that it may not have contained significant amounts of free oxygen until ca 2 Ga. There are many different definitions of the term æreducingÆ, but the criterion adopted here is whether crustal iron was limited to Fe2+, or whether Fe3+ was also widespread, ie was there scope for redox changes in the state of iron? Significantly, major Australian banded iron formations span this period of inferred atmosphere transition, eg Mt Goldsworthy, Mt Tom Price, Middleback Ranges. Geological evidence for a reducing Archaean atmosphere is both ambiguous and controversial (see review by Phillips, Law and Myers, 2001). Many earlier ideas (eg no Archaean redbeds; all very large iron ore deposits being post-Archaean) have been disproved by dating, whereas other evidence (eg homogeneous detrital gold grains, inferred palaeosols) has not withstood geological scrutiny. The interpretation of some data sets (eg inferred detrital uraninite and pyrite in some Archaean meta-sedimentary rocks) is still controversial. In fact, some lines of evidence now suggest that oxygen was present in the atmosphere well before 2.5 Ga (eg sulfates in the Pilbara craton, carbon distribution in clastic sedimentary rocks). An oxidising Archaean atmosphere has important implications for the development of iron formations. First, the atmosphere is an obvious potential source of oxygen to stabilise ferric iron minerals. Second, reduced fluids in equilibrium with ferrous iron are commonly inferred to transport iron in solution to the depositional site. The redox state of the atmosphere thus provides critical constraints on the solution chemistry of surface waters, effective transport paths for iron and particularly on viable precipitation mechanisms. Iron formations developed from fluids in equilibrium with the atmosphere also have the potential to provide important constraints on the evolution of EarthÆs early atmosphere. If an oxygenated atmosphere is a necessary condition for the development of iron formations, then the Archaean atmosphere must have been oxidising since at least 3.5 Ga. If the redox state of the atmosphere is not a necessary condition, then the time distribution of iron formations cannot be used to provide constraints on atmospheric evolution. Given these uncertainties, models for the genesis of iron ore deposits of Archaean or early Proterozoic age should not rely on a reducing atmosphere in the absence of independent evidence and the alternative of an oxidising atmosphere should also be considered.

Jan 1, 2002

By Daryl R. Tweeton

The Bureau of Mines measured the geochemical changes as H2S04 was used for in situ uranium leaching by Rocky Mountain Energy Company near Casper, Wyoming. Cores and ground water were analyzed before leaching. Water samples were taken from observation wells located between injection and production wells as the leach solution was brought up to full strength in several steps. Measurements were made of pH, Eh, temperature, conductivity, total dissolved solids, dissolved oxygen, HC03, U, V, Na, K, Ca, Mg, SO4, C1, Mo, Mn, Fe, Al, Si, F, P, As, and Se. The data were gathered to assist in geochemical modeling of leaching and to study the potential environmental effects of acid leaching. Environmental considerations appear favorable. For example, the concentration of Se, a toxic element often found in uranium deposits, stayed below the EPA standard for drinking water.

Jan 1, 1979

By E V. Kislov

"An EXTENDED ABSTRACT is available for download. A full-length paper was not prepared for this presentation. The Northern Baikal Ni-Cu province is located in Buryatia, south-east Siberia, and geologically is part of the Baikal-Muya volcano-plutonic belt. It is known for numerous PGE-Ni-Cu-bearing mafic-ultramafic intrusions of Neoproterozoic age formed in various geodynamic settings. All these deposits can be regarded as a single Ni-Cu ore cluster located near the Kholodninskoe Pb-Zn deposit, which is ready for mining. In addition, there are less studied, small dyke-like bodies with sulfide mineralisation that formed in a rift setting and may be enriched in Ni, Cu and PGE. Individually, the known bodies are of poor commercial value by their resources, but their close spatial association (&lt;30 km) may make these PGE-Ni-Cu deposits economic in the future. This extended abstract seeks to provide a geological framework of the North Baikal Ni-Cu-PGE province, specifically at the north-eastern Synnyr rift hosting numerous small subvolcanic bodies with Ni-Cu sulfide mineralisation. Some small subvolcanic bodies contain industrial level Ni-Cu deposits (Shanuch, Cabanga-Musongati, Voisey’s Bay, Jinchuan, etc).CITATION:Kislov, E V, 2015. North Baikal region Ni-Cu deposits , in Proceedings PACRIM 2015 Congress, pp 297–302 (The Australasian Institute of Mining and Metallurgy: Melbourne)."

Mar 18, 2015