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By J. J. Kramer, G. W. Wiener, K. Foster

The effects of the primary grain size and sheet thickness on the secondary growth rates of grains with (100) surface planes were studied in 3 pct Si-Fe sheets. This secondary grain growth was carried out under conditions in which the {100} plane had the lowest surface free energy. The value of the surface energy difference, between the (100) plane and the random matrix planes was found to he only about 3 pct of the grain boundary energy, indicating that most of the driving force for secondary growth is supplzed by grain boundary energy. A method for obtaining cube texture in 3 pct Si-Fe sheets by a secondary recrystallization process has been reported.' It has been demonstrated that a difference in surface free energy between the (100) plane and other planes is responsible for this growth, where the (100) plane has the lowest surface energy. A semiquantitative relation has been derived for secondary grain growth in sheets where primary grain growth has proceeded until the grains have grown through the sheet and the average grain diameter in the plane of the sheet is from one to two times the sheet thickness. Then, the linear growth rate, G, for the secondary grains can be given by where M is the grain boundary mobility, is the grain boundary free energy, is the average primary grain radius, A is the average difference in surface free energy between the (100) plane and planes of other orientations, t is the sheet thickness, and C is a term first proposed by zener6 which acts as a negative driving force, the effect of inclusions in holding up grain boundary motion. Since the problem of grain growth being discussed is under conditions where the matrix grain size is at least equal to the sheet thickness, the radius r is, of course, a function of the sheet thickness. The term B/r is the grain boundary driving force normally associated with inclusion inhibited or texture inhibited secondary recrystallization. Here, however, the term is modified to account for the fact that growth occurs in thin sheets. The term is the additional driving force available because of the difference in surface free energy. The purpose of the present work has been to evaluate the driving force terms of the growth equation by studying growth rates of (100) secondary grains as a function of sheet thickness and primary grain size. From these data it has been possible to determine the relative values of grain boundary energy, surface energy difference, and the inclusion term, C. EXPERIMENTAL PROCEDURE A 3 pct Si-Fe alloy was melted and cast under a helium atmosphere using electrolytic iron and a pure commercial grade of silicon as raw materials. The alloy was hot and cold rolled to a thickness of 0.6 mm, and samples approximately 5 in. long by 1 1/4 in. wide were cut from the cold-rolled sheets. Four different primary grain sizes were obtained

Jan 1, 1963

By James A. Wasson

This report summarizes the results and conclusions reached by various investigators who have attempted to determine the extent to which hydraulic fracturing will affect the secondary recovery of crude oil by waterflooding. It also discusses the most advantageous use of this well-stimulation method in waterflood projects. A thorough search of the literature was made, and pertinent information was abstracted from appropriate reports. A carefully designed and controlled program of formation fracturing is an effective aid in waterflooding because it increases water-injection and oil- production rates. Generally, fracturing has resulted in little or no reduction in ultimate oil recovery, but under certain circumstances recovery has been substantially increased.

Jan 1, 1963

By H. W. Kilau

Thermodynamic calculations indicate that an electrochemical cell might serve as an analytical device for determining the composition of high-purity metals. An equation, readily derived, for the cell voltage, E, is as follows: [E I RT In F NFe unknown sample T of L NFe standard] The cell, however, must come to equilibrium, must be reversible, and must have no thermal effects or complicating side reactions whose magnitude is indeterminable. This Bureau of Mines investigation explores the feasibility of an electrochemical technique for the analysis of high-purity iron. Experiments were conducted using room-temperature aqueous cells and high-temperature molten salt cells. The room-temperature cells proved to be irreversible. The high-temperature cells utilizing FeCl2 and a eutectic mixture of KC1-LiCl were reversible, but did not attain a constant voltage necessary for analytical considerations.

Jan 1, 1963

By Robert S. Warfield

The Bureau of Mines investigated a geologically favorable area in the Beluga River coalfield in south-central Alaska to determine if there were sufficient minable coal reserves for onsite utilization to meet the projected thermal power needs of the Anchorage area. A program of diamond core drilling and sampling delimited a shallow saucerlike structure estimated to contain indicated reserves of more than 20 million tons of subbitminous coal in a seam over 50 feet thick that could be mined by opencut methods. A large sample of fresh coal was taken across the full width of the seam for washability studies. This sample, with 4 volume-percent of clay partings eliminated, contained 24.4 percent moisture and 16.8 percent ash and had a calorific value of 7,162 Btu per pound. The studies indicated that mechanical cleaning would be of doubtful value.

Jan 1, 1963

By W A. James

The use of spectrographic semi-quantitative analysis has recently been of considerable value in establishing the geological relationships in a complicated orebody. The principal minerals found in the Mount Pleasant orebody are cassiterite, stannite, sphalerite, molybdenite, wolframite, chalcopyrite and galena, associated with arsenopyrite, pyrite and fluorite. In addition to the large number of minerals, a further com-plication is the non-uniform distribution of the economic minerals, with one mineral being the only one present in major amounts in one area and another mineral being predominant in another area. At the same time, all minerals are present to a minor extent throughout the deposit. This heterogeneity made it advisable to analyse all exploration samples thoroughly. Analysis by conventional means would have resulted in prohibitive costs. By the use of emission spectroscopy, however, it was possible to obtain, quickly and relatively inexpensively, a reasonably comprehensive picture of the orebody un-der investigation.

Jan 1, 1963

By Tanner A. C, Harraway D. H

Various circuits were tried at Mount Isa Mines during the period 1959 to 19G3 with the objective of improving the differential flotation of galena and sphalerite. Many benefits and disadvantages of the various circuits were revealed. An analysis' of ore characteristics and their effect on flotation was made -and resullted in the design of a proposed circuit which is currently in the process of installation.INTRODUCTIONSince 1936 when lead-zinc sulphide flotation commenced at Mount Isa, at least three types of ore have been encountered.Each ore has presented problems to flotation metallurgists.The three types of ore are,1. partially oxidized upper level sulphide ore,2. Black Star ore from the lower levels with its carbonaceous fraction, and3. Black Rock ore which is similar to 2, but more free milling.In retrospect a number of the metallurgical successes of the past were short lived. Often flowsheets or 0perating practices were designed to solve a single metallurgical problem associated with the current ore being treated. As the ore changed the problem would vanish and the method originally taken to counter the problem could become unnecessary or deleterious to the treatment of the new ore. The general lesson learnt from-the past-is-that thetreatment of Mount Isa lead-zinc ore involves a number of equally major problems...

Jan 1, 1963

By G. L. Alston

Rigid urethane foam can be used effectively for improving mine air conditioning systems by reducing heat and moisture transfer from mine rock to ventilating air and from mine rock to ventilation ducts, for erecting mine ventilation stoppings and overcasts, for sealings around door frames and bulkheads to prevent air leakage, for preventing spalling and sloughing of roof and rib and for erecting fire-resistant powder magazines and transformer or compression stations. Rigid urethane foam is a tough, cellular material, made by nixing diisocyanate and polyether polyol resin in accurate proportions through an applicator system, then the two chemicals react, the mixture expands thirty times its original volume with 85 to 95 percent closed cells. Within seconds, the mixture solidifies and takes a preset which will adhere to overhead or vertical surfaces. It will adhere to brattice cloth, steel, wood, concrete and rock, Excessive wetness will reduce the adherence, but in such cases adherence can be improved by preliminary application of an absorbent dust such as cement.

Jan 1, 1963

By E. Maré

Some of the members will probably ask themselves what close relationship exists between hydro-metallurgy and a wet scrubber, but we are sure that as soon as deeper thought is given to the matter it will be realised how vital scrubbing, operations are in metallurgical plants. In ordinary metallurgical installations or pyro-metallurgical processes ore concentrates are first of all shifted from place to place and dust is created. In other cases the ores or concentrates are crushed or dried or roasted, and in each one of these operations dust and fumes, are created. All suspended particles and fumes originating from the abovementioned conditions not only, in many instances, provide health hazards which disrupt production and endanger the personnel in the plant, but also are the source of economic losses through extra maintenance and wear to moving machinery due to abrasion and corrosion. Further losses are incurred by the waste of fine, very often valuable, components. The Party who once said that in several metallurgical plants the bulk of the profits was discharged into the atmosphere by the stack wasn't stretching the truth. There is a place in Africa where a gold producing concern used to lose over 5 oz. of fine gold per day out of a total production of 3000 oz. per month. In another instance, copper concentrate going as high as 80% Cu was discharged into the atmosphere at the rate of 4 tons per day. Realising the value of removing and collecting solids and fumes created in metallurgical plants, a thorough study was made of the available plant and equipment offered on the market. Some units were found very efficient, but very expensive; some others also very efficient but with temperature and maintenance limitations. Some others were also efficient but prohibitive from the point of running costs.

Jan 1, 1963

By E. T. Turkdogan, P. Grieveson, J. F. Beisler

Experimental results are given for the rate of reduction of silica from silicate melts by paphite-saturated iron in the presence of carbon monoxide. It is shown that, when gas bubbles are present at the slag-metal interface, the interfacial chemical reaction is the rate-controlling process in the transfer of silicon from slag to metal. From the silicon-concentration profiles in the metal sample, the diffusivity of silicon in paphite-saturated iron is found to be (5.4 * 0.4) x 10 sq cm per sec at 1600°C. Some consideration is given to the transport of oxygen from the slug-metal interface to the walls of the gvaphite metal container as becoming the rate-controlling process in the absence of gas bubbles at the slag-metal interface. ATTEMPTS were made by Fulton and chipman1 to investigate the kinetics of reduction of silica from calcium alumino-silicate melts by graphite-saturated iron in an atmosphere of carbon monoxide. In these experiments with 400 to 500 g of metal and slag, both phases were stirred in such a manner that the interface was essentially undisturbed. Initially, the graphite-saturated iron contained about 15 pct Si and, after about 8 or 10 hr of reaction time at 1600°C, the silicon content of the metal in- creased by about 0.2 pct. In a written discussion on this paper of Fulton and Chipman, schuhmann2 pointed out the possibility that this observed slowness of the reduction of silica could be due to the transport of oxygen across the liquid metal boundary layer at the slag-metal interface. Although this explanation of Schuhmann is quite feasible for the experimental data of Fulton and Chipman on silica reduction, such a reasoning should not be extended to other rate data on slag-metal reactions unless sufficient evidence is available satisfying the boundary conditions for such a transport process. The hydrodynamics of stirred liquids are very complex and even for a simple method of stirring there is no exact mathematical solution which will predict the mass transfer coefficient accurately. The best available solution of this problem is that given by Lewis' and later modified by mayers~ for a two-liquid system where liquids are stirred by counter-rotating stirrer blades without disturbing the interface. In such a system the mass transfer coefficient is estimated from an empirical relationship using the data on viscosity and density of the two liquids, rate of revolution, the length of stirrer blades, and the diffusivity of the element which is transferred from one phase to the other. It was found in these investigations' that the estimated and observed mass transfer coefficients, in systems containing two immiscible aqueous solutions, agreed within *40 pct. Although this is not considered to be an unreasonable error for the study of industrial processes, uncertainties of this magnitude cannot be tolerated in any theoretical study of reaction kinetics. In view of the complexity of the

Jan 1, 1963

By W. J. Boone

Experimental determinations were made of vapor-liquid equilibria data for a helium-nitrogen-methane system. A mixture composition was chosen to approximate the crude helium to be produced Or conservation that will eventually be further refined to obtain pure helium. Although there are publications of studies of the vapor-liquid equilibria of helium-nitrogen, helium-methane, and nitrogen-methane binary systems, there is little indication of work done on the ternary system of helium-nitrogen-methane. The experimental data presented in this report supplement the information available for the binary systems. The equilibrium vapor-liquid data and equilibrium vaporization coefficients are presented in tabular form. Graphs are employed to show an extensive amount of the data.

Jan 1, 1963

By James B. Meredith

The European Economic Community (The Common Market) is now shifting from I a coal oriented to an oil oriented economy. The proportion of energy supplied by oil has increased from only 13% in 1950 to 38% in 1962, and will approach 50% by 1970. In the past five years Common Market petroleum demand has in- creased 15% per year compared with only 3% per year in the United States. This rapid shift to oil can be explained by looking at oil's competition, First; there is simply not enough other energy - European coal, natural gas and hydro-electric power - to meet the demand, Secondly, oil?s primary competing energy in the Common Market is coal, and Community coal is high-priced - it costs more than two and a half times as much as U. S, coal at the pithead. The third reason for the shift to oil is consumer preference for the ease of handling, convenience and cleanliness of liquid fuels. As these reasons suggest, much of the shift to oil and the resulting growth in demand would have occurred whether or not the Common Market organization had existed. On the other hand, the Common Market has stimulated the use of oil by causing a higher rate of energy consumption, and oil has been the beneficiary of most of this growth.

Jan 1, 1963

By R. H. Richman, II Conard G. P.

AS part of a study of deformation twinning in bcc crystals, solid solutions of beryllium in iron have been found to twin profusely when strained slowly at room temperature. This note reports some crystal-lographic aspects of the operative mechanical twin modes in a quenched Fe-5 wt pct Be alloy. After melting twice under a partial pressure of helium, the alloy was homogenized, cut into pieces 7 to 10 mm on an edge, solution treated at 1130°C,1 and quenched. Debye-Scherrer patterns confirmed

Jan 1, 1963

By W G. Brese

The attention of the world is being focused on the spectacular rise of elemental sulphur production in Alberta. In the short space of a decade, production has increased from less than 10,000 long tons, in 1952, to al-most 1,000,000 long tons in 1962. Moreover, 1963 sulphur production is expected to rise by 50 per cent to approximately 1,500,000 long tons, and further increases are forecast for ensuing years. The reason for this dramatic in-crease in elemental sulphur production, particularly in the last year or two, is that Alberta elemental sulphur is recovered in association with the production of sour natural gas. When very large volumes of natural gas began moving to U.S. markets in the latter part of 1961, the resultant increase in sour gas production led to a marked increase in the production of sulphur. Consequently, Canada, mainly on the strength of sulphur produced in Alberta, will soon become the second largest producer of sulphur in the Free World

Jan 1, 1963

By R. E. Hook, H. J. Garrett, A. M. Adair

X-ray diffraction and metallographic techniques were employed to examine the impurity phases occurring in as-swaged and recrystallized chromium produced fvom high-purity iodide chromium crystals. Chromium oxides are found to form in a consistent manner associated with the temperature of recrystallization. Microscopically observable second phase particles of Cr203 are observed to form intergranulurly beginning at 1300T. Beginning at 1500°C. Cr30, is formed intergvanulurly, atzd at 1600°C and above Cr30, is also formed in association with migrating grain boundaries. Geometrical traces formed by particles of this high temperature oxide uithin the grains rez)eal the histmy of grain boundary motion. X-ray evidence is presented which suggests the existence of a high temperature form of Cr203. Other impurity phases in addition to the oxides of chromium are also present. THE partitioning Of impurity elements between grain boundary aid lattice sires, either as solutes in solution or as second phases, may exercise an important influence on the mechanical behavior of metals and alloy systems. This partitioning of impurities could have a direct bearing on the iecrys-

Jan 1, 1963

By W. E. Adkins

Ore and waste haulage usually constitute one of the major cost items in the operation of an open pit mine. This has always been true at the Chino mine, one of Kennecott Copper Corporation's western mines, located in southwestern New Mexico. The Chino Mines Division is an integrated operation. The open pit mine, dump leaching operation, and a precipitating plant are located at Santa Rita, New Mexico, and a power plant, mill, smelter, and fire refinery are located in Hurley, New Mexico, about nine miles south of the mine. Approximately 22,000 tons of ore are mined and processed each day; in addition, approximately 42,000 tons of waste are removed from the pit. Originally the pit was located along the side of Santa Rita Creek but it has deepened and expanded so that at the present time, it could better be described as a nearly circular pit about one to 1.5 miles in diameter. The bottom is at an elevation of 5750 feet, the west rim near the ore gathering yard is at an elevation of 6230 feet, and the highest bench on the east side of the pit is at an elevation of 6750 feet, giving a vertical mining depth of 1000 feet. The train waste dumps reach a maximum elevation of 6580 feet. At the present time, Chino uses electric locomotives, off-the- highway trucks, and a skip system for mine haulage.

Jan 1, 1963

By R. G. Ward, A. E. El-Mehairy

A technique was developed to calculate the density of liquid metals from the profile of a weighed levitated drop obtained by emitted light photography and calibration. The density of liquid copper was determined over the temperature range 1370" to 2100°K and expressed with the equation: The molar volumes and thermal coefficients of expansion are calculated. Copper, upon melting, was found to expand 3.34 pct. A knowledge of the density of liquid metals is essential as it is a parameter appearing in most theories of the liquid state. The liquid density is also necessary for the calculation of the commercially important contraction occurring on solidification. Unfortunately good density values are rarely available and the present work was undertaken to establish a new method of density determination free from the limitations of the existing methods. For liquid metals with high melting points, the variation and the limited number of density values reported in the literature have been caused primarily by difficulties in technique, a matter which has been adequately discussed by Urbain.' In all the methods used for measuring the density of the high-melting liquid metals there are sources of error, and corrections have to be made. For example, in the method of balanced columns, the formation of gas bubbles in one or both arms was a great source of error. In the pyknometer3 and immersed-sinker methods, corrections of certain volumes for thermal expansion to the operating temperature exceed 4 pct. In the maximum-bubble method5 a correction for the thermal expansion of the bubble-tube is used (about 1.6 pct); a second correction takes into account the change in the volume of liquid displaced by the bubble-tube (about 3.5 pct). Another method used is based on the shape of a drop of liquid, at rest on an inert refractory plaque, obtained photographically or radiographi-cally. The volume is calculated from the shape, which is sensitive to the surface tension and supporting material, by some intricate empirical relation. The drop contour changes with 90 deg rotation of the support.7 The application of all methods is limited by reaction between liquid metal and the apparatus. The successful stabilization of a mass of liquid metal during levitation melting8 afforded a technique for measuring the density of liquid metals out of contact with solid materials. The technique was developed by using copper as the density of liquid copper has already been studied extensively, thus allowing comparison with the new method. It consists of calculating the volume from the dimensioned profile of the levitated drop obtained by emitted-light photography and careful calibration. The molten egg-shaped drop spins around the magnetic axis of the coil (lined vertically) at a speed which seems to increase with increasing temperature. The method does not involve corrections and the experimental setup allows the use of vacuum or special atmospheres. The maximum operating temperature is limited by excessive evaporation of metal from the droplet. EXPERIMENTAL Levitating System. A stabilizing ring was used in conjunction with a 3-turn levitating coil energized by a 450-kc per sec, 10-kw Toccotron with a high current-low voltage output stabilized to f 1 pet.' APyrex glass tube with a Pyrex Optical flat window inserted through the coil and ring allowed the use of special atmospheres during levitation melting, as shown in Fig. 1. Optical System. Fig. 1 shows the optical arrangement used to photograph the profiles of the drop, parallel and perpendicular to the vertical spinning axis, simultaneously on the same frame of a high-speed 35-mm film. The optical system was adjusted to avoid any distortion of the profiles and to ensure that both profiles are in focus. The length of path from object to objective was about 30 cm, and a magnification factor close to 1 was obtained with the single-lens reflex-camera system. Temperature Measurement and Control. In operation, the specimen temperature was constant to 5 C for a fixed power input to the levitating coil and fixed rate of gas flow through the tube. The temperature was measured by an automatic two-color pyrometer (Coloratio) checked at the melting

Jan 1, 1963

By John Plecash

This paper comprises a general outline of all of the developments, including the history, geology, mining, milling, power and transportation installations, at the gold mining operation of La Luz Mines Limited and the copper mining operation of its wholly-owned subsidiary, Rosita Mines Limited, both located in north-central Nicaragua. The low-grade, gold-bearing ore-bodies of La Luz Mines, contained in highly fractured and folded Lower Cretaceous sedimentary rocks, were from 1909 to 1928, mined and treated by primitive methods by the La Luz and Los Angeles Mining Company. The abandoned property was acquired by La Luz Mines Limited in 1936, and was equipped with modern machinery and put into production in 1939. Between 1939 and 1948, the daily rate of production was in-creased from 300 tons per day to 2,-000 ton per day. The ore reserves available for open-pit mining were depleted in 1954. Since then, the entire production has come from under-ground operations.

Jan 1, 1963

By J. J. Kramer, W. A. Tiller, G. F. Bolling

The temperatures of solid-liquid interfaces have been measured during the growth of Sn-Pb alloy crystals which exhibited a cellulur substructure. A simple descriptive theory was used in combination with this data and the other measurable growth variables to predict some features of the solute segregation such as the intercell excess concentration and the depth of cell grooves during freezing. The effective distribution coefficient at the tip of a cell, a, was predicted and experimentally found to vary in the range, 1 >a > k0. At the lower limit, the severe segregation that must arise between dendritic cells was substantiated by various observations such as the existence of a second Phase even for alloys of only 0.2 wt pct Pb. ThE cellular morphology of a solid-liquid interface is known to coincide with the formation of a zone of constitutional supercooling ahead of the interface during growth.' The occurrence of various cell structures, (two-dimensional cells, regular cells, dendritic cells), has been quantitatively investigated,'2,4 but the segregation of solute which arises as a consequence of this mode of growth has only been examined qualitatively. An indirect method of obtaining the solute concentration at the tip of a cell cap during solidification has been de-

Jan 1, 1963

By James R. Welty

Heat content values were experimentally determined for yttrium metal between temperatures of 400° and 1,300° K and for iron pentacarbonyl between 301° and 380° K. The drop technique was used; that is, a sample of material sealed in a protective capsule was heated to 3 desired temperature in a furnace and then dropped into an ice calorimeter. A revised technique for determining heat content values from calorimetric data is described. Heat content and corresponding entropy-increment data above a reference temperature of 298.15° K are presented in tabular form. Equations for heat content and heat capacity as functions of temperature were derived for each substance. These equations are [Y (c): HT-H298.15 = 1.2041T 1 3.393 x 10-3T2- 0.4176 x 10' T"1 + 739.9 cal/mole Cp = 1.2041 + 6.786 x 10-3T + 0.4176 x 106-T-2 cal/deg mole Fe (CO) E, (1) : HT - H298.15 = 55.636T - 16,588 cal/mole Cp = 55.636 cal/deg mole]

Jan 1, 1963

By L. B. Pankratz

High-temperature heat-content values of gallium and scandium sesquioxides were measured over the temperature range from 298° to 1,800° K. The results fill gaps in the thermodynamic information for these compounds; no previous similar data existed. The heat-content values were combined with heats and entropies of formation to obtain free energies of formation of gallium and scandium sesquioxides to 2,000° K. The thermodynamic stabilities of the sesquioxides of aluminum, gallium, scandim, and yttrium were compared.

Jan 1, 1963