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Institute of Metals Division - Production of High-Purity Aluminum Crystals by a Modified Strain-Anneal Method (TN)By H. P. Leighly, F. C. Perkins
THERE have been several statements in the literature about the difficulty of producing single crystals of high-purity (99.99pct) by the strain-anneal method. Consequently, investigators tend to employ low-purity aluminum for their single-crystal experiments, or else resort to the Bridgman or other techniques which depend on solidification for the production of single crystals. The following paragraphs describe a solid-state method for the manufacture of single crystals of high-purity aluminum which should provide crystals with greater perfection than those formed by solidification. The starting material for this method of producing single crystals was secured from the Aluminum Corp. of America and has a purity of 99.99 pct, the balance being trace amounts of impurities. Specimens approximately 1 by 4 in. are sheared from sheet having a nominal 0.050 in. thickness. The specimens are given a preliminary anneal at 640°C for approximately 3 hr in order to remove fabrication strains and to produce an average grain size of about 1/4-in. diam. The specimens are then etched in Tucker's etchant (45 pct HC1, 15 pct HNO3, 15 pct HF and 25 pct H2O) to remove the oxide film. Critical strain is applied by wrapping each specimen about a 1 3/4 in. round and subsequently straightening it against a flat surface. The high-purity aluminum sheet is sufficiently soft that this operation can be accomplished by ordinary finger pressure. The specimens are immediately annealed again at 640°C for 3 hr and reetched for examination. Ordinarily, considerable growth of certain of the grains will have occurred, and occasionally a single crystal will be produced on the first attempt. The procedure of alternately straining, annealing and etching is repeated until the majority of a batch of specimens contains usable crystal sizes. Typical examples are illustrated in Fig. 1. The greatest changes in crystal sizes are produced in the initial treatments. As the average crystal sizes get coarser in the later treatments, the sever- ity of the strain must be increased in order to produce grain boundary- migration. This increase in severity is effected by decreasing the diameter of the round used for straining (to 1 1/2 in., for example) and/or wrapping the specimens about the round twice, with opposite faces in contact with the round, before flattening. Usually the strain treatments described are not severe enough to produce nucleation in coarse grain high-purity aluminum. The growth of grains occurs by strain-induced grain-boundary migration. It has been observed that the grain boundaries move most readily during the first hour or so of each annealing treatment and that the rate of movement decreases with extended holding times at temperature. Prolonged annealing treatments are therefore not usually beneficial. Similarly, the rate of growth of each crystal appears to depend upon the orientation of the crystal with relation to those of its neighbors. Frequently island grains are formed after the initial heat treatment as the result of slow grain-boundary migration. These sometime become stationary during later heat treatments. Twin orientation interfaces are frequently developed during annealing. These imperfections can usually be removed by increasing the severity of strain to produce actual nucleation of new grains of more favorable orientation at the imperfection interfaces. The largest single crystals produced in our laboratory by the above method measured 4 by 1 by 0.050 in. Examination of Laue back-reflection patterns from a limited area of the specimens, gave no evidence of polygonization. Probably there is some indication of polygonization in the original grain area provided a more sensitive technique is used for detection. Experiments to produce wider specimens were less successful, possibly because wider sheets increase the complexity of the strains induced by deformation and promote widespread nucleation. Grain boundary migration occurs preferentially in a direction parallel to the longitudinal axis of the specimen. The choice of specimen geometry with respect to the rolling direction of the sheet appears to be immaterial in regard to the production of single crystals.
Jan 1, 1961
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Institute of Metals Division - Recovery in Single Crystals of ZincBy J. Washburn, R. Drouard, E. R. Parker
Temperature dependence of the rate of recovery in zinc single crystals after a simple shear deformation at low temperature was investigated. Some tentative suggestions regarding the annealed and strain-hardened states of a crystal are discussed. RECOVERY may be defined as the gradual return of the mechanical and physical properties of strain-hardened metal to those characteristic of the annealed material; an increase in temperature increases the rate of recovery. The annealing process in strain-hardened polycrystalline metals is complicated by the inhomogeneity of strain which always exists in aggregates. Polygonization in bent regions of the crystals and growth of new almost strain-free grains starting at points of severe local distortion1-:' make it almost impossible to isolate and study the recovery process. Homogeneously strained single crystals, however, do not polygonize or re-crystallize and hence they can be used advantageously to study recovery. In such crystals strain hardening is completely removed by recovery alone. Since recovery is a process whereby certain lattice disturbances introduced by plastic flow are gradually reduced, a knowledge of the rate and temperature dependence of this process for various conditions of prestrain might be helpful in formulating a model of the strain-hardened state. For simplicity it seemed desirable to limit the type of prestrain to the simplest obtainable, i.e., simple shear strain. In the experiments to be described, recovery was studied by observing changes in the stress-strain curve of prestrained zinc single crystals held for various times at temperatures above that employed for straining. Single crystals were grown from the melt by a modified Bridgeman technique from Horse Head Special zinc 99.99 pct pure, and from spectrographically pure zinc 99.999 pct pure. They were grown as 1 in. diameter spheres and acid-machined' to the final specimen contour. The test section was a cylinder about 1/8 in. high and 3/4 in. in diameter. The conical sections adjacent to the test section were cemented into the grips so the load could be transmitted to the crystal as uniformly as possible. The specimens were oriented so that in testing the maximum shear stress was applied along one of the slip directions, [2110], in the (0001) plane. Details of the production and testing of such specimens have been presented.' Each test was carried out according to the following schedule: 1—The crystal was strained at — 50°C until it reached a maximum shear stress, ,,,. The strain rate was approximately 5 pct per min in all cases. 2—After straining, the crystal was unloaded before the temperature was changed. Unloading required about 3 min. 3—The temperature of the specimen was then increased from — 50°C to the temperature, T, of recovery. This change in temperature was completed in a time of less than 2 min. The specimen remained at temperature, T, for a time, t, which differed for the various specimens. 4—Thereafter the temperature was again reduced to — 50 °C in approximately 3 min. 5—While at —50°C, the stress-strain curve after recovery was obtained. 6—The specimen was then unloaded and annealed for 1 hr at 375 °C in a helium atmosphere to bring about complete recovery. Cooling to room temperature after anneal required 90 min. 7—The same crystal could be re-used for another test because the plastic properties after annealing closely duplicated those of the original crystal. The specimen was immersed during the test in a bath of methyl alcohol which, through a system of tubes, could be pumped through either of two heat exchangers to regulate the temperature; this was accomplished by circulating the liquid through coils immersed in a bath of acetone and dry ice for cooling or in a bath of warm water for heating. Test temperatures were thus maintained constant within ±1°C. The — 50°C temperature was low enough so that no measurable recovery occurred during unloading and reloading. The stress-strain curve continued after recovery along a path below, but approximately parallel to, the path of a curve obtained in an uninterrupted test. Fig. 1 shows some of the results from a specimen of 99.999 pct Zn. The amount of downward displacement of the curve due to recovery was a
Jan 1, 1954
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General Design Sulphide Ore PlantBy Wilbur Jurden
THE writer's first experience with a nonferrous reduction plant of great magnitude was at the Washoe reduction works of Anaconda some 35 years ago. Here was a plant which had been planned with remarkable skill and foresight considering the time and the state of development of copper-plant practice in the year 1902. The designer utilized topography to fullest extent to provide proper sequence of operations and, what is most remarkable, to leave adequate space for future developments, most of which at that time were unknown. However, the practice then was to locate the various units of the reduction works at the most advantageous points of the existing terrain with little regard for tramming or other auxiliaries and then connect these various units by the essential trackage, conveyor systems, piping, etc., as the need developed. This occasionally led to undesirable track arrangements, sharp curves, and steep grades, especially when it became necessary to extend various portions of the plant. Conveyor systems also became rather complicated, running as they did at various angles, and such items as piping and electrical distribution were often found to be in the wrong place, entirely inadequate in size, or awkwardly arranged for any kind of extension. This condition was not peculiar to Anaconda, for all copper plants at that time were built in the same manner and it was the constant association with these difficulties which, in the year 1925, influenced the layout of the Andes Copper Mining Co. plant. In that plant all trackage was laid out straight and level, all conveyors at right angles to each other with minimum length and number of transfers. All buildings were placed parallel and the main structures were complete for all purposes so that auxiliary buildings and dog houses would not be added later. Piping and electrical work was provided for in the original layout and carefully designed to avoid additions and alterations, and careful study given to every movement of material throughout the entire plant so that it would be accomplished with the least possible effort. Naturally it was hardly expected to attain all these objectives perfectly but our efforts did succeed in creating a plant which was unique and outstanding for its time-1927. It was also most gratifying to find that these design principles contributed to considerable savings starting right in the drafting room, carrying through the construction and ultimately yielding savings in operations and manpower. Not only that, but such a plant gives the observer an impression of symmetry and order, is more attractive to the workmen, and unquestionably eliminates many accident hazards. However, the Andes plant buildings were fitted to the existing terrain instead of having terrain created to fit the buildings-an item which we found advantageous to correct on the next large plant. At Morenci in 1939, all of the desirable features of the Andes plant such as parallel buildings, etc., were incorporated; but we went one step further-power shovels were brought in to make the terrain fit the reduction works. The result at Morenci is well-known and needs no elaboration here, but the success achieved by the design methods used for this and previous plants naturally influenced and guided the layout of the Chuquicamata sulphide plant which is the largest yet conceived. Chuquicamata Plant Design At Chuquicamata several factors not encountered previously complicated the problem to a great extent. The most desirable location for the smelter would allow smelter gases to blow directly into the open-pit mine already producing 60,000 tons of oxide ore per day and employing 1550 men. This, of course, would be a serious condition and, therefore, we were forced to move the smelter to a less desirable location but followed our previous experience at Morenci and made the terrain fit the job. The most difficult problem, however, was the provision for receiving various types of ore both by rail and conveyor. These consisted of: 1-Sulphide-bearing residue from the stockpile from which oxide copper had previously been leached. 2-Sulphide-bearing residue coming direct from the leaching vats. 3-Sulphide ore crushed at the existing crushing plants and hauled to the concentrator in cars. 4-Sulphide ore from the new crushing plant adjacent to the concentrator. 5-Sulphide ore obtained
Jan 1, 1952
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Coal - Froth Flotation in Durham Division of the National Coal BoardBy H. Macpherson
Durhm has a well earned reputation for supplying some of the finest coking caals in the world. The caals, in general, vary in rank from 301 to 501/2. Durham has traditionally produced foundry coke for the major proportion of the foundries in Great Britah. Durham coals can be described as clean, soft coals, which yielded, with the old hand methods of coal getting, low ash small coal because the extraneous shale was normally harder than the coal and occurred in larger pieces. Under these conditions, with a plentiful supply of cheap labor, it used to be sufficient, at most collieries, to hand clean the large sizes of coal which could then be remixed with the untreated small coal to produce carbonization coals, ready for the coke ovens, at under 5 pct ash. With the introduction of mechanical methods of coal mining, the coal gradually required more cleaning. The first method adopted to resolve this problem was the introduction of pneumatic dry cleaners for the small coal. Although such machines had little effect on the fine coal (say below 1/8 in.), they could clean the intermediate sizes of coal. This, coupled with hand cleaning the larger sizes above 1-1/2or 2 in., resulted in a combined run-of-mine mixture below 6 pct ash, capable of maintaining the quality and reputation of the cokes produced. In more recent years, the intensification of mechanization and power loading, coupled with gradual exhaustion of the cleaner seams, has created the need for a more complete method of coal cleaning. This particularly applies in the fine sizes (say below 1/50 in.) which normally vary, under present day conditions, between 15 and 35 pct ash and are much too dirty to be included in the raw state in a carbonization mixture. This pronounced change has been accelerated because legislation controlling the dust conditions of mine airs for the prevention of pneumoconiosis has resulted in tk~e extensive use of water underground and a consequent increase in moisture content of the run-of-milie output. The presence of damp fine coal decreast the efficiency of prescreening and dry cleaners, so that this type of preparation for low ash coking coals is decreasing, although it is still used satisfactorily for industrial coals in the medium ash range. Table I shows the gradual increase in mechanization, the reduction in manpower, the increased use of explosives per ton of coal extraction, and the increase in the proportion of coal cleaned by mechanical means in Great Britain. Although similar figures are not available for Durham Div. until after the date of nationalization of the coal industry, it is probable that the increase in mechanical cleaning, particularly by dry cleaners, was more marked in the Durham collieries than elsewhere in the country. As dry clealiers were replaced by coal washeries in the Gritish ccal industry, no special attempts were made to recover the slurry, with the result that large outflows of dirty water were allowed, deposits of slurry came in to lagoons and neighboring streams, and a proportion of fine material was lost from the coking coal. This position, coupled with the higher moisture of the washed coking coal, resulted in adverse effects on coke oven throughputs and coke quality. It is now realized that the natural coal fines are an essential ingredient of coking coals in obtaining the correct coke structure in metallurgical cokes. This, together with economic pressure, led to the introduction of flocculation and filtration plants for the recovery of slurries, and later, when the ash contelits of the filter cakes were too high, to the introduction of froth flotation equipment. After this position had been reached, the tailings from the froth flotation pIants were, in many cases, still allowed to constitute an undesirable effluent. Recent legislation on river pollution has changed this picture; it is now necessary to provide a circuit which is completely closed so far as solids are concerned. The gradual increase in the coal cleaned by wet methods and froth flotation in Durham Div, is shown in Table 11. It is now an accepted feature of new Washeries that. froth flotation should be an integral part of the washing process from the initial installation of the plant.
Jan 1, 1962
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Institute of Metals Division - Columbium-Vanadium Alloy SystemBy O. N. Carlson, H. A. Wilhelm, J. M. Dickinson
On the basis of microscopic studies, melting-point observations, and X-ray analyses, a phase diagram is proposed for the Cb-V system. A complete series of solid solutions is formed with a minimum in the solidus at 1810°C near 35 wt pct Cb. No compounds or intermediate phases were found in the system above 650°C. THERE is an ever increasing need for better structural metals and alloys for use in nuclear reactors. In addition to the normal properties of engineering structural materials, such as high temperature strength, resistance to corrosion, and fabric-abil~ty, the nuclear properties of the material must be considered. In a nuclear reactor it is important to conserve neutrons, so a material which removes these neutrons from the reaction excessively is considered to have unfavorable nuclear properties. In nuclear-reactor design the engineer must have nuclear as well as other data available on alloys in order to make a wise selection of materials. Due to the fact that many of the common structural materials have undesirable nuclear properties, it is vital that new alloys of metals having more favorable nuclear properties be investigated. Columbium and vanadium are both high melting metals, both exhibit resistance to chemical attack, and no great difficulty is encountered in fabricating them into desired shapes. With proper treatment both metals can be cold rolled extensively without failure. In addition they have desirable nuclear properties for certain types of reactors. Therefore, the alloys of columbium and vanadium should be of interest in the atomic energy program. Since an alloy-development program is enhanced by a knowledge of the phase equilibria of the components, this investigation was undertaken to establish the phase diagram for the Cb-V system. According to the Hume-Rothery rules for alloying,' the chemical similarity, crystal structure, and atomic-size factor are favorable for a complete series of solid solutions for this system. Both elements are in the same family of group V of the periodic table and thus are quite similar chemically. The crystal structures of columbium and vanadium are compatible for extensive solid solubility, since both have body-centered-cubic structures. The atomic diameters of columbium and vanadium are 2.85 and 2.62Å, respectively. This difference of slightly more than 8 pct is well within the 15 pct maximum difference allowed for extensive solid solubility. Experimental Procedures Source of Materials: Columbium powder and sheet trimmings were obtained from the Fansteel Metallurgical Corp. According to the manufacturer the metal contains less than 1 pct impurity. An analysis of the metal showed approximately 1800 ppm C in the powder while the sheet trimmings contained less than 500 ppm C. Spectrographic analysis showed minor amounts of Ca, Cr, Fe, Mn, Si, Ti, V, and Zr in both forms of the columbium. No commercial source of vanadium having the ductility and purity desired was available to the authors at the beginning of this investigation. As a result, all of the vanadium used in this study was prepared by the bomb reduction of vanadium pen-toxide with calcium employing the method reported by Long.' Yields of massive vanadium normally were about 80 pct. Chemical analysis of the vanadium prepared in this manner showed the presence of 200 to 500 ppm N and 800 to 1000 ppm C. Minor amounts of Ca, Fe, Mn, Si, Zr, Cr, and Cb were detected by spectrographic analysis. This vanadium metal was ductile and was cold rolled into 5 mil sheet. Annealing was not necessary during this rolling and the metal retained its cold-rolling characteristic after are-melting. Preparation of Alloys: The Cb-V alloys were prepared by melting pieces of vanadium sheet togethel-with columbium in the form of sheet or pellets of powder. The melting was carried out under argon in conventional arc-melting equipment employing a tungsten electrode and a water-cooled copper crucible. Each alloy was remelted three or four times, inverting the alloy after each melting in order to assure complete mixing. Alloys normally were obtained as round flat disks, weighed approximately 70 grams, and had roughly the shape of a disk 1 1/2 in. in diameter and 1/4 in. thick. Half of each alloy
Jan 1, 1955
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Institute of Metals Division - A Texture Study in Silicon IronBy C. G. Dunn, P. K. Koh
THE primary recrystallization texture in cold-rolled silicon iron, which is the matrix texture for developing the Goss texture or the cube-on-edge texture by secondary recrystallization at temperatures near 900°C,1-5,21 has not been adequately described. Thus from the present available information, it is not possible to explain satisfactorily both the grain-growth selectivity of the matrix and the often observed magnetic torque curve, which itself provides some information on the texture. Also lacking is information on the special annealing texture that develops in this material when the annealing temperature is 1200°C or higher and the rate of rise to temperature is extremely rapid. From the work of May and Turnbull5 and from unpublished work, it was known that isothermal annealing near 1200°C tends to reduce the extent of secondary recrystallization and that a much weaker cube-on-edge texture results if appreciable normal grain growth replaces secondary recrystallization. Koh and Dunn6,7 have obtained additional information on complex primary recrystallization textures from further studies made after normal grain growth. In these instances the initial textures were retained during normal grain growth. A similar result reasonably could be expected in the present study except for the presence of a grain growth ihibitor1-5,8,9.21 and its tendency to allow only a few grains to grow. However, any information on the orientations of grains in the special annealing texture, even if far from representative of the initial matrix texture, would provide useful information on the nature of the matrix texture. In the present texture study the method of Newkirk and Bruce,10 which is based on the methods of Geisler" and Schwartz, 12 is used to obtain a complete (110) pole figure of the primary recrystallization texture. The high-temperature annealing texture is determined simply from the orientations of a large number of selected grains. The kinetic nature of the process that produces the annealing texture is treated elsewhere13 and it is shown that a form of secondary recrystallization with a very high rate of nucleation occurs during rapid annealing at high temperatures. EXPERIMENTAL PROCEDURE Commercial 0.014-in. cold-rolled silicon iron strip (3.16 wt pct Si), prepared by two stages of cold rolling with an intermediate short anneal, was given a decarburizing 3-min anneal at 800°C. Me-tallographic studies indicated complete recrystallization. Short-time anneals at 900° C and at higher temperatures proved that secondary recrystallization had not begun at 800°C, in fact, the short additional anneals were still in the induction period of secondary recrystallization. A rapid rise to an annealing temperature of 1260°C (2300°F) was obtained in a BaC12and NaCl fused salt bath. The structures that resulted from anneals in the range 12- to 1000-sec duration were relatively finegrained, even though the growth was a form of exaggerated grain growth13 or secondary recrystallization with a high nucleation frequency.= Many of the grains were large enough for an X-ray study using a 5-mil X-ray beam. A transmission Laue Camera and an optical-mechanical stage for moving the grains into the X-ray beam were used. A total of 325 grains were X-rayed in this manner and the grain orientations determined. Complete (110) pole figures were obtained for the primary recrystallization texture using CoKa radiation at 30 kv in the back-reflection range, such as (220) for (110) poles, as described recently by Newkirk and Bruce.10 The low voltage serves to reduce the spurious white radiation to a minimum. A filter of 0.001-inch iron foil was located in front of the detector slit for transmission and in front of the beam slit for back reflection. A new and improved specimen holder extended the useful tilting angle range for transmission to 70 deg instead of 60 deg as previously reported.' A torque magnetometer was used to obtain the magnetic torque curves for a number of l-in. diam disk specimens. RESULTS The (110) pole figure of the material after recrystallization at 800°C is shown in Fig. 1. The positions of the pole concentrations are found to be
Jan 1, 1961
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Minerals Beneficiation - Energy-Size Reduction Relationships in ComminutionBy R. J. Charles
SEARCH for a consistent theory to explain the relationship between energy input and size reduction in a comminution process has accumulated, over the years, an enormous amount of plant and laboratory data. Although some correlation of these data has been possible for purposes of engineering design and for the advancement of research in fracture, there is still great need of a means of predicting behaviour of a solid when it is reduced in size by mechanical forces. The best known hypotheses proposed to describe the energy-size reduction relationships in crushing and grinding stem from a common origin. The present article analyzes problems of comminution in the light of the precepts of this origin. Its object is to reconcile points of difference between these well known hypotheses and to present relationships more widely applicable to comminution studies. Theoretical Considerations: Most existing relationships between energy and size reduction of a brittle solid stem from a single, simple, empirical proposition.' Although this proposition can be demonstrated by observation and experiment, no theoretical derivation is yet possible. Mathematically, the proposition may be stated as follows: dE = -Cdx/xn [1] where dE = infinitesimal energy change, C = a constant, dx = infinitesimal size change, x = object size, and n = a constant. Eq. 1 states that the energy required to make a small change in the size of an object is proportional to the size change and inversely proportional to the object size to some power n. No stipulations are placed on the exponent n in either magnitude or sign. In 1867 Rittinger2 postulated that the energy required for size reduction of a solid would be proportional to the new surface area created during the size reduction. As far as can be determined there is as yet no physical basis for Rittinger's hypothesis. Rittinger's hypothesis can be stated mathematically as follows: E, = K(oa-a-0 . [2] Er = energy input per unit volume, K = a constant, <ti = initial specific surface, and o2 = final specific surface. In the size reduction of particles of size x, to particles of another smaller size, x2, Eq. 2 becomes the well known relation: ET = K' {l/x2-l/xx) [3] where K' is a constant. Eq. 3 may be arrived at from the proposition given in Eq. 1 by integrating and by assigning a value of 2 to the exponent n. J dE = J - C dx/x2 E = Kt (1x - 1x) where K' = C. In 1885 Kick3 proposed the theory that equivalent amounts of energy should result in equivalent geometrical changes in the sizes of the pieces of a solid. For example, if one unit of energy reduced a number of equal-sized particles to particles of one half the size, then the same amount of energy applied to the particles resulting from the first test should result again in a size reduction of one half or a final size one quarter the original size. The Kick concept may be expressed as follows: Ek = K" log x1/x2 [41 K" = a constant and E, = energy per unit volume. The expression for Kick's law may be arrived at by again integrating Eq. 1 and in this case assigning a value of 1 to the exponent n. dE= J - C dx/x Eh = - C In {x/x2) = K" log (x,/x,) where K" = 2.3 C. Application of Kick's and Rittinger's laws to comminution has met with varied success. Gross and Zimmerley4 and Piret5 have shown that Rittinger's equation applies under certain conditions of experimentation. Walker and Shaw6 express the belief that in metal turning and shaping and in grinding of both metals and minerals the production of very fine particles (less than lP) follows Kick's hypothesis, whereas Rittinger's concept is valid for the size reduction of coarse particles. For the practical case of crushing and grinding, however, neither of the above hypotheses has received general acceptance. Bond' has lately proposed that since neither Kick's nor Rittinger's hypotheses seem correct for plant design work, an energy-size reduction relationship somewhere between the two would be more applicable. The fundamental statement of Bond's work
Jan 1, 1958
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Institute of Metals Division - Determination of Number of Particles Per Unit Volume From Measurements Made on Random Plane Sections; The General Cylinder and the EllipsoidBy 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
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Institute of Metals Division - Solute Segregation During Dendritic GrowthBy 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 '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,' Smith, Tiller, and Rut-ter,' 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:' or diffusion controlled solute movements in the liquid without any convective mixing.' 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 '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
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Reservoir Engineering - General - Reservoir Performance During Two-Phase FlowBy W. T. Weller
In Part I, a study of pressure build-up curves calculated for conditions under which both oil and gas flow led to the conclusion that the presence of a dispersed free gas phase in an oil reservoir must be taken into consideration to estimate accurately average reservoir pressure and permeability from build-up curves. Familiar methods based on the assumption of no free gas can be extended to the two-phase case by using total compressibility and mobility in place of single-fluid compressibility and mobility. These methods give correct values for average pressure and permeability when gas saturation is small. Errors become larger as the gas saturation increases. However, for the use to which the results will be put, the methods are satisfactory for reservoir engineering purposes. An improved method of calculating the performance of depletion-type reservoirs is presented in Part 2. Because the mathematical relationships describing simultaneous flow of oil and gas are quite involved. simplifying assumptions are made to provide means of obtaining approximate solutions of reasonable accuracy. One such approximate method now in use is the constant-GOR solution. It involves the assumption that at any instant, the ratio of total gas flow rate (both free and disolved) to oil flow rate is the same at all points in the reservoir. The approach is not applicable unless the free gar saturation in the reservoir is everywhere greater than the critical gas saturation. This paper presents a modification which, by avoiding the constant-GOR assumption, makes the method applicable to all reservoir conditions, and so far appears to be more accurate than the constant-GOR solution and to he comparable in required compuctation time. PART I— BUILD-UP CURVE ANALYSIS INTRODUCTION Pressure build-up characteristics of shut-in wells have been used for many years by engineers to evaluate average reservoir pressure, effective permeability thickness of the pay section, effectiveness of well completion (skin effect) and reservoir size. A number of methods of analysis have appeared from time to time."" Without exception, these methods are based on the assumption that the reservoir contains but one fluid of constant small compressibility and constant mobility. It has been suggesteda" hat these single-fluid methods may be applied to data from reservoirs containing both oil and gas by substitution of some effective total properties of the multiphase system in place of the corresponding single-phase properties. The present investigation was undertaken primarily to evaluate this approach. METHOD A number of theoretical build-up curves were calculated for conditions of two-phase flow, under the assumption of certain reservoir and fluid properties, and were analyzed by single-fluid methods with appropriate total compressibility and total mobility values for the corresponding single-fluid properties. Results of the analyses were compared with the assumed conditions. The theoretical build-up curves were completed by procedures similar to those of West, Garvin and Sheldon." Since these calculations require a considerable amount of computer time, an attempt was made to derive an approximate calculation method. The attempt was unsuccessful for calculating build-up curves, but the effort did result in a new approximate method of calculating the performance of solution gas drive reservoirs, which appears to be an improvement over the constant-GOR method" used previously (see Part 2). The West, Garvin and Sheldon calculations involved the following assumptions: (1) the reservoir is circular and completely bounded, with a completely penetrating well at its center; (2) the porous medium is uniform and iso-tropic, with a constant water saturation at all points; (3) gravity effects can be neglected; (4) compressibility of rock and water can be neglected; (5) the composition and equilibrium are constant for oil and gas; (6) the same pressure exists in both the oil phase and the gas phase; and (7) no afterproduction occurs, i.e., the well is shut in at the sand face for build-up. These assumptions make it possible to describe two-phase flow of oil and gas by the partial differential equations:
Jan 1, 1967
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Technical Notes - Discontinuous Crack PropagationBy L. D. Jaffe, H. C. Mann, E. L. Reed
It has been generally believed that fracture originates at a point and, if the stress is suficient, propagates across the material from this point. Evidence to the contrary is given in Fig 1. This micrograph shows an area close to the fracture of a steel containing The material had been quenched from 1675°F and tempered at 1150°F as a round about 10 in, in diam, and had a static tensile strength of 132,000 psi and a static yield strength of 105,000 psi. The steel was broken in 3000 cycles of reversed bending at a nominal max. fiber stress of 110,000 psi at a speed of 10,000 rpm. It was in the form of a standard R.R. Moore specimen with 45" V-notch, 0.015 in. radius and 0.220 in. diam at base of notch. The fractured edge in Fig 1 is part of the central portion of the specimen which broke during the final sudden fracture. Attention is directed to the short cracks which appear as dark lines within the specimen. Similar cracks were found in another specimen of the material, broken in 1,798,000 cycles at a nominal stress of 40,000 psi. The cracks were found in several areas close to the path of the final sudden fracture. This final fracture appeared microscopically to be wholly brittle and transcrystalline. Closer to the surface of the specimens, near the path of progressive fracture, which presumably advanced gradually during many cycles, there was microscopic evidence of some local deformation, but no microcracks. Neither were microcracks observed in areas distant from the main fracture path. The following explanation is offered: In the sudden fracture of the specimen, a crack propagates along a crystallo-graphic plane, with little or no plastic deformation of the adjacent material, until it reaches a grain boundary or a particle of carbide or inclusion which stops its advance. (The particle or boundary may be outside the plane of polish and not visible in the micrograph.) A stress concentration occurs about the end of the stopped crack. One or more new cracks are likely to start in the zone of this stress concentration. They may lie in the same grain as the first crack or in an adjacent grain. New cracks may occasionally start in a nearby but not adjacent grain whose orientation with respect to the stress leads to more ready fracture than does that of the grain between. Once started, these cracks propagate along crystallographic planes in their grains and the process repeats. This leads to discontinuous, branching chains of microcracks. As the process continues, microcracks probably tend to link up by fracture of intermediate material under the influence of increasing stress concentration. Occasionally, too, there may be a series of nearby grains of similar orientation so that there is a certain continuity of fracture across them. In either case the effective size of a crack is increased, resulting in greater stress concentration at its ends and a greater likelihood of further increase of size of the continuously-fractured region. When one continuous crack crosses the entire specimen, macroscopic fracture has occurred. The fractured edge of the specimen in Fig 1 represents a series of microcracks which became continuous across the entire specimen. The short, dark-appearing cracks in the figure did not become continuous over a large area. The row of microscopic stress concentrations at their ends may link up with those of the "main crack" outside the plane of polish. The above explanation does not imply that microcracks develop at the same rate in all portions of the specimen. They will develop most rapidly where the macroscopic tensile stress and macroscopic stress concentration are greatest. Viewed on a scale large compared to the grains, the fracture would appear to progress continuously across the specimen. Although Fig 1 shows a specimen broken in a fatigue test, it is believed that the microcracks discussed do not depend on the repetitive nature of the stressing used, since they are in the region where "sudden" fracture occurred, presumably in a single stress cycle. The whole process of microcrack propagation outlined above is thought to have occurred during this single cycle. It is believed that discontinuous crack propagation may be universal in brittle transgranular fracture of crystalline solids. Further experiments are under way.
Jan 1, 1950
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Technical Notes - Diffusion of Boron in Alpha IronBy P. E. Busby, C. Wells
FURTHER study of data used in determinations of 1—rates of diffusion of boron in austenite and 2—solubilities of boron in the a and phases of iron and steel' has provided an equation for the diffusion of boron in a iron. In brief, the previously published data were accumulated from the results of deboron-izing (and decarburizing) experiments carried out in the range of 700° to 1300°C. Diffusion coefficients (D?) for boron in austenite were calculated using the Grube solution of Fick's law. However, only solubility values were estimated from the discontinuous concentration-penetration curves, Fig. 1, which are characteristic of diffusion in two phases. Dr. Carl Wagner' has recently provided a solution for calculating D values from penetration curves of this type as follows: Cl1.1 —C8/C8- C11.1 = vp ? e ? erf (?) and D = ?/4?2 t where C11,12, C8, C11, and E have the values shown in Fig. 1. D is the diffusion coefficient, sq cm per sec; t is time of deboronizing anneal, see; and ? is a di-mensionless parameter. For a given diffusion experiment, the value of ? can be readily obtained by graphical solution from a plot of y vs the right-hand part of Eq. 1. D may then be evaluated from Eq. 2. The avplication of this solution to previously re-ported results, of which excerpts are given in Table I, permits the calculation of diffusion coefficients for boron in a iron. On the basis of these meager data, it is tentatively concluded that the diffusion of boron in a may be represented by the equation Da = 1011 e-92,900/RT where R is the gas constant, cal X 0C-1 X mol-1; and T is the absolute temperature, OK. Although the frequency factor, 106 sq cm per sec, is admittedly several orders of magnitude higher than expected, the value of Q, 62,000 cal per mol, appears reasonable and is, in fact, very similar to that for the self-diffusion of iron. It is pertinent to mention at this point that the value of Q obtained for the diffusion of boron in austenite by means of the Wagner solution is 19,000 cal per mol and is in excellent agreement with the value previously reported1 in the equation DT = 2xl0-3 e-21,000/RT [4] which was determined by the application of the Grube solution to other data. The fact that determined constants A and Q in the equation D? = A e-Q/RT were practically the same, independent of whether the Wagner or Grube solutions were used in determinations of D values, strengthened the authors' belief that the computed values of D (Table I) using the Wagner solution are reliable. The relative values in Eqs. 3 and 4 for the diffusion of boron in the a and ? phases, respectively, suggest that boron forms a substitutional solid solution in a iron and an interstitial solid solution in ? iron. The same tentative conclusion has been reached by McBride et al.3 on the basis of relative solubilities, atom diameter, and the size of the interstitial hole in a and ? iron. In connection with the data for test 14 listed in Table I, it is of interest to calculate the solubility of boron in a iron using the D value given by Eq. 3. As might be anticipated from the small movement of the interface in test 14, proper substitutions in Eqs. 2 and 1 give a low value, approximately 0.0004 pct B, at 850°C. Apparently at 835°C (test 13) it is possible to obtain 0.0018 pct B, and at 850°C only 0.0004 pct B into solution in the a phase before a second phase appears. These observations are consistent with the Fe-B constitution diagram proposed by McBride, Spretnak, and Speiser.3 References P. E. Busby, M. E. Warga, and C. Wells: Diffusion and Solubility of Boron in Iron and Steel. Trans. AIME (1953) 197, p. 1463; Journal of Metals (November 1953). 'W. Jost: Diffusion in Solids, Liquids, Gases. (1952) pp. 69-71. New York. Academic Press Inc. "C. C. McBride, J. W. Spretnak, and R. Speiser: A Study of the Fe-Fe2B System. Trans. ASM (1954) 46, p. 499.
Jan 1, 1955
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Extractive Mettallurgy Division - Engineering Aspects of Ion Exchange in HydrometallurgyBy R. D. MacDonald, John Dasher, A. M. Gaudin
ION exchange is a widely used unit operation in water treatment and elsewhere in chemical industries. It has occasionally been used in hydro-metallurgy for treating plating, pickling, and rayon wastes Concerning ion exchange in extractive hydrometallurgy—for treating ore leach solutions— the literature prior to the Geneva Conference has given only hints."-" Yet most of the ore leach plants now being built or completed in the last three years use ion exchange for this purpose. Most of these plants are used for extracting uranium. The overall process for leaching low grade uranium ores and the history of its development have been given in the authors' previous papers.',' The object of this paper is to discuss certain engineering aspects of the new application of ion exchange to recover dissolved values from ore leach solutions. Necessarily the illustrations will be taken from the first application—to uranium metallurgy. Although ion exchange processes have been devised in which separation of spent residue from pregnant liquor is not required, as in the RIP process,"-'I only ion exchange operation, in which the resin is contacted with a clear solution, will be discussed in this paper. Uranium exists in acid leach liquors mainly as the cation UO," and can be adsorbed completely by cation exchange resins, but the adsorption is not selective as other cations such as Fe++, Fe+++, Al+++, Mg++, Mn", and Ca++ are also adsorbed. Uranium, however, forms complex anions with sulfate, phosphate," Carbonate"~"~ and even with chloride if the solution is strong enough.15 These anions can be adsorbed by anion exchange resins. The strong base anion exchangers have a very strong preference for these complexes and hence this adsorption is very selective. In this paper, the examples concern acid sulfate leach liquors from which uranium is adsorbed as UO,(SO,),-% and UO,(SO,),". Materials and Equipment Ion Exchange Material—Ion exchange materials include natural and synthetic; organic and inorganic; cationic and anionic; and weak, intermediate, and strong varieties. They consist of fragments or beads normally in the size range —16 to $50 mesh. The newer varieties have been developed to have greater stability, chemical strength, and/or capacity than earlier varieties. The resin used for uranium recovery is a strong base anion exchanger.* To make * Such as Rohm and Haas Amberlite IRA-400 series, British Permutit DeAcidite FF. Permutit lonac SE. and Dow Nalcite SAR. this resin, styrene plus a few percent divinyl benzene are polymerized into long chains with occasional cross links. This resin in bead form is then reacted to introduce quaternary amine groups onto most of the aromatic rings.' These resins are water-avid gels of specific gravity of about 1.1, which shrink and swell by osmosis when the ionic content of the surrounding solution is changed. The beads which are shown in Fig. 1 can be broken like an onion by rapidly replacing 15 pct H,SO, with water. This organic gel can also be broken by mechanical handling as by a centrifugal pump. Otherwise it is remarkably stable. It is unharmed by fairly strong acid or alkali, oxidizing or reducing agents, and heat up to 70°C. The strong base resin when completely in the chloride form (with a chloride anion on each quaternary amine group) holds over 107 g of C1- per dry kg. As all these chloride ions can be displaced by other anions, the resin has an exchange capacity of over 3 g equivalents per dry kg. However, the resin is sold and used by moist volume. The moist resin contains about 50 pct water, weighs about 43 lb per cu ft, has 40 pct voids, and an exchange capacity of over 1 g equivalent per liter of bed volume. Ion Exchange Equipment—Ion exchange equipment used for recovery of uranium from leach solutions is substantially identical to that developed for water treatment and other applications.'" The resin beds are held in closed tanks or columns which, in the uranium plants, have been standardized at 7 ft diam and 12 ft high. The resin bed
Jan 1, 1958
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Minerals Beneficiation - The Use of a Caved Block as an Ore Pass and Its Application to Open-Pit MiningBy H. Carroll Weed
By caving a block into the workings of its open pit and using the block as an ore transfer, the lnspiration Consolidated Copper Co. has solved a transportation and sizing problem, making possible a great expansion of open-pit methods as applied to Inspiration ore-bodies. FROM 1915 to 1948 the entire production of Inspiration Consolidated Copper Co. was supplied from underground mining. The sole method used was block caving. Underground haulage and hoisting facilities were designed and geared to large-scale production. Beginning in 1948 open-pit mining was substituted for block caving in a portion of Inspiration's Live Oak orebody. The idea proved so attractive that before the Live Oak pit had come into production, another pit on the Colorado orebody (now the Thornton pit) had been laid out and stripping started. It should be noted that these orebodies were not new and the entire program was one of changed methods of mining. Since part of these orebodies had already been mined by block caving methods, it must be recognized that haulage levels had been established under the area or adjacent to it. The orebodies lay on the south side of Inspiration Ridge, while the shafts, crushers, and treatment plants are all on the north side of this ridge. The existing main crushing plant was designed to take a maximum of 12-in. material, and all ore was sized to this dimension by passing through grizzlies in the stopes. In the original planning for open-pit work much thought was given to the transfer of ore to existing underground levels for haulage and hoisting from the regular shafts. If this could be done the necessity of crossing the ridge could be eliminated. Final decision called for cutting a road through the ridge, installation of a primary crusher at an elevation of 3968 ft on the north side of the ridge, and railroad haulage with existing facilities to the main coarse crusher. This decision was brought about by the difficulties of properly sizing and transferring to underground haulage large tonnages of coarse breaking oxide which lay on the upper benches of the proposed pit. Trucking over the ridge on a 7 pct grade would give a cheaper and more flexible operation in handling this material. The benches in the pits are laid out at 50-ft inter-vals and designated according to elevation above sea level. The lowest bench in the original pit was laid out at 3500-ft elvation. All haulage roads are on a 7 pct grade and a vertical lift of 468 ft was considered about the maximum economically possible from a cost standpoint. After 2 years' operation the advantages of pit mining, both from the standpoint of costs and flexibility of operation, became more and more apparent. Studies were then started to develop the extension of open-pit mining to more of the ore reserve than had been planned originally. The idea of transfer raises was again explored. Obviously, as elevation of the pit was lowered, shorter transfer raises would be needed to reach the main haulage levels. Transportation from the lower elevations to the rim of the pit by belt conveyor or skip hoisting was also considered. However, it was recognized that sizing would be required both for conveying and regulation of feed size to the main crusher plant. This would necessitate a fixed or portable crusher located somewhere in the pit. It was known that the sulphide ore at the lower elevations was softer and easier to break than the overlying oxide of the upper benches. This sulphide ore is very suitable for grizzly sizing. Calculations indicated that for ore mined on 3650 elevation, costs for trucking to the primary crusher, crushing, and delivery by railroad to the coarse crusher would equal costs for dropping the same material to the 600 level, hauling underground, and hoisting directly to the coarse crusher bins, provided a suitable method of sizing and transferring could be developed. Above 3650 elevation costs would favor surface haulage; below they would favor underground haulage. The idea of caving an underground block from the 600 haulage level directly into the bottom of the pit
Jan 1, 1954
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The Development of Open Stoping in Lead Orebodies at Mount Isa Mines LimitedBy I. A. Goddard
INTRODUCTION This paper deals with the development of the sublevel open stoping (SLOS) method in lead orebodies at the Isa Mine of Mount Isa Mines Limited, during the last ten years. Open stoping in different forms has been used at the Isa Mine for many years. Prior to the period under review, stopes were small, pillars were not always recovered, and scrapers extracted the ore. By the end of the sixties, the use of load-haul-dump units was becoming more widespread. Wagner ST5's were the mucking units for the lead cut and fill stopes. Some of the open stopes in 5 orebody above 13 level had 100 kW slushers, but the more southerly stopes were the sites for the introduction of diesel front-end loaders for extraction. In the early seventies, new methods were used in the block of six stopes in 2 and 5 orebodies between 8 level and 13 level and a trial stoping project was undertaken in 7 orebody between 11 level and 13 level to determine possible stope dimensions for the extraction of the Racecourse orebodies below 13 level. By the mid-19701s, stoping was well underway in 5, 7 and 8 orebodies between 13 level and 15 level, using the 'triplet' system, incorporating cemented hydraulic fill to allow greater pillar recovery. As the eighties were entered, development of the Racecourse orebodies below 15 level commenced, as did preparations for 1 orebody in the upper levels of the north end of the mine. In both cases, the pillar recovery method has been changed to reduce the amount of cemented fill required for pillar recovery. GEOLOGY Most of the lead orebodies at Isa Mine lie chiefly to the north of the central shaft complex. They are bedded sulphide deposits in a host rock called Urquhart Shale, which dips at roughly 650 to the west. The main minerals are galena and sphalerite, with the silver mineral, freibergite, being contained in the galena. To the hangingwall of the sequence are the Black Star orebodies (1, 2 and 5) which are relatively wide, pyritic and with low to above average grade lead. The Racecourse orebodies (6 to 16) lie to the footwall, and have a large variation in width, low to high grade lead, and gradation in the lead to zinc ratio from north to south. Stope outlines are often determined by economic or engineering considerations rather than geological. The published extraction reserves are 56 million tonnes of primary ore, containing 150 grams of silver per tonne, 6.4% lead and 6.5% zinc. Traditionally, it has been regarded as lead ore, although the dominant revenue earner varies from time to time. In the Black Star orebodies, the ore and hangingwalls are more competent and open stoping has long been used. The major Racecourse orebodies which have been open stoped are 7 and 8 orebodies. This has been where the orebodies are wider (to the south) and where hangingwall conditions allow. This latter aspect has been greatly influenced by the presence of 'silica dolomite1. This tough, relatively homogeneous, non-bedded rock is, in fact, the host rock for the copper mineralisation at Mount Isa, and provides a competent hangingwall for some of the lead stopes. While the shale's bedding and jointing has a major influence on the ground conditions, there is a major fault system which causes local problems. The principal virgin stress direction is perpendicular to the bedding, but the local stress situation is complicated because of shielding by filled stopes in the hangingwall copper orebodies and because of the interaction between orebodies being extracted to the footwall. Most development on strike is mined with a 'shanty-back’, with the back being as close to normal to the bedding as possible. This is near parallel to most jointing and the principal stress direction. Figure 1 is a plan view of 14 level north, which provides a representative horizontal section through the orebodies. A typical cross section is shown in Figure 2. The narrow, parallel footwall orebodies can be seen to differ from the wider hangingwall orebodies.
Jan 1, 1981
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Institute of Metals Division - Titanium Binary Alloys - DiscussionBy O. W. Simmons, L. W. Eastwood, C. M. Craighead
H. Schwartzbart and W. F. Brown, Jr.—The authors have divided the effects of recovery on the true stress-true strain curve into two types; metarecovery, which effects only the first part of the curve or the yield strength, and orthorecovery, which effects the flow stress at any strain. Both of these are said to be true recovery effects, involve no recrystallization, and are explained by the removal of two different types of imperfections caused by work hardening. However, there seems to be some question as to whether the data are sufficiently conclusive to exclude, as an explanation of the authors' results, a mechanism based on the relief of residual stresses between the grains or slip bands and recrystallization. It appears that metarecovery could be interpreted in the same fashion as a customary interpretation of the Bausch-inger effect. The balanced system of internal stresses which exists between grains in a strained specimen due to varying orientation and, hence, yield strengths, of the different grains is responsible for a reduced yield strength in compression following pre-tension, and, similarly, for an elevated yield strength in tension following pre-tension. If the specimen is now heated so that the internal stresses are relieved by creep, then the yield strength in tension following tension will have been reduced and in compression following tension will have been raised. There seems to be a very strong case for the lack of recrystallization in the aluminum investigated by the authors, if one defines recrystallization as the presence of visually detectable new grains or accepts the X-ray evidence as conclusive. One must remember, however, that the appearance of spots on the back-reflection X-ray patterns cannot be taken as the time when recrystallization first started. The areas of recrystallized strain-free material must first have grown to a size large enough to give distinct spots on the patterns and this may take some time. Averbachl7 in an investigation of brass has shown that recrystallization can be detected by extinction measurements at temperatures lower than those based on hardness or X-ray line width determinations. It can be seen from fig. 10 that the rate of recrystallization is extremely low over a considerable time period at the onset of the process. Observations on the rate at which small amounts of recrystallization effect the flow stress would have given further insight as to whether undetectably small amounts of recrystallization might have been responsible for orthorecovery. Also, the question arises as to whether the effects observed in fig. 6 for various times and temperatures could not have been obtained if the time at 212°F were sufficiently long. In addition, the argument that the curve in fig. 10 is not sigmoidal seems weak in view of the scattering of the points. It is conceivable that an accurate determination of the curve for the first 100 hr would exhibit a relationship other than the one drawn. There is one point we would like to raise about the condition of the starting material. The authors annealed their material at 750°F for 15 min to remove the effects of any previous work hardening or machining strains. Reference to the work by Anderson and Mehl shows that this treatment may not have completely recrystallized the aluminum, so that the starting material may have had some strained areas. Higher temperatures or longer times may have been required to remove the effects of any small strains. We would like to mention some results of tests being conducted at the Lewis laboratory of the National Advisory Committee for Aeronautics in an investigation of the Bauschinger effect in relation to fatigue. Tests were performed on annealed electrolytic copper and several annealed brasses. Specimens were pre-strained 1 pct in tension and then tested in compression or tension with and without intermediate stress-relieving annealing treatments at 500°F for various times. Specimens heated at 500°F for 10 1/2 hr showed an elevation of the flow curve in compression and an approximately equal lowering of the flow curve in tension when compared with the curves for the un-heat treated specimens. After approximately 0.8 pct strain, all flow stresses coincided and were equal to the flow stress of the virgin material at this strain. This behavior is consistent with the metarecovery observed for aluminum by the authors and for which a residual stress model can be used. On the other hand, increas-
Jan 1, 1951
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Extractive Metallurgy Division - The Fume and Dust Problem in IndustryBy H. V. Welch
In this paper, as prepared for delivery at the Southern California regional meeting on Oct. 14, 1948, it was thought best to interpret the term "economics" in a rather broad manner and to include, in addition to the material losses and recoveries and associated monetary values (Part I), a limited discussion of the increased difficulties or the particular problem and the special requirements, as the particle sizes of the suspended particles range down from the relatively coarse to 100, to 10, to 1 micron or even to a fraction of one micron (Part II). Further, it is not quite in order to overlook entirely the community and individual health problems, although space requires the economics of this to be considered only very incompletely. Therefore, Part III, covering this phase of the subject, is very limited. This paper, then, is divided into 5 parts or headings as follows: I Losses and/or values in suspended solids. II Particle size. III Dust and fumes in community and individual living. IV Means and Procedures for dust and fume collection. V Description or examples of specific equipment in service and of the several types used for dust and fume collection. Because of the wide extent and wealth of subject material available and the space and time limitation imposed, presentation and discussion are less than originally planned. I—Losses and/or Values in Suspended Solids The weight involved in moving streams of industrial plant gases is commonly not appreciated, neither is their carrying power in the weight of solids maintained in suspension and moved with the gas stream from a point of origin or pick-up to a point of dissipation or settlement. These, however, are major weight figures; for example, in a modern iron blast furnace there may be five tons of gas for every ton of iron produced and by the time this blast furnace gas has been burned in stoves or under boilers the weight of gas discharged to atmosphere is on the order of eight times the weight of iron produced. Similarly for nonferrous metallurgy there may readily be from 10 to 20 times the weight of gases discharged to atmosphere as there is metal produced. A cement kiln in operation or a kiln in service to produce metallurgical lime may have on the order of 5 to 6 times the weight of stack gases as of clinker or lime produced, and at least the cement kiln, because of the very fine nature of its feed, is a very heavy dust producer. It may be noted that there have been two developments in progress for nearly three decades. Both are extraordinary in the industrial economics effected and in their ready availability to ever larger units of operation and their ever widening importance in industry, and both are productive of great quantities of finely divided material in furnacing. The first of these is the flotation process for ores, especially the metallics such as copper, lead, and zinc; and the second, powdered fuel combustion for power plant, industrial plants and metallurgical operations. Today, new developments, for example, flotation for the nonmetallics such as higher grade limestone for cement manufacture which requires still finer grinding and the powdered-coal-fired boilers with production ratings of over 1,000,000 lb of steam per hr, bring still more concentrated and hugely increased quantities of stack emission. Perhaps the honors for the greatest interest in the quantities and values escaping in waste furnace and equipment gases belong to the nonferrous metallurgical operations. Their record of achievement in the installation of dust and fume collection equipment, largely baghouses or Cottrell electrical precipitators, is exceeded by no other industry. Something of the magnitude and variety of equipment utilized in such recovery systems was covered by the writer in two papers presented to the Institute some 10 years ago.1,2 It is not intended to repeat the material of those articles, but it is thought that they complement this offering and should be noted. COPPER ROASTERS As the copper roasters are the first of the series of furnaces handling the copper-bearing concentrates in the usual copper smelter of today, it is in order to make them the first consideration. Multiple hearth sulphide roasters, not hard driven, often maintain their dust loss through exit gases at 3 pet or below of feed to furnace; in hard-driven or maximum-driven furnaces, exit gas losses often approximate 7 pet of charge with a ±2 pet variation for special conditions prevailing at some plants. A 5 pet loss of feed in a roaster gas exit, unless reclaimed, often makes the difference between a profit and loss operation, and in many cases substantial recovery is the very basis of dividend payments. As there is available very practical and successful equipment for the collection of the
Jan 1, 1950
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Geological Engineering - A Curricular Outcast?By P. J. Shenon
ENROLLMENT in geological and mining engineering curricula is declining at an accelerated rate despite the greatest need for trained men ever extant in the minerals industry. Industrial and military demand is mounting, but the number of freshmen selecting the mineral field continues to fall. Estimates on the needs of industry range as high as 30,000 new engineers a year. The current deficit is more than 60,000 engineers less than the 350,000 to 450,000 which eventually will be needed. The indisputable fact is that the colleges are turning out fewer and fewer engineers despite the greatest enrollment in colleges and universities ever experienced in the United States. In 1950 a record 52,000 young men stepped out of the confines of ivy covered walls with engineering degrees in their hands. By 1951, however, the number dropped to 41,000 and present enrollment indicates a national graduating class of only 25,000 for 1952. No letup in the drop is forecast. About 19,000 can be looked for in 1953 and 1954 may reach an unhappy 12,000. It becomes clear that something must be done to attract high school graduates to engineering. One immediate possibility could be to make the course burden carried by the engineering student somewhat lighter. The prescribed curriculum in many schools is such that the student takes the path of least resistance, and instead of training for an engineering future, studies for a vocation which will allow him to learn and at the same time get at least a nominal enjoyment out of college life. Review geological and mining curricula of 20 colleges and it will be found that the engineering student is a veritable pack mule compared to a lad taking liberal arts or some other non-technical program of study. The curriculum for geological engineering at one school calls for 202 semester hr, with almost 23 hr carried per semester. Multiply this figure by three hr, the minimum supposedly to be devoted to a credit and you get 69 hr per week. With a bare minimum of 84 hr for sleeping and eating, about two hours a day remain for recreation. However, the load of other schools investigated is about 19 hr. The University of Utah requires 238 quarter hr for graduation with a degree in geological engineering, while requiring only 183 quarter hr for baccalaureate degree from University college, Utah's liberal arts school. It can be stated with a measure of surety that the same proportions exist in other universities. The first step would be for ECPD to review its requirements for mining and geological engineering. It must recognize that mining and geological engineers operate in a specialized field, as do other types of engineers. Although a geological engineer may not design a bridge, as pictured by the ECPD Committee on Engineering Schools, his field of design calls for similar engineering precision, a knowledge of materials, construction methods, economic considerations, and financing. Six schools have been accredited by the ECPD. What is the basis for approval and can the requirements be modified and still be kept in line with the needs of the geological engineer? Course work from school to school varies with the exception of mathematics, chemistry, and physics. Even in those courses the not inconsiderable variation lends dubious creditability to the mean. One accredited school requires 7 1/3 semester hr of chemistry, compared with 24 hr required by another, making an average for the six schools of 17 1 /3 hr. Required credit hr in mechanics ranges from 4 to 18 and in surveying from 2 to 15. Several non-accredited schools require more hr than do the accredited schools in some courses. Why is the engineering student forced to carry such a back-breaking load? The answer is of course fairly obvious. He is irrevocably set apart from the rest of the student body because of the nature of his life's work. He is training for a place in a world where technology is becoming increasingly involved. He must be prepared to do a job now-and not later. Mining and geological engineering require the same essential backgrounds as other engineers, and more. The "more" is a knowledge of mining methods, metallurgy and geology for the mining engineer. The geological engineer must know in addition, mineralogy, petrography, and geophysics. The load is compounded finally by the addition of liberal arts courses. Should anything be done to relieve the situation? Today's engineer must be a whole man, capable of handling the tools of communication and with an understanding of the economics of industry. He must be able to write clear simple English, and he must be man who can think from some other position than bent over a work table. He must be aware of the history of his country and to some extent that of the world. Not all schools share this view. Only two of the accredited schools require history courses. However, five of the non-accredited schools make it mandatory. Four accredited and five of the nonaccredited schools require economics. Courses in mathematics, physics, and chemistry are fundamental in engineer training. The average for the accredited schools could serve as a guide in
Jan 1, 1952
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Institute of Metals Division - Preferred Orientations in Iodide Titanium (Discussion page 1563)By J. P. Hammond, C. J. McHargue
The wire textures for cold rolled and recrystallized iodide titanium and the sheet textures for this material produced by cold and hot rolling, and recrystallization at a series of temperatures were determined. 'The effect of the a + ß transformation on the sheet texture was noted. UNTIL recently it was believed that all hexagonal close-packed metals deformed by slip on the basal plane, (0001), and that rolling should tend to rotate this slip plane into the plane of the rolled sheet. The pole figures of cold rolled magnesium' are satisfactorily explained on this basis. There is a tendency for the <1120> directions to align parallel to the rolling direction, and the principal scatter is in the rolling direction. Zinc% as a rolling texture in which the hexagonal axis is inclined 20" to 25" toward the rolling direction. Twinning is believed to account for the moving of the basal plane away from parallelism with the rolling plane. The texture of beryllium3 places the basal plane parallel to the rolling plane with the [1010] direction parallel to the rolling direction, and the scatter from this orientation is primarily in the transverse direction. Cold rolled textures reported for zirconium' and titanium5 how the [1010] directions to lie parallel to the rolling direction and the (0001) plane tilted by approximately 25" to 30" to the rolling plane in the transverse direction. Rosi has recently reported that the mechanisms for deformation in titanium are distinctly different from those commonly reported for hexagonal close-packed metals. The principal slip plane is the prismatic plane, {1010), with some slip also occurring on the pyramidal planes, (1011). However, there is no evidence for basal slip. The slip direction is reported to be the close-packed digonal axis, [1120]. In addition to the twin plane commonly reported for metals of this class, {1012), Rosi found the twin planes (1122) and {1121), with the dominant twin plane being (1121). Information regarding the recrystallization and hot rolling textures of hexagonal close-packed metals is limited. Barrett and Smigelskas report that rolling beryllium at temperatures up to 800°C and recrystallization at 700°C produce textures not differing from the cold rolled sheet texture.3 McGeary and Lustman find that hot rolling at 850°C produces the same basic texture in zirconium as rolling at room temperature.' These investigators also report that the texture for sheet zirconium recrystallized at 650 °C differs from the cold rolled orientation inasmuch as the [1120] direction, instead of the [1010] direction, is parallel to the rolling direction. In the case of titanium, it is not possible to deduce which direction is preferred in the recrystallized state from the pole figures presented by Clark." The purpose of this paper is to report an extensive investigation of the preferred orientations in iodide titanium. Since the deformation mechanisms for titanium are different from those commonly given for hexagonal close-packed metals, it is not surprising to find distinct differences between the textures of titanium and other metals of this class. Materials and Methods This investigation was carried out on iodide titanium obtained from the New Jersey Zinc Co. with an analysis as follows: N2, 0.002 pct; Mn, 0.004; Fe, 0.0065; A1, 0.0065; Pb, 0.0025; Cu, 0.01; Sn, 0.002; and Ti, remainder. The crystallities of titanium were broken from the as-deposited bar and melted to form 20 g buttons on a water-cooled copper block in a vacuum arc-furnace. Hardness tests conducted on the material before and after melting differed by only two or three Vickers Pyramid Numbers, indicating no or insignificant contamination. The buttons were hot forged, ground, and etched to sizes and shapes suitable for the rolling schedule, and vacuum annealed at 1300°F. Specimens for determination of the wire textures were reduced 91 pct in diameter to 0.027 in. in 24 steps using grooved rolls. In order for the orientation of the central region to be studied, portions of these wires were electrolytically reduced to a diameter of 0.005 in. using the procedure described by Sutcliffe and Reynolds.' The sheet textures were determined on titanium cold rolled 97 pct to a thickness of 0.005 in. A reduction of approximately 10 pct per pass was used, and the rolling direction was changed 180" after each pass. Specimens used for determination of the recrystallized textures were annealed in evacuated quartz tubes at 1000°, 1300°, and 1500°F. The grain size of the 1000°F specimen was sufficiently small to give satisfactory X-ray patterns with the specimen stationary. However, it was necessary to scan the surface of the other recrystallized specimens. The microstructure of each annealed specimen was that of a recrystallized material. The diffraction rings all showed the break-up into spots typical of recrystallized structures.
Jan 1, 1954
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Part VII – July 1969 – Papers - Dynamic X-Ray Diffraction Study of the Deformation of Aluminum CrystalsBy Robert E. Green, Kenneth Reifsnider
Several experiments have been performed in order to illustrate the application of a recently developed X-ray image intensifier system to metallurgical investigations. In the present work the system has been used to study the instantaneous alterations in Laue transmission X-ray diffraction patterns during tensile deformation of aluminum single crystals. Expem'mental results are presented which demonstrate the capability of the system for crystal orientation, for following orientation changes due to lattice rotation during tensile deformation, and for showing changes in the homogeneity of the lattice planes along the specimen length as a function of strain rate. RECENTLY, a new X-ray system has been developed which incorporates a cascaded image intensifier and permits direct viewing and recording of X-ray diffraction patterns produced on a fluorescent screen.1"3 In the present work the results of several experiments are presented which demonstrate the usefulness of this system for metallurgical applications. EXPERIMENTAL PROCEDURE A schematic diagram of the experimental arrangement is shown in Fig. 1. In this system a Machlett AEG-50-S tungsten target X-ray tube, normally operated at 50 kv and 40 ma, serves as the X-ray source. The X-ray tube is placed in direct contact with a 10-in.-long collimator, which transforms the X-ray beam from one with a circular cross section to one with a rectangular cross section 3 in. high and 1/6in. wide. By blocking off all but a small portion of the rectangular slit, it is possible to work with the more conventional "pinhole" collimated X-ray beam commonly used for obtaining Laue diffraction patterns. In the present work the test specimens were 99.99+ pct aluminum single crystal wires & in. in diam and 3 in. long. For the deformation tests the wire crystals were mounted in a special set of grips in a table model Instron machine so that diffraction patterns could be recorded during specimen deformation. For the orientation tests the wire crystals were mounted in a rotating goniometer so that diffraction patterns could be recorded during specimen rotation. At a distance of 3 cm from the specimen axis, a 6 in. diam DuPont CB-2 fluorescent screen is positioned to transform the X-ray image to a visible one. A Super Farron f/0.87 72 mm coupling lens, corrected for 4 to 1 demagnification, transmits the visible image to the image tube. The image intensifier used is a three-stage magnetically focused RCA type C70021A with an S-20 input photocathode and a P-20 output phosphor. The tube has unity magnification and useful input and output screen diameters of 1.5 in. The image on the output phosphor is of sufficient intensity to be viewed directly, to be recorded cine-matographically, or to be displayed by vidicon pick-up on a television monitor. The recording device most commonly used is a 16 mm Bolex motion picture camera fitted with a Canon f/0.95, 50 mm lens. The overall gain of the system is 16,000 for direct viewing and 2240 for recording on 16 mm movie film. The resolution of the system is limited to 1 line pair per mm which is approximately that of the fluorescent screen. This system has been used for cine recording of transmission Laue X-ray diffraction patterns with exposure times as short as 1/220 sec and for vidicon television pick-up and display at a scan time of 1/30 sec. Quantitative information may be obtained from each frame of the movie film, by either stopping the vertical slit down to a point source in order to obtain a conventional Laue photograph or else by retaining the linear beam and introducing fiducial marks as described in a previous paper.4 In either case, each frame may be enlarged to appropriate size for analysis by either using a photographic enlarger and making prints of the desired frames, or, more conveniently, by using a microfilm reader. EXPERIMENTAL RESULTS The first series of photographs which are presented in Fig. 2 serves to demonstrate the usefulness of the system for crystallographic orientation determination. This series of prints, made from enlargements of a 16 mm movie film, shows the dynamic Laue transmission patterns produced by an aluminum single crystal wire which was rotating about the wire axis when the patterns were recorded. The movie films were taken at 16 frames per sec and the crystal was rotated at a rate of 15 rpm.
Jan 1, 1970