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By Strathmore R. B. Cooke, Thomas E. Ban

MUCH experimental work has been performed on the mechanism of agglomeration and pelletizing of moist ore and concentrates and on the process of firing agglomerates, but except for the work of Tigerschiöld and Ilmoni1 much of the published information is empirical, and the literature contains no information concerning the structure of fired pellets. Results of a preliminary study of the microstructures occurring in pellets produced both in the laboratory and on a pilot-plant scale are presented in this paper. Most of the results were obtained from pellets prepared from Mesabi magnetic taconite, but through the courtesy of the staffs of the Minnesota Mines Experiment Station and the Bethlehem Steel Co., fired pellets produced from limonite and hematite ores and from Lebanon magnetite have also been examined. The work has been restricted almost entirely to pellets produced without additives, the exceptions being those in which coal was. added to the filter cake before rolling. Schwartz has described the microstructures occurring in ore sinters produced under reducing conditions.2 Many of the structures and constituents he describes are common to fired pellets, but the constituents normally occur in markedly different proportions. His statement that "in all satisfactory sinter the amount of hematite is small, perhaps not over 2 or 3 per cent" is inapplicable to pellets produced by pilot plant operation or by any process in which air is not deliberately excluded. Pilot plant pellets contain over 90 pct by weight of hematite, and those produced in the smaller furnaces of the Minnesota Mines Experiment Station contain more than 80 pct of that constituent. Preparation of Specimens It is difficult to examine unfired pellets microscopically because of their insufficient coherency to withstand sectioning and polishing. Fired pellets sometimes lack coherency and frequently contain holes which are troublesome during polishing. Impregnation of both air-dried and fired pellets is readily accomplished by the use of methyl methacrylate monomer.3 The dry pellets are covered in a test tube with excess monomer, to which a small amount of accelerator has been added. When the test tube is placed in a cooling bath and evacuated with an aspirator, most of the entrapped air is removed, and disruption of weak pellets by boiling of the monomer is reduced to a minimum. Polymerization is then effected by immersion of the test tube in a water-bath at about 45°C, this temperature being held for 4 or 5 days. The test tube may then be broken away from the solidified mass and the pellets sectioned by a carborundum wheel or a diamond saw. Where time is important, impregnation is carried out at a higher temperature by Meyer's method.4 Air-dried pellets must be impregnated with especial care; otherwise swelling occurs and the solids are displaced. It is more important to be certain that the monomer forms a reasonably complete network throughout the specimen than that all entrained air is removed, and for this reason the vacuum technique may be omitted. Impregnated agglomerated products and pellets are extremely coherent, section well, and may be polished either by hand or by machine. Hand polishing is not satisfactory for the examination of conditions existing at the boundaries of grains, and for this machine polishing must be used. The Graton-Vanderwilt machine gives excellent results, provided that pressure on the specimen is considerably in excess of that recommended by the manufacturer. Mineralogy of Fired Pellets Only two opaque iron minerals, magnetite and hematite, have been recognized in pellets. The complete identity of these artificial minerals with their corresponding natural counterparts is shown by their mineralographic characteristics and their X-ray structures. Wüstite has not been found. Slag is the most common transparent constituent of fired pellets. Occasionally conditions have been appropriate for the crystallization of fayalite from the slag, and at other times another crystalline sil-

Jan 1, 1952

By W. A. Backofen, D. H. Avery, W. F. Hosford

Sheets of the magnesium alloys AZ31B, HK31A, and ZE10A in several different tempers were tested in tension and determinations were made of the ratio of width-to-thickness strain. A marked increase in the ratio with tensile straining and a dependence upon alloy and test direction are rationalized in terms of a balance between the amounts of basal and prism-plane slip. All such variations are related, in turn, to the prevailing crystallographic texture. Fracture appearance is explained on the basis of anisotropy in plastic flow, and implications for developing texture -hardening effects in these alloys are discussed. ThE crystallographic texture or preferred orientation of a given material is determined by details of processing history. Such texture is known to influence many aspects of material behavior, in particular both the yielding and strain-hardening characteristics which are of special interest in the present work. Traditionally, the resulting plastic anisotropy has not been regarded as especially desirable. Earing in drawn sheet is perhaps the most common example of an unwanted effect of texture. However, it has also been recognized that suitable textures may be usefully employed to improve drawability,1,2 as a specific example, and generally to control yielding resistance under combined-stress loading.374 Texture would seem to be a detail of structure not yet exploited to nearly the fullest extent. A convenient basis for characterizing anisotropy in plastic behavior is the ratio of width-to-thickness strains obtained in a tension test;5&apos;6 the parameter is frequently labeled "R" and its value is revealing with respect to the nature of the prevailing texture. R gives a useful measure of a material&apos;s "thinning resistance". For an isotropic material, R = 1. With R > 1 the increased through-thickness strength in a sheet means greater resistance to yielding under biaxial tension, or "texture hardening";3&apos;4 if R < 1 the result may be a "texture softening" under the same loading conditions.4 Most R data relate to steel sheets for deep-drawing applications. Values for steel and other materials of cubic structures are not often much greater than 1 and nearly constant with strain in testing.1,2,7,8 To explore the implications of plastic anisotropy further, it was felt that experiments with much more strongly textured materials would be useful, and this led to the choice of magnesium alloys. The "ideal" sheet texture for magnesium contains the (0001) plane in the rolling plane, which ought to lead to R values approaching infinity. However, departures from the ideal texture, the possibility of slip in non-close-packed directions, and deformation by twinning would all be expected to introduce some range of R. Accordingly, studies on these materials were undertaken. EXPERIMENTAL Alloys in sheet form, Table I, were selected to obtain a variation in crystallographic texture, in the expectation that this would be reflected in differences in plastic anisotropy. Pole figures constructed by the Schulz surface-reflection technique9 were provided with the experimental materials by the Dow Metal Products Co. Profiles of pole density along great circles through the rolling (0 deg) and transverse (90 deg) directions were prepared from the pole figures and are collected in Figs. 1 and 2; considerable departure from the "ideal" (0001) alignment in the rolling plane is evident, with the largest angular spread in both directions being found in the ZEl0 alloy. Results of tensile tests on full-thickness specimens of 6-in. gage length by 1/2-in. width are given in Fig. 3 as engineering stress-strain curves* in rolling and transverse directions. All tests but one were made at a constant drive rate of 0.02 in. per min, and the final values of percent elongation at fracture, over the initial 6-in. gage length, are noted at the ends of the curves; one test on ZE10A-

Jan 1, 1965

By A. Styka, G. Fischer, S. Tour

Described herein are the results obtained during research work involving coating titanium alloys with molybdenum by vapor-deposition methods. Results show that the method can be used successfully to deposit hard adherent wear-resistant coating of methodmetallic molybdenum on titanium or titanium alloys without changing the microstructure of the titanium base. PRODUCTION and use of titanium and its alloys have increased tremendously in the past few years. The physical, mechanical, and chemical properties of this engineering metal have caused considerable enthusiasm among metallurgists and engineers. However, as with all materials, there are some drawbacks. For example, titanium is susceptible to seizing and galling on wearing surfaces. In order to produce a good wear-resistant surface, many investigations have been conducted evaluating oxidizing, carburizing, nitriding, carbonitriding, sili-conizing, and chromizing of titanium. All of these processes require high temperatures for rather extensive periods of time. It has been possible to produce hard surfaces on titanium and its alloys by a number of these processes at the expense of a deterioration of the physical properties of the base material. A practical solution to the problem of providing titanium and titanium alloy parts with a satisfactory wear-resistant nongalling surface must be one that does not involve excessive temperatures for long periods of time. Sam Tour & Co. Inc. has completed a research and development contract for the United States Army Ordnance Corps on vapor deposition of molybdenum on titanium and titanium alloys. On the basis of results obtained from the research program, titanium alloys can be coated successfully with molybdenum to provide a hard wear-resistant surface without harm to their base mechanical properties. The remainder of this article is a description of the techniques used to apply the coating and the results obtained from wear tests on molybdenum-coated titanium. Theory Basically, the technique used was the application of molybdenum by a vapor-deposition method, thermal decomposition of molybdenum hexacarbonyl [Mo(CO)] with hydrogen as the carrier gas. The selection of this method was based chiefly on the following considerations: 1—low plating temperature which would minimize excessive grain growth, 2— low decomposition temperature of the carbonyl, 3— possibilities of controlling the hardness of the plate by adjusting the carbon content using the plating temperature and pressure as the primary variables, 4—use of high vacuum, thereby avoiding unnecessary oxidation and other complex reactions with the atmosphere. Free energy data1 show the strong tendency for titanium to combine with O2 N2 or carbon from normal temperatures to temperatures above its melting point. To maintain the titanium in a film free condition, the use of as high a vacuum as possible is indicated. The literature&apos; indicates that the reaction product of hydrogen with titanium is unstable in vacuum at around 400°C. 5—Although it is indicated from the thermodynamic standpoint that there is little possibility of removing carbon from either titanium or molybdenum, the work of Lander and Germer -ndicates that the use of a suitable H,/CO ratio is somewhat effective in minimizing carbon deposition. 6—Availability of molybdenum carbonyl. In the simplest form, the conditions of equilibrium3 in chemical reactions involving decomposition of carbonyl are as follows: Mo (CO) ? Mo + 6CO 2CO * C + CO,. The plating rate is proportional to the rate of evolution of CO from the decomposed carbonyl, i.e., it is proportional to the pressure of the gaseous decomposition products. Carbon released from CO gas is the significant constituent for the variability of the physical properties of the product. High carbon deposition is favored by increasing pressure. Limitations are imposed in the selection of plating temperature and pressure. Excessive temperature re-

Jan 1, 1956

By R. E. Miner, J. K. Jackson, D. F. Gibbons

Internal-friction measurements were made during isothermal aging treatments of 18 pct Ni maraging-steel wires between 420° and 612°C. A sharp initial drop in the internal-friction level was interpreted in terms of a rapid dislocation recovery reaction. The rate of the recovery was found to be independent of temperature. Truncation of the recovery reaction was apparent in those systems that exhibited the rapid age-hardening characteristics of the maraging steels. It is proposed that this initial hardening response is the result of a low activation energy preprecipitation reaction involving molybdenum. A gradual rise in the internal-friction level at longer aging times was associated with the precipitation of a molybdenum-containing precipitate. CONSIDERABLE research effort has recently been devoted to the mechanisms responsible for the high strength and toughness of 18 pct Ni maraging steels. These bcc martensitic alloys are found to harden during aging at temperatures between 400° and 600°C. The aging response is very rapid with more than half the total hardness increase occurring within the first few minutes of aging, Fig. 1. Precipitate particles have been observed in the later stages of aging by a number of investigators.&apos;-&apos; While the identity of the precipitates remains the subject of some controversy, one or more of the intermetallic compounds, Ni3Mo, Ni3Ti, and Fe2Mo, are almost certainly involved. Heterogeneous nucleation of precipitates at dislocations has been noted8 and cobalt is believed to enhance the formation of fine, homogeneously distributed particles by lowering the solubility of the alloying elements in the martensitic matrix.3,7 Transmission electron microscopy studies of the initial hardening behavior have not been fruitful. Strengthening mechanisms based on atomic ordering have not been generally supported by X-ray and neutron-diffraction experiments.9 In the present investigation, the aging reaction was studied using isothermal-aging internal-friction measurements. The marked sensitivity of internal friction to short-range diffusion and precipitation processes has provided a convenient tool for the elucidation of the strengthening mechanisms operative in the maraging steels. EXPERIMENTAL PROCEDURE An upright torsion pendulum was used to measure the internal friction of several maraging steels during isothermal aging. The pendulum was placed in an atmosphere of helium at a pressure slightly less than atmospheric. To permit measurement of internal friction during the first minutes of aging, the specimens were rapidly heated by passing a current through them in a manner similar to that described by Ang and Wert.10 Thermal gradients in the specimen were largely eliminated by using specially designed specimen grips11 which produced temperature variations of less than 1 pct over 90 pct of the specimen length and less than 3 pct over the entire length at aging temperatures up to 620°C. A proportioning strip-chart program controller was employed to maintain constant specimen temperature during treatments of up to 36 hr duration. A number of vacuum-melted laboratory heats having compositions near that of a typical commercial 18Ni-7Co-5Mo-0.4Ti alloy were investigated. The amount of cobalt was varied from 0 to 7 wt pct in five of the heats. Either molybdenum or titanium was omitted in the remaining two heats. The alloy desig-

Jan 1, 1967

By E. O. Wagner, V. F. Parry

This paper summarizes investigations during 1949 on three pilot plants for drying low-rank fine coal by entrainment in hot gases. Detailed operating results on processing seven coals having moisture ranging from 24 to 62 pct, formulas and data for calculating performance of large units, and general conclusions on the problem of drying fine coal are presented.

Jan 9, 1950

By Terry E. Perkins, Len Marnewecke

Installation of a relatively simple, low-cost analog mill control system at Amax Lead Co. of Missouri&apos;s Buick concentrator has paid off handsomely. The system, which provides the capability of handling mill circuit upsets and ore changes while maintaining a desired particle size, is expected to generate annually a return on investment of several times its capital cost. In addition, the system stresses simplicity of field instrumentation and control strategy, leading to better operator acceptance and understanding, and its capital cost makes it very attractive for the specific installation when compared to more complex schemes using mass flow measurement and computers for calculating circulating load to infer particle size. This system has the advantage of utilizing an actual measurement for control, rather than a difficult-to-maintain inferred value.

Jan 2, 1978

By Chester Washburne

LEASING the Teapot dome to the Mammoth Oil Co. is the culminating anticlimax of the "conserva-tion movement." It is just the touch required to make a full fiasco of the whole affair. If the revered wielder of the "Big Stick" were still with us, we could hear it fall harder than it did on Ballinger. Of all the oil reserves set aside by presidential decree, there was only one which certainly could con-serve much oil for the future. This was Naval Reserve No. 3, on the Teapot dome, Wyoming. After secret negotiations, carefully guarded from the press and from the knowledge of other oil men, we are suddenly informed that this last and only known chance to save much oil for future naval needs has been given away for early development.

Jan 6, 1922

By John W. Tieman

Research on processes to remove sulfur oxides from flue gas has been in progress for many years. Pioneers in this field were the British who, in the early 1930&apos;s, installed a full-scale flue gas scrubbing unit on a 120 MW boiler using alkaline water from a Thames estuary plus chalk. Since that time, various methods have been studied by many investigators. Federal laws covering air pollution started with the 1955 Air Pollution Control Act. With the advent of the Air Quality Act of 1967, and subsequent publishing of criteria and available technology for control of sulfur oxides in January 1969, the clamor for information on commercially available control techniques to remove sulfur from fossil fuels has rapidly increased.

Jan 8, 1972

By S. G. Malghan

Steel consumption forms a significant part of the operating cost of a minerals processing plant. An estimated 250 kt (276, 000 tons) of steel in the US and over 500 kt (551, 000 tons) worldwide are consumed each year in wet grinding alone. The depletion of ore grades and the need for finer grinding of abrasive ores are expected to increase steel consumption even more. Through continued research and development by the mining industry and the suppliers of steel products, several methods to reduce steel consumption have evolved. This paper critically reviews the mechanisms involved in steel wear and the currently available methods, materials. and operating conditions for reducing steel consumption. Particular attention is given to liner design modifications and substitution of rubber liners for steel liners.

Jan 1, 1983

By D. J. Crouse, W. D. Arnold

The potential behavior of radionuclides released in an underground nuclear detonation to fracture copper ore for subsequent in-situ leaching and copper recovery was studied with regard to contamination of the copper product and hazards to operating personnel. The laboratory test results indicate that only small fractions of the radioactive fission products would be dissolved on leaching the ore. Tritium (as tritiated water) would be the dominant radionuclide in the circulating leach liquor, assuming use of a fusion explosive. The test results showed solvent extraction to have important advantages over cementation for recovering copper from the leach liquors. While the radioactivity of the copper metal product produced by either method should be extremely low, the solvent extraction process provides a more effective separation of copper from the radioactive contaminants and entails fewer radiation protection problems. For these reasons it is the preferred process.

Jan 1, 1976

By J. P. Morgan, J. R. Dawson

A review of Jones & Laughlin&apos;s Vesta coal preparation plant flowsheet in 1959 indicated that, of the three sizes making up the company&apos;s metallurgical product, the -48-mesh fraction offered the greatest potential for improvement. Efforts to improve quality and yield were directed toward the use of froth flotation. After laboratory and plant tests were completed, it was decided that treatment of the entire -@-mesh fraction of the coal mix by flotation was a significant step forward in providing better coal quality and recovery. Reduction of ash in the metallurgical coal from 6.75 to 6.25% provided material savings at the coal washer, coke plant and blast furnace. The Vesta preparation plant of the Jones & Laughlin Steel Corp. is located on the Monongahela River, eight miles south of Brownsville, Pa. This plant is capable of cleaning 2400 tph of a mixture of Pittsburgh seam high volatile coals from the Vesta and Shannopin mines to produce a metallurgical coal of 6.75% ash and a steam coal containing 14% ash. Heavy media vessels are utilized to upgrade the coarse coal while launders and tables handle the -1/4-in. fraction of the raw coal feed. Cleaned -1/4-in. coal goes to boot classifiers where the 48 mesh material settles and is removed by bucket elevators. This 1/4x48 mesh material is then sent to centrifugal dryers for dewatering. As designed, the -48 mesh fraction overflows the boot as a 7 to 8% solids slurry and is recovered by cyclones and a thickener and then dewatered by filtration. The products of the heavy media circuit, the launder-table-boot-dryer circuit and the cyclone-thickener-filter circuit, are combined to constitute the shipped metallurgical coal. The Vesta-Shannopin mix is combined at Jones & Laughlin&apos;s Pittsburgh and Aliquippa Works with purchased low and medium volatile coals for the production of metallurgical coke. A review of the preparation plant flowsheet in 1959 indicated that of the three sizes making up the metallurgical product, the -48-mesh fraction, containing 16.7% ash, offered the greatest potential for improvement of coal quality. This fraction was considered low, averaging 55%, while the rejects averaged only 33% ash. It was evident that while the boot overflow fraction represented only 6% of the product mix, a reduction in ash to 6 or 7% would reduce the ash of the metallurgical coal by 0.5%. The original plant flowsheet handling the boot overflow (Fig. 1) consisted of ten 14-in. cyclones treating 70% of the overflow and producing a 48x150-mesh underflow and a -150-mesh overflow. The cyclone overflow was combined with the remaining 30% of the boot overflow to constitute the feed to a 150-ft thickener. The cyclone underflow and the 48x325-mesh thickener underflow were fed to vacuum disk filters for dewatering prior to combination with the coarse metallurgical coal. The thickener overflow stream containing the -325-mesh material was split, 40% being recycled directly to the plant water system and 60% being flocculated and clarified in an 85-ft thickener. The underflow of this thickener was pumped to waste. Efforts to improve quality and yield on the -48-mesh coal were directed toward the use of froth flotation early in the investigation. A review of the fine coal flowsheet indicated that three streams should be considered for treatment by froth flotation. These were the -325-mesh thickener overflow, the -150-mesh cyclone overflow and the -48-mesh boot overflow. Flotation of the thickener overflow was considered basically to improve recovery by upgrading the reject stream so that it could be fed to the filters along with the thickener and cyclone underflows. The overflow from the thickener contained 3.7% solids and had an ash analysis of 33%. Flotation of the cyclone overflow and boot overflow were considered to upgrade coal quality as well as yield. Treatment of the cyclone overflow, a 5.4% solids slurry averaging 27% ash, would eliminate the coal thickener and provide a feed of flotation concentrate and cyclone underflow to the filters. Treatment of the boot overflow would eliminate both the cyclones and thickener and feed only flotation concentrates to the filters. Flotation feed in this

Jan 1, 1962

By G. W. P. Rengstorff, H. B. Goodwin

A method is described for purifying iron in batches of 150 Ib or more. Oxygen, carbon, nitrogen, and sulphur are removed from flakes of electrolytic iron by treatment in wet and then dry hydrogen. A special consumable-electrode arc furnace is used to remove hydrogen and to melt the flakes into ingots. A LTHOUGH iron and steel have been made and used for hundreds of years, there are still wide gaps in the knowledge of these metals. One reason for this is that the true properties of the base metal, iron, are not well known, simply because really pure iron has never been readily available for research purposes. Commercial iron, and even the "pure" irons which are readily available, are really complex alloys of iron with oxygen, nitrogen, hydrogen, carbon, sulphur, silicon, and other elements. With such materials, it has not been possible to prepare steels and other iron-base alloys in which all elements are present in exactly controlled amounts. It is an almost impossible task to determine the separate effects of each element or the intereffects of several elements unless alloys can be prepared containing only the desired elements. The ability to make controlled alloys of low impurity content is of far more than academic interest. It will assist in the study of such practical problems as the brittle failure of ship hulls or high pressure gas pipelines, determination of the factors which affect the deep-drawing properties of steels, the improvement of magnetic and electrical properties, the phenomenon of aging, and many others. In 1949, the American Iron and Steel Institute asked Battelle Memorial Institute to prepare high purity iron on a larger scale than had been attempted up to that time. The work was directed toward the preparation of iron as low as possible in carbon, oxygen, nitrogen, hydrogen, and sulphur because these are the contaminating elements of major interest in many research investigations on iron-base alloys. The initial goal was to prepare iron with not more than a few thousandths of one percent of each of these impurities. The purpose was to set up a "bank" of high purity iron on which researchers could draw when a supply was needed and which could be replenished from time to time as the stock became depleted. Of several possible purification methods, heating in hydrogen was selected as the most promising for the removal of both carbon and oxygen from solid iron. Metallic impurities are not removed by hydrogen. Electrolytic iron was chosen as a starting material because it is the most readily available form of iron low in metallic impurities. Decarburization and desulphurization were obtained by annealing in wet hydrogen at relatively low temperatures. The optimum temperature, as found by previous investigators,&apos; is about 1400°F. This treatment also removes nitrogen. Deoxidation is favored by dry hydrogen and higher temperature. There is evidence from previous work that an anneal at 2200°F in dry hydrogen will deoxidize the iron, reduce the nitrogen content, and reduce the sulphur content. These facts suggested the use of a two-stage process: treatment in wet hydrogen followed by treatment in dry hydrogen. To carry out the purification process in a reasonable time, it was necessary that the iron be in thin pieces. Flakes of electrolytic iron were used. Because most research requires that the iron be in massive form, it was nccessary to melt the purified iron to consolidate it into large pieces. For this work, it was decided to prepare ingots weighing at least 15 lb by using a cold hearth arc-melting process in which the iron was melted in an inert atmosphere of argon or helium. This method of melting was selected because the water-cooled copper crucible is not wet by the iron and does not contaminate it as a refractory crucible would. Because the crucible is also the ingot mold, contamination from mold materials was also eliminated. Contamination from electrodes was avoided by making them from purified electrolytic iron. The melting procedure finally developed was an adaptation of the Kellogg electric ingot process.&apos; Two batches of purified iron weighing about 100 Ib each in ingot form were prepared with analyses as shown in Table I. The remainder of this paper describes the procedures in more detail. In general, the process con-

Jan 1, 1956

By G. L. F. Powell, L. M. Hogan

Large degrees of undercooling have been produced in bulk samples, 400 g, of copper and Cu-O alloys by melting in a slag of commercial soda-lime glass. The maximum degrees of undercooling obtained for copper, hypoeutectic and hypereutectic Cu-O alloy samples were 208°, 218°, and 97°C, respectively. No grain refinement as a function of undercooling was observed for the pure copper samples although in Cu-O alloys there was a marked decrease in grain size at degrees of undercooling greater than 150°C. The grain size change is the result of recrystallization during or immediately following the freezing process. THE first report of a large degree of undercooling in a bulk sample of metal was that by Bardenheuer and Bleckmann1 who produced 258°C undercooling in a 150-g sample of iron by melting in a glass slag. Garbeck2 extended this technique to nickel, cobalt, and copper and reported maximum undercoolings of 220°, 230°, and 60°C, respectively, while Fehling and schei13 undercooled a large number of metals as 2 to 20-g samples slagged in glass. Subsequently, one of the authors4 applied the glass slag technique to bulk samples, -500 g, of silver and obtained a maximum undercooling of 250°C. It was concluded that impurities which normally catalyze nucleation at small degrees of undercooling could be removed by oxidation and solution in a glass slag. Large undercooling of bulk samples of iron, nickel, cobalt, and their alloys has also been reported by other authors.8&apos;10&apos;11 Of the five metals mentioned above, copper was the only one which had not been undercooled by at least 200°C in the form of a large bulk sample. Since copper exhibits high liquid solubility for oxygen, as do iron, nickel, cobalt, and silver, it was considered that a much larger degree of undercooling than that observed by Garbeck for copper should be possible. This was obtained by modification of the technique applied previously to silver and the results of undercooling experiments with 400-g samples of copper form part of this paper. The undercooling behavior of Cu-O alloys was also studied, and the influence of a small oxygen content on the grain structure of undercooled copper was observed metallographically. 1) EXPERIMENTAL The copper was obtained as oxygen-free high-conductivity copper, the major impurities of which were Fe 0.01 pct, Zn 0.015 pct, and Si 0.02 pct. Melting was carried out in an open-ended vertical cylindrical fur- nace wound with Kanthal wire. A schematic diagram of the experimental setup is shown in Fig. 1. The undercooling technique previously used for silver4 involved preoxidation of the samples by melting the silver in contact with the atmosphere. The oxygen content was subsequently reduced by freezing the samples under a glass slag, whereby the oxygen was evolved as gas and the continuous glass cover over the surface prevented re-solution of oxygen when the sample was remelted. Since oxygen is not released as gas when a Cu-O alloy is frozen. the technique had to be modified for use with copper. Also, copper is oxidized during fire refining so that an in situ preoxidation treatment of the samples was not considered to be a prerequisite to large undercooling. Experimentation proved that this supposition was correct. Instead, it was found that care was necessary during melting of the copper under glass to minimize oxygen pickup. Samples of copper weighing 400 g were prepared by adding 50-g pieces of copper to a vitreous silica crucible partly filled with soda lime glass at a temperature of approximately 1000°C. Each piece was quickly immersed in the glass slag and held at this temperature until the oxide coating on the surface decomposed. This change was easily observed and coincided with the formation of gas bubbles in the glass

Jan 1, 1969

By P. J. Root, J. E. Warren

An idealized model has been developed for the purpose of studying the characteristic behavior of a permeable medium which contains regions which contribute significantly to the pore volume of the system but contribute negligibly to the flow capacity; e.g., a naturally fractured or vugular reservoir. Unsteady-state flow in this model reservoir has been investigated analytically. The pressure build-up performance has been examined in some detail; and, a technique for analyzing the build-up data to evaluate the desired parameters has been suggested. The use of this approach in the interpretation of field data has been discussed. As a result of this study, the following general conclusions can be drawn: 1. Two parameters are sufficient to characterize the deviation of the behavior of a medium with "double porositym from that of a homogeneously porous medium. 2. These parameters can be evaluated by the proper analysis of pressure build-up data obtained from adequately designed tests. 3. Since the build-up curve associated with this type of porous system is similar to that obtained from a stratified reservoir, an unambiguous interpretation is not possible without additional information. 4. Differencing methods which utilize pressure data from the final stages of a build-up test should be used with extreme caution. INTRODUCTION In order to plan a sound exploitation program or a successful secondary-recovery project, sufficient reliable information concerning the nature of the reservoir-fluid system must be available. Since it is evident that an adequate description of the reservoir rock is necessary if this condition is to be fulfilled, the present investigation was undertaken for the purpose of improving the fluid-flow characterization, based on normally available data, of a particular porous medium. DISCUSSION OF THE PROBLEM For many years it was widely assumed that, for the purpose of making engineering studies, two param- eters were sufficient to describe the single-phase flow properties of a producing formation, i.e., the absolute permeability and the effective porosity. It later became evident that the concept of directional permeability was of more than academic interest; consequently, the degree of permeability anisotropy and the orientation of the principal axes of permeability were accepted as basic parameters governing reservoir performance. 1,2 More recently, 3-6 it was recognized that at least one additional parameter was required to depict the behavior of a porous system containing regions which contributed significantly to the pore volume but contributed negligibly to the flow capacity. Microscopically, these regions could be "dead-end" or "storage" pores or, macroscopi-cally, they could be discrete volumes of low-permeability matrix rock combined with natural fissures in a reservoir. It is obvious that some provision for the inclusion of all the indicated parameters, as well as their spatial variations, must be made if a truly useful, conceptual model of a reservoir is to be developed. A dichotomy of the internal voids of reservoir rocks has been suggested.7,8 These two classes of porosity can be described as follows: a. Primary porosity is intergranular and controlled by deposition and lithification. It is highly interconnected and usually can be correlated with permeability since it is largely dependent on the geometry, size distribution and spatial distribution of the grains. The void systems of sands, sandstones and oolitic limestones are typical of this type. b. Secondary porosity is foramenular and is controlled by fracturing, jointing and/or solution in circulating water although it may be modified by infilling as a result of precipitation. It is not highly interconnected and usually cannot be correlated with permeability. Solution channels or vugular voids developed during weathering or burial in sedimentary basins are indigenous to carbonate rocks such as limestones or dolomites. Joints or fissures which occur in massive, extensive formations composed of shale, siltstone, schist, limestone or dolomite are generally vertical, and they are ascribed to tensional failure during mechanical deformation (the permeability associated with this type of void system is often anisotropic). Shrinkage cracks are the result

By J. S. Browning

The U.S. Bureau of Mines has been experimenting with flotation processes to separate the spodumene-beryl ores mined at Kings Mountain, N.C. The success to date as well as the present status of the process is discussed. Further experimentation is underway and studies will be made on the milling costs involved in the flotation process. The pegmatites of the Kings Mountain-Lincoln ton, N.C., area constitute the largest known domestic reserve of beryl and spodumene. The reserve is estimated to contain 90 million tons of pegmatic material with 1,280,000 tons of recoverable Li,O(lithia) as spodurnene.&apos; The pegmatites also contain 0.4 to 0.5 pct beryl disseminated throughout the orebodies. The pegmatites may contain a potential reserve of 240,-000 tons beryl, equivalent to approximately 34,000 tons of BeO. Different flotation methods for separating beryl from feldspar or quartz, or both, have been developed by various investigators.2-7 On the other hand, published information is limited on concentration of spodumene-beryl ores. As the response of beryl and spodumene to flotation is essentially the same, a successful separation of the two minerals depends upon use of a selective depressant or a selective collector for one of the minerals. Several years ago, the U.S. Bureau of Mines, recognizing the need for developing a large domestic supply of strategic beryl, undertook studies to develop improved methods of recovering this mineral. Because of the low beryl content of the pegmatites, economic production of the beryl entails its recovery as a byproduct of spodumene flotation. Thus, the development of procedures that would provide for maximum recoveries of the spodumene, as well as the beryl, was a primary objective of the studies. Tests were made on run-of-mine ore and spodumene flotation tailing from the Foote Mineral Co.&apos;s spodumene concentrator at Kings Mountain (Fig. 1). Pet-rographic analyses of the ore and flotation tailing are given in Table I. Detailed analyses and examinations of the ore and tailings revealed that the beryllium was present in the form of a low-alkali beryl. The crystals were small, rarely larger than 14-mesh diam, and were clear and colorless. About 10 pct of the Li20 content of the ore was present in the mica and feldspar components of the pegmatite. In some weathered ores the associated clays also contained small amounts of lithia. This is typical of pegmatites in the Kings Mountain area. LABORATORY TESTS In the past, a vigorous chemical treatment of the spodumene surfaces with acid or caustic soda has been considered essential for satisfactory selective flotation of the spodumene from the other minerals in pegmatites. Many tests were made during this investigation to determine if chemical treatment of the spodumene could be eliminated in favor of a reagent combination that would depress the other minerals while selectively floating the spodumene. A simple reagent combination and process was developed that gave better spodumene recovery and grade of concentrate than the more elaborate acid or caustic treatment methods previously used. The finely ground ore pulps were conditioned with either an ammonium, alkali, or alkaline earth lignin sulfonate and sodium fluoride, and the spodumene was floated and cleaned using oleic acid as the collector. The spodumene tailing was deslimed, conditioned with sulfuric acid and coco amine acetate, and floated to reject mica. The mica tailing was thickened and conditioned with hydrofluoric acid, then washed to remove the acid. The washed pulp was conditioned with sodium hydroxide for pH control, and the beryl was floated and cleaned with oleic acid as the collector. Table II summarizes the results of the laboratory test work. About 77 pct of the spodumene and 75 pct of the beryl were recovered from the pegmatitic material. The spodumene concentrate assayed 6.1 pct Li20 and 0.01 pct BeO, and the beryl product assayed 3.0 pct Li20 and 1.57 pct BeO. Similar results were ob-

Jan 1, 1961

By E. W. Greig

This paper is an account of exploration for bauxite in the Amazon Basin, Brazil, and particularly of the discovery, exploration and development of the Trombetas deposits by Alcan. A general report of the Trombetas Project has already been published in E/MJ(Anon. 1975) to which the reader is referred for details on ownership, infrastructure and construction as well as the proposal for mining and treating the bauxite. A regional account of bauxite in and around the Guyana Shield and the northern part of the Brazilian Shield is included to help explain the geology of the Trombetas deposits and their relation to other bauxites in northern South America. It is suggested that all these deposits formed during Tertiary time under similar geologic conditions.

Jan 1, 1979

By W. A. Tiller, S. O’Hara

Grain refinement in stirred melts has previously been shown to arise from dendrite segmentation. The present work discusses experiments capable of distinguishing between remelting and mechanical effects which result from fluid motion. Nucleation of still un-dercooled Sn-1 pct Pb melts with a single-crystal seed shows that the grain size of the resulting ingots decreases as the undercooling at nucleation increases up to about 1Z0C, then increases again for larger undercoolings. Pure melts exhibit little refinement as a result of nucleation at any undercooling up to 12°C. The presence of fluid motion gives rise to grain multiplication in pure melts, but the magnitude of this effect is partly obscured by solid-state pain growth. The results indicate that two grain-multiplication pvocesses can operate, one which involves dendrite remelt ing, and another associated with fluid motion. Small ingot experiments indicated that an equiaxed transition can be caused by fluid motion. THE presence of forced convection during recales-cence of undercooled Sn-1.3 pct Pb melts has been shown to give rise to extensive grain refinement during solidification of small ingots of this alloy.&apos;&apos;2 In Ref. 2, this refining was shown to result entirely from dendrite fragmentation and not from any nucleation mechanism. The purpose of the present work is to establish what processes lead to dendrite segmentation. Experiments were therefore carried out to determine the resulting structure of both pure tin and Sn-1 pct Pb melts, nucleated at various undercoolings by single-crystal seeds in the absence of forced or natural convection. By comparing the information obtained from these experiments with the results of Refs. 1 and 2, the effects of fluid motion on the ingot structure, and the details of the segmentation mechanisms, should become clear. The results of these experiments should also be helpful in understanding the solidification structures of larger ingots since natural convection, which is known to play an important role in determining ingot structure13 differs only in degree from the fluid-motion effects studied here. I) EXPERIMENTAL PROCEDURE The apparatus shown in Fig. 1 was constructed to permit controlled nucleation of stirred or unstirred supercooled melts using a seed oriented in the tin dendrite growth direction. Because the melts, in all cases, were capable of larger supercoolings than the one used in each experiment, the structure observed always resulted from a single nucleation event at the surface. The sequential procedure was as follows: Tin was melted under purified hydrogen and the oxide removed at a temperature of 450°C . Electromagnetic stirring was then used to clear the surface completely and during this time the guide tube was lowered underneath the melt surface. A pointed Czochralski-like crystal was then propagated from a specially prepared tin dendrite seed4 inside the guide tube while the temperature of the bulk melt was held just above the melting point, ensuring a perfectly clean seed which was epitaxial with the original dendrite. The dendrite and epitaxial seed, still in the guide tube, were withdrawn from the melt which, in turn, was undercooled to 2C° below the temperature at which the nucleation experiment was to be performed. The melt was held there for several minutes, both in stirred and in still-melt experiments. The temperature was next raised to the required value and the melt nucleated by the carrot seed inside the guide tube, the heater power being shut off just after nucleation. In experiments where quenching after nucleation was required, a high-density graphite crucible was used, but otherwise the procedure was as described above. The temperature gradient in the melt before nucleation was kept below 1C° per cm by carrying the experiment out just below the center of the heater shown in Fig. 1.

Jan 1, 1968

By John A. Church

IN May, 1878, I had the honor of presenting to the Institute, at the Chattanooga meeting, some observations upon the heat of the Comstock Lode, and since then the subject has attracted some attention and criticism, in the course of which, I have observed errors of apprehension which I beg leave to correct now. Mr. John Arthur Phillips discussed it before the Geological Society, his paper being printed in the Quarterly Journal for August, 1879.* His criticism is based upon that part of my paper in which I quote a number of analyses of the mine waters, to illustrate the fact that the heat does not come from the oxidation of pyrite. I pointed out that these waters contain only an insignificant proportion of sulphuric acid, and not enough to account for even one per cent. Of * A Contribution to the History of Mineral Veins. By J. Arthur Phillips, Esq., F.G.S. Quarterly Journal of the Geological Society for August, 1879.

Jan 1, 1880

By G. G. Waddell, T. J. Crocker, S. S. M. Chan

A successful engineering structural design often depends upon a thorough understanding of the material properties of the structure. It is no exception when designing a supporting system for stable underground openings. For this reason, studies were made in the deep mines of the Coeur d&apos;Alene mining district to obtain engineering properties of rocks and rock masses immediately surrounding underground openings. In this paper, data concerning laboratory tested physical properties of rocks and in-situ deformation behavior of rock masses from the Galena, Lucky Friday, and Silver Summit mines of the district are presented. Interpretations of the data so obtained and suggestions for the use of the results of the investigations as design criteria are also outlined.

Jan 1, 1973

By H. Sato, R. J. Lipp, I. Iwasaki, K. A. Smith

Selective desliming holds much promise for upgrading low-grade, finely disseminated iron ores that are not readily amenable to conventional flotation. The process is extremely sensitive to the presence of calcium and magnesium ions that are in process water or are released by constituent minerals. The effects of these two alkaline earth ions on quartz were compared through streaming potential measurements, flocculation and cationic flotation tests, abstraction tests and scanning electron microscope studies. Calcium ion, adsorbed as CaOH+, and magnesium ion, attached by heterocoagulation as Mg(OH)2 precipitate, were responsible for the flocculation of quartz suspension and for the depression in cationic flotation of silica in alkaline pulp solutions. Magnesium hydroxide coating could be removed, similarly to adsorbed calcium ion, by complexation with EDTA and polyphosphates.

Jan 1, 1980