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By A. P. Pipilen, M. Weintraub, W. F. Hosford, A. A. 230-000-000-006 Orning

In a study of the principal factors affecting the transport of coal-water mixtures through a centrifugal pump and a pipeline, the interrelation between solids concentration, velocity, and pressure drop was established for a minus 2-in. bituminous lump coal in concentrations up to 48% by weight. Optimum concentrations were found to exist for maximum capacity of a given pipeline and for minimum energy requirements per ton of coal. Coal size degradation by particle fracture took place in the pump; abrasion and attrition to form fines took place in both pump and line. A novel system of studying flow of solid-liquid mixtures in pipelines by the determination of relative sound intensities was developed. The hydraulic transport of minerals is in part an established art and in part a relatively new field of industrial technology. The established art developed especially where the mineral was under water, where water was used in hydraulic mining, or where large quantities of water had to be pumped from the mining site to expose the mineral. Power requirements and limited life of pumps and pipelines, under such conditions, were relatively unimportant. Examples may be found in dredging, and in hydraulic mining and transportation of phosphate rock.' In the design of a coal pipeline the most needed information relates to flow characteristics, power requirements, pressure drop, size degradation, and size segregation as a function of solids-water ratio and size distribution of the mineral. A considerable amount of information has become available concerning pressure drop and energy requirements.2'3 These topics were therefore not studied intensively. Coal degradation, however, has not been clearly delineated. Lammers and coworkers4 showed that coal may be severely degraded in size but did not distinguish between degradation produced in the pump and in the line. It is the primary purpose of this paper to outline techniques used to acquire some of the much needed design data. A full report of the investigation is to be published by the Bureau of Mines at a later date. APPARATUS AND PROCEDURE The apparatus for circulation tests (hereafter referred to as Type III tests) consisted essentially of a loop and a centrifugal solids handling pump, with attendant instrumentation, and coal weighing and feeding equipment. It also included an adequate water supply, as shown in Fig. 1. The selection of 6-in., schedule 40, carbon steel pipe was based on the top size of coal to be used. Assuming that the top size of coal should not exceed 1/3 the inside diameter of the pipe, a 6-in. pipe would accommodate 2-in. coal, a realistic size for transport from the mine face. An 872-ft loop was constructed first. Later a few tests were made with a lengthened circuit of 1361 ft by superimposing an additional loop on the original one. All bends used were of 3-ft radius. A noisemeter microphone, taped to the pipe at various points, but generally about 50 ft downstream of the pump, was used to sense segregation of the coal and the length of slugs of coal in water. To measure the stream velocity, radioactive sources were encapsulated in plastic cubes. The specific gravity of the blocks was adjusted to 1.3 and 1.8 to simulate low ash and high ash coal particles. Their passage through the pipeline was detected by a Geiger counter. Because the repeated circuits of the Type III tests did not permit coal degradation in the line to be distinguished from that produced by the pump, the two

Jan 1, 1964

DEVELOPMENT of a chemical process for the extraction of pure metals from mill concentrates or metal scrap has progressed beyond the pilot plant stage and may prove an important adjunct to present smelting and refining methods if initial commercial operations prove economically successful. Developed by the Chemical Construction Corp., the new process involves the treatment of oxide and sulphide ore concentrates by chemical methods, instead of the usual smelting and refining techniques. Several of the many applications are now scheduled for commercial use. Refiners using the new process will prepare ore concentrates by standard flotation methods, introduce the concentrate as a slurry into an autoclave along with water and an acid or ammonia. From the resulting leach solution, recovery of individual metals is made by use of suitable reducing agents. By varying conditions during treatment, different metals in the ore are produced separately as pure powders, which may be pressed into forms ready to market, or in the case of copper, extruded as rods or pipe. The reagents are generally recovered. By manipulating the variables during reduction, selective separation of nickel, and/or cobalt, and/or copper can be made simultaneously. The separation is a continuous operation. Low metal prices are not immediately in view because of the tremendous demand at this time. However, reduced metallurgical treatment costs will allow economical mining of orebodies with lower metal content, permitting increased production to meet demand. Although the practical horizon for use of the new process appears to be limitless, one factor may enter into its employment. Just how low grade a concentrate can be economically used is unknown. In addition, for present practical considerations, only metal below zinc in the electromotive series may be processed. Each commercial application requires specific technique adaptation and pilot-plant data for engineering design. A nickel-cobalt-copper process has been researched and piloted in collaboration with Sherritt Gordon Mines, Ltd., for the firm's Lynn Lake properties. In addition, processes were tailored for cobalt concentrates of Howe Sound Mining Co., and National Lead Co., in view of the urgent need for this specific metal. Major General William N. Porter, president of Chemical Construction, says of the new process, "piloting experience has shown that production cost, from ore concentrates to pure metals should be considerably below current costs." Other savings may be realized by cutting transportation and personnel costs, and by reducing the time lag between mining and pure metal from months to a matter of hours. First commercial use of the process will start sometime this summer. Chemico is slated to finish building a $2.5 million cobalt refinery for Howe Sound Mining near Salt Lake City. The plant is expected to raise world cobalt production by 40 pct. The plant will process 35 tons of 20 pct cobalt concentrates from Howe Sound's Blackbird mine near Cobalt, Idaho, daily. Yearly production is expected to reach 2000 tons of pure metal, about one half of U. S. consumption in 1950. Steps in the Howe Sound application of the process are: 1. Acid oxidation leach. 2. Filtration (residues thrown away are insoluble compounds-gangue, iron, arsenic). 3. Cementation (for Cu removal because Cu content is too low for recovery). 4. Reduction from ammoniacal solution. 5. Separation of Co and Ni as mixed metals (95 pct Co and 5 pct Ni). 6. Recovery of ammonium sulphate. Under construction at the Fredericktown, Mo., mine of National Lead is a $5 million refinery sched- [ ]

Jan 1, 1952

By N. S. Stoloff, R. G. Davies

The annealing behavior of a heavily cold-worked FeCo-V alloy has been studied at temperatures both above and below Tc, the critical temperature for ordering. It was found that re crystallization and grain growth can take place below Tc in the ordered state and that, in agreement with results for fcc alloys, order retards grain growth. The activation energy for pain growth is -55 kcal per mole in the disordered condition; it was not possible to assign a value to the activation energy for grain growth below Tc because the degree of order is changing rapidly over the temperature interval investigated. Precipitation of an fcc y phase was observed upon annealing the cold-worked alloy at temperatures of 675°C and below. SINCE it is known that diffusion constants are greatly affected by long-range order,' it is not unreasonable to anticipate that order will influence the diffusion-controlled phenomena of recrystallization and grain growth. In the course of a study of strain aging of ordering alloys around the composition Ni3Fe Vidoz, Lazarevic, and cahn2 noted that a disordered cold-worked alloy annealed at a temperature T1 just below Tc will order but not recrystallize; Tc is the critical temperature for order. The same alloy annealed at a temperature T2 just above Tc, or an alloy of different (nonordering) composition annealed at either T1 or T2, will recrystallize after equivalent amounts of cold work. Initially Selisskii and coworkers,3,4 who examined a series of cold-worked and annealed bcc Fe- Co alloys, reported that alloys forming the B2 FeCo super lattice could not be recrystallized below Tc. However in a later paper5 it was shown that FeCo ordered alloys could be recrystallized below Tc. Thus the first question to be answered by the present investigation was whether or not a heavily cold-worked Fe-Co-V alloy could be recrystallized below Tc. When it was found that the alloy would indeed re-crystallize below Tc, the influence of long-range order upon subsequent grain growth was studied. EXPERIMENTAL PROCEDURE The grain-growth measurements were made upon FeCo-2 pct V wire of 0.031 in. diam; the alloy was the same as that used in an earlier study of the mechanical properties of FeCO-v.6 The wire was produced by cold swageing and drawing a rod 0.125 in. diam that had been quenched into iced brine from 850°C to disorder the alloy; the initial grain size was 0.05 mm. Rates of grain browth were measured after isother-mally annealing the wire in the temperature range 675° to 825°C; T, is -720°C. Grain diameters were measured on the transverse cross section of the wires. The line-intercept method of determining the grain diameter was used; conventional light photomicrographs were taken when the grain size was greater than 10 . Carbon replicas were produced and examined in the electron microscope if the grain size was less than Dislocation configurations after recrystallization anneals were studied by electron transmission microscopy of foils produced by cold rolling a 0.125-in.-thick strip of the quenched material to 0.012 in. The foils, after heat treatments similar to the wire samples, were thinned by electropolishing in a chromic-

Jan 1, 1967

By R. H. Frazier, F. W. Boulger

THE performance of welded structures is closely associated with the ductile-to-brittle transition temperature of the steel from which they are made. A low transition temperature is desirable because it indicates that the steel is less likely to fail suddenly at low ambient temperatures. Structures such as bridges, ships, storage tanks, and pipelines are usually made from hot rolled semikilled steel. Changes in rolling practice or chemical composition appear to be the most practical methods for improving the toughness of such materials. This results from the fact that production is likely to be seriously curtailed if improvements were obtained by recourse to heat treatment or complete deoxidation. This paper discusses the effect of variations in carbon and manganese contents on the properties of semikilled steels. The transition temperature, a property to which considerable importance is attached, varies with specimen configuration, testing method, and criterion of performance. Both the Navy tear test' and the keyhole Charpy test were used in the investigation. According to the terms used by Vanderbeck and Gensamer,V he tear test was used to measure a fracture transition and the Charpy test to measure a ductility transition. In either case the specimens absorb considerably less breaking energy in tests below the transition temperature than in tests above the transition temperature. Decreasing the testing temperature of notched-bar specimens seems to be equivalent in its effect to increasing the severity of loading on fabricated structures. Therefore, structures built from steels exhibiting lower transition temperatures in laboratory tests are expected to be less susceptible to sudden brittle fractures in service. Consequently, changes in composition which lowered the transition temperature of the experimental steels were judged desirable. Materials and Methods The steels for this study were made in a laboratory induction furnace and rolled to 3/4 in. plate, using a finishing temperature of 1850°F. Precautions taken to insure reproducible melting and testing practices are discussed in detail elsewhere.' All tests were made on hot rolled steels. The analyses of the experimental steels are given in Table I. The list includes steels with manganese contents ranging from 0.21 to 1.46 pct, at each of five carbon levels. The phosphorus, silicon, sulphur, and nitrogen contents of the steels are reasonably constant. The tensile and notched-bar properties of the experimental steels are presented in Table 11. Both upper and lower yield points are listed, and all values are averages for duplicate specimens. Transition temperatures based on three criteria are given. The keyhole Charpy transition temperatures are the temperatures at which the energy-temperature curves based on averages of four specimens cross the 20 and 12 ft-lb levels. Both definitions of Charpy transition temperatures have been used by other investigators. Charpy tests were made at intervals of 10°F, using a pendulum with an available striking energy of 220 ft-lb and a velocity of 18.1 ft per sec. The specimens were oriented parallel to the rolling direction and notched normal to the surface of the plates. The tear test transition temperatures are based on the usual' criterion of the highest temperature at which at least one of four specimens exhibits brittle behavior. The dimensions of the tear test specimens are shown in Fig. 1. The specimen is loaded eccentrically in tension, with pin and shackle fixtures, through the large holes while submerged in a liquid bath at the proper temperature. A specimen developing a fracture area with less than 50 pct shear or ductile texture is classed as brittle. Tear tests were made at intervals of 10°F.

Jan 1, 1955

By L. G. Jones

An approximate method of calculation is developed in this paper which allows duplication of radial unsteady-state gas flow computer results where Darcy's law applies, such as those reported by Aronofsky and Jenkins and Bruce, Peaceman, Rachford, and Rice. Moreover, the new calculation method can be used to obtain results for radial unsteady-state gas flow obeying the quadratic flow law proposed by Duwez and Green. Means are discussed for predicting well behavior at single or superimposed flow rates in finite or infinite reservoirs, determining reservoir rock properties from well-test data, reproducing and interpreting back-pressure test data, and determining the radial extent and reserves of gas reservoirs from well-test data. Example calculations are presented for gas flow following both Darcy's law and the quadratic flow law. INTRODUCTION Since the publishing of U. S. Bureau of Mines Monograph 7,1 most gas-well testing methods have been based on the equation q = y (pl2 - pw2)a, where q = production rate, pl and pw, are formation pressure and sandface pressure, respectively, and y and a are constants to be obtained from test data. These methods, used for predicting both deliverability and "open-flow" capacity of gas wells, have been useful and accurate in many cases but unsatisfactory in others. Even at best, however, they do not supply information about the formation or lead to an understanding of nonsteady-state gas flow in porous media. Many theoretically based studies2-4 of gas flow obeying Darcy's law have been made.' Since the partial differential equations which result from combining Darcy's flow law with the continuity equation are nonlinear, most of the published research consists of either numerical solutions or analytical solutions for linear approximating equations. Such solutions have been of limited value in field work due to their unhandy form and their failure to correlate most field data. There is evidence5,6 which indicates that Darcy's law is inadequate to describe gas flow at some flow rates of practical interest. A quadratic flow law: which reduces to Darcy's law at low rates, is more successful in accounting for experimentally observed behavior. This flow law has been applied successfully to a few hypothetical reservoir cases in work which has recently been published.10 However, these numerical solutions of the equations involved have been successful only on a special analog computer. Routine applications to field cases would be awkward and have not been attempted. The present paper describes an approximate method for computing nonsteady-state gas flow solutions which has been completely successful in predicting the results for both Darcy flow and quadratic flow obtained by elaborate numerical methods. The new calculation method allows determination of the observable variables in gas-well testing at constant rates. It is similar to the scheme of using a succession of steady states suggested by Muskat7 in that it makes use of steady-state and material-balance equations. It also is similar to the work of Aronofsky and Jenkins2 in that the new method includes Aronofsky and Jenkins' stabilized flow equation as a special case. It improves upon both of these calculation schemes in that it accurately describes all portions of reservoir history and suggests means of determining reservoir rock properties from well-test data. This paper deals only with production from a reservoir, in which case the rate is defined as being negative. The reservoir studied here is a homogeneous, disk-shaped porous body of uniform thickness, with all boundaries sealed except the inner radial boundary of the well.

By F. W. Luersson

High carbon, low phosphorus steel can now be made from pig iron containing 0.7 pct P or more, in a commercial sized open hearth furnace. No external heat is required for refining, and steel produced is identical with basic open hearth steel. THE classical Thomas process, which requires liquid pig iron containing over 11/2 pct P, yields a product relatively high in phosphorzs and nitrogen. Unless large quantities of recarburizers are added to the refined steel, the product is low in carbon content. Thus, the Thomas process is not well suited to American raw materials, and its product is often not acceptable according to the standards set by American industry. The shortcomings of the Thomas process have long been recognized; with the advent of low cost oxygen, studies were initiated to develop pneumatic processes which would conceivably overcome the inherent objections to Thomas steelmaking. Several such modified basic pneumatic processes have been tested experimentally in commercial trials during the past decade. Probably the most widely publicized of these developments has been the oxygen converter process as practiced in Austrial,2 and in Canada.8 n this process, oxygen is substituted for air and introduced above the liquid bath in order to increase the heat available to the metallurgical system. This avoids the need for high phosphorus raw materials and gives a product low in nitrogen. In this process, the phosphorus content in the final product depends, to a considerable extent, on the total amount of that element in the burden. The rotary furnace4 which is now in commercial operation at Domnarvet Steelworks, Sweden, is producing low phosphorus steel from iron containing 1.8 to 2 pct P. One or more early slags are removed and by this means high carbon steels of open hearth quality can be produced. At this stage of development there is some question as to the applicability of the rotary process to large heats. Another development has been the use of oxygen in combination with either steam6 or carbon dioxide yn the basic bessemer, thus avoiding the introduction of nitrogen gas into the refining system and giving a product relatively low in nitrogen content. A double slag process has been used in Europe7 in conjunction with a regular Thomas converter, by means of which it is possible to obtain a phosphorus content in the product approaching that obtained in basic open hearth steels. The Turbo-Hearth process:' which uses the side blowing principle so as to produce low nitrogen steel from normal American pig irons, has been developed experimentally in this country. A process fitted to U. S. raw materials All of the preceding processes, with the exception of the rotary furnace, suffer from the common shortcoming that they cannot be adapted to the production of high-carbon, low-phosphorus steels unless large proportions of recarburizers are added. In 1947, a program was initiated by the Inland Steel Company1' to study an oxygen steelmaking process specifically designed to utilize the full range of phosphorus analyses encountered in American pig irons and to give finai products with phosphorus and nitrogen contents comparable to steel produced by the basic open hearth process. Some of the objectives of the proposed process are: 1) the process should be able to accommodate molten pig iron conta;rl;rrg up to 1 pct P., 2) sne process should be subject to close control of carbon analysis, 3) the process should be capable of producing high carbon

Jan 1, 1958

By M. P. Tixier, M. Gondouin, G. L. Simard

In the quantitative interpretation of the SP logs, the electrochemical component is generally taken equal to — K log Rm /Rw where K has the theoretical value corresponding to solutions of pure sodium chloride. This method may be misleading when relatively large quantities of salts other than NaCl are present in form-rrtion waters—as is generally the case for low salinities —or in gyp-base muds. In such cases recourse is made in the field to changing the K value or to adding a correction term to the equation on the basis of local experience. An investigation has been made in the laboratory of the influence of HCO3, SO4=, Ca++, and Mg++ on the amplitude of the SP deflection, which included in par-ricular determinations of the activity coefficients of Ca++ and Mg++. The theory, the experimental techniques and a tentative method for applying the results are described. So far, applications to actual field cases where chemical analyses of waters were available have provided an excellent confirmation of the proposed method. The case of the SP in very salty brines is also considered and it is shown that the use of activity data for sodium gives satisfactory results. HISTORICAL In early times of electrical logging, the SP curve was used exclusively as a tool for the location of permeable beds and the definition of their boundaries. Later, with the introduction of methods of quantitative analysis, attention was called to the possibility of deriving from the SP log some information on the formation water resistivity, which constitutes one essential element for the computation of water saturation from log data. The first laboratory experiments' in 1932 had shown that, as a result of electrochemical phenomena arising at the contact of the niud and the formation, the amplitude of the deflection of the SP curve was, at least partly, a function of the salt concentration of interstitial water and accordingly of its resistivity. It was indicated that the amplitude of the electrochemical component of the SP should be equal to K log R1/R2, R1 and R2 being the resistivities of the mud and of the formation water respectively. However, the exact value of the K coefficient was not determined at that time because the surface clay used for a laboratory model was far from an ideal shale membrane. Consequently, the way was not yet open towards quantitative interpretation. In the early forties, Tixier reported2, on the basis of field log observations, the following equation for the case of NaCl solutions, SP = -71 log f1c1/f2c2, c1 and c2 being the concentrations and f1, f2 the mean activity coefficients. The local variations observed in the empirical values of K, chiefly in the Rocky Mountains, led him to advance the opinion that, besides the relative amounts, the nature of the salts present in the solutions had a bearing on the magnitude of the SP. At about the same time Mounce and Rust- ad published laboratory results which emphasized the part played by the shale in the generation of the SP. On the basis of laboratory tests and theoretical considerations, Wyllie in 1948' published the following equation of the electrochemical SP for the case of NaCl solutions, SP= - 71 log (a1)m/(a2)m

Jan 1, 1958

By William R. Barton

Iron and steel slag represent man's most successful attempt to date to profitably utilize a solid waste. Its consumption represents a solution to a solid waste problem and also represents tonnage of natural aggregates that will not have to be mined with concomitant disturbance of the land. Slag has been produced as long as iron has been made; but until a little more than 50 years ago, it was mostly a waste product to be disposed of with as little effort and cost as possible. Huge piles of waste slag were generated over the years of iron and steelmaking. Sporadic use was found for small amounts starting with slag (from Catalan forges) used for road bases by the Roman Empire. The first recorded sustained commercial use was, as is often the case in man's history, for making war. Some profit- conscious munitions maker in the 16th century realized that he could make cannon balls of slag instead of the more precious iron. Other small-volume uses gradually developed: cast building blocks, slag-lime mortars and cements, slag wool, ballast, road base, and, finally, in concrete. But it was not until after World War II that the true potential of blast-furnace slag as a construction aggregate was really recognized. Now nearly all blast-furnace slag produced is used, and much of the earlier stock- piles in the U. S. have been reduced or entirely consumed. Steel slag for aggregate use has been in commerce for only the past 10 years, and use has increased rapidly (10-50% per year) during the past 5 years as blast-furnace slag supplies became depleted. However, much remains to be accomplished in determining character and optimum conditions of use for various types of steel slags before such slags will realize their full use potential. Although slag represents only 2% of construction aggregate materials used in the U.S., its production involves certain features that make its production record far more important than national tonnage figures would indicate. Its source is in iron and steel production and concomitantly slag availability is restricted to those areas where iron or steel is produced. In such areas, it often represents one of the principal aggregates marketed and, because of special properties that make slag a selected aggregate for certain uses, the tonnage imbalance may be overcome by the importance of its contribution to quality or special characteristics of end products. The location and number (Fig. 1) of slag plants handling this annual production is governed by the geographic makeup of the iron producing industry. Prior to the period marked by World War 11, most blast furnaces were in the Great Lakes area-Pittsburgh, Cleveland, Chicago, Gary, Buffalo, Detroit, Youngstown, and Toledo, with exceptions at Baltimore, Bethlehem, and Birmingham. Since that time, iron and steel facilities have been established in Texas, Utah, and California. Today 85 slag plants in 15 states provide employment for almost 2000 persons. The slag plants also recover almost 4 million tons of slag-encrusted iron each year for return to the blast furnaces. Much of the success in developing uses for slag can be attributed to the efforts of the National Slag Association founded in 1918. Since then, it has conducted numerous field and laboratory investigations to demonstrate the properties and uses for slag and slag products. These investigations have resulted in total recognition of blast-furnace slag as a construction material of consequence. The American Society for Testing & Materials Designation C125 recognizes blast-furnace slag as "the nonmetallic product consisting essentially of silicates and aluminosilicates of

Jan 1, 1975

By Ralph E. Esarey, Robert G. Reno

DriLLing activity and prospecting for oil and gas increascd in Indiana in 1941 over the previous year. The greater part of the drilling and development continued to centralize in the Indiana portion of the Interior Coal Basin, in the southwestern part of the state, but other parts of the state were not neglected. Many wildcat wells were drilled, including a series of core tests through the mantle of drift on the southern flank of the Michigan Basin. These core tests have been followed by several unsuccessful production tests. Production tests were made also along the axis of the Logansport-Kankakec branch of the Cincinnati Arch. In all, 411 field locations and 141 wildcat wells were completed in Indiana during 1941; that is, a total of 552 wells, an increase of 3 2 wells over the previous year. The field tests resulted in 260 oil wells, 57 gas wells, and 94 dry holes; wildcats included 16 oil wells, 3 gas wells and 122 dry holes. At the end of the year, 53 field wells and 34 wildcats were drilling. Gibson and Posey Counties led the state, with 154 and 155 wells drilled, respectively. However, 125 wells produced oil in Gibson County, while 98 produced oil in Posey County. Twenty-five per cent of all wells drilled were wildcat; II per cent of these produced oil and 5 per cent produced gas. Grifin field continued to lead in drilling activity, with 157 successful wells and 20 dry holes (including important wells defining the field). Production is found in five pay zones (Tar Springs, Waltersburg, Elwren, Aux Vases and McClosky). It produced a major part of Indiana's estimated 7,200,000 bbl. of oil during the year. Heusler field, Posey County, expanded with 11 oil ells and 4 dry holes in the Waltersburg and Tar Springs. Vienna field, Posey County, completed four oil producers in the Mansfield sandstone, between 1200 and 1250 ft. The College field, discovered late in 1940, received three oil producers and two dry holes in the Aux Vases. Two new fields were discovered in Posey County during the year: Lamott pool, in the Tar Springs, at 1950 ft., had initial production of 55 bbl. on discovery. One producer and one dry hole have been drilled since. Mt. Vernon pool found saturation in both the Waltersburg and Cypress formations. The discovery well tested about 1000 bbl. per day; it tested the McClosky at 2764 ft. Seven producers have been drilled since the October discovery. Welborne-Switch pool found oil in the Cypress sand at approximately 2500 ft., with an initial production of 33 bbl. One more well in the area proved a dry hole. Gibson County had the following discoveries in 1941: The Patoka field was opened by a McClosky producer of 300 bbl. Another producing well has been drilled. An attempt was made to extend the Illinois Mt. Carmel field into Gibson County, Ind., and one producer of 24 bbl, was completed on the Indiana side. A dry hole has since been drilled, one location south. One small well was completed in the Mans. field at 1105 ft. in sec. 31, T.2 S., R.12 W., Gibson County promising a new field

Jan 1, 1942

By T. L. Berger, M. C. lnman, M. F. Rose

AFTER shock loading, mechanical twinning has been observed by several authors1-4 for a variety of fcc metals and alloys. It has been shown2,3 that low stacking fault energy materials deform primarily by the formation of mechanical twins and stacking faults during dynamic loading. Further, Inman, Murr, and Rose2 have shown that a correlation exists between the average hardness and the volume percent of mechanically twinned material in stainless steel. It has been observed in nickel' that mechanical twins are produced during shock deformation if the peak pressure associated with the shock wave is greater than 350kbar. It is the purpose of this work to discuss shock-hardening mechanisms in nickel and to determine to what extent the initial condition influences the final response. The "flying plate technique" was used to generate planar shock waves with peak pressures as high as 710 kbar. The details of the technique5" have been discussed elsewhere and will not be repeated here. The material used in this study was polycrystalline nickel of 99.98 pct purity and had an initial grain size of 0.18 mm. Prior to any deformation, all samples were given a stress-relief anneal of 6 hr at 600°C in a vacuum furnace. After annealing, the initial condition of the samples was changed by cold rolling individual samples from 0 pct to a maximum of 80 pct reduction in thickness. This provided samples with controlled initial histories for shock deformation. Immediately after shock loading, the specimens were slowed and quenched by suitable arrangement of buffer material and water bath. This technique minimized specimen damage and the effects of shock heating on the samples. Since deformation twins in high stacking fault energy fcc metals are only produced at high stress levels, the initial defect configuration prior to mechanical twinning should greatly influence the number of twins formed. In fact, Zukas and Fowler7 have found that prestraining in iron and steel greatly suppresses the formation of mechanical twins during the shock deformation process. Following the methods of Warren and warekois8 and Cohen and Wagner,9 X-ray diffraction profile analysis was performed to determine the incidence of stacking faults and mechanical twins in the deformed nickel. Analysis was made on samples in the annealed, cold-rolled, shock-loaded, and cold-rolled—shock-loaded states. The estimated accuracy of the peak position measurements is *0.01 deg in 2?. Therefore the accuracy in the measurement of the relative peak shifts between the (400) and (222) diffraction line profiles is on the order of *0.04 deg in 2?. None of our measurements indicated peak shifts greater than 0.04 in 28. This would correspond to a fault density of -1 pct and sets the limit on the sensitivity of our instrument. Similarly, analysis of the shift in the center of gravity of the diffraction line profiles yields the minimum measurable value of the twin fault probabilitya to be -0.002. Fig. 1 shows mechanical twinning in nickel shock-loaded to 400 kbar. In this photograph, fault intersections are clearly visible. The thickness of the individual fault lamellae was determined from the image widths of their lines of intersections by the

Jan 1, 1968

By Robert G. Reno, Ralph E. Esarey

DriLLing activity and prospecting for oil and gas increascd in Indiana in 1941 over the previous year. The greater part of the drilling and development continued to centralize in the Indiana portion of the Interior Coal Basin, in the southwestern part of the state, but other parts of the state were not neglected. Many wildcat wells were drilled, including a series of core tests through the mantle of drift on the southern flank of the Michigan Basin. These core tests have been followed by several unsuccessful production tests. Production tests were made also along the axis of the Logansport-Kankakec branch of the Cincinnati Arch. In all, 411 field locations and 141 wildcat wells were completed in Indiana during 1941; that is, a total of 552 wells, an increase of 3 2 wells over the previous year. The field tests resulted in 260 oil wells, 57 gas wells, and 94 dry holes; wildcats included 16 oil wells, 3 gas wells and 122 dry holes. At the end of the year, 53 field wells and 34 wildcats were drilling. Gibson and Posey Counties led the state, with 154 and 155 wells drilled, respectively. However, 125 wells produced oil in Gibson County, while 98 produced oil in Posey County. Twenty-five per cent of all wells drilled were wildcat; II per cent of these produced oil and 5 per cent produced gas. Grifin field continued to lead in drilling activity, with 157 successful wells and 20 dry holes (including important wells defining the field). Production is found in five pay zones (Tar Springs, Waltersburg, Elwren, Aux Vases and McClosky). It produced a major part of Indiana's estimated 7,200,000 bbl. of oil during the year. Heusler field, Posey County, expanded with 11 oil ells and 4 dry holes in the Waltersburg and Tar Springs. Vienna field, Posey County, completed four oil producers in the Mansfield sandstone, between 1200 and 1250 ft. The College field, discovered late in 1940, received three oil producers and two dry holes in the Aux Vases. Two new fields were discovered in Posey County during the year: Lamott pool, in the Tar Springs, at 1950 ft., had initial production of 55 bbl. on discovery. One producer and one dry hole have been drilled since. Mt. Vernon pool found saturation in both the Waltersburg and Cypress formations. The discovery well tested about 1000 bbl. per day; it tested the McClosky at 2764 ft. Seven producers have been drilled since the October discovery. Welborne-Switch pool found oil in the Cypress sand at approximately 2500 ft., with an initial production of 33 bbl. One more well in the area proved a dry hole. Gibson County had the following discoveries in 1941: The Patoka field was opened by a McClosky producer of 300 bbl. Another producing well has been drilled. An attempt was made to extend the Illinois Mt. Carmel field into Gibson County, Ind., and one producer of 24 bbl, was completed on the Indiana side. A dry hole has since been drilled, one location south. One small well was completed in the Mans. field at 1105 ft. in sec. 31, T.2 S., R.12 W., Gibson County promising a new field

Jan 1, 1942

By A. L. Labbe, J. J. Donoso

Hard-won experience in the operation of smelting plants has pointed the way to the most efficient design and economical operation of a baghouse system for recovery of metallurgical fumes. This paper treats of the principles governing bag filtration and the factors most directly affecting bag life. Methods for temperature conditioning of smoke previous to filtering are described and the evolution of bag shaking mechanisms is brought up to date. THE history of the bag filter process, as applied to the recovery of metallurgical fumes, goes back to 1876, when the Lone Elms Works of Joplin, Missouri, erected a two-section baghouse for filtering fumes from Scotch Hearth lead smelting furnaces. By modern standards this installation was crude, but the basic operating principles remain essentially the same today. Great progress, however, has been made in the mechanization of the process by the use of devices for mechanically and automatically cleaning bags of adhering fumes, in the use of instruments for recording and controlling the variables affecting baghouse operation, and in the conditioning of the smoke previous to filtering. The principles governing bag filtration of fumes were investigated in 1929 by A. J. Seitz of American Smelting and Refining Co., and he arrived at the following conclusions: 1. Pressure on Bags at Constant Volume: The rate at which the pressure builds up in a bag with constant volume is directly proportional to the time, with the same kind of smoke and dust burden (fig. 1). 2. Pressure on Bags for Change in Volume: With equivalent smoke and dust burden, the bag pressure increases with the square of the increase in volume. The rapid increase in pressure is due to (1) increase in volume, (2) increase in amount of dust on the bag, and (3) more intense packing of the dust at higher velocity (fig. 2). 3. Effect of Intensive Filtering on Pressure: Since the pressure builds up directly as the square of the volume, with the same smoke and dust burden, it is necessary to shake the bags in that increased ratio, and vigorously, to keep the pores of the bag open and pressure down. This increases the wear on the bags and the dust losses. 4. Effect of Shaking on Dust Losses: The losses are in direct proportion to the frequency of shaking because the loss takes place immediately after shaking, before the bag seals itself. Tests show that with hand shaking the last 20 pct of the removable dust requires seven times more shaking per unit weight of dust than the first 80 pct. 5. Effect of Fineness of Dust on Losses: The fineness of the dust particle increases the loss in two ways: (1) When the bag is clean a greater percentage of it will pass through before the bag seals itself; (2) fine material penetrates farther into the bag pores, building up pressure faster and necessitating more shaking, thereby increasing the loss. The physical principle of operation of the bag filter is simply the separation of solids from a gaseous carrier through a porous medium, and is analogous to the filtration of solids from liquid carriers. Basically, the mechanics of the process are as follows: Fume-laden gases drawn from the operating fur-

Jan 1, 1951

By Renato G. Bautista, Theodore D. Tiemann

A kinetic study of the hydrogen reduction of taconite from the Wisconsin Gogebic range was made over the temperature range from 500° to 1000°C on eleven size fractions from 4 to 150 mesh. Two stages of reduction were observed, a rapid initial reaction followed by a slower reaction presumably taking place at an internal receding FexO-Fe interface. Calculated mean activation energies for the two reactions were 7800 and 14,600 cal per mole respectively. In recent years there has been an increased interest in the direct reduction of iron oxide ores to metallic iron by means of gaseous reducing agents such as hydrogen and carbon monoxide.1,2 These investigations have been motivated by the desire to develop a process that will by-pass the blast furnace in the production of steel. The majority of these processes have been developed to produce metallic iron by direct reduction from high-grade iron oxide ores.3"5 Very little work has been done on the low-grade siliceous iron oxide ores.6"8 The work reported here is directed principally towards the fundamental aspect of the reduction reactions of siliceous iron oxide ores, since the practical aspects of the gaseous reductant process were discussed previously. The ore used in the investigation was obtained originally from the United States Bureau of Mines10 trench sample of the Yale member of the Wisconsin Gogebic range iron formation. The Yale taconite has an average analysis of 28.2 pct Fe and approximately 50 pct SiO2. Chemically, these nonmagnetic taconites contain on the average about 53 pct silica and 30 pct Fe. An average analysis calculated fron the USBM10 figures for a composite of the five members (Norrie, Plymouth, Pence, Pabst, and ale) of the iron formation is given in Table I. Mineralogically, based on previous X-ray diffraction and other studies, the principal minerals are hematite (Fe2O3), geothite (Fe2O3.H2O), and quartz (SiO2). Minor amounts of iron containing silicates, siderite (FeCO3) and magnetite (FeO. Fe2O3) are present.10,11 The iron minerals and the quartz are finely disseminated requiring extremely fine grinding for liberation. For the experimental work, the ore sample was screened into a number of size fractions, the analyses and densities of which are given in Table II. EXPERIMENTAL PROCEDURE The reduction experiments were carried out in a 24 in. by 2 in. ID nichrome-wound vertical-tube furnace mounted on a stand. A 1 1/2 in. OD zirconium-oxide combustion tube was used inside the furnace to contain the atmosphere. To the top of this combustion tube was joined a pyrex ground-glass joint to which was attached a glass bulb with a small (1.0 mm) opening at the center, and with two outlets controlled with a stopcock on each side. A pyrex-glass joint with connections to three stopcock joints for introducing hydrogen, nitrogen, and mixtures of hydrogen and nitrogen gas was joined to the tapered bottom of the combustion tube. The sized ore fractions were contained in a 1 in. diameter by 1 1/2 in. 150-mesh nickel screen basket. The basket was suspended in the furnace from a balance by means of a supporting nickel wire which hung freely inside the combustion tube. The furnace temperature was controlled by a Leeds and Northrup Speedomax Type G controller, connected to a chromel-alumel thermocouple placed

Jan 1, 1962

By M. P. E. Desvaux, P. Charsley

OLIP-line observations on copper alloys, using the electron microscope, have been made by a number of workers,13 but this work has been confined to a brass. In a CuAl alloys Koppenaal4 and Koppenaal and Fine5 have made observations with the optical microscope and by the use of interferometry. They found that the observed slip step heights inside the Liiders bands accounted for only 42 pet of the total macroscopic strain. The suggestion was put forward that optically unresolvable slip in other parts of the specimen accounted for a major part of the macroscopic strain. This is surprising since it is known from other workers that slip in a brass is inhomogeneous; i.e., large amounts of slip occur on individual {lll) closelys paced than being shared by a large number of closely spaced planes. Furthermore, a brass and a CuAl alloys with high concentration of aluminum exhibit similar deformation characteristics and slip-line patterns. Prior to investigations into the behavior of copper and a CuAl alloys under reversed stresses in tension and compression, some preliminary experiments have yielded results which the authors think resolve this discrepancy, and throw some further light on the behavior of a CuAl in tension. An experiment was carried out on a 10 at. pet CuAl single crystal, of gage length 7.5 cm, diameter 3.1 mm, and orientation shown in Fig. 3 (inset), for the purpose of resolving the above discrepancy. The specimen gage length was electropolished for 10 min in a 50:50 orthophosphoric acid (SG=1.75)-distilled water system, with 2 v across the cell and a current density of 0.5 amp per sq cm. The cathode was made of copper. After a tensile strain of 0.067 ± 0.001, intense slip was observed over a length 2 cm of the gage length whilst the rest of the specimen was relatively undeformed. In the lightly deformed region, slip bands of mean width 20 /x were spaced about 1 mm apart on average. The transition from the heavily slipped region (usually called a Liiders band) to the lightly deformed region was gradual, the slip-band density increasing as the "Liiders band" was approached. In the latter, the slip bands became so close together that, to the naked eye, the specimen appeared to be continously slipped, and the typical microtopography of this region is shown in Fig. 1. Twelve electron micrographs were taken at random from replicas of the Liiders-band region, and the widths of the slip lines were measured. The slip lines account for an over-all tensile deformation of 7.0 ± 0.7 pet, after allowing for the lengths of the un-slipped regions, which is in good agreement with the macroscopic strain. The distribution of slip-line widths was also measured and is shown in Fig. 3. Since Koppenaal could not resolve slip lines with height less than 540A (limit of resolution represented by dashed line), then it was deduced that he could have measured only about 50 pet of the deformation within the 'Liiders Band'. It is concluded, contrary to the suggestion of Koppenaal,5 that virtually all the macroscopic strain is accommodated within the "Luders band" and that there is no need to invoke fine slip distributed uniformly over the gage length.

Jan 1, 1967

By O. A. E. Jackson

In all three principal dunite dikes, minute disseminated grains of pyrrhotite are to be seen in the fresh rock in amounts less than 1 pct. Traces of nickel have been reported from many such specimens. Nickeliferous pyrrhotite is the principal nickel-bearing mineral, although olivine contains very minor amounts of nickel in solid solution, substituting for magnesium and iron. Such occurences are of no economic significance. Nickel analyses of possible economic significance (up to 3 pct Ni) have been returned from samples taken near the margins of the two large western dunite dikes. These samples were from schistose zones along and within the dike walls. The mineralized shear zones, up to 30 ft wide, strike N 30 W and dip from 65" to 90" west. They consist of layers of hard, fresh, green-gray dunite, mineralized with finely disseminated pyrrhotite. These layers alternate with layers of soft, black, oxidized schistose dunite up to 1 ft wide, well mineralized with pyrrhotite and tabular-fractured pentlandite in crystals up to 1/4-in. diam. Sulfides identified in polished sections were chiefly pyrrhotite and pentlandite, with much smaller amounts of chalcopyrite. There are two varieties of pyrrhotite. One develops a fine polish and conforms to published descriptions. The other is slightly darker and browner, does not polish as well, and displays flamelike growth or intergrowth structure when etched with nitric acid fumes. Pyrrhotite and pentlandite crystallized contemporaneously in the form of veins in the olivine and as fillings of the interstices of euhedral olivine crystals. Chalcopyrite replaces the other sulfides. The most striking feature of the deposits is their occurrence in intimately fractured and schistose zones in the dunite where faulting has been localized along the contacts of the sediments and the dunite dikes. Though far too little detailed work has been done to be certain, there appears to be a higher concentration of sulfides in the shear zones along the margins of dike apophyses, sediment reentrants, and strike and dip irregularities. Much more study would be required in order to submit a plausible theory of formation of the nickel deposits, supported by laboratory and field evidence. Results of the present study, especially localization of the metals by fracturing, certainly indicate that the nickel concentrations were brought about by precipitation of nickel sulfides from fluids that used the fractures as a means of ingress. Studies of nickel sulfide deposits throughout the world have demonstrated that such sulfides were deposited at considerable depths and at temperatures of several hundred degrees. This would rule out the possibility of groundwater as the transporting medium. The two possible sources of hot nickel-bearing fluids are quartz diorite and gabbro. The first possibility is that large volumes of fluids, expelled from the quartz diorite magma during its crystallization, obtained a supply of nickel by altering the nickeliferous olivine of the dunites. The likelihood of this process is lessened by the recognition that, although the dunites show some alteration to serpentine, talc, and trem-olite, they are for the most part remarkably fresh outside the schistose zones. The worldwide association of nickel with basic rocks, together with the presence of pyrrhotite in thin films on joint planes of the gabbro on Jumbro Mountain, favors the gabbro source. The writer extends thanks to C. Phillips Purdy, Jr., project chief of American Metal Climax Inc., for giving him the opportunity to study these deposits. He is also indebted to the officers of American Metal Climax Inc. and Discovery Mines Inc. for permission to publish this article.

Jan 1, 1961

By M. D. Hassialis

[Surface Areas of Concentrates and Collector Coatings (T.P. 2002, by A. M. GAUDIN and G. S. PRELLER, Min. Tech., May. Discussion by M. D. HASSIALIS and the authors) . I Activation of Minerals and Adsorption of Collectors (T.P. 2082 by J. ROGERS and K. 1'. SUTHERLAND, Min. Tech., Nov. Discussion by A. F. TAGGART and the authors). . . . 3 Correlation between Mineral Behavior in Cataphoresis and in Flotation (T.P. 2005 by A. If. GAUDIN and S. C. SUN, Min. Tech., May. Discussion by M. D. HASSIALIS). . . . . . 8] Surface Areas of Concentrates and Collector Coatings M. D. HASSIALIS.*-In the current flotation theories there exists a common gap spanned by a common assumption pertaining to the arrangement and orientation of the collector ions at the solid surface. Also common is the belief that contact angle and flotation performance are dependent upon the arrangement and orientation of collector ions. This stimulating and informative paper sheds some light upon this general problem. One of the indices of arrangement is the area available per collector ion; in this connection, Gaudin and Preller have applied the B.E.T. method for surface determinations. In a surprising number of cases, their results show a greater specific surface for tailing than for concentrate. This cannot be accounted for by the differences in specific gravity and is attributed to the presence of clay minerals of "primary" sluices in the tailing. This is not a satisfactory explanation, for experience shows that when free slimed clay minerals are present in a flotation cell they will be carried mechanically into the concentrate. A part of the answer to the decreased specific surface of the concentrate would appear to be its usual flocculated condition, yet this should not entirely account for the large spreads reported. The possibility occurs that the nitrogen adsorption isotherms for clean mineral and collector-coated mineral are different. If that were true, and if the coated mineral surface exhibited decreased adsorptive powers, the discrepancy might vanish. In discussing the disposition of collector ions at mineral surfaces, the authors adopt the more consistent viewpoint that there exists some agreement between the ions of the substrate and those of the superstrate. In the case of xanthate ions on galena, a possible arrangement is shown in Fig. 2. This arrangement shows every xanthate ion being shared by two lead ions, whereas the chemical composition calls for two xanthate ions for each lead ion (p. g). This whole discussion is misleading. In the first place, it is known that xanthate ions are not abstracted by unoxidized galena, hence Fig. 2 should show as the substrate not Pbs but PbS„ Om. It would be equally erroneous to use the lattice arrangement of PGSO4, since the surface properties of xanthate-conditioned anglesite differ from those of xanthated galena. It is highly probable that the state of the galena surface exploited in its flotation is ephemeral, since weathered galena is only poorly, if at all, collected by xanthate. Just how a substrate of oxidized galena is to be pictured depends upon one's conception of the transformation from galena to anglesite. This writer is inclined to the following sequence of events. Surface sulphide ions undergo progressive oxidation. As more oxygen is taken up by the sulphide ions they become displaced from their equilibrium positions in the galena lattice, thus accommodating for the larger volume of the S„ Om ions. Concomittant with this change the forces acting on the lead ions

Jan 1, 1946

By D. Harker, E. Epremian

The constitution of the nickel-tungsten system has been studied by a number of investigators, the most recent of which are Ellinger and Sykes.1 On the basis of metallography, electrical resistivity and hardness measurements and some X ray diffraction work, they constructed a consitution diagram (Fig 1). Ellinger and Sykes report a0 for the alpha face-centered cubic phase (nickel saturated with tungsten) as 3.66?.‡ The gamma phase (tungsten saturated with nickel) is given as body-centered cubic, but no value of a. is recorded. At 43 pct tungsten by weight (approximately 20 at. pct) a beta phase is reported, but structure and lattice parameter are not known. Primarily on the basis of metallographic evidence, they conclude that beta is a new phase and rule out the possibility of formation of a superlattice since they- observe a new phase in the microstructure. Grube and Schlecht2 report an ordering reaction in a system similar to the Ni-W (Ni-Mo) and Harker3 has shown that NirMo forms a superlattice upon the pre-existing face-centered cubic lattice of the alpha phase. Elliniger arid Sykes observed a change in the diffraction pattern of a 4.3 pct W alloy upon aging and attributed it to the formation of a new phase. Thus, there appears to be some question as to the character of the beta phase reported by Ellinger and Sykes. The purpose of the present work is to determine precisely the structure and nature of the beta phase in the Ni-w system of X ray diffraction methods. Experimental Procedure One inch diameter ingots of 43.66 pct, 40.15 pct and 34.06 pct .tungsten by weight (19.8, 17.6 and 14.1 at. pct respectively) were melted and cast under vacuum from electrolytic nickel and pure wire filament grade tungsten. The ingots were soaked for 16 hr at 1300°C in a hydrogen atmosphere furnace, then swaged at this temperature and finally drawn to 0.020 in. diam wire. Some of the bar stock was retained in 1/2 in. diam rod for hardness and metallographic studies. Wire samples for diffraction work were sealed in evacuated quartz tubes and subjected to the various solution and aging heat treatments in a hydrogen furnace. X ray photograms were taken in a Debeye-Slierrer camera using copper K radiation filtered by nickel foil. Results X RAY DIFFRACTION The lattice parameters of the alpha and gamma phases at saturation were determined by an X ray photogram of the 19.8 at. pct W alloy after solution heat treatment at a temperature well within the alpha-gamma range above the peritectoid temperature (17 hr at 1150°C—oil quenched). The alpha phase was found to be face-centeted cubic with a. of 3.594 ± 0.001?, while the gamma phase was determined as body-centered cubic with a. of 3.158 ± 0.001?. Exactly the same phases and parameters were ohtained with the 17.6 at. pct W alloy for the same solution heat treatment. Thorough analysis was made of an X ray photogram of a 19.8 at. pct alloy sample in the quenched and aged condition (solution treated 1T hr at

Jan 1, 1950

By Joseph L. Gillson

BRAZIL has had an industry based on ocean beach deposits of heavy minerals containing monazite, zircon, rutile, and ilmenite for well over 40 years, but except at the very earliest period, prior to 1906, and again during World War 11, has this industry been at all comparable in size with similar operations in other countries. Limiting factors have been neither a lack of reserves nor lack of markets (except for zircon). Although poor local transportation and shipping facilities have handicapped the development in Brazil, these conditions were perhaps equally bad (when mining operations started) in the Indian State of Travancore, and in New South Wales and Queensland, Australia, in which states the principal production of beach deposits of heavy minerals has occurred. The outstanding restraints on the Brazilian industry have been the lower quality of the Brazilian minerals, the relative small size of individual deposits that were known until recently, the lack of interest of Brazilian investors in mining ventures, and the unfavorable climate for investment of foreign capital under Brazilian mining law. The lower quality of the minerals is indicated by the fact that the Brazilian monazite carries only 5 to 6 pct Tho2*, and the ilmenite 561/2 pct TiO2, whereas the corresponding Travancore minerals carry 9 pct Tho, and 60 pct TiO, respectively. The Brazilian zircon is a dirty brown color (which can be removed readily) as compared with the gleaming whiteness of the Australian zircon. An inadequate market for the abundant zircon that will be available in any operation in Brazil is certainly a heavy restraint, since otherwise it could be an important byproduct. The oxide of zirconia, baddeleyite, that has come from Brazil is from other sources.' Since the Brazilian beach sands carry only a little rutile, that mineral has not been available as a valuable byproduct to help finance the operations. Substantial tonnages of rutile have been exported from Brazil. The sources of this mineral are stream placers and residual deposits over gneisses in the States of Goyaz, Minas Geraes, Ceara, etc. (Leonardos,' and Chambers". With these handicaps, Brazilian production from beach sands has been marginal, and there has been only one consistent producer. This is a company, originally French, which was called Companie de Franco-BrazilliCne, but, with the downfall of France in 1940, became Brazilian under the name Monazita e Ilmenita do Brasil ("Mibra"). This company has operated several deposits in the vicinity of Guara-pary, in the State of Espirito Santo. Its office and plant has been at Guarapary. Recently a company called, "Fomil" (Fomento Monazita-Ilmenita) started operations. This company was organized by the Foote Mineral Co. of Philadelphia, and such share as a foreign company can hold under Brazilian law has now been acquired by the Lindsay Light and Chemical Co. of Chicago. When the writer went to Brazil in the fall of 1940, he found that no general survey of the beaches had been made except for a thorough study of part of the area by Abreu.4 The paper by Miranda6 had not then been written. The federal Geological Survey and Department of Mines knew only of the existence of the deposits in Espirito Santo south of Vitoria, and had a hazy idea that others might be found north of Vitoria. One deposit in Bala was known in Rio, but the larger one at Guaratiba was not known, although a Frenchman had prospected

Jan 1, 1951

By R. H. Hopkins, R. W. Kraft

X-ray and metallographic analysis reveal that the preferred cryslallograPhic relationships in direc-tionally solid~fied Pb-Sn eutectic specimens can be stated: interface growth direction, Experiments in which tin single-crystal seeds were used to nucleate the eutectic demonstrate that the normal lamellar structure observed at steady state can be forced to break down initially to a semide-generate structure when the crystallograPhic direction of the tin seed does not lie within the preferred eutectic interface plane. A normal structure eventually develops by preferred grain growth. X-ray topo-graphs and rocking curves substantiate that the perfection of eutectic samples increases as growth proceeds until steady-state conditions prevail. RECENT years have seen substantial progress made in the understanding of eutectic solidification through both intensive theoretical1'' and experimental investigations (see Ref. 7 for a review and extensive bibliography of both aspects). Several important observations concerning the nucleation and growth aspects of binary eutectic solidification have been brought to light. Briefly some of these include the nonrecipro-cal nucleation of one phase upon another,'j9 the tendency for a specific low-index direction of one or both phases of the eutectic to be aligned in the growth direction during unidirectional solidification,'0711 and the production of lamellar microstructures having a preferred interface plane between "11-13 phases. Questions quite naturally arise as to the mechanism by which preferred grain growth evolves during eutectic solidification and what relationships (if any) connect the initial nucleation of one phase upon another with the preferred growth directions and interface planes observed after a few centimeters of growth in many systems. This study was initiated in an attempt to answer these questions. An experiment was devised in which both the nucleation and growth steps in the crystallization of a binary eutectic, Pb-Sn, could be correlated with subsequently developed eutectic morphology and crystallography. This was accomplished by nucleating the eutectic upon a tin single crystal seed and then causing the eutectic to grow from the seed by directional freezing. The morphology of the structures produced in this manner was then monitored metallographically and the orientation relationships and substructural perfection determined by X-ray analysis. The information thus ob- tained was correlated to the growth history of the samples. EXPERIMENTAL DETAILS The eutectic of composition 38.1 wt pct Pb and 61.9 wt pct sn14 was prepared by accurately weighing lead and tin of 99.999+ (from ASARCO and Lytess Metals and Chemicals, respectively), melting in a clean Pyrex beaker under an argon blanket, and casting into the proper crucible for resolidification as described below. Tin seeds were grown by the method of ~halmers," saw-cut, oriented by the Laue method, and soldered to the pull rod of the Czochralski puller. All seeds were given a final electropolishing (to assure the removal of any deformed material from the cutting operation) and acetone degreasing immediately prior to the nucleation experiment in which they were to be used. Eutectic samples were unidirectionally solidified in a horizontal graphite boat1' or by pulling from the melt16 with tin (or graphite) seeds. A flowing argon atmosphere was employed in all experiments and growth rates and temperature gradients, constant for a given run, varied from 2 to 4 cm per hr and 8" to 15°C per cm over the course of all the experi-

Jan 1, 1969

By Joseph L. Gillson

BRAZIL has had an industry based on ocean beach deposits of heavy minerals containing monazite, zircon, rutile, and ilmenite for well over 40 years, but except at the very earliest period, prior to 1906, and again during World War 11, has this industry been at all comparable in size with similar operations in other countries. Limiting factors have been neither a lack of reserves nor lack of markets (except for zircon). Although poor local transportation and shipping facilities have handicapped the development in Brazil, these conditions were perhaps equally bad (when mining operations started) in the Indian State of Travancore, and in New South Wales and Queensland, Australia, in which states the principal production of beach deposits of heavy minerals has occurred. The outstanding restraints on the Brazilian industry have been the lower quality of the Brazilian minerals, the relative small size of individual deposits that were known until recently, the lack of interest of Brazilian investors in mining ventures, and the unfavorable climate for investment of foreign capital under Brazilian mining law. The lower quality of the minerals is indicated by the fact that the Brazilian monazite carries only 5 to 6 pct Tho2*, and the ilmenite 561/2 pct TiO2, whereas the corresponding Travancore minerals carry 9 pct Tho, and 60 pct TiO, respectively. The Brazilian zircon is a dirty brown color (which can be removed readily) as compared with the gleaming whiteness of the Australian zircon. An inadequate market for the abundant zircon that will be available in any operation in Brazil is certainly a heavy restraint, since otherwise it could be an important byproduct. The oxide of zirconia, baddeleyite, that has come from Brazil is from other sources.' Since the Brazilian beach sands carry only a little rutile, that mineral has not been available as a valuable byproduct to help finance the operations. Substantial tonnages of rutile have been exported from Brazil. The sources of this mineral are stream placers and residual deposits over gneisses in the States of Goyaz, Minas Geraes, Ceara, etc. (Leonardos,' and Chambers". With these handicaps, Brazilian production from beach sands has been marginal, and there has been only one consistent producer. This is a company, originally French, which was called Companie de Franco-BrazilliCne, but, with the downfall of France in 1940, became Brazilian under the name Monazita e Ilmenita do Brasil ("Mibra"). This company has operated several deposits in the vicinity of Guara-pary, in the State of Espirito Santo. Its office and plant has been at Guarapary. Recently a company called, "Fomil" (Fomento Monazita-Ilmenita) started operations. This company was organized by the Foote Mineral Co. of Philadelphia, and such share as a foreign company can hold under Brazilian law has now been acquired by the Lindsay Light and Chemical Co. of Chicago. When the writer went to Brazil in the fall of 1940, he found that no general survey of the beaches had been made except for a thorough study of part of the area by Abreu.4 The paper by Miranda6 had not then been written. The federal Geological Survey and Department of Mines knew only of the existence of the deposits in Espirito Santo south of Vitoria, and had a hazy idea that others might be found north of Vitoria. One deposit in Bala was known in Rio, but the larger one at Guaratiba was not known, although a Frenchman had prospected

Jan 1, 1951