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By R. B. Sudderth

The recovery of copper by various combinations of processes centered around liquid ion exchange has certainly been accepted as a technically superior entity when compared to the widely applied classical method of cementation. While the technical aspect of liquid ion exchange processes has received much attention and acclaim through actual operating data, in particular the ease of handling solutions, percentage recovery, reduction of pollution, etc., the corresponding economic data has either gone unpublished or has been held confidential. Much of this economic data has now been made available for publication; and with this data, we at General Mills Chemicals, Inc., will attempt to present an accurate economic analysis of some liquid ion exchange plants and an economic comparison between these plants and the typical cementation facility.

Jan 1, 1974

PROF. Henry Louis, Newcastle-on-Tyne, England (communication to the Secretary): I have read this paper with much pleasure. It presents a very accurate summary of a very interesting district. Like the authors, I was struck by the extreme General View, near French Co.'s Cyanide Works, Showing Horse-Whims, etc. flatness of this region, which looks strange to a gold-miner accustomed to other reef-districts. This prevailing absence_of relief in the contours is shown in Figs. 1 to 4, from photographs taken in August, 1897, some of which also show the horse-whims used here for hoisting. The flatness of contour is due, no doubt, to the fact that the rocks are similar in structure over large areas and are easily decomposed. I am quite at one with the authors in looking upon the so-called " placers " as the result of decom-

Jan 1, 1899

By M. B. Truehaft

Expectations for coal in the early to mid-1970s prompted the government and industry to pursue research and development programs to increase underground and surface mining coal Productivity and net coal recovery. Several programs concerned advanced surface mining methods for thin seam coal recovery. Three such programs, along with related areas of interest, presented in this paper are: extended depth augering for trench-strip applications; high recovery auger heads for enhanced recovery; and variable wall mining in low cover longwalls. Conceptual development is examined, prototype testing is discussed, and potential operations are considered.

Jan 1, 1985

By C. L. Baker

The district of Catoree, San Luis Potosi, ranks among the first half-dozen silver-producing camps of Mexico. Mining has been more or less continuous there for 150 years. The large producing mines, Mapnni, Mazapil, Palomas, Musquiz, Minas Viejas, now for the most part idle or abandoned, are grouped around the head of two valleys: one, which drains to the west, falls 2000 ft. (610 m.) in 41/2 mi. (7.2 km.) between the main Catorce and the western foot of the range and is characterized by steep canon walls; the other, east of the main town of Catoree from which it is separated by a high divide, heads in a number of steep tributaries above the basin in which lies the town of Potrero and flows nearly north for 10 mi. (16 km.) to the northern base of the range; below Potrero, it has for the most part gently sloping valley walls and a broad valley floor. The Sierra Catorce is the highest range of the region, the summits reaching altitudes of over 11,000 ft. With the exception of a few cliffs of the erosion escarpment of the lower limestone and the canon walls below the main town of Catoree, which is the highest town in Mexico, the gently rounded slopes are characteristic of a maturely eroded mountain range composed of folded sedimentary rocks. As is usual in desert regions, the heavy-bedded limestones are the most resistant to crosivc forces. Folded into anticlines, they form the mountain ranges; and the intermontane valleys and basins, originally carved out of less resistant shales, clays, marls and sandstone?, are covered by debris forming a mantle with surface gradually rising upwards toward the hills. In time, the debris buries, in deposits formed from their own ruins, all but the highest summits of the original mountains: some of this region has already nearly reached this stage. Most of the debris is firmly cemented by calcium carbonate (caliche). Solution of the limestone by meteoric waters afforded the supply of lime carbonate, which has been redeposited upon evaporation of the waters as a cement binding the boulders, pebblcs, and finer detritus. According to tradition, the higher portions of the Sierra Catoree were forested with pines and cedars but none remain within the mining district, although cedar is found farther south in the range. The vegeta-

Jan 1, 1922

By H. F. Gossenberger, J. J. Tietjen, J. J. Gannon, C. J. Nuese

External quantum efficiency measurements at 300" and 77°K are presented for vapor-grown GaAs and GaAs1-xPx electroluminescent diodes as a function of junction depth and doping. In GaAs, external efficiencies are found to decrease exponentially with increasing junction depth, defining an average absorption coefficient of 900 cm-1 at 300°K and 350 cm-1 at 77°Kfor epitaxial layers of p-type GaAs. It is shown that photon absorption losses dominate at room temperature and, in fact, account for most of the external efficiency degradation between 77° and 300°K. Healever, the internal ('junction) quantum efficiency is also found to decrease by a factor of 3.5 between 77" ALTHOUGH rapid progress has been made in recent years with GaAs, Gap, and their alloys for use in electroluminescent diodes, there are still important unknown factors related to the performance of these de- and 300°K. The dependence of GaAs efficiencies on donor and acceptor concentrations is presented, illustrating best efficiencies at donor concentrations of 1.5 to 2x 1018 cm-3 . External efficiencies are found to be independent of acceptor concentrations less than 3 x 1019 cm-3 but to degrade at higher doping. The fabrication of GaAsi-xPx electroluminescent diodes is briefly discussed. External efficiencies here for planar uncoated diodes are about 0.035 pct at 300°K and 0.4 pct at 77°for x = 0.42. A brightness of about 8500 ft-Lamberts is attained at 77°K and of 315 ft-Lamberts at 300° K. for curvent densities of 10 amp per sq cm. vices. For example, although the external efficiency is known to decrease by factors of typically 10 to 30 between 77°K and room temperature, the exact causes of this are still uncertain. Experimental results of ill' and carr2 with zinc-diffused electroluminescent diodes suggest that this external degradation is almost entirely due to increased absorption losses at room temperature, with a relatively temperature-independent internal efficiency; recent calculations by Gonda et al.3 corroborate this hypothesis. In contrast, Pilkuhn and Rupprecht4 find the internal efficiency of solution-grown GaAs laser diodes to degrade from 100 to 66 to 40 pct as the temperature is increased from

Jan 1, 1969

By John Birkinbine

Much has been contributed to the Transactions of the Institute concerning the construction and operation of American blast-furnares ; but the following compilation is offered as possibly furnishing additional information upon the general features, dimensions, locations, capacities, etc., of the blast-furnaces of the United States; while, incidentally, the ores upon which they rely are noted in a general way. The paper is presented chiefly as a compilation, and the figures given are selections from most reliable sources, or averages calculated from official statistics, placed for convenient reference, with a view of assisting those who consult the Transactions in determining the present relative merits and importance of various sections of the country. The scope of the paper has been restricted to as few topics as possible, and all the details of special plants, or notable outputs have been ignored. While every effort has been made to give correct figures and data, the changes which are constantly taking place in the iron-producing industry, will, undoubtedly, by the time the paper is in print, develop some errors. It is difficult to determine which of the blast-furnace plants of the country should or should not be considered as upon the active list. A number which have not been in operation for years are still reported as active, some of which will scarcely be put in blast again, and others are handicapped so that they can only operate in times of abnormal profits. It is therefore scarcely probable that there are over 600 blast-furnaces in the United States which can properly be considered as active; but so many considerations affect the various plants, that, it being impossible to determine the exact number, I have relied upon the annual reports presented to the American Iron and Steel Association. Concerning the number of plants which could be stricken from the list, the Secretary of this Association says: "In January last (1885) we enumerated 669 furnaces, which included many stacks which had not been in blast for a very long time, and others which could not be operated except during short periods of exceedingly high prices for pig iron. We have gone over this list very carefully and have eliminated 10 anthracite, 19 bituminous, vol. xiv.—36

Jan 1, 1886

By Ralph Hultgren, Prodyot Roy

Manganese vapor pressures from 1250° to 1500°K were measured by conventional Knudsen and torsion-effusion methods in twelve Fe-Mn alloys with compositions from 9 to 80 at. pct Mn. The Knudsen re-sults agveed approximately with previous measurements found in the literature which indicated the solutions were nearly ideal. However, except for the higher manganese compositions, the initial torsion readings indicated much (up to 50 pct) higher vapor presszcres than the Knudsen method. These high readings decreased steadily with time. The results are interpreted as due to depletion of surface concentration of manganese during evaporation. Thus the initial torsion readings are the most nearly correct and Knudsen methods on alloys are to be regarded with suspicion unless it can be demonstrated that diffusion rates are rapid enough to replenish surface concentrations depleted by evaporation. For the lowest manganese contents and highest temperatures, depletion causes initial torsion readings to be too low. FEW thermodynamic data are available for alloys of the high-melting transition metals due primarily to experimental difficulties at the high temperatures involved. Measurement of vapor pressure is one of the most promising techniques to be applied to this problem. From the vapor pressure of a component of an alloy phase, its activity or its partial molar Gibbs energy can be directly calculated. From measurements over a sufficient range of temperatures and compositions the partial and integral Gibbs energies, enthalpies, and entropies may be determined through Gibbs-Duhem integration. For solid phases of variable composition, which commonly are found in alloys, measured vapor pressures are low because of depletion of the surface concentration of the more volatile component as it is selectively vaporized. Diffusion from the interior tends to restore the depleted concentration. The seriousness of the effect depends on the relative rates of diffusion and vaporization. Although depletion has been recognized as a factor,' direct measurements of its rate are lacking and quantitative estimates of its effect on measurements are uncertain. In the present work the vapor pressures above a series of Fe-Mn alloys have been measured by the torsion-effusion method. This method permits a measurement of the vapor pressure of manganese as soon as the sample comes to temperature and continuously throughout the run. The rate of decline of the apparent vapor pressure measures the rate of depletion and the torsion reading at zero time should be correct. At high manganese concentrations (70 and 80 at. pct Mn), the torsion reading remained nearly constant; surface depletion was negligible. There was a slow drop in measured pressure due to bulk loss of manganese from the sample. However, for lower manganese contents, especially at high temperatures, the depletion effect was considerable and the apparent vapor pressure decreased steadily with time. For these alloys the Knudsen method should give pressures which are too low. The measurement of pressure in the Knudsen method cannot be made until enough manganese has been vaporized to be weighable. The Knudsen result is therefore an integrated average between the initial and final vapor pressures. To verify this, conventional Knudsen measurements were also made with results in approximate agreement with previously published Knudsen measurements for these alloys. As expected, for the lower manganese contents the initial torsion readings of pressure were as much as 50 pct higher than the Knudsen. THE APPARATUS The apparatus, shown in Fig. 1, is capable of operating to temperatures up to 2000°K. A vacuum of 5 x 10"6 mm Hg can be maintained. Temperatures were measured to +3° by a W-Re thermocouple placed in the dummy cell, N. The torsion cell consisted of two alumina crucibles with holes in their covers. They were placed in the molybdenum holder shown suspended from the torsion wire. Rectangular torsion wires (1 by 4 mm) were found to have superior sensitivity and less residual distortion than circular (2-mm-diameter) wires. The precision of angular measurement was found to be *0.025 deg; the variation is no doubt due to temperature fluctuation and vibration. For the Knudsen experiments the alumina cell was set on the support, N. SAMPLE PREPARATION 800-g samples were prepared by melting together electrolytic iron and electrolytic manganese and pouring the melt into a water-cooled copper mold. Melting and pouring were done under a helium at-

Jan 1, 1965

By A. H. Miller

TEMPERATURE considerations are of prime importance in the manufacture of steel products-front the time the metal is produced in the melting furnace, where the chemical reactions have a direct dependence on the temperatures of the bath, to the final machining of work on which the expansion due to the rise in temperature of the forgings during machining must be allowed for. Methods employed and difficulties encountered in some of the more important steps are here outlined. These methods are the result of years of experience, with many methods of temperature determination, and have been successful in routine works practice in the manufacture of high-quality steels. In the operations of melting, forging, and heat treatment, if the product is to be of the best quality each operation must be carefully followed through. A high-quality product cannot be obtained even with the best heat treatment if the steel is poorly melted, and, conversely, the best steel ever made may he spoiled by inefficient heat treatment. To perform the best work in any of these operations, temperatures must be accurately regulated.

Jan 8, 1919

By I. D. Shah

A roasting procedure for synthetic copper sulfide which results in a reproducible transient melting at 450° and 470°C is described in this paper. Possible causes for this melting phenomenon are suggested, and also a procedure to avoid it during the roasting. This melting is believed to be responsible for the occasional occurrence of stickiness in the commercial roasting of copper sulfide concentrate. Many workers have studied the roasting of copper sulfides, but only Lewis et al. have reported that fusion and, in some cases, fusion with "boiling" occurred in the neighborhood of 450°C. The DTA and TGA apparatus, the materials used in this investigation, and the discussion of chemical reactions occurring during the CuS roasting are described in an earlier publication. CuS, in the form of either pellet or powder, was heated at 280° to 330°C in a flowing air or 30% 02: 70% N2 atmosphere. Heating was continued at this temperature until no further weight increase due to sulfates formation was observed on the TGA thermogram. This is believed to be due to the inability of SO, to diffuse out from the sulfate layer on the surface of the pellet, thus halting the sulfate-forming reactions. Hereafter, the sample oxidized in this manner will be referred to as "partially oxidized CuS." X-ray analysis and microscopic examination of a polished cross section of a partially oxidized CuS pellet showed the following order of layers starting from the center of the pellet: Cu2S, Cu2O, CuO • CUSO4, and CuSO4. A bare thermocouple inserted in the center of a partially oxidized CuS pellet (2.5 g) did not indicate any noticeable change in the temperature of the pellet when melted at 450° to 470°C in an inert or oxidizing atmosphere. During the preparation of a partially oxidized pellet, the temperature of a CuS pellet increased by 50°C due to the exothermic formation of sulfates in air at 320°C. The endothermic peak associated with the melting phenomenon at 450°C is shown in [Fig. 1.] A CuS pellet (0.2 g) was oxidized in flowing air (150 cc per min) at 10°C per min up to 320°C and held there for about 2 hr. Then, N2 replaced air and heating was continued up to 500°C. The exothermic peak at 320°C represents an overall formation of sulfates, and an endothermic peak at 450° to 470°C represents the melting phenomenon. To observe the melting visually, a small (50 mg), partially oxidized CuS pellet was heated (in static air) in a hot-stage microscope. The melting phenomenon was observed on an auxiliary TV screen. The sample

Jan 1, 1976

By F. B. Sherman, Keros Cartwright

Sanitary land filling has become one of the most widely used methods of disposing of solid refuse. A principal concern of regulatory agencies and the public itself is that landfill operations do not degrade the physical environment, including water resources, and the ground-water reservoir in particular. Knowledge of ground-water and engineering geology can guide landfill operations into suitable terranes or develop measures to compensate for natural limitations at a particular site. Experience and research in Illinois suggest four activities relating to landfill disposal that warrant attention by geologists and engineers: (1) regional delineation of favorable and unfavorable hydrogeologic conditions to facilitate planning and preliminary screening of potential landfill sites; (2) site evaluations, with considerations of geologic materials, topography, water levels, flow systems, and local occurrence and use of water resources; (3) research on aspects of the hydrogeologic environment that control effects of, or are modified by, landfills; and (4) formulation of practices in the siting, construction, and operation of landfills that prevent, mitigate, or isolate deleterious effects. The first two activities are basically in the domain of earth science, requiring the application of fundamental concepts of geology and hydrology and conventional site-exploration methods. The third activity, research, requires contributions from geology as well as other disciplines, including soil physics, sanitary engineering, and chemistry. The fourth calls for policy decisions by regulatory agencies and elected officials, using the contributions of scientists and engineers. Throughout history, man has disposed of unwanted materials by dumping. As urbanization has increased, haphazard dumping practices have given way to disposal under more controlled conditions because of increasing congestion of population and production of waste and greater concern for public health and environmental amenities. Many states and communities have already outlawed open dumping and open burning of refuse. The only practical methods of disposal of large volumes of refuse, therefore, are contained, high-temperature incineration, or burial in a sanitary landfill. In Illinois, regulation of solid waste disposal has been delegated to the Environmental Protection Agency. Each session of the legislature since 1965 has passed increasingly strict laws regulating waste diposal. As a result, the work of evaluating sanitary landfill sites has increased significantly for both the Department of Public Health, now the Environmental Protection Agency, and the Illinois State Geological Survey, which advises the Agency on matters of ground-water geology and pollution. In fact, our ground-water staff spends as much time on studies relating to waste disposal, primarily sanitary landfills, as on ground-water resource studies. Many other geological agencies are experiencing similar demands for increased assistance in solving waste-disposal problems. This paper summarizes some of the salient features of the sanitary landfill concept, describes activities of the Illinois Geological Survey in ground-water and engineering geology relating to landfills, and suggests policies that need consideration. A sanitary landfill is located and operated in such a way that vermin and pests, nuisances, and degradation of air and water are kept at acceptable levels. Some of the physical requirements of a sanitary landfill are all-weather roads for year-round access, fences to retain blowing paper, a daily cover of at least six inches of suitable earth material, and a final cover of at least 2 ft of earth material. Dumping into or adjacent to standing water generally is not allowed. Two common operating techniques are used. In the first, trenches are dug, the refuse is placed in them, and the earth removed from the trenches is used to cover the waste. In the second method, area fill, refuse is placed in low ground and covered with earth from adjacent high areas. The hydrology of the site is a prime consideration in locating sanitary landfills. Putrescible refuse, if saturated above field capacity, produces a leachate that usually has a high concentration of dissolved solids.2 As the leachate also acts as an agent for transporting bacterial pollutants, it constitutes a potential pollution hazard. To reduce the production of leachates, the topography of the landfill area should be such that surface water will not flow into or through the fill. Operations that will result in refuse disposal below or near the highest known water-table elevation may be required to take corrective or preventive measures to protect the ground water. In practice, under humid conditions such as prevail in Illinois, locations where disposal can take place above the water table are relatively few because surficial materials are commonly fine-grained, which permits slow gravity drainage and results in high degrees of saturation (100% moisture content) near the surface. At some sites, although disposal has taken place above the water table, ground-water mounds have developed, resulting in permanent saturation of the refuse. Permeability barriers usually are required to protect the ground-water reservoir from degradation by leachates. The convention in Illinois is to have a minimum of

Jan 1, 1972

By C. R. Hayward

THE CHAIRMAN (ALBERT SAUVEUR, Boston, Mass.).-I am sure we are indebted to Prof: Hayward for his addition to our knowledge of the influence of sulphur on steel. As he has said in this paper, sulphur has had many defenders in recent years. It seems to me, however, that, while it may be old school to believe in the detrimental action of sulphur, it is not yet old school to believe in segregation; that while it may be that 0.1 per cent. of sulphur has no very great effect on the physical properties of steel, a ladle analysis of 0.1 per cent. of sulphur may readily result in 0.2 or 0.3 per cent. sulphur being present in the segregated portion of the ingot, and that, it seems to me, might be a rather serious matter. J. S. UNGER, Pittsburgh, Pa.-Prof. Hayward has presented the results of an investigation along a line to which I have devoted considerable time and attention, and I am particularly pleased to note that his results are in accord with my own and further tend to prove the fact that the old, established prejudice against sulphur is based more on belief than actual facts. I have felt for years that tooo much stress was placed on the harmful influence of certain elements in steel such as sulphur, phosphorus, copper, etc., but it has only been within recent years that efforts have been made to, establish the truth. Practically all the investigations made to date have proven that these elements within reasonable limits are harmless and, in fact, that for certain purposes the addition of these elements is beneficial. In referring to copper, J. E. Stead, Vice-President of the British Iron and Steel Institute, said at their last meeting: "Even today one comes across steel specifications in which copper is barred, which can only be regarded as ail indication of ignorance, if not stupidity, of those who prescribe the composition of steel, for it has been long ago proved that copper in steel, instead of being an evil, is quite harmless, and is sometimes distinctly beneficial." Sulphur owes its evil name to the early days of the manufacture of steel. Chemical analyses were crude, and failure due to either poor raw materials or metallurgical treatment were many. Sulphur being a comparatively easy element to determine with reasonable accuracy, particular attention was called to the amount of sulphur, and the failure was attributed to it, without giving any consideration to other causes. A pre-

Jan 4, 1917

By J. L. Jernegan

IN this paper I propose to give a short and, I must confess, a rather incomplete description, as regards many details, of the process used in Chicago, Ill., for smelting the argentiferous ores of the far West, and shall confine myself in this description, principally, to the process used at the Chicago Silver Smelting and Refining Company's Works, known as the Balbach process, as all the other smelting works in that city follow the same method, with the exception of one, which has the Cordurié, process for the desilverization of argentiferous lead. In all, there are five silver smelting and refining works in and near the city of Chicago. The Chicago Silver Smelting and Refining Company's Works are situated at the little station of South Lynne, about seven miles south from Chicago. The plant at these works consists of one horizontal steam-engine, principally used for running the ore pulverizer, four reverberatory smelting-furnaces, connected by horizontal flues with a common chimney 85 feet high, three lead-softening furnaces, one so-called zinc or mixing furnace, one separating furnace or liquation hearth, one lead-refining furnace, three zinc distillation retorts, one English cupellation furnace, supplied with blast by a No. 3 Sturtevant blower, which is run by a small steam-engine having a vertical tubular boiler, and an assay office, in which there are two wind-furnaces of the ordinary construction, and also a small muffle furnace. The assay office is supplied with all the necessary apparatus and reagents for fire assaying. There are also a superintendent's office, various store-rooms for coke and charcoal, and for the preparation of fire-clay, etc. Recently a small slag hearth (Krummofen) with one tuyere, has been put up for the purpose of working over such slags as assay too high in silver and lead to be thrown away, of which there are large amounts. The principal ore worked while I was in the employ of the company was that of the well known Emma mine in Utah, and also small quantities of Colorado ore. The character of the Emma ore is well known to most members of the Institute. In consists principally of ferruginous mixtures of carbonate and oxide of lead, oxide

Jan 1, 1874

By R. H. B. Jones

THIS paper reviews pertinent geology of the Biwabik iron formation, Mesabi Range, Minnesota. This iron formation is divisible into four members. Each member is distinctive and contains marker horizons, which are recognizable throughout all phases of alteration from lean, fresh rock to high-grade iron ore. Some beds have a larger magnetite content than others. During the process of ore genesis, which is essentially an oxidation process, the magnetite content is lowered. Alteration from iron formation to ore includes both oxidation of iron minerals and silica removal by leaching and these distinct processes progress at variable rates for different locations and structures. Magnetic intensities, of each horizon of the iron formation are dependent chiefly upon its preoxidation magnetite content, upon the subsequent degree of oxidation, upon the character of the enclosing rocks, and on the extent of fracturing, folding, or faulting. The results of a number of magnetic surveys are described and are correlated with results of drill-hole and mine exploration and development. The magnetic anomalies obtained are discussed in relation to phases of formation of ore within the iron formation.

Jan 1, 1946

By Earle E. Schumacher, W. C. Ellis

For the purpose of developing combinations of higher strength and conductivity than are obtainable by heat treatment alone in the age-hardening copper alloys, an investigation has been made of the effects of combinations of heat treatment and strain hardening on the properties in question. The investigation was limited to a study of the alloys containing nickel and silicon; nickel, silicon and cadmium; and cobalt and silicon. The experiments made in the course of the study arc described in this paper in three groups: 1. The effect of hard drawing subsequent to heat trcatment on the mechanical and electrical properties of the alloys. 2. The effect of low-temperature aging on the properties of heat-treat,ed and hard-drawn alloys. 3. The effect of strain on the rate of aging of quenched nickel-silicon-copper alloys. Preparation and Compositions or the Alloys The alloys were prepared by melting cathode copper in an electric resistance furnace and adding sufficient of the hardening elements to bring the compositions to the desired values. The purities of the hardening elements were as high as could be obtained in commercial practice. The metals were what are designated in the trade as electrolytic nickel, cobalt rondelles, commercial stick cadmium and fused silicon. The alloys

Jan 1, 1931

By R. L. Curfman

From January 1, 1965 through July 5, 1970, the very difficult potash ore body of Texasgulf Inc. near Moab, Utah was mined by conventional methods. The mine was gassy, the temperature was high and structural conditions precluded a satisfactory or economical extraction ratio due to the undulating configuration of the ore horizon. In 1966, 67, and 68, alternative mining methods were considered, among which was solution mining of the ore body. Cost studies indicated that the use of crystallizers to evaporate the large amounts of water attendant to solution mining offered no chance of economic success. In 1969 additional testwork and cost studies were carried out utilizing solar evaporation. These studies showed economic potential and justified additional investigation. As a result of these studies, Texasgulf now gathers potash solids from these solar evaporation ponds, (Fig. l), after pumping them from the underground mine as brine. The investigations were concentrated in four basic areas : (1) area evaporation rates and crystal growth habits; (2) underground solution tests including heat transfer rates; (3) accelerated evaporation tests to provide material for metallurgical testing, and (4) tests of evaporation pond lining materials and application techniques, along with area surveys to ascertain if sufficient earth was available in the near vicinity to con-

Jan 1, 1974

By R. Scot Clark

The reactively sputtered silicon dioxide capacitor -was developed for use in the monolithic integrated circuit, thereby requiring the capacitor to be fabricated on an oxidized silicon slice. The silicon dioxide film is formed by reactively sputtering silicon in a 50 pct Ar-50 pct 0, atmosphere and the physical properties are indistinguishable from silica. A practical upper limit of capacitance per unit area of 0.25 pf per sq mil is reached with the capacitors fabricated from the Si0, film. Methods shown to enhance this value are double stacking the thin-film capacitors and addition of aluminum to the silicon cathode during sputtering to form an aluminosilicate dielectric. A major contribution to the field of diffused integrated circuits would be the addition of auxiliary passive devices for replacement of diffused passive devices which are currently being fabricated for many integrated circuits. This accomplishment would increase the flexibility of the diffusion process in order to concentrate more on transistor parameters rather than on fabricating diffused resistors and capacitors. To pursue this technique, a thin-film SiOz capacitor was developed which has _ proven applicable to many integrated circuits. Although the SiOl capacitor has an application, the major deterrent from extending the integrated circuit into many useful areas such as low-frequency linear application is the low dielectric constant of SiO, and the low usable capacitance in an integrated circuit. This paper will cover the sputtering techniques used for forming the SiO, film, the physical and electrical properties of sputtered SiO,, and yield information concerning the application of these capacitors to integrated circuits. REACTIVE SPUTTERING Reactive sputtering is simply the sputtering of a metal or semiconductor in glow discharge in the presence of a reactive gas. The material to be sputtered is seen in Fig. 1 as the cathode of the system and is bombarded with positively charged ions of the ambient gas. In this investigation, the ambient gas is composed of 50 pct Ar and 50 pct O2 at a pressure of approximately 2.5 X l0-' Torr. The ions are accelerated toward the cathode in the cathode dark space by the electric field and upon striking the cathode effect a momentum energy transfer to the surface atoms. The transferred energy is sufficient to dislodge a surface atom or atoms and these particles diffuse through the glow discharge to the collector or anode. Several mechanisms of oxidation in the reaction chamber can be considered during reactive sputtering. 1) The surface of the cathode is oxidized and the oxide is subsequently sputtered. 2) Oxidation and sputtering occur simultaneously. 3) Sputtering of the cathode material is followed

Jan 1, 1965

By William Loblowitz

A simplified system of flotation testing has been developed recently at the Bureau of Mineral Research of Rutgers University. The technique involves the known principle of skin flotation and can be used with minute quantities of sample and reagents in a beaker. A vessel containing the conditioned sample with added water and flotation reagents is held inclined and rotated slowly. Water-repellent particles come in contact with air and float on the surface of the liquid, while wettable particles are submerged. The float is poured off and filtered whereas the nonfloat remains in the beaker. The filtrate may be returned to repeat the process. This procedure can be made quantitative. Separations are obtained and are remarkably complete and repeatable. The effect of different reagents, optimum quantities, pH and other variables can be determined in a fraction of the time required for conventional testing. However, the method gives no information on the effect of frothers and the quality of froth to be expected in a cell, and it is not practical for particles finer than 200-mesh. Unlike other preliminary tests, separate float and nonfloat products are obtained, and their contents can be determined quantitatively by chemical analysis or grain counts. After the optimum reagent combination has been determined, the effect of fines and frothing may be verified in the conventional flotation cell. On the other hand, agglomeration-tabling can be directly duplicated from beaker tests. Procedure: Five to ten grams of sample are weighed into a 100-ml beaker. Flotation reagents and a small initial quantity of water are stirred together; additional water is then added to produce the proper water-solids ratio. The beaker is then tilted to 45" and rotated slowly. After three to five rotations, liquid and float are poured off and filtered; the filtrate may be recycled until the separation is completed. One test generally requires less than 10 min. Reagent concentration and pH remain quite constant because of the recycling of the filtrate. Two to four tests may be made simultaneously, and the effect of varied conditions may be observed by comparison. Considerable time is saved in preparation and handling since small quantities of sample suffice for a series of systematic tests. Repeatability One test was repeated four times under constant conditions. The sample used was a quartz sand containing approximately 24 pct feldspar and some clay aggregates. The +28-mesh grains had been screened out, and most of those finer than 100-mesh had been removed by hydraulic classification. The results are presented in Table I. For comparison, 500 g of the sample were separated by agglomeration-tabling using the same reagent combination and quantities as given in Table I. The weight percent float was 18.3 pct, composed almost entirely of feldspar and with only traces of quartz. Most of the remaining feldspar was recovered in a middling product with 2.2 pct by weight.

Jan 1, 1952

By R. F. Campell, W. L. Jensen

IT is not uncommon for martensitic high carbon steels having a coarse austenite grain size to exhibit microcracks when polished and etched and examined with a microscope, as described by Davenport, Roff, and Bain.' Whether such cracks exist before etching or are the result of acid attack during etching has been debated from time to time. Fig. 1 illustrates the effect of electrolytic polishing, mechanical polishing and etching subsequent to each polish on microcracks produced by oil quenching from 1800°F a steel containing 1.14 pct C, 0.23 pct Mn, 0.33 pct Si, and 0.45 pct Mo. The austenite grain size was 3-4 on the ASTM scale. Grinding on lead laps followed by either electrolytic polishing with acetic anhydride-perchloric acid solution' or mechanical polishing with Linde "B" alumina on "microcloth" (sometimes referred to as Gamal cloth) revealed microcracks without conventional etching, as shown in Fig. la and b, respectively. These same fields, after subsequent etching with saturated picral, are shown in Fig. lc and d, and the cracks are seen to be typical microcracks; moreover, the cracks appear to be broader and longer than before etching. Although the microcracks were revealed by electrolytic polishing alone, the possibility of acid attack was present; however, the mechanical polish was accomplished without any intermediate etching to remove disturbed metal, hence this is regarded as definite evidence that microcracks are present before etching.

Jan 1, 1954

By M. I. Sherman, J. D. H. Strickland

PRELIMINARY experiments in these laboratories showed that whereas pyrite1 produced only sul-fate the action of aqueous chlorine solutions on most other sulfide ores resulted in the formation of a mixture of sulfate and elemental sulfur, the production of the latter being favored by a very dilute solution of oxidant. The reactions taking place were obviously complex and only a detailed kinetic study could be expected to clarify the position and enable a prediction to be made of conditions leading to the rapid formation of metal salt and the economically desirable elemental form of sulfur. Galena was chosen for the first investigation as it is of widespread occurrence and is representative of a simple cubic lattice sulfide containing the monosulfide unit, S2-. Experimental Procedure The apparatus and general technique used in this work have already been described.' Analyses for chlorine and sulfate were carried out by the same methods as those used for pyrite. The lead in 1 ml aliquots of solution was determined polarographi-cally, after destroying chlorine with hydrazine hy-drochloride and making solutions 0.5 molar with hydrochloric acid. A large sample of Kansas galena, assaying at better than 98 pet PbS, was crushed and wet sieved to give fractions of —10 + 14, —20 + 28, —28 + 35, and —48 + 65 Tyler screen. The particles were almost perfect cubes and the apparent surface Per gram was calculated assuming each particle a cube Of side equal to the mean mesh opening. A volume shape factor, calculated as for pyrite, was exactly unity. The main apparatus was unsuitable for direct visual examination of the ore particles during the reaction. For this purpose a small cell from a Spekker Absorptiometer optical flats 1 cm apart) was l by a greased microscope slide after filling with oxidant solution. One or two ore particles were placed in the cell and the solution was stirred by a glass covered speck of iron wire activated by an external rotating magnet. The surface of an ore particle was examined under a binocular microscope at between 10 and 40 magnifications. Results Experiments were made under a wide variety of conditions, the form of presentation of the data being illustrated by Fig. 1, where the concentrations of chlorine, sulfate, and sulfur are plotted against time. The fictitious concentration of solid sulfur is used for convenience and is the molarity of sulfur which would be recorded if the elementary sulfur formed during the reaction were dissolved in the liquid iii the reaction vessel. As some lead sulfate is occluded with the sulfur on the ore particles the amounts of sulfur and sulfate formed during a reaction cannot be calculated

Jan 1, 1958

By H. M. Chance

The great outspread of the coal measures over portions of thirtyone of the sixty-seven counties of Pennsylvania, and the large number of workable seamy comprising the coal series,—together with some workable seams lately shown to belong to the (so-called) barren measures,—-create the impression that these fields contain a practically inexhaustible supply of fucl, and those who have estimated or attempted to estimate their available tonnage have generally promulgated this view. But the actual total contents of this coal-field is of no importance to us at present; calculations including all seams, whether thick enough to mine or not, whether pure enough to furnish a marketable fuel or not, whether accessible at reasonable depth or not, are of no practical value. As coal producers, we are interested not in the total contents, but in the total amount of easily accessible coal of good quality contained in beds thick enough for remunerative mining. The estimates contained in this payer refer exclusively to workable and accessible coal of commercial value,—we may call it available" coal. I am not aware that any one has as yet attempted to estimate in

Jan 1, 1882