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By M. L. Millican

The objective of this study has been to develop a method of log interpretation in the Delaware sand whereby the effects of the shale contained within the sand can be recognized and accounted for in a quantitative solution for porosity and water saturation. Both theoretical and empirical considerations are discussed. A simplified interpretation chart is presented which provides a means of amending the conventional porosity resolution of the Sonic log to compensate for the presence of shale. The amount of shale within the sand and its degree of lamination may be inferred from a calibrated gamma ray log. The resulting porosity value may then be used in conjunction with a knowledge of the formation resistivity to determine water saturation. Of added interest, particularly in the Delaware sand, is an approximation of permeability which may be derived empirically from the simplified chart. The discussion is illustrated by field examples. INTRODUCTION The performance of the Sonic log in defining the porosity fraction in clean, consolidated formations is well known, particularly in sandstones that are well compacted and free of shale. An approach to Sonic log porosity determination in shaly sands has been recently developed.' This method involves correcting the Sonic log readings by means of an a factor, where a is the ratio of the pseudo-static SP to, the static SP, and is a function of the amount of shale present. This method is dependent upon a contrast between the salinities of the drilling fluid and the connate water in the formation, inasmuch as this contrast produces the SP effect. In wells drilled with salt mud, the contrast, and with it the means of obtaining the a correction, disappear. In the Delaware basin, the large majority of rotary wells drilled to the uppermost sands of the Bell Canyon group employ salt mud as the drilling fluid. These sands have been the objective of most of the drilling exploration in the basin to date. A comparison of porosity values in these sands, as determined by core analysis, to Sonic log readings has indicated that a correction for the shaliness of the sand is needed. In the absence of an SP curve to determine the correction factor, the porosity resolution of the Sonic log in these sands has been questionable.

By Chester A. Fulton

In Polk County, Florida, the mining of raw phosphates began some 50 years ago with dredging operations on the Peace River, and in other near-by places by removal of shallow overburden with negroes and wheelbarrows, or with mules and scrapers, and the excavation and screening of deposits found close to the surface. There were many individual operations of comparatively short life. Later steam shovels removed the overburden, and still later hydraulic methods were substituted for the steam shovel. Within the last 10 years large electrically operated draglines have almost entirely replaced hydraulic mining for overburden removal. The matrix is still mined by hydraulic giants and pumped to the washer or recovery plant. The many small operations have long since disappeared and the most desirable phosphate lands have gradually been acquired through purchase or merger by the seven companies that are operating in the field today. These companies are producing and selling about 2,000,000 long tons of phosphate per annum, or about two-thirds of what the industry likes to think is the normal output, with 1929 and 1930 in mind. To produce these 2,000,000 long tons of raw phosphate, they mine and treat about 1,000,000 tons of tailings from older and less efficient operations, about 11,000,000 tons of matrix, and remove from above this matrix some 22,000,000 tons of overburden. The mining practice that has made possible the excavation and handling of 34 million tons of material to win but 2 million tons of merchantable product, selling for probably an average of only $4 per long ton when dried, should be of interest to the mining profession, though little has been written of it. The Florida Pebble Field, as it has come to be known, comprises an area (Fig. 1) within a radius of about 18 to 20 miles centering around Mulberry in Polk County, a small town 30 miles east of Tampa, Florida's largest port on the Gulf coast. The geology1 of these phosphate pebble deposits may be described briefly. A fairly pure limestone was altered to a secondary apatite.

Jan 1, 1938

By Chester A. Fulton

In Polk County, Florida, the mining of raw phosphates began some 50 years ago with dredging operations on the Peace River, and in other near-by places by removal of shallow overburden with negroes and wheelbarrows, or with mules and scrapers, and the excavation and screening of deposits found close to the surface. There were many individual operations of comparatively short life. Later steam shovels removed the overburden, and still later hydraulic methods were substituted for the steam shovel. Within the last 10 years large electrically operated draglines have almost entirely replaced hydraulic mining for overburden removal. The matrix is still mined by hydraulic giants and pumped to the washer or recovery plant. The many small operations have long since disappeared and the most desirable phosphate lands have gradually been acquired through purchase or merger by the seven companies that are operating in the field today. These companies are producing and selling about 2,000,000 long tons of phosphate per annum, or about two-thirds of what the industry likes to think is the normal output, with 1929 and 1930 in mind. To produce these 2,000,000 long tons of raw phosphate, they mine and treat about 1,000,000 tons of tailings from older and less efficient operations, about 11,000,000 tons of matrix, and remove from above this matrix some 22,000,000 tons of overburden. The mining practice that has made possible the excavation and handling of 34 million tons of material to win but 2 million tons of merchantable product, selling for probably an average of only $4 per long ton when dried, should be of interest to the mining profession, though little has been written of it. The Florida Pebble Field, as it has come to be known, comprises an area (Fig. 1) within a radius of about 18 to 20 miles centering around Mulberry in Polk County, a small town 30 miles east of Tampa, Florida's largest port on the Gulf coast. The geology1 of these phosphate pebble deposits may be described briefly. A fairly pure limestone was altered to a secondary apatite.

Jan 1, 1938

By William H. Shockley

There was an extensive mining and industrial exploitation of Russia, about 20 years ago, by Belgian, French and British capitalists; but the results were discouraging. It is said that the Belgian and French public together lost approximately $400,000,000, chiefly in the coal and iron industry of southern Russia. This loss is largely accounted for by the fact that most of the companies were formed, as usual in " boom" times, to sell stock; and that thorough investigations were not made. I11 1906, renewed interest was taken in Russian mines, especially in those of gold and copper, and a considerable literature is growing on this subject; but as yet I have seen no account of one of the large Russian mining estates. The following notes on such property, where the conditions are so different from those in the mining regions of the United States, should be of interest: This inadequate and probably somewhat inaccurate account is made up, partly from my own notes made on the ground, in the summers of 1904 and 1905, and partly from a volume on the geology and resources of the estate issued several years ago, containing surface- and mine-maps, and from a pamphlet published in 1904, giving a general account of the condition and prospects of the property. This pamphlet includes a report made in 1899 by Arthur L. Pearse, a member of this Institute. Both these books are in Russian, and were prepared by the Bogoslovsk Mining Co., which owns and operates the property. Articles in many other languages have appeared dealing with various matters connected with the estate; but I know of no other general account of it. In numerous books and articles on the Urals and Siberia, however, localities are described in which somewhat similar conditions prevail. Recent papers by

Jan 1, 1909

By F. Benard

Recovery of selenium and tellurium at Copper Cliff by the Ontario Refining Co. has been previously described by the writer.l During 1935 a new building was erected to house this operation and description of the new plant and process form the subject of this paper. The building, of modern steel and tile construction, covers an area of 5900 sq. ft. with a volume of approximately 165,000 cu. ft. The large monitored center bay is flanked by two smaller outside bays, one of which is devoted to the tellurium section. All equipment, ceilings and upper walls, are treated with aluminum paint, giving good illumination and facilitating good housekeeping, essential from a health standpoint in handling material of this nature. Equipment Layout and type of equipment conforms to the requirements of the process as described below. In the selenium section, storage tanks, neutralizing tanks and precipitators are of steel construction, lead-lined and arranged for gravity flow (Fig. 1). The neutralizing tanks are equipped with water-cooled lead coils for controlling solution temperature, agitation being accomplished with compressed air. The precipitators are provided with mechanical agitators, and sulphur dioxide is introduced into the solution through 1/2-in. lead pipes leading from a manifold attached to the cover of the precipitator. Each precipitator has internal cooling coils and an air-jet exhauster to carry off fumes. Neutralized solutions are filtered in a 29-plate wooden filter press using heavy cotton duck as a filter medium, forced feed being maintained by a Welmet centrifugal pump. Dilute solutions are concentrated by evaporation in a vacuum evaporator, constructed of cast hard lead. Heat is supplied by an outside steam chest operating under 15 Ib. steam pressure. The solution is circulated through the steam chest by a pump of antimoniallead at a rate approximating 400 cu. ft. per min. The evaporator is evacuated by a water-jet condenser that creates a vacuum of 26 in. of mercury under normal operating conditions. The capacity of the vessel is 60 cu. ft. and the rate of evaporation 25 cu. ft. per hour.

Jan 1, 1944

By Robert I. Jaffee, Bruce W. Gonser, Eugene M. Smith

THERE has been little investigation of the gold-germanium binary alloys. Haughton1 does not mention any work on the system. In a review article commemorating the fiftieth anniversary of the discovery of germanium, E. Einecke2 mentioned a gold germanium eutectic at 24 atomic per cent Ge (10.4 weight per cent) melting at 359°C., but did not give the source of his information. From measurements of electrical conductivity, J. 0. Linde3 estimated that at least o.6 weight per cent germanium is soluble in gold. The recent availability of germanium in this country in commercial quantities has led to interest in its properties and its alloys. This study is part of a program of investigation on germanium alloys; work on ternary alloys involving germanium and gold will be reported later. In this investigation, the composition and melting point of the Au-Ge eutectic reported by Einecke has been found to be substantially correct. Eutectic composition has been placed at 12,0 per cent germanium, however. An alloy of 10.4 per cent Ge, Einecke's value, was found to have a few gold dendrites in it. The eutectic temperature has been determined as 356.0 ± 0.5°C., slightly less than the temperature of 359°C reported by Einecke. The liquidus curves and the solid solubility of germanium in gold have been determined, and are shown in Fig. I. MATERIALS AND ALLOYING The germanium used in this investigation was prepared by the Eagle-Picher Lead Co. from pure germanium oxide, by reduction in clay crucibles with sodium cyanide. The regulus is quite pure, assaying over 99.9 per cent Ge. High-purity gold obtained from Handy and Harmon was used. Alloying was carried out in graphite crucibles in an atmosphere of purified hydrogen. The temperature was brought up to 1050° to 1100°C., and the metal was allowed to freeze in the crucible. Prepared in this way, the gold dendrites in hypoeutectic alloys were somewhat segregated at the bottom and sides of the ingot, and on the hypereutectic side the lighter primary germanium tended to gather at the top. Most of the alloys were made from virgin metal. Low-germanium heats were made by alloying pure gold with the eutectic. Melting losses were consistently a few milligrams or less, and the composition could safely be taken from the intended analysis. The 30 per cent and 50 per cent germanium heats for thermal analysis were made in part from remelted higher germanium heats, and they may be off composition as much as one per cent. Because of the high cost of materials, the weight of heats for thermal analysis were 15 to 20 grams and heats for metallographic, X-ray, and hardness specimens were 2 to 4 grams.

Jan 1, 1945

By W. J. Taylor

Nature has furnished us with fuel in three forms, solid, liquid, and gaseous; solid, the most common; liquid, containing the greatest energy; gaseous, the most convenient for use. The tendency of the day is to the conversion of solid and liquid fuel into the gaseous form. There is magic in the word gas to many men who through ignorance or indifference imagine that by mere conversion into gas an immense quantity of energy can he added to fuel of other forms, forgetful of the law of nature, that. the conversion of any substance from one form to another involves a loss of effective energy, and therefore that if in certain cases more duty can be obtained out of the gas resulting from a given amount of coal than the coal itself will supply when used direct, the cause lies solely in the more efficient utilization of the fuel in its gaseous state. Nevertheless, new processes for making gas are constantly crowded upon our notice with claims of less cost for manufacture and delivery than natural gas, and often of far more energy for the product than is contained in the coal or oil from which it is made. I was recently asked to examine a new process of this kind. From an analysis shown me the calorific energy of the gas approximated 375 heat-units per cubic foot; on ascertaining the quantity of gas claimed to be made from a given amount of solid and liquid fuel, it appeared, that for every 325 heat-units contained in the latter 900 heat-units were alleged to he delivered into the gas, or nearly three times as much energy as the original fuel really held. The extravagant claim of some oil-gas advocates is still frequently heard, that by vaporizing oil with steam and then passing the mixture through a coil of hot iron pipe, an oil-water-gas containing 26,600 heat-units is formed from 1 pound of oil carrying originally 21,000 heat-units, while the only energy expended on the gas has been by the introduction of a -little steam and a little extraneous heat. Theoretically, 1 pound of oil converted into water-gas carries 26,600

Jan 1, 1890

By Ronald W. Klusman, Erik B. Nelson

The Front Range portion of the Colorado Mineral Belt is an extensive area of mineralization with mining activity dating from 1859 with the discovery of large gold deposits. After an initial boom period and gradual diminishing production, present activity is restricted to molybdenum in Clear Creek County, uranium in Jefferson County, and several small operations extracting gold and silver in Clear Creek and Gilpin Counties. Gold and silver have dominated the production in the Front Range, though the complex mineralization created milling and smelting problems and it is postulated that considerable amounts of precious metals remain in the mine dumps. This area is plagued by a severe mine drainage problem, with Clear Creek most impacted by many draining mines and tailings in the basin. Boyles et al. Moran and Wentz, Wentz, Wildeman et al., have examined various aspects of the impact of mine drain¬age in the Clear Creek basin. The primary objective of this study was to collect data on the tailings, drainages, and leaching experiments in order to make preliminary suggestions for reducing the impact while recovering metal values to offset treatment costs. A variety of leaching experiments were performed on tailings from the Nevada Gulch area in the Central City mining district. Leachings were performed in vertical tubes indoors and wooden boxes exposed to the outside environment. In the leaching experiments, the leaching solution, grain size, and residence times were varied, while forced aeration was used in some experiments. Bacterial nutrient 9K° and mine drainage were used in some of the experiments. A total of 14 additional tailings samples were analyzed for base and precious metals. The composition of the mine drainage and tailings used in the leaching experiments, as well as data on the additional samples are shown in [Table 1]. Leachate samples were taken periodically for analysis until compositions leveled off. Results and Discussion Leaching with distilled water was used as a control and best illustrates the basic behavior of the leaching process for zinc in a vertical tube [(Fig. 1)]. More acidic leachings increased concentrations of metals as did smaller grain sizes, though the time required increased significantly. Mine drainage with its high concentration of dissolved iron sometimes decreased the heavy-metal concentration in the leachate due to oxidation of Fe 2 and precipitation of Fe(OH)9 which absorbs some of the dissolved heavy metals. In the larger scale experiment carried out in the simulated leaching pad, substantial concentrations of metals were attained in the final leachate after one month. In this experiment the leachate was not recycled, but allowed to saturate the tailings continually with evaporation loss made up by additions of Quartz Hill drainage and nutrient 9K. The concentration of the metals in the leachate and the increase over the input solution are given in [Table 2]. Heap leaching of low-grade copper and uranium ores is successfully carried out in many districts, enhanced by the metabolism of autotrophic bacteria of the Thiobacillus-Ferrobacillus group. These ubiquitous organisms enhance metal leaching, and general aspects of heap leaching are discussed by Malouf, Trudinger, Pings, and Duncan et al. Conclusions and Recommendations Returning to the primary objective, how to reduce the mine drainage impact and recover metal values, we need to consider how the data may suggest avenues toward this objective. Boyles, et al., considered various

Jan 1, 1977

By Frederic Benard

Recovery of selenium and tellurium at Copper Cliff by the Ontario Refining Co. has been previously described by the writer.l During 1935 a new building was erected to house this operation and description of the new plant and process form the subject of this paper. The building, of modern steel and tile construction, covers an area of 5900 sq. ft. with a volume of approximately 166,000 cu. ft. The large monitored center bay is flanked by two smaller outside bays, one of which is devoted to the tellurium section. All equipment, ceilings and upper walls, are treated with aluminum paint, giving good illumination and facilitating good housekeeping, essential from a health standpoint in handling material of this nature. Equipment Layout and type of equipment conforms to the requirements of the process as described below. In the selenium section, storage tanks, neutralizing tanks and precipitators are of steel construction, lead-lined and arranged for gravity flow (Fig. 1). The neutralizing tanks are equipped with water-cooled lead coils for controlling solution temperature, agitation being accomplished with compressed air. The precipitators are provided with mechanical agitators, and sulphur dioxide is introduced into the solution through 1/2-in. lead pipes leading from a manifold attached to the cover of the precipitator. Each precipitator has internal cooling coils and an air-jet exhauster to carry off fumes. Neutralized solutions are filtered in a 29-plate wooden filter press using heavy cotton duck as a filter medium, forced feed being maintained by a Welmet centrifugal pump. Dilute solutions are concentrated by evaporation in a vacuum evaporator, constructed of cast hard lead. Heat is supplied by an outside steam chest operating under 15 Ib. steam pressure. The solution is circulated through the steam chest by a pump of antimonial lead at a rate approximating 400 cu. ft. per min. The evaporator is evacuated by a water-jet condenser that creates a vacuum of 26 in. of mercury under normal operating conditions. The capacity of the vessel is 60 cu. ft. and the rate of evaporation 25 cu. ft. per hour.

Jan 1, 1943

By Frederic Benard

Recovery of selenium and tellurium at Copper Cliff by the Ontario Refining Co. has been previously described by the writer.l During 1935 a new building was erected to house this operation and description of the new plant and process form the subject of this paper. The building, of modern steel and tile construction, covers an area of 5900 sq. ft. with a volume of approximately 166,000 cu. ft. The large monitored center bay is flanked by two smaller outside bays, one of which is devoted to the tellurium section. All equipment, ceilings and upper walls, are treated with aluminum paint, giving good illumination and facilitating good housekeeping, essential from a health standpoint in handling material of this nature. Equipment Layout and type of equipment conforms to the requirements of the process as described below. In the selenium section, storage tanks, neutralizing tanks and precipitators are of steel construction, lead-lined and arranged for gravity flow (Fig. 1). The neutralizing tanks are equipped with water-cooled lead coils for controlling solution temperature, agitation being accomplished with compressed air. The precipitators are provided with mechanical agitators, and sulphur dioxide is introduced into the solution through 1/2-in. lead pipes leading from a manifold attached to the cover of the precipitator. Each precipitator has internal cooling coils and an air-jet exhauster to carry off fumes. Neutralized solutions are filtered in a 29-plate wooden filter press using heavy cotton duck as a filter medium, forced feed being maintained by a Welmet centrifugal pump. Dilute solutions are concentrated by evaporation in a vacuum evaporator, constructed of cast hard lead. Heat is supplied by an outside steam chest operating under 15 Ib. steam pressure. The solution is circulated through the steam chest by a pump of antimonial lead at a rate approximating 400 cu. ft. per min. The evaporator is evacuated by a water-jet condenser that creates a vacuum of 26 in. of mercury under normal operating conditions. The capacity of the vessel is 60 cu. ft. and the rate of evaporation 25 cu. ft. per hour.

Jan 1, 1943

By William H. Shockley

Though China has been widely explored by mining engineers during the past dozen years, comparatively little has been published concerning its mineral resources. The few moilographs scattered through the transactions of various societies contain far less information than the private reports made to the numerous syndicates which have sent out engineers. The best general account of the geolopy and mineral resources of China is to be found in the works of von Richthofen,' a remarkably gifted observer. The observations recorded here in this paper were made in the service of the Pekin Syndicate (which has kindly given me permission to publish them), during the first months of 1898, among the coal- and iron-fields of southeastern Shansi. This is one of the largest anthracite-regions known, the area being

Jan 1, 1904

By David Scott

THE MOGOLLON mining district, New Mexico, has received little public attention, although for 15 years it has been the leading silver producer of the state; it is situated in a region remote from the principal lines of travel, and its activities have usually been limited to the operations of two or three companies. The value of the total production of the district in the 44 years of its history has been estimated at $15,000,000. For the years 1904 to 1917, inclusive, the output was: gold, $4,370,000; silver, 10,042,000 oz.; copper, 874,862 lb.; total value, approximately. $10,500,000. In 1913 the district contributed 80 per cent. of the total silver production of New Mexico, but in 1917 only 41 per cent., due to serious interruption in the operations of the leading producer. Since 1914 the silver output has diminished one-half, and the present high value of silver is nearly offset by the increase in cost of production. The output of gold has rarely exceeded 35 per cent, of the total for New Mexico. The ratio of silver to gold, by weight, has averaged 46:1 based on the whole output of the district. LOCATION AND TOPOGRAPHY The town of Mogollon is 75 mi. (121 km.) by a poorly located highway from the nearest railroad terminals, at Silver City and Tyrone. All supplies are transported by motor trucks and teams. The area, sometimes called the Cooney Mining District, lies on the western flank of the Mogollon Mountains, which occupy the western part of Socorro County. The elevations drop steeply on the west to the valley of the San Francisco River, adjacent to the Arizona boundary. The topography is very rugged, the whole area being sharply dissected; deep canyons with steep gradients and rugged walls are characteristic of the whole western-slope of the Mogollon Range. The main canyons run east and west, and usually maintain a flow of water during the entire year. As would be expected in a region of such deep dissection, the

Jan 2, 1920

By J. E. Spurr

Jan 1, 1903

By N. C. Nissen, J. A. Thomas, A. Illis, K. N. Subramanian

Successful miniplant and laboratory testwork has indicated that high purity selenium can be produced from copper refinery slimes. The recovery technique fits into existing unit operations, and the selenium recovery in the new process was close to 99%. This recovery virtually eliminated any selenium being processed through the smelting stage. In addition, miniplant tests conducted at Inco Metals Co.'s J. Roy Gordon Research Laboratory in Mississauga, Ontario, have demonstrated the reliability of the process with respect to extractions, product quality, filtration characteristics, and effluent disposal. Inco's copper refinery at Copper Cliff, Ontario, produces about 500 t/d of copper with the anode slimes fall typically averaging 0.5% of the throughput. Investigations relating to the treatment of slimes within Inco's R&D have been conducted on several occasions since 1959, when the available alternatives such as acid or alkaline pressure leaching, aqueous or high temperature chlorination, roasting, smelting, etc., were considered. Interest in slimes processing was revived recently to meet increasingly stringent environmental standards and to replace equipment of a relatively old plant.

Jan 11, 1978

By ED. E. Furman, R. H. Atkinson

HITHERTO the practical creep testing of precious metals has received little or no attention. The only previous creep tests of precious metals have been made with wires under conditions such as to yield much more rapid rates of creep than in engineering tests.', ' Up to the present time the value of creep bars of adequate size, in the absence of real need for engineering data, has deterred investigators. However, the increasing use of platinum at high temperatures has demonstrated the need for reliable creep data for the guidance of engineers, especially those engaged in designing certain specialized chemical plant equipment. In order to supply this need, creep tests were conducted at 1382°F (750°C) on 0.290 in. diam specimens of platinum, 90 pct Pt, 10 pct Rh and palladium. The platinum was high purity, nominally 99.95 pct Pt. The 90 pct Pt, 10 pct Rh was of the same high quality as is used for making gauzes for the catalytic oxidation of ammonia. The palladium was also of high purity; two batches of palladium bars were tested, one deoxidized with calcium boride and the other with aluminum. Spectrographic examination of the palladium confirmed its good quality; the only significant impurities apart from the residual deoxidizers were traces of silicon and lead. Procedure The creep bars, which were furnished by Baker and Co. to our specification, were 6 ¾ in. in overall length with a 4½ in. (4 in. gage length) reduced section 0.290 in. in diam and had the ends threaded (?-NC16). It may be of interest that the bars were valued at up to $600 each. The specimens were supplied in a 50 pct cold-worked condition to facilitate attachment of the creep extensometer, which was of the push rod type. Because of the softness of the platinum and palladium, the extensometer rings were secured to the test section by means of circular knife edges instead of the usual pointed set screws. The extensometer rods extended through the bottom of the furnace and readings were taken with a 0.0001 in. "Last Word" dial gage fastened to the rods for the duration of the test. The bars were directly loaded by hanging weights from the lower specimen grip. All tests were conducted at 1382°F ± 2°F, and an effort was made to maintain the temperature gradient over the test section within 2°F. The ends of the furnace tube were packed with asbestos wool, which allowed a very slow circulation of air through the tube. Annealing was accomplished in the creep furnace before the load was applied. The platinum and palladium specimens were annealed at the test tem- perature for about 17 and 24 hr respectively; in the case of the rhodioplatinum it was found expedient to anneal for 1 hr at 1922°F (1050°C). Pilot samples cut from the same stock as the bars were used to check annealing procedures. Pertinent measurements of grain size and hardness were recorded. Results and Discussion The creep data obtained are given in Table I and the creep curves are plotted in Figs. 1, 2, and 3. Two platinum specimens, tested under a stress of 250 psi, had almost identical creep rates at 2000 hr, namely 0.000008 and 0.000009 pct per hr. A third platinum specimen, stressed at 400 psi, had a creep rate at 2000 hr of 0.000026 pct per hr; the reason for a rather sharp decrease in creep rate during the period from 1200 to 1600 hr is unknown. As it was thought that 90 pct Pt, 10 pct Rh would have a lower creep rate than platinum, the first sample was tested at 400 psi; however, the creep rate was approximately 50 pct greater. Microex-amination revealed that differences in grain size might be responsible for the unexpected result, as annealing at 1382°F developed an average grain diameter of 0.0021 in. in the rhodioplatinum specimen compared with 0.004 in. in the platinum bar. Annealing the alloy for 1 hr at 1922°F (1050°C) increased the average grain diameter to 0.0032 in. and materially improved the creep resistance, making it much better than platinum. A second specimen annealed at 1922°F (1050°C) and tested under a stress of 550 psi had a creep rate of 0.000022 pct per hr at 2000 hr, which was still substantially lower than that shown by the specimen annealed at 1382°F (750°C) and stressed at only 400 psi. In contrast to the creep behavior of the platinum and rhodioplatinum specimens, the palladium bars, whether deoxidized with calcium boride or aluminum, were characterized by high first stages of creep. However, after about 1200 hr of test, the creep

Jan 1, 1952

By Frederic Benard

RECOVERY of selenium and tellurium at Copper Cliff by the Ontario Refining Co. has been previously described by the writer.1 During 1935 a new building was erected to house this operation and description of the new plant and process form the subject of this paper. The building, of modern steel and tile construction, covers an area of 5900 sq. ft. with a volume of approximately 165,000 cu. ft. The large monitored center bay is flanked by two smaller outside bays, one of which is devoted to the tellurium section. All equipment, ceilings and upper walls, are treated with aluminum paint, giving good illumination and facilitating good housekeeping, essential from a health standpoint in handling material of this nature. EQUIPMENT Layout and type of equipment conforms to the requirements of the process as described below. In the selenium section, storage tanks, neutralizing tanks and precipitators are of steel construction, lead-lined and. arranged for gravity flow (Fig. 1). The neutralizing tanks are equipped with water-cooled lead coils for controlling solution temperature, agitation being accomplished with compressed air. The precipitators are provided with mechanical agitators, and sulphur dioxide is introduced into the solution through 3-in. lead pipes leading from a manifold attached to the cover of the precipitator. Each precipitator has internal cooling coils and an air-jet exhauster to carry off fumes. Neutralized solutions are filtered in a 29-plate wooden filter press using heavy cotton duck as a filter medium, forced feed being maintained by a Welmet centrifugal pump. Dilute solutions are concentrated by evaporation in a vacuum evaporator, constructed of cast hard lead. Heat is supplied by an outside steam chest operating under 15 lb. steam pressure. The solution is circulated through the steam chest by a pump of antimonial lead at a rate approximating 400 cu. ft. per min. The evaporator is evacuated by a water-jet condenser that creates a vacuum of 26 in. of mercury under normal operating conditions. The capacity of the vessel is 60 cu. ft. and the rate of evaporation 25 cu. ft. per hour.

Jan 1, 1938

By John W. Burd

A system is described for the simultaneous deposition of epitaxial layers on as many as eight substrates. A high degree of uniformity of both physical and electrical characteristics is achieved in the films. Variation of film thicknesses is consistently less than ±10pct within a wafer and from wafer to wafer within a run with the variation typically on the order of 55 pct. Composition variation of GaAs1-x PX layers within a wafer and from wafer to wafer within a run is consistently less than 51 pct. Electrical evaluation of the films by several techniques indicates excellent doping uniformity within a wafer and from wafer to wafer within a run. Mobilities for lightly doped GaAs films at 300°K are consistently >6000 cm2 v-1 sec-1 and mobilities > 7000 cm2 v- 1 sec-1 are regularly attainable. Techniques for the preparation of material with carrier concentrations from 1 x 1015cm-3 to 1 x 1019 cm-3 n-type and 5 x 1016 to 5 x 1018 cm-3 p-type are discussed. METHODS for the preparation of 111-V compounds by vapor phase reactions have been extensively reported in the literature.1-6 Almost all of the apparatus described for these various methods are suitable for processing one or at the most a very limited number of wafers simultaneously. With the recent rapid advances in the use of vapor grown GaAs for microwave oscillators and GaAs1-xPx as visible light emitters the requirements for these materials are steadily increasing. In order to satisfy these requirements it is necessary to move from a laboratory scale apparatus to one which is capable of processing a large number of wafers simultaneously. Desirable features would be a high degree of uniformity among the wafers and good reproducibility from run to run. The apparatus to be described fulfills these requirements very well. DISCUSSION The various methods reported in the literature can be classified under three headings: 1) closed tube, 2) open tube, and 3) the close-spaced method. Of these three the open-tube method is the most amenable for scale-up to a manufacturing process. It is the most versatile and the various operating conditions can be more precisely controlled than with the other two methods. A number of chemical reactions may be used to achieve vapor-phase growth of 111-V compounds. Sev-era1 of the more generally used reactions are shown in Fig. 1. All of these reactions have the following points in common: 1) generation of a volatile group III(Ga) species by the reaction of the transport agent (halide or HC1) with either Ga or GaAs, 2) introduction of the Group V(As and/or PI component, 3) a method of adding dopant, if desired, and 4) a region in which deposition from the vapor will occur and form as a single crystal epitaxial film on the substrates. The laboratory scale reactors permit the hot re-actant gases to flow into the relatively cooler deposition zone and pass successively over the several substrates which are arrayed along the long axis of the tube parallel to the gas flow. With this arrangement the composition of the reactant stream is continually changing as solid material is deposited on each successive substrate. As a result of this changing gas composition the reaction driving force also changes from substrate to substrate and the degree of uniformity of layer thickness, doping level, and so forth, is poor. This effect can be partially overcome by imposing a controlled temperature gradient along the deposition region to compensate for change in gas composition. However, even when this is done variations in layer thickness on the order of 30 to 40 pct are common and as high as 50 pct are frequently experienced between adjacent wafers in the tube. To expand this arrangement to a large number of wafers would only increase the nonuniformity from the first to last wafer in the line. From the above discussion the two undesirable features of changing gas composition and temperature gradient become evident. A reactor system which eliminates or minimizes these undesirable features is one in which the apparatus is mounted vertically as shown schematically in Fig. 2. The vertical mounting permits the disposition of a number of substrates on a suitable support so that all wafers are at the same vertical height in the furnace and hence at essentially the same temperature. By using only a single row of wafers the reactant gas mixture passes over only one substrate in its path through the reactor. Thus the two undesirable features of changing gas composition and temperature gradient are minimized. An additional design feature which further minimizes temperature variations is rotation of the substrate holder. Rotation serves to integrate any radial temperature gradient existing around the resistance heated furnace. A photograph of a reactor assembly at the completion of a run is shown in Fig. 3. MATERIAL PREPARATION Apparatus. Although any of the several chemical systems shown in Fig. 1 are adaptable for use in this apparatus the one generally used is System 2, the hydride synthesis system. This system has been de-

Jan 1, 1970

By W. M. Myers

THE hydraulic properties exhibited by the calcination products of certain limestones were recognized at an early datemore than 2000 years ago. It was known that calcined limestone with the addition of other minerals would react with water and produce an insoluble and stable product. This material could be cast in desired forms or could be used as a cement for the unification of other materials in large masses or for bonding brick or masonry structures. Cements are essentially mineral glues and it is their ability to unify other materials plus their fluidity when first mixed with water, enabling the mass to assume any desired shape, that has made them so extraordinarily useful to modern industry. Like other glues, cements do not exhibit their maximum strength when used alone and only when mixed with proper aggregates do their optimum properties appear. The resulting concrete, a mixture of cement, mineral aggregates and frequently of reinforcing steel, exhibits the most desirable properties of the individual constituents with regard to tensile strength, stability and permanence. The speed with which such mixtures can be -prepared and installed in place with mechanical equipment has facilitated their adoption by the engineering profession concerned with the construction industries. The development and application of improved methods of manufacture have resulted in such economies that the finished product can be sold at a remarkably low price. In addition, the necessary raw materials are of such common occurrence and wide geographic distribution that the manufacture of cement was established in 34 of the 48 states by 1946. Plants under construction will add to this number. In recent years the industry has been characterized by the development of a number of new cements designed to possess special properties essential for use in unusual environments. These have introduced the use of some new raw materials and also have complicated the processes of manufacture. In the following pages, the major varieties of cement of commercial importance are treated in the chronological order of their appearance on the market.

Jan 1, 1949

By W. P. Sykes

IN CONNECTION with a study of tungsten steels, Honda and Murakami1 reported an investigation of the system iron-tungsten. This report included a tentative equilibrium diagram, photomicrographs of various alloys in the series, and qualitative measurements of hardness and magnetic properties. The present investigation originally had as its object the study of the hardness and tensile properties of a series of carbon-free iron-tungsten alloys. But, as the work progressed it became evident that the system possessed other features of interest, so the scope of the investigation was enlarged. MATERIALS The iron powder used in preparing the alloys was obtained as follows: Iron oxalate was precipitated from a ferrous-sulfate solution by the addition of a solution of oxalic acid. This oxalate, after thorough washing, was ignited to iron oxide, which after reduction in hydrogen at about 1000° C. yielded iron powder containing but about 0.2 per cent. iron oxide and about 0.005 percent. carbon. Tungsten metal in the form of powder, such as is used in the manufacture of filaments for incandescent lamps, was the other constituent. This material analyzed 99.8 per cent. tungsten and contained no carbon, The metal powders, in the desired proportions, were mixed by tumbling and formed, under pressure of 20 tons per sq. in., into rods 3/8 by 3/8 by 10 in. To form the alloys without contamination, sections of the pressed rods were placed on alundum slabs and heated in an alundum tube wound with a tungsten resistor and packed in heat-insulating material. While the resistor was heated, a stream of hydrogen was continually passed through both the tube and the case containing it. The tungsten winding on the tube, as well as the material heated within the tube, was thus protected from oxidation. Such a furnace will operate constantly

Jan 2, 1926

By S. Luszcz, R. W. Vook, Fred Witt

In situ X-ray investigations were made on polycrys-talline silver films deposited by vacuum evaporation on (111) CaF2 and (100) NaCl single-crystal substrates at 80°K. The films were evaporated and annealed in an X-ray diffractometer attachment having a residual gas pressure of 2 x lo-' Torr. All measurements were made without exposing the films to the atmosphere. Measurements were made on the films in the as-deposited state and after various annealing treatments. The intrinsic stacking and twin fault densities, the magnitudes of the uniform and nonuniform strains, and the crystallite sizes were determined. In addition the textures in the films were measured qualitatively. The results obtained for the as-deposited films on single-crystal substrates are in substantial agreement with previously reported results for silver films deposited on glass. Intrinsic stacking and twin faults, as well as uniform and nonuniform strains, were present in these films. During the various annealing treatments (up to 350°C) the faults and nonuniform strains annealed out. Considerable grain growth and texture changes occurred also. The effects were much greater for the NaCl substrate than for the CaFz substrate. The relative magnitudes of the grain growth in the variously oriented grains could be explained qualitatively in terms of the thermal strains and strain energies introduced into the differently oriented grains during the initial, irreversible anneal. These strains were due to the different thermal expansion coefficients of the film and substrate. X-RAY diffraction measurements on evaporated films deposited on substrates at low temperature have the advantage that many of the imperfections introduced into the film during deposition are "frozen in". Thus, the influence of a very important experimental variable, substrate temperature, on the imperfection structure of evaporated metal films may be studied. Moreover, the effects of annealing such films makes possible the study of thermally activated recovery processes in these films. The present study was designed to determine the influence of single-crystal substrates on the resultant film structure relative to the previous results obtained using glass substrates.' To this end great care was taken to keep the experimental variables the same in the two cases. Different experimental conditions would, of course, result in films having different physical properties. Again the initial substrate temperature was in the neighborhood of 80°K and the films were subsequently annealed to 350°C. The pure metal silver was chosen for evaporation, primarily because of its relatively low stacking fault energy and consequent high fault density in the as-deposited state. The silver films were formed by evaporation onto air-cleaved {ill} CaF, and (100) NaCl surfaces cooled to 80°K in an X-ray diffractometer attachment2 having a base residual gas pressure of 2 X l0-' Torr. The films were not exposed to the atmosphere until all of the X-ray data had been recorded. In this way one of the most important experimental variables, environment, could be well-controlled and reproduced. X-ray measurements were made at the temperature of deposition and included determinations of the diffraction line peak positions, line shapes, and integrated intensities. The peak position measurements were used to determine the intrinsic stacking fault densities and the average uniform strain in the film. The shapes of the diffraction lines provided information on the twin fault density, true crystallite size, and average nonuniform strain. The preferred orientation in the film was determined qualitatively from the integrated intensities. I) EXPERIMENTAL PROCEDURE The evaporator attachmentZ was charged with 99.999 pct Ag pellets positioned in a tantalum filament which had been outgassed previously at l0-8 Torr. The CaFz and NaCl single crystals were cleaved in air and then placed in position in the chamber so that their cleavage surfaces were on the diffractometer axis. The chamber was prepumped using a sorption pump, sealed off, and then baked at 150°C for 24 hr. The ion pump operated during the bakeout cycle. The substrate was then heated to 500° C by means of an auxiliary heater and kept hot until the rest of the chamber was cooled slowly to room temperature. This bakeout procedure consistently resulted in an ultimate pressure in the low lo-' Torr range. The substrate was then cooled down on 80°K. Its temperature was monitored by a thermocouple wedged into the rear of the copper substrate holder. The diffracted intensity and peak position of the 111, 222, and 333 CaF, lines were measured prior to evaporation. Nickel-filtered, pulse-height-discriminated copper radiation was used. Similar measurements were made for the 200 and 400 lines from NaC1. These measurements were used as a lattice parameter check and to determine the thickness of the evaporated silver films from the attenuation of the substrate lines. The evaporation rates were approximately 3A per sec for both films while the maximum pressures during evaporation were 3 x lo- ' and 7 x 10"8 Torr for the CaF, and NaCl cases, respectively. The film thickness was measured by the attenuation of the CaF, and NaCl substrate lines and by at optical interference method. Values of 1700 and 1500A, respectively, were obtained for the silver

Jan 1, 1969