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By J. R. Long, T. R. Graham

THIS report is concerned with part of a series of investigations carried on by the Federal Bureau of Mines on alloys, particularly nonferrous alloys, made with electrolytic manganese. A broad general program instituted after commercial quantities of electrolytic manganese became available was necessary in order to compare the effects of electrolytic manganese with those of the ordinary commercial grades. Representative analyses of these two materials show the commercial manganese metal to contain up to 2 per cent iron, a maximum of I per cent silicon and 0.06 per cent carbon, while the electrolytic manganese rarely exceeds 0.01 iron, 0.02 sulphur, with no silicon or aluminum. In the literature, the emphasis has been largely on high-strength casting alloys containing up to 5 per cent manganese, and few data are available on wrought manganese alloys. These factors, coupled with the strategic position of copper and zinc, have given impetus to the Bureau's War Research Program for the development of alloys containing nonstrategic manganese for the purpose of supplementing or providing alternates for the more strategic metals. The alloy reported here was studied, along with several other ferrous and nonferrous alloys, as possible cartridge-case material, and was chosen after a review of the properties of the ternary alloys of copper-manganese-zinc. PRELIMINARY WORK In a cursory survey of this system, alloys ranging from 60 to 95 per cent copper, 0 to 50 per cent manganese, and 5 to 40 per cent zinc were investigated. The alloys containing 60 per cent copper were found to fall into the two-phase alpha plus beta region of the system, and since those containing 70 per cent would not permit a saving, only alloys containing 65 per cent copper were considered. The tensile properties of these 65 per cent alloys are plotted in Fig. I as a function of manganese content for annealed material and for four conditions of cold-work In the annealed condition the increases in strength and decreases in elongation are minor up to 15 per cent manganese; beyond this, the changes become more significant. In the cold-worked condition, the first 5 to 10 per cent of manganese appears to have the greatest strengthening, effect, the rate of increase dropping off as the manganese increases beyond this amount. These effects are more pronounced with moderate than with severe cold reduction. It is also interesting to note that while the elongation of annealed material drops regularly with increasing manganese, the elongation in the cold-worked state is relatively little affected by increasing manganese content, particu-

Jan 1, 1944

By Allen F. Agnew

Detailed stratigraphic studies in the Wisconsin-Illinois-Iowa district have made it possible to map the folds and faults that controlled the deposition of the zinc-lead ore. Prospecting on the basis of this mapping and prospecting in lower zones that are potentially ore-bearing have led to discoveries of ore. GEOLOGIC studies for the Federal and State governments in the Wisconsin-Illinois-Iowa zinc-lead district were begun in 1835, and subsequent surveys were made in the three states at intervals until 1916, see Table I. The current study of the district, Fig. 1, by the U. S. Geological Survey was begun in 1942 in the hope that a systematic investigation would help increase production of zinc and lead, then in extremely short supply. Major emphasis of the USGS program was on detailed mapping of the geologic structure and ore deposits. Preliminary maps and reports covering localities of intensive mining activity have been published during the course of this study, Fig. 2. By 1950 the objectives of the study by the USGS were revised; 71/2-min quadrangles of relatively unprospected localities as well as intensively mined localities are now being mapped in Wisconsin. Since 1945 the investigation in Wisconsin has been made in cooperation with the Wisconsin Geological and Natural History Survey, and since 1951 the geologic mapping of areas of particular interest in Iowa has been performed in cooperation with the Iowa Geological Survey. At intervals since 1943 the Illinois State Geological Survey has mapped the geologic structure and ore deposits of localities in the Illinois part of the mining district, see Fig. 2. Geology was applied by mining company personnel as early as 1853, but only sporadically, with periods of greater application between 1890 and 1925. Much of the so-called geologic work was in reality mining engineering. Since 1946 the major mining companies in the district have employed geologists who have successfully applied geologic techniques in the search for ore. History of Mining Occurrence of galena in the district was known as early as 1658 or 1659, when French explorers heard of lead mines that were apparently in the vicinity of Dubuque, Iowa. In 1690 a trading post was established near Dubuque to obtain galena. The first significant attempt at mining by white men took place in 1788 when the Indians granted to Julien Dubuque mining rights for 20 miles along the west side of the Mississippi River, including the vicinity of Dubuque, Iowa. By 1805 lead was being mined near Galena, Ill. In 1819 permanent settlement of the region was begun, and most of the important lead-producing areas had been found by 1830, see Fig. 3. Lead production in the Wisconsin-Illinois-Iowa district between 1830 and 1871 far exceeded that of any other district in the U. S.' Smithsonite was first mined in 1859, and sphalerite was mined as early as 1867. After 1873 the production of sphalerite exceeded that of smithsonite. In 1873 annual zinc production from the district first equaled lead production, and from then until 1893 production of zinc and lead was roughly the same. Since 1893 the ratio of zinc to lead mined has generally ranged between 5:l and 20:l. In 1942 the Wisconsin-Illinois-Iowa zinc-lead district ranked 14th among zinc-producing districts of the U. S. From 1946 until February 1953 the dis-

Jan 1, 1956

By P. K. Weimer

Coinpletely integrated thin-film circuits inco?,porating more than 1000 active and passive elements have been fabricated reproducibly in the laboratory by evaporation of- all components. A 180-stage modified shift register comprising 540 CdSe TFT's, 360 resistovs, and 180 capacitors was deposited upon a glass substrate during one pump-down of the vacuum systeitl. Experimental units have been operated for more than 5000 hr at temperatures uP to 85°C without failure of any slages. The present pupper reviews the charvactevistics of evaporated thin-film transistors (TFT's) and discusses their application to integrnted circuils. INTEGRATED circuits most widely used today are based upon silicon technology, with the circuits formed on the surface of a block of single-crystal silicon1 or on a block of sapphire 2,3 upon which a thin layer of silicon has been deposited. Transistor patterns and interconnections are defined by photographic procedures using photoresist masking. Large groups of transistors are produced in batches which undergo many processing steps, some of which are carried out at elevated temperatures. Passive elements are formed by treatment of the semiconductor surface or are deposited by evaporation alongside the active elements. The size and complexity of the circuits are limited by defects in the devices and by the size of the available single-crystal chips. Capacitative coupling to the semiconducting substrate may also limit useful size and frequency response of the circuits. An alternative approach to integrated circuits is based upon the deposition by evaporation of all circuit components upon a noncrystalline, insulating substrate such as glass.4 Thin-film field-effect transistors,1'6 known as TFT's, can be deposited in large arrays on glass or plastic substrates at the same time the associated passive elements are being deposited. Although still in the research stage the all-evaporated approach is expected to offer certain advantages for many applications. In particular, the use of thin films upon a noncrystalline substrate offers the prospect of producing complex, large-area circuits not now feasible with single-crystal silicon. Important applications of this type include memory arrays for computers and imaging devices for television. The ease with which the evaporated TFT's can be deposited may permit continuous, automated production methods not possible with high-temperature batch processing. Recent advances7'8 in the fabrication of thin-film transistors have led to greatly improved reproduci-bility and life of the TFT's. Experimental circuits having over 1000 active and passive elements deposited upon a common glass substrate are currently being produced in the laboratory. The present paper reviews recent progress in the development of the TFT and in its application to integrated circuits. I) DESCRIPTION OF THE THIN-FILM FIELD-EFFECT TRANSISTOR The TFT is a field-effect transistor of the type having the control gate separated from the semiconductor by a thin insulating spacer. Although its operation resembles that of the silicon MOS transistorg its construction is based entirely on thin-film techniques. Fig. 1 shows a cross-sectional view of an evaporated TFT deposited upon a glass substrate compared with a silicon MOS transistor deposited upon single-crystal sapphire.3 The semiconductor in the TFT is a poly crystal line layer, of a material which can be readily evaporated, such as cadmium sulfide, cadmium selenide,l0 or tellurium." Silicon monoxide layers have usually served as the gate insulator, but other oxides, sulfides, and fluorides may be used. Film thicknesses range from a few hundred to a few thousand angstroms. The source, drain, and gate electrodes in the TFT are of metal. Qpical source-drain gap dimensions are 0.0003 x 0.030 in., with a gate strip whose width slightly overlaps the source and drain. The source and drain electrodes should make low impedance contacts to the semiconductor. With cadmium sulfide films, gold is a satisfactory material for underlying electrodes, while aluminum is preferable for overlying electrodes.12 Considerable variation in design of the TFT is permissible, with the electrodes being

Jan 1, 1967

By Shiou-Chuan Sun

THIS paper presents the design and operation of a frothmeter capable of measuring the frothing characteristics of pine oils and other frothing reagents. The experimental data show that the froth-ability of pine oil is governed by: 1—rate of aeration, 2—time of aeration, 3—height of liquid column, 4—chemical composition of pine oil, 5—pH value of solution, 6—temperature of solution, and 7—concentration of pine oil in solution. The effect of mineral particles on the behavior of froth also was studied, and the results can be found in a separate paper.' The results also show that the relative froth-abilities of pine oils in the frothmeter generally correlate with those in actual flotation, provided that other factors are kept constant. In addition to pine oils, the other well-established flotation frothers were tested, and the results are included. In this paper, compressed air frothing is the frothing process performed by means of purified compressed air, whereas sucked air frothing is the frothing process accomplished by purified air sucked into the glass cylinder by a vacuum system. The term vacuum frothing denotes that froth was formed by degassing of the air-saturated liquid under a closed vacuum system. Apparatus The frothmeter, shown in Fig. 1, is capable of re-producibly measuring the volume and persistence of froth as well as the volume of air bubbles entrapped in the liquid and is capable of being used for compressed air frothing, sucked air frothing, and vacuum frothing. Fig. la shows that for compressed air frothing, the apparatus consists of an airflow regulating system, 1-3; a purifying and drying system, 4-8; a standardized flowmeter to measure the rate of airflow from zero to 500 cc per sec, 9; and a graduated glass cylinder, 13; equipped with an air regulating stopcock, 10; an air chamber, 11; and a fritted glass disk to produce froth, 12. The fritted glass disk, 5 cm in diam and 0.3 cm thick, has an average pore diameter of 85 to 145 microns. The pyrex glass cylinder has a uniform ID of 5.588 cm and an effective height of 63 cm. The inside cross-sectional area of the glass cylinder was calculated to be 24.53 sq cm, or 3.8 sq in. For sucked air frothing, Fig. lb shows that the apparatus for compressed air frothing is used again, with the following modifications: 1—compressed air and its regulating system, 1-3, are eliminated; and 2—a vacuum system, 16, equipped with a vapor trap, 15, and a vacuum manometer, 17, is added. The vacuum system can be either a water aspirator or a laboratory vacuum pump. Any desired rate of airflow can be drawn into the glass cylinder, 13, by adjusting the opening of the air regulating stopcock, 10. The sucked air stream is cleaned by the purifying and drying system, 4-8, before entering the glass cylinder, 13. When this setup is used for vacuum frothing, the air regulating stopcock is closed. The frothmeter has been used for almost 3 years and has proved to give reproducible results, as illustrated in Table I. With a magnifying glass and suitable illumination, the frothmeter also can be used to study the attachment of air bubbles to coarse mineral particles.' Experimental Procedures Except where otherwise stated, the data presented were established by means of the compressed air method. The volume and persistence of froth were recorded respectively at the end of 4 and 6 min of aeration at a constant rate of airflow of 29.3 cc per sec, which is equivalent to 71.6 cc per sq cm per min, or 462.6 cc per sq in. per min. The aqueous solution for each test, containing 1000 cc of distilled water and 19.2 ± 0.5 mg frothing reagent, was adjusted to a pH of 6.9 0.2. The volume of froth is expressed as cubic centimeter per square centimeter and is equivalent to the height of the froth column (the distance between the bottom and the meniscus of the froth). The volume of froth was obtained by multiplying the height of froth by the cross-sectional area of the glass cylinder, 24.53 sq cm. Before each test, the glass cylinder, 13, was cleaned thoroughly with jets of tap water, ethyl alcohol, tap water, cleaning solution, tap water, and finally distilled water. The cylinder with stopcock,

Jan 1, 1953

By Donald W. Petrasek

The effects of selected alloying elements on the elevated-temperature tensile properties of copper alloy -tungsten fiber reinforced composites were invcstigated. A cornparison of the elevated-temperature tensile properties of copper alloy - tungsten fiber reinforced composites, representing soluble systems. was made with copper - tungsten fiber reinforced composites, representing a mutually insoluble system. A linear relation between tensile strength and volume percent fiber content existed at elevated temperatures for all the systenzs investigated. The copper alloy composites were weaker in tension at high volume percent fiber contents than copper composites in which alloying with the fiber did not occur. The tensile strength of the alloyed tungsten fiber decreased with increasing penetration of the alloying element into Ihe tungsten fiber. THE technique of combining strong fibers with relatively weak matrix materials so that the fibers are load-carrying members has been utilized for many years in the reinforcement of plastics with glass fibers. This type of strengthening is currently being extended to include the reinforcement of metals with metallic fibers. Investigations of the room-temperature tensile properties of metal-fiber-reinforced metallic composites have been numerous,'-" but the study of tensile properties at elevated temperatures has been limited. In previous work done at the Lewis Research Center' composites consisting of mutually insoluble constituents were investigated. Composites were made of copper reinforced with uniaxially oriented tungsten fibers. The stress-strain behavior and tensile properties of the composites were related to the tensile properties of the base materials. The tensile strength of the composite was directly proportional to the volume percent of tungsten fiber present, and the full strength of the fiber was realized. Few metal fiber - metal matrix systems exist that are mutually insoluble, and those that do exist are not generally practical. An extension of this work was an

Jan 1, 1967

By E. R. Buchanan, R. E. Reed-Hill

Cylindrical magnesium single crystals were deformed in torsion. The axis of torsion was the basal pole. Five crystals were deformed to different strains between 0.08 and 1.03 and then sectioned in order to determine their dislocation densities using the transmission electron microscope. The work hardening rate of all specimens was at least an order of magnitude higher than that normally associated with easy glide in a tension test and comparable to that obserzed in stage B of a tension test. The correspondence between stage B in a tension test and the initial stages of a torsion test is believed to result from the fact that in both cases deformation occurs in a structure containing roughly equivalent densities of the dislocations associated with the three basal slip vectors. THERE are three basic ways of changing the shape of a crystal using slip dislocations. The crystal can be sheared along a slip direction in a slip plane; it can be bent about an axis in the slip plane normal to the slip direction; and, if the slip plane contains multiple slip directions, it can be twisted or rotated about the slip plane normal. Of the three processes, generally known as translational, flexural, and rotational slip, only rotational slip has not been extensively investigated. The object of the present research was to obtain basic information about this phase of crystalline plasticity. This paper is concerned with some aspects of the stress-strain curves obtained by twisting magnesium crystals about their basal poles. Magnesium was selected for four reasons. One, its recovery rate at room temperature is relatively low. Two, single crystals may be easily grown. Three, at room temperature the critical resolved shear stress for basal slip is about two orders of magnitude lower than that for nonbasal slip, so that rotational slip might be expected to occur primarily by basal slip. Finally, relationships between flow stress, shear strain, and dislocation density have been determined for tensile deformation of magnesium crystals,' thereby providing a basis of comparison for the torsional results. EXPERIMENTAL PROCEDURES Crystals were grown from 0.5 in. diam extruded sublimed magnesium rod furnished by the Dow Chemical Co. who reported that it contained in weight percent less than 0.0003 Al, 0.01 Ca, 0.01 Cu, 0.0012 Fe, 0.001 Mn, 0.0005 Ni, 0.003 Pb, 0.001 Si, 0.01 Sn, and 0.02 Zn, with the balance magnesium. All crystals were grown in a dried argon atmosphere using Jill-son's2 modified Bridgman technique. Two different methods were used to obtain crystals with the basal plane normal to the specimen axis. These included direct growth from seeds of the proper orientation, and spark machining (trepanning) of 0.5 in. diam cylinders from larger (1.5 in. diam) randomly grown crystals. The crystals thus produced were polished in a 20 pct HC1 water solution and then etched in a 1 pct HC1 water solution to develop etch pits lying in rows parallel to the basal plane trace. The crystals were then revolved about their axes on the stage of a low-powered microscope. Torsion specimens were prepared only from those crystals whose axes were normal to the rows of etch pits. It is estimated that this simple orientation method was accurate to about 51 deg. 1.625 in. long cylinders were next cut from these selected crystals and then acid machined in a 20 pct HC1 water solution into torsion specimens with a 1 in. long by 0.30 in. diam reduced gage section. Following this, they were annealed in air at 400°C and furnace cooled to room temperature. The specimens were given a final polish in a 10 pct HC1 water solution, rinsed in ethanol, dried, and cemented into brass grips with an epoxy resin. In addition to the torsion specimens, several tensile specimens with their basal planes at 45 deg to the stress axis were also prepared with similar dimensions except that the gage sections were increased to 4 in. in length. The torsion specimens were tested in the apparatus

Jan 1, 1970

By R. A. Morse, W. O. Keller

The properties of limestone reservoir rocks such as the distribution and degree of continuity of the pore systems, and the relative volumes and permeabilities of the systems making up the complex cause large variations between performance of individual limestone reservoirs and their susceptibility to secondary recovery methods. The effects of these factors on the mechanism of fluid flow cannot be adequately evaluated with presently developed concepts, laboratory data, and geological information. The observance and interpretation of the performance of individual limestone reservoirs provides, at present, the most adequate approach for evaluating the integrated effects upon performance of the many. now immeasurable variations in the properties of limestone reservoirs. INTRODUCTION The development and application of techniques for increasing the efficiency of oil recovery from natural reservoirs is a problem of primary importance to the industry. During the past several years, a great deal of effort has been expended by the technical personnel of the industry toward the improvement of present known methods of oil recovery. and evaluating the factors which control the susceptibility of particular reservoir types to economic application of secondary recovery methods. Providing adequate and accurate laboratory data on the properties of the reservoir rock and its contained fluids. together with good production statistics, are available, methods have been evolved for estimating with reasonable accuracy the performance of an oil reservoir under either continued natural depletion or conditions imposed by introducing additional displacing fluid into the reservoir from an extraneous source through the injection of gas and/or water. The susceptibility of limestone reservoirs to secondary recovery by gas injection is very much dependent upon gas-oil relative permeability relationships for the reservoir in question. In a rock formation in which the porosity is of the intergranular type such as is found in sand stones and some non-fractured dolomites, a representative sample of the pore structure can be obtained in a small core plug. In this type of reservoir, it has been shown that relative permeability data obtained from laboratory experiments can be Properly applied to evaluate the flow relationships actually observed during the depletion of a reservoir. In addition, a good idea of the fraction of the reservoir which will be swept by the injected gas may be obtained from the spacing pattern used and the permeability profile of cored wells. From these data, it has been demonstrated that reliable estimates of performance and recoveries under gas injection operations can be made for reservoirs in which the Porosity is of the intergranular type. Limestone reservoirs on the other hand often present much more complex problems. One reason that the performance of limestone reservoirs is so variable is that there may be, in reality. two or more pore systems, the integrated performance of which will depend upon the physical properties of each system and their inter-relationship. For instance, in a limestone reservoir, the main pore structure, as far as void spaces for storage of hydrocarbons is concerned, may be represented by the intergranular openings of the rock. Usually in limes and dolomites, the intergranular pore openings are very small and the matrix permeabilities extremely low. Often, as in the case of Many dolomite and oolitic lime reservoirs, this is the only pore system, and performance is observed to be very similar to that of a sand stone of similar permeability. However, in the great majority of' the limestone reservoirs, there is present, in addition to the intergranular pore system, a complementary system of openings caused by fracturing or solution.',' The openings in the latter system are usually many times more permeable than the intergranular pore system due to their much larger size, and may contribute almost all the fluid carrying capacity of the formation, even though their volume may be a very small part of the total pore space in the reservoir. Obviously, the performance of such a complex under either primary or secondary control will deend upon the distribution and degree of continuity of both systems, the relative volumes and permeabilities of the

Jan 1, 1949

By T. V. Philip, R. E. Lenhart

When commercial silicon iron sheets of varying magnetic quality are isothermally annealed at high temperatures, extremely large grains develop in the material having good magnetic properties. These grains are of the (110) [001] orientation and are formed by secondary recrystallization. The primary driving force for this secondary recrystallization is grain boundary free energy. For the secondary grains, activation energies of 103 kcal per mole for nucleation, and of 75.5 kcal per mole for growth, were obtained. The activation energy for nucleation of the secondary grains is consistent with a model involving redistribution of a precipitate acting as the primary grain growth inhibitor. SINGLY oriented silicon iron sheet was first produced in 1935.1 The material as commercially produced today has a very highly developed preferred orientation or texture; up to 95 pct of the grains are crystallographically oriented with their (110) planes in the plane of the sheet and their [loo] directions parallel to the rolling direction. This texture, usually written as (110) [00l], is referred to as the "GOSS" or the "cube-on-edge" texture. Because the magnetic properties of this material are superior to those of the nonoriented sheets in the direction of rolling, the oriented silicon iron has acquired tremendous industrial importance especially in the manufacture of transformer cores and other electrical equipment. The commercially produced material is essentially an iron-silicon alloy containing about 3 1/4 pct Si with minor impurities totaling less than 0.15 pct. The silicon steel heat is melted in the open hearth or electric furnace. The ingots are hot rolled, with or without being slabbed, to strips of 0.100 to 0.080 in. thickness. They are then cold reduced to an intermediate thickness, recrystallized, cold reduced to final thickness, decarburized, and finally annealed at a high temperature. During this high-temperature anneal, extremely large grains with the cube-on-edge texture are produced in the sheet. Several papers have appeared in the literature2-10 relating to the production of the Goss-textured material. Most of these describe the textures produced on cold rolling and on subsequent annealing of single crystal or polycrystalline silicon iron. May and Turnbull11,12 have recently shown the necessity of a second-phase dispersed impurity in the material for the production of the Goss texture. However, none of these papers describes in detail the nucleation and growth kinetics of the (110) [001] grains during the final high-temperature anneal.* The present work, therefore, is an attempt to understand the nucleation and growth kinetics of the cube-on-edge grains in the silicon iron sheet during the final high-temperature anneal.

Jan 1, 1962

By John Chipman, Theodore B. Winkler

In order to understand more fully the complexities of the reactions occurring between the liquid steel and the slag in the basic open-hearth steelmaking furnace, investigations in this country and. abroad have turned to laboratory equilibrium studies. This paper is one of a series of reports on investigations being conducted at the Massachusetts Institute of Technology. The experimental work was completed early in 1942. The slag systems found in the basic open hearth are very complex, being made up of at least eight major components and as many others whose effect might be classified as minor. The first two papers of the series, by Fetters and Chipman,l,2 as well as the paper by Taylor and Chip-man,3 dealt with the simplest possible slag system that would resemble those found in the basic ope), hearth—the slag system consisting of CaO-MgO2-SiOz-FeO. (Taylor's rotating induction furnace eliminated the necessity of contamination of the slag by MgO.) Having arrived at some reasonable conclusions regarding the physical chemis- try of the reactions between molten iron and the simple slags at equilibrium, the next step was to investigate more complex slag systems. The major purpose of the present investigation was to determine what factors control the distribution of phosphorus between molten iron and the more complex basic slags at equilibrium, and to what extent these factors are influential. The slags used contained CaO, MgO, SiO2, FeO, Fe2O3, P2O6, MnO, Al2O3 and CaF2, but not all of the slag samples contained all of these components at one time. Review of Literature Although a number of interesting papers have been published on the subject of dephosphorization of an iron bath, there are as yet no results from laboratory studies that give thoroughly reliable information on the dephosphorization reaction. Even for the supposedly simple Fe-O-P system involving iron-phosphorus melts and iron oxide-iron phosphate slags, the experimental results are contradictory and no formulas have been established that adequately fit the equilibrium conditions. The Fe-O-P system has been studied by Schackmann and Krings,4 von Samson-Himmelstjerna,6 Oelsen and Maetz,6 Bischof and Maurer,7 Diepschlag and Schürmann,8 and Herty,9 and the results of their investigations appear in Table I. A number of different equilibrium constants and distribution . Ratios

Jan 1, 1947

By Theodore B. Winkler, John Chipman

In order to understand more fully the complexities of the reactions occurring between the liquid steel and the slag in the basic open-hearth steelmaking furnace, investigations in this country and. abroad have turned to laboratory equilibrium studies. This paper is one of a series of reports on investigations being conducted at the Massachusetts Institute of Technology. The experimental work was completed early in 1942. The slag systems found in the basic open hearth are very complex, being made up of at least eight major components and as many others whose effect might be classified as minor. The first two papers of the series, by Fetters and Chipman,l,2 as well as the paper by Taylor and Chip-man,3 dealt with the simplest possible slag system that would resemble those found in the basic ope), hearth—the slag system consisting of CaO-MgO2-SiOz-FeO. (Taylor's rotating induction furnace eliminated the necessity of contamination of the slag by MgO.) Having arrived at some reasonable conclusions regarding the physical chemis- try of the reactions between molten iron and the simple slags at equilibrium, the next step was to investigate more complex slag systems. The major purpose of the present investigation was to determine what factors control the distribution of phosphorus between molten iron and the more complex basic slags at equilibrium, and to what extent these factors are influential. The slags used contained CaO, MgO, SiO2, FeO, Fe2O3, P2O6, MnO, Al2O3 and CaF2, but not all of the slag samples contained all of these components at one time. Review of Literature Although a number of interesting papers have been published on the subject of dephosphorization of an iron bath, there are as yet no results from laboratory studies that give thoroughly reliable information on the dephosphorization reaction. Even for the supposedly simple Fe-O-P system involving iron-phosphorus melts and iron oxide-iron phosphate slags, the experimental results are contradictory and no formulas have been established that adequately fit the equilibrium conditions. The Fe-O-P system has been studied by Schackmann and Krings,4 von Samson-Himmelstjerna,6 Oelsen and Maetz,6 Bischof and Maurer,7 Diepschlag and Schürmann,8 and Herty,9 and the results of their investigations appear in Table I. A number of different equilibrium constants and distribution . Ratios

Jan 1, 1947

By S. F. Urban, G. Derge

At the time this investigation was initiated variations were observed in the quality of different heats of basic electric-furnace steels, although they had been made under purportedly similar conditions. This indicated that these variations were related to normally unobserved variations in the character of the bath, especially during the "refining" period. Although the slags used for this operation are commonly referred to as "reducing" slags, and are regarded as having a "deoxidizing" action on the bath, no reliable measurements of this action were available. It was decided, therefore, to study the behavior of oxygen in the metal for ' large enough number of heats to learn its normal variations and to relate these variations to regularly observed conditions of operation. The most important general conclusion reached was that the time a heat is held under a reducing 'lag should be reduced to a minimum, which was about an hour and a half under the conditions studied. Beyond this time no observable beneficial effects are obtained from the reducing slags, insofar as oxygen and sulphur content of the bath are concerned. It is likely that added time may increase hydrogen content as well as heat costs. The oxygen content of the bath is never reduced below the amount in equilibrium with the carbon. Concurrently with this work, J. S. Marsh1 presented data that supplement and support many of the results of this paper. Procedure The work was done in two different electric-furnace shops of the same plant. The selection of heats was made primarily with regard to the convenience of heat schedules. companion slag and metal samples were taken just prior to slag-ofi and throughout the refining period for an initial set of 17 heats, and before slag-off and near tap for an additional I3 heats. slag Sampling presented no particular problem; a spoonful of slag was poured onto a metal plate and when sufficiently cool was sealed in an airtight container. Sampling the metal for oxygen presented a more complex problem. Because of the lack of previous experience in sampling electric-furnace baths, a number of methods were compared. Chilled Wedge Samples2 An unkilled metal sample is removed from the furnace in a well-slagged car-bometer spoon and poured immediately into a heavy copper mold designed to provide rapid freezing. Three different types of molds were used to determine the optimum for electric-furnace hats. The Big wedge Mold (a) was a 4 by 4 by 4-in. split copper mold, yielding a wedge-shaped casting I in. wide, 1 1/2 in. long, and 34 in. maximum thickness, and was finally adopted as the most satisfactory design.

Jan 1, 1948

By W. A. Scheuch, J. Walter

Ordinarily secondary copper, unless electrolytically refined, is reclaimed directly as foundry ingots used in the manufacture of copper-rich alloy castings. This use does not require the elimination of the impurities to the degree required if the recovered'metal is to be used for electrical purposes where a high electrical conductivity is of prime importance. However, as a part of the general policy of reusing its own scrap and by-products wherever possible, the Western Electric Co. at its Hawthorne Works is recovering its secondary copper as wire bars which are delivered to its own rod and wire mill and there processed into wire of high electrical conductivity. This departure from the usual recovery scheme has been accomplished through the careful classification and sorting of the material entering the furnace charges and the careful control of the subsequent melting and refining in a reverberatory furnace. Tests conducted over a period of approximately four years have shown that the quality of wire bars produced from selected secondary copper is equal to that of wire bars produced by the electrolytic refineries. The interest which has been exhibited in the process by those who have seen it has prompted the following general description. It is the authors' opinion that the recovery of secondary copper will become more and more an important factor in the copper production industry. The description is largely of the refining furnace and its operation, but it must be remembered that careful classification and sorting of the scrap materials to eliminate impurities are just as important as the furnace operation toward obtaining a satisfactory final product. Classification and sorting do not lend themselves easily to description; they must, just be done. It should also be recognized at the outset that constant intelligent supervision is requisite to the success of the process because there are so many ways in which impurities can find their way into the final product. Secondary Copper Used for Wire Bars Only clean secondary copper of the grades known to the trade as Numbers 1 and 2 are melted for wire-bar manufacture. This material, supplemented by that obtained from various manufacturing processes

Jan 1, 1930

By Charles O. Burgess

The improvement in the quality of cast iron by means of alloy additions has been a metallurgical accomplishment of recent years. Work in this field has shown that chromium is one of the most effective of such additions but, in general, the influence of chromium has been studied only in connection with other alloying additions, with irons other than foundry irons, or with relatively high percentages of chromium. The present study was initiated for the purpose of determining the influence of small additions of chromium (0.25 to 1.00 per cent) on the quality and resultant properties of cast irons of various foundry grades. The effect of small chromium additions on cast iron was investigated with particular reference to casting characteristics, hardness vs. section, strength, machinability, heat resistance and structure. Material Tested Three separate types of cast iron were investigated as to the effect of small chromium additions. The first series of these irons was prepared from remelted foundry cast iron at the Union Carbide and Carbon Research Laboratories, and the other two series consisted of cupola melts made under usual operating conditions. The first series was made by melting 30-lb. charges of foundry scrap iron containing 2.86 per cent carbon, 2.72 silicon, 0.50 manganese, 0.062 sulfur and 0.794 phosphorus in a carbon resistance furnace. The chromium was added as high-carbon ferrochrome just before pouring. The irons were cast at approximately 1250" C. (2282" F.). The analysis and physical properties of these irons are given in Table 1, test 1. The second set of cast irons was made in a cupola in accordance with normal practice, the charge containing approximately 42 per cent steel scrap and the chromium additions being made to the ladle. Analysis and tests of these heats are shown in Table 1, test 2. A small amount of copper was present in heat C of this series. Further data on the effect of chromium on strength were obtained from a third series of 13 cupola heats containing from 0.06 to 0.50 per cent chromium and made without steel additions. The heats were all

Jan 1, 1933

By W. A. Griffith

The fundamental principles and modern techniques of experimental planning and data analysis, applicable to any type of research, are particularly important in flotation experimentation. Since they constitute the modern science of experimentation, they should be among the working tools of any scientist, research engineer, or plant operator engaged in flotation investigates. This chapter is a review of these principles and techniques. Equipment and procedures for the actual conduct of experiments will not be discussed here since these subjects are well covered elsewhere in this volume. Neither will any attempt be made to impart a working knowledge of statistical methods of data analysis since this would be impossible in the space allotted, and many excellent texts are available to the diligent inestigator.1-4 The objective here is simply to interest the reader in the application of statistical techniques to flotation experimentation by illustrating their utility in situations frequently encountered, and to point out the principles of experimental planning necessary for their proper use. Any conscientious metallurgist engaged in flotation experimentation or operations is well aware of the inherent complexity of the flotation process, and of the often frustrating difficulties this introduces into experimentation. The raw materials normally treated by the process are complex both physi- cally and chemically, and often highly variable even when from the same source. The flotation process itself is characterized by a very large number of potentially important process variables. Many of these are beyond the con- trol of the metallurgist, and some cannot even be measured quantitatively with available instruments. Those which can be measured and controlled with reasonable precision often produce effects which are intricately interrelated. Not only are the variables many, but the physical and chemical mechanisms by which they function are imperfectly under stood. To compound the difficulty, experimental techniques are relatively crude. Controls are not very precise, and the human factor looms large in most flotation experiments. These situations lead inevitably to experimental data of a relatively low degree of precision or reproducibility. Some are inclined to think that these conditions are unique to flotation experimentation. They are not. The experimental problems met by the agronomist, the biologist, the social scientist, and others are equally complex. Investigators in these fields pioneered in the development of methods for handling just such situations by proper experimental planning and the application of statistical methods in the analysis of data. Their pioneering work has grown into a well established modern science of experimentation which has spread into every field of science. This science is based upon statistical

Jan 1, 1962

By Howard Scott

INVAR is the preeminent low-expansion metal by virtue of the fact that it can be prepared with a zero coefficient of expansion at atmospheric temperature. This fact suggests that there is little room for improvement in the expansion properties of the low-expansion nickel steels. The inference is true, however, only so far as the expansion at and near atmospheric temperature is concerned, because the expansivity of invar starts to increase rapidly on heating above 100° C. and soon reaches the value of copper. Guillaume1 met this situation by increasing the nickel content above that of invar. By that expedient, alloys having low expansivity under higher temperatures were obtained, but not without a large increase in minimum expansivity. The increase in minimum expansivity with increasing nickel content severely limits the technical applications of these alloys at high temperatures. Prospects of improving the expansion characteristics of the nickel steels is offered by alloying. Search for an advantageous alloying addition by analogy with other alloy systems, however, is not productive because the low-expansion characteristic is unique with that system. The rule of mixtures usually gives a fair value of the expansivity of other solid-solution alloys, but in the iron-nickel systems gives a value of 18 X 10-6 per deg. C. whereas the actual value is 1 X 10-6 per deg. C. Apparently suitable additions are not to be deduced from such ingenuous considerations. Recognition of the fact that the temperature range of low expansivity in nickel steels is terminated with loss of magnetism affords a more promising basis for the selection of an advantageous element. One may expect from that fact that additions of nonmagnetic elements to the iron-nickel alloys are detrimental to the low-expansion characteristic. Indeed, carbon, manganese, silicon, copper and chromium are detri-mental to the expansion properties and no nonmagnetic element is reported to be beneficial. From the same viewpoint, the addition of a magnetic metal offers prospects of improvement. As two of the three ferromagnetic elements are already present in the

Jan 1, 1930

By I. W. Alcorn

THE cost of drilling in the past few years of proration and ever decreasing allowables has received increasing thought and study. It seems to parallel the strides made with respect to pumping problems in 1932 and 1933. Low profit margins stimulate the search for economies. Any discussion of slim-hole drilling involves a multitude of abstract values, and the problem can be attacked only by a study of records and rational thinking. In a measure, traditional methods must be studied with a questioning attitude. The words "slim hole" may be somewhat misleading, as the term is entirely relative. For that reason I wish to define it as used in this discussion. On the Gulf Coast, I would define a normal hole as one in which 10 3/4-in. surface casing has been set and below which a 9 7/8-in. hole is dug. With this as a datum, holes of larger diameter below surface would be called "large holes," with 12 1/4 in. as the "extra large" class and holes of smaller diameter classed in the slim-hole range, 6 1/4 in. representing about the minimum size. The optimum size has not been definitely determined, but the preference is for a program that would call for setting 8 5/8-in. surface casing and digging a 7 3/4-in. hole. Different sections of the country might very properly deviate from this practice because of differences in depth, formations, regulations, or other factors. This paper will be confined to a discussion of the drilling of exploratory wells, as the drilling of this class of wells is quite a different problem from that of drilling a proven field, although many of the same considerations apply in both cases, as will be apparent. Although for many years shallow slim-hole and core-test holes of small diameter had been dug, it was not, I believe, until the fall of 1937 that serious consideration was given to its application in drilling wells 7000 ft., 8000 ft. and 9000 ft. deep on the Gulf Coast. This does not mean that nearly all such wells drilled on the Gulf Coast now are of the slim-hole variety, but only that efforts have been aimed in that direction with very encouraging results and there has been a very definite trend to reduce the size of holes, a trend that probably will continue. As to exploration policy, there appear to be two distinct and opposite views. The one usually followed in the past was more or less designed to "shoot the works" on one well. Generally on the Gulf Coast, the depth at which production might be obtained is limited by the drilling equipment and economics. With this thought in mind, wildcat wells are often planned with the idea of carrying the depth to 10,000 ft., or even 15,000 ft. All of the possible hazards are anticipated and the general drilling and casing programs are so predicated. Such wells contemplate the drilling of large-diameter holes; the setting of at least one protective string of casing and an extensive coring policy, all of which finally adds up to an expensive well. As opposed to this general policy is the slim hole. This, on the Gulf Coast, recognizes that new discoveries represent gam-

Jan 1, 1941

Discussion of the paper of C. W. WASHBURNE, presented at the Pittsburgh meeting, October, 1914, and printed in Bulletin No. 93,. September, 1914, pp. 2365 to 2378. ROSWELL H. JOHNSON, Pittsburgh, Pa.-It seems to me rather important to bear in mind one thing which is sometimes lost sight of, that the marine sedimentary rocks are laid down in water. We have to start with an initial charge of water. That being so, and the surface tension between the water and the -oil being as slight as it is, as referred to by Mr. Washburne,. the phenomena of capillarity are bound to be most important as between the liquid surface and the gas surface. So far as the liquid-gas surface is concerned, capillarity, in my opinion, is of the utmost importance, and it seems to me this paper of Mr. Washburne's is of great value to us for that reason. Starting out as we have, with our attention concentrated upon gravitational sorting, we have had to wait for the discussion of movement furnished by Munn, and this discussion of capillarity by Washburne, for a more balanced view of the situation. It seems to me that in the accumulation of oil and gas we have a problem of the interworking of gravitational sorting, capillarity, viscosity, immiscibility, and movement. All five things seem to me to be important. I would have expected Mr. Washburne to have given a fuller treatment of the relation of movement to capillarity. In my own experiments I find that gravitation and capillarity alone seem remarkably impotent when everything is at rest, but if I furnish a little movement, gravitation and capillarity step in and accomplish a great many results that one would not expect. Take a horizontal tube and fill a portion at the middle with an ordinary sand saturated with oil, and then put water and sand in each end, and the tube may remain at rest a very long time without that oil distributing itself along the top of the tube. But with a little motion that oil will gradually work up to the upper side. So gravitation and capillarity alone are rather impotent unless they get this element of movement. It would not be necessary to have very extensive movement, but some degree of movement is essential. Now if natural gas, in addition to the method of origin by the action of bacteria on organic matter in mud, may also arise by pressure at great depth, as the overburden is added, a great deal of motion may result. I think more motion is produced in this way than by the descent of meteoric waters.

Jan 4, 1915

By A. E. Lehman

A RECENT demand for some form of panoramic display of an important railway line, showing its branches, connections, and terri tory controlled by it, revealed to the writer the advantages of' a topographical model or relief map fix this purpose. Hitherto, maps of this nature have been used chiefly for scientific and geographical purposes, and confined to a comparatively narrow field of service. They deserve to become more popular and to have their advantages better understood. Much has been written and accomplished in this direction by Prof. Lesley, Messrs. Harden, Moulten, de Mendonca Cortez, and others; but I believe their pub lished descriptions of the methods employed in the construction of these models are confined to those used by themselves. It is the writer's aim to present in condensed form these various methods, and some suggestions of practical value as to the most economical course of procedure, as well as to mention some of the uses that may be made of the results obtained Methods of Construction.—Many different materials have been prepared and used in the preparation of relief maps, such as metal, clay, plaster, gypsum, wax, putty, Card-board, papier-mache, wood, and compositions of varions kinds, with results more or less success ful : wood, however, in the writer's experience, has been found to be by far the most satisfactory, combining the advantages of stability, accuracy and ease of handling. The following is a brief description of several of the methods used in constructing topographical models : When clay, wax, putty, compositions or materials of a plastic nature are used, the operator carries his work up from its base by means of measurements or by the eye, manipulating and shaping the material as best he can, ac cording to such features of his subject as he wishes to delineate. This process requires remarkable skill, and given this, will probably fall short even then of an approximation to accuracy; lacking essential elements of detail nil over the work and exactness, particularly in position and elevation of the most important points in the territory mapped. When either of the above mentioned materials or compositions are used, metal or wooden pins are sometimes driven into the base or level datum plane of wood, the top of these pins giving the eleva-

Jan 1, 1886

By S. F. Urban, G. Derge

At the time this investigation was initiated variations were observed in the quality of different heats of basic electric-furnace steels, although they had been made under purportedly similar conditions. This indicated that these variations were related to normally unobserved variations in the character of the bath, especially during the "refining" period. Although the slags used for this operation are commonly referred to as "reducing" slags, and are regarded as having a "deoxidizing" action on the bath, no reliable measurements of this action were available. It was decided, therefore, to study the behavior of oxygen in the metal for ' large enough number of heats to learn its normal variations and to relate these variations to regularly observed conditions of operation. The most important general conclusion reached was that the time a heat is held under a reducing 'lag should be reduced to a minimum, which was about an hour and a half under the conditions studied. Beyond this time no observable beneficial effects are obtained from the reducing slags, insofar as oxygen and sulphur content of the bath are concerned. It is likely that added time may increase hydrogen content as well as heat costs. The oxygen content of the bath is never reduced below the amount in equilibrium with the carbon. Concurrently with this work, J. S. Marsh1 presented data that supplement and support many of the results of this paper. Procedure The work was done in two different electric-furnace shops of the same plant. The selection of heats was made primarily with regard to the convenience of heat schedules. companion slag and metal samples were taken just prior to slag-ofi and throughout the refining period for an initial set of 17 heats, and before slag-off and near tap for an additional I3 heats. slag Sampling presented no particular problem; a spoonful of slag was poured onto a metal plate and when sufficiently cool was sealed in an airtight container. Sampling the metal for oxygen presented a more complex problem. Because of the lack of previous experience in sampling electric-furnace baths, a number of methods were compared. Chilled Wedge Samples2 An unkilled metal sample is removed from the furnace in a well-slagged car-bometer spoon and poured immediately into a heavy copper mold designed to provide rapid freezing. Three different types of molds were used to determine the optimum for electric-furnace hats. The Big wedge Mold (a) was a 4 by 4 by 4-in. split copper mold, yielding a wedge-shaped casting I in. wide, 1 1/2 in. long, and 34 in. maximum thickness, and was finally adopted as the most satisfactory design.

Jan 1, 1948

By D. F. Kaufman, V. V. Damiano, G. J. London, L. R. Aronin

Beryllium bicrystals were Prepared by a seeding and floating zone-melting technique from high-purity beryllium single-crystal material. The starting material was given six floating zone purification passes prior to producing the bicrystals. Symmetric, asymmetric, and antisymmetric bicrystals were tested in tension. Included were bicrystals with boundaries both parallel and perpendicular to the tension axis. Modified symmetric bicrystals were also examined in detail. In these cases, the angles made by the slip planes with the boundary were not equal. Failure by (0001) cleavage, (1180) cleavage, and boundary separation were all observed depending on the orientation of these cleavage planes and the boundary with respect to the tension axis. Failure occurred on whichever system experienced the greatest normal stress. The origin of the fractures observed and the operative dislocation mechanisms were investigated by frac-tography and transmission electron microscopy. The results indicate that low-angle boundaries form in close proximity to the bicrystal boundary and act as sites for crack nucleation. It has been concluded that, although macroscopic compatibility was satisfied in many of the bicrystals examined, the bicrysta1 boundary was effective in Producing "early" failure by local bend plane formation as plastic deformation proceeded, followed by cleavage initiation and crack propagation. SINGLE crystals of high-purity beryllium oriented with the basal plane inclined 45 deg to the tension axis exhibit a critical resolved shear stress of about 300 psi and 200 pct extension by slipping only on the basal plane before failure by cleavage on that plane. Single crystals, oriented with the basal plane parallel to the tension axis, deform by prism slip at a critical resolved shear stress of 9000 psi and exhibit an extension of over 100 pct before failure in a ductile manner.' In contrast to the behavior of single crystals, poly-crystalline beryllium deformed in tension or bending exhibits little or no ductility at room temperature. Beryllium's lack of ductility at room temperature has been attributed to its lack of a sufficient number of independent slip systems. Beryllium has only four independent slip modes at room temperature and according to the Taylor2 and von Mises3 criteria at least five independent shear modes are necessary to completely satisfy the strain compatibility conditions at all the boundaries in a random polycrystalline sample. Studies of beryllium bicrystals thus appear to provide a convenient way in which to determine whether the condition of strain compatibility is a necessary and sufficient condition to prevent failure and whether obviously incompatible boundary conditions result in boundary separation. Bicrystal studies, although not providing all of the constraints encountered in polycrystalline samples, do allow one to select very specific orientation relation-

Jan 1, 1969