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By R. M. Caves

High-purity dense tungsten coating is obtained by means of a modified de Boer-van Arkel iodide process using tungsten bromides. The all-glass reaction system is pumped, baked, and sealed (pinched-off) at about 10-7 mm Hg pressure. The bromides then formed in situ are decomposed, depositing tungsten on heated tungsten surfaces. Heating of the specimen is done inductively in a novel arrangement that avoids electrodes of glass-to-metal seals. The tungsten, deposited at specimen temperatures from 2000° to 2800°F and bulb (halide) temperatures of 225" to 725°F, was adherent and uniform, and ranged in thickness to 1/8-in. REFRACTORY metals are of interest at NASA for use in hypersonic aircraft, in rocket engines, and in other thrust devices where very high temperatures are encountered. Tungsten, with a melting point about 6100° F, is potentially very useful for some of these applications. Considerable research on tungsten and its alloys is currently being conducted at the NASA Lewis Research Center. In this tungsten research program, there is need for a method of depositing high-purity, nonporous tungsten coatirlgs. Metallurgical bonding of the coating both to itself and to the substrate is required. In addition, it is necessary to be able to deposit thin, uniform coatings on substrates of a variety of shapes and sizes for laboratory test purposes. A survey of the methods previously used for depositing tungsten coatings indicated that none would likely meet these requirements for high purity, good uniformity, and high density except thermal decomposition of the halides. The method for coating that was selected for investigation was the thermal decomposition of tungsten bromide. This is a variation of the van Arkel and de Boer iodide process established years ago and recently reviewed.1,2 This process is applicable to the transition metals in general. More recently, the application and techniques were extended with chlorine3 and fluorine,4 and included the coating of tungsten. This is believed to be the first report on the use of the bromide for tungsten coating. Bromine was chosen over the other halogens because it promised a lower temperature for tungsten

Jan 1, 1962

By W. T. Cardwell, R. L. Parsons

This paper discusses the practical problem of estimating a single equivalent permeability for an oil reservoir, or a portion thereof, whose actual permeability varies in an irregular manner. Limiting averages for general types of permeability variation are developed, and illustrated by examples involving important, specific types of variation. Introduction The theory of the flow of fluids through porous media1"4 is becoming increasingly important in predictions of oil-reservoir behavior. In practical applications, however, reservoirs are seldom found to which simple theory strictly applies. Actual reservoirs have complicated shapes and nonuniform permeabilities and porosities. This paper discusses the problem of estimating a single equivalent permeability for an oil reservoir, or a segment of an oil reservoir, whose actual permeability varies in an irregular manner. The equivalent permeability of a reservoir segment is defined as the permeability of a homogeneous segment of the same dimensions that would pass the same flux under the same pressure drop- It is the permeability value that can be used in simple theoretical formulas to calculate the reservoir behavior. To the authors' knowledge, previous theoretical calculationst on systems of nonuniform permeability have been carried out only by Muskat'"; and he has not dealt with irregular variations, except in writing down the general differential equation for the pressure in variably permeable systems.lb In practical work, many calculations necessarily have been made to estimate equivalent permeabilities from the permeabiiity profiles obtained by core analyses. Regarding such calculations, Johnston and Sherborne6 say: Simple arithmetic and weighted averages have been tried on many wells and it has been found that, where frequent sampling has occurred, the arithmetic average is as satis- factory as a weighted average. It is possible that the application of statistical methods to the analysis of permeability data as recently presented by Law8 may prove fruitful. L,, has made a valuable contribution in showing how statistical analyses may aid in picturing the characteristics of a reservoir from those of a necessarily limited number of core samples. It is believed however that the particular problem of the estimation of equivalent permeabilities can be most directly approached from a fluid dynamical viewpoint as given in the present paper. An example is presented of the use of the conclusions herein in conjunction with Law's method. Theory In order to approach the problem of heterogeneity simply, it is interesting to consider a square block composed of four smaller, homogeneous, square blocks of porous medium, two of which have a

Jan 1, 1945

By J. B. Morgan

The mechanical behavior of MgCu2 from 20 o to 725°C has been determined by "brittle-ring" tensite-test techniques, axial compression, and bending experiments. Compressive ductility begins at 450°C (0.65 T/Tm) and slowly increases with increasing temperature white the tensile ductility is characterized by an abrupt brittle-ductile transition at 600°C (0.8T/Tm). The compressive strength increases eightfold from room temperature to 400°C with a "normal" decrease as the temperature is further increased. The tensile strength goes through a rather abrupt threefold increase above 600°C with a subsequent decrease at higher temperatures. The slip system is (111)[110] and the twinning system is (111)[112]. At high temperatures MgCu2 is quite rate-sensitive, and dynamic yield points are observed that are extremely orientation-dependent. The high-temperature creep behavior under constant load is characterized by an increasing strain-rate with time. The general characteristics of the mechanical behavior make it possible to classify MgCu2 with those materials in which initial mobile dislocation density and the dislocation velocity-stress dependence are significant in determining mechanical response. Mgcu2 is the C15 prototype of the cubic Laves phase. Its range of homogeneity extends from 32.8 to 35.5 at. pct Mg at 500°C and narrows at lower temperatures. The lattice parameter is reported to vary from 7.02 to 7.05A,1 and the compound is completely ordered to the melting point of 819°C. MgCu2 has a brassy metallic appearance, is extremely brittle, and many of its physical properties are intermediate between those of the constituent elements: the electrical resistivity is 3.5 x 10-6 ohm-cm, Young's modulus is 10x 106 psi, the shear modulus is 6 x l06 psi, and the thermal coefficient of expansion is 18.7 x 10-6 cm per cm per "C from 20" to 250°C. Usually, properties of intermetallic compounds as functions of temperature have been determined by hardness, compression, or impact behavior, and almost all of these experiments have been performed on polycrystalline materials. Tammann and Dahl,2 for instance, determined the onset of ductility in a series of binary intermetallics by ball-hardness measurements and found the onset to range between 0.71 and 0.96 T/T,. Lowrie's3 investigations included some tensile properties, and he found ductility beginning around 0.65 T/Tm for most materials examined. His work did include some data on polycrystalline, nonstoichiometric MgCu2, however. The present work is an attempt to extend the examination of the particular compound MgCu2 in single-crystal form in order to aid the formation of general concepts about mechanical be-

Jan 1, 1965

By H. I. Aaronson, H. A. Domian

The self-diffusivity of Ag10 has been measured as a function of temperature and composition in AgMg. a CsCl-type intermetallic compound with a substitutional defect structure on both sides of the stoichiometric (50 at. pct Mg) composition. These measurements show that In D increases linearly, and both In Do and Q decrease linearly with deviation from stoichiometry. The slopes of these lines are significantly steeper in magnesium-rich alloys. Equations for the variation of Q with composition have been derived by application of the theory of random walk processes on the assumption that diffusion in compounds of this type takes place by the six-jump cycle mechanism of Huntington, Elcock, and McCombie. The favorable agreement obtained with experiment furnishes fresh support for the correctness of this assumption. A principal result of this treatment is that. although the concentration of vacancies is considerably higher in the silver sublattice than in the magnesium sublattice, the acfivation energies for movement of the magnesium sublattice vacancies are so much lower that these vacancies are responsible for effectively all diffusion of silver in this compound. A tendency for vacancies of both types to be kinetically bound to wrong atoms is also noted. THIS study was undertaken to examine the influence of substitutional defects upon self-diffusion in an intermetallic compound, AgMg, with a CsCl-type crystal structure. The CsCl structure is exception- ally simple. At the equiatomic or stoichiometric composition in a binary alloy, it consists of two interpenetrating simple cubic sublattices, each of which is exclusively populated by the atoms of one species. When atomic size and other factors are favorable, deviations from stoichiometry can be entirely accommodated by the substitution of atoms of the species present in excess of 50 at. pct on the sublattice of the other species on a one-for-one basis. Under this condition, the only vacancies present are those formed by thermal activation. The excess atoms thus incorporated into the sublattice of the minority species may be considered as substitutional defects in this sublattice. Several X-ray studies have shown that the defect structure of AgMg is entirely of the substitutional type on both sides of the stoichiometric composition.1"3 The thermodynamic investigation of Kachi indicates that, aside from a low level of thermal disorder and these constitutional defects, order is maintained to the solidus temperature. This compound is therefore a particularly useful vehicle for a study of the influence of substitutional defects upon diffusion kinetics. Other advantages of AgMg for this purpose include: the broad composition region, as much as approximately 10 at. pct on either side of the stoichiometric (50 at. pct Mg), in which the compound is stable; the comparatively low temperature range of the solidus (820°C and below),5 making diffusion anneals near this range experimentally convenient; the reasonably good machinability of the compound, permitting utilization of the standard sectioning method of radiotracer analysis; and the availability of a good tracer, A for one of the constituent species. While this investigation was in progress, Hagel and westbrooks reported data on the self-diffusion

Jan 1, 1964

By R. F. Lynch, J. D. Wood

The Al-1.0 pct Mg alloy 565 7 was studied using optical microscopy and electron microprobe X-ray analysis. Constituent particles were found to exist inter-dendritically in the as-cast material in a region of precipitate free a -aluminum. Five phases besides a fine precipitate and a-Al were identified in the cast structure: Fel3, Fe2Al7, Mg2Al3, CUMgAl2, and Cu2FeAl7. Thermal treatments conducted for 100 hr at 1180°, 1130°, 1080°, 1030°, 980°, and 880° F revealed a general dissolution and spheroidization of the in-terdendritic constituent network observed in the cast structure. The principal constituents present in the thermally treated structures were FeAl3 and Fe2Al7 with the relative amount of Fe2A17 to FeAl3 increasing with a decrease in the treatment temperature. The phases Present in the wrought structure were identical to those observed after the thermal treatments, with the constituent particles strung out in the direction of rolling. ALLOY 5657 is a nonheat-treatable commercial purity Al-1.0 pct Mg alloy utilized extensively because of its bright finishing characteristics. This investigation was conducted to determine the constituents present in 5657 alloy, and to study the effect of extended thermal treatments on morphology. Numerous studies have been carried out to establish the equilibrium diagrams for various aluminum systems,1-3 with phase identification based on X-ray analysis, morphology, and the etching response of relatively large particles. Phragmen4 conducted a study of the phases in aluminum eutectic systems and compiled a "corrected" table of etching responses, drawing on his work plus that of Schrader,5 Keller and Wilcox,6 and Mondolfo.7 A review of the original work of Keller and Wilcox, and Mondolfo, which was concerned with the constituents found in commercial alloys, reveals that in numerous cases their etching responses differ from those reported by Phragmen and from each other. These inconsistencies may occur because a specific constituent will react to a given etch in a varying manner depending upon its size, the elements dissolved in the phase, the other constituents surrounding a phase, and the solute content of the matrix. Work with a commercial orientation was conducted on alloys 2024 and 3003 by Sperry8,9 and on alloy 3003 by Barker,10 where the relationship between the phase diagram and the nonequilibrium structure of an alloy was examined. Backerud11 investigated the A1-Fe binary system and found that at high cooling rates the equilibrium eutectic reaction forming a-A1 and FeA13 is replaced by another lower temperature eutectic reaction forming a-A1 and metastable FeAl6, a constituent first identified by Hollingsworth et al.12 Most of the above mentioned studies were conducted on materials having a significantly greater alloy content than 5657 alloy, where the relatively small size and sparse distribution of second phase particles hinders the process of identifying constituents. EXPERIMENTAL PROCEDURE Material with a composition as given in Table I was examined in the as-direct chill cast, hot rolled and cold rolled conditions, and after thermal treatment of the cast structure. Thermal treatments were terminated by a water quench. Microscopic examination was conducted under various lighting conditions following the application of standard etchants as specified in Table 11. A semi-quantitative electron microprobe X-ray analysis was conducted for Al, Mg, Fe, Cu, Si, Zn, and Ti. RESULTS AND DISCUSSION Microstructure of the As-Cast Material. Particles of second phase material were found to exist inter-dendritically, principally in regions of precipitate free a-Al, as illustrated in Fig. 1. Adjacent to the ingot edge was a region of inverse segregation, resulting in an increased amount of second phase material containing large sized particles which aided in phase identification. Phase Identification. Cast Structure. Five phases besides a-Al and a fine precipitate were identified using optical microscopy and electron microprobe X-ray analysis, as presented in Tables II and III, respectively. FeA13 and Fe2A17 are often found with Fe2A17 forming a sheath around the core of FeAl3, resulting from an incomplete peritectoid reaction. These phases have a nearly identical appearance under white light, although they are easily differentiated under crossed polarizers, as characteristically illustrated in Figs. 2(a) and 2(b), respectively. Microprobe analysis con-

Jan 1, 1970

By E. S. Davenport, R. J. Hafsten, R. A. Grange

The influence of austenite grain size upon the hardenability of steel is now fairly well understood; for a given austenite, increasing the grain size increases the depth of hardening, and, since the latter is related to the fundamental transformation behavior of austenite, it follows that austenite decomposition must, in general, be retarded by increasing grain size. To date, very little quantitative information bearing directly on the effect of austenite grain size upon the progress and result of isothermal transformation has been published. Davenport and Bain,' and Zimmerman, Aborn and Bain2 have shown that the transformation is definitely relarded in hypereutectoid plain carbon steels at temperatures near and above the upper region of rapid transformation (Ar') when the austenite grains are increased in size. More recently, Griffiths. Pfeil and Allen3 investigated the effect of a series of different heating (austenitizing) temperatures upon the progress of isothermal transformation at 1245°F. (675°C.) and 745ºF. (395°C.) in a medium carbon, low-alloy steel; while they reported no measurements of the austenite grain size, their results suggest that increase in grain size retards austenite transformation at 1245ºF. (675°C), but has no appreciable effect at 745°F (395°C.). The present paper deals with the results of a study of the isothermal transformation of austenite in a single commercial alloy steel in which a fine-grained or a coarsegrained state was induced by appropriate selection of austenitizing temperature. The data are presented in the form of isothermal transformation diagrams, which clearly show that coarsening the grains lessens the rate of transformation of austenite to proeutectoid ferrite and pearlite—that is, at temperature levels above about 1000°F. (540°C.)—but is without significant effect at lower temperatures where the transformation product is bainite or martensite. It is to he presumed that the foregoing statement would be valid, at least in principle, for many other grades of steel; it confirms again that the mechanism of transformation to a pearlitic structure is fundamentally different from that to an acicular structure. A number of related observations were made, which seem to throw some light on the transformation process as it takes place in alloy steels, particularly at temperature levels in the vicinity of 1000ºF. (540°C.), where the transition from lamellar to acicular structures occurs. These data are discussed briefly in the belief that they may lead to a clearer understanding of this aspect of the subject. Material and Experimental Procedure The material investigated was a cornmercial grade of S.A.E. 4140 steel, the composition of which was as follows: 0.37 per cent C, 0.77 per cent Mn, 0.98 per cent Cr and 0.21 per cent Mo. It was hot-rolled to a 1 1/8-in. round bar and normalized by air-cooling from 1800°F. (980°C.).

Jan 1, 1941

By R. J. Hafsten, E. S. Davenport, R. A. Grange

The influence of austenite grain size upon the hardenability of steel is now fairly well understood; for a given austenite, increasing the grain size increases the depth of hardening, and, since the latter is related to the fundamental transformation behavior of austenite, it follows that austenite decomposition must, in general, be retarded by increasing grain size. To date, very little quantitative information bearing directly on the effect of austenite grain size upon the progress and result of isothermal transformation has been published. Davenport and Bain,' and Zimmerman, Aborn and Bain2 have shown that the transformation is definitely relarded in hypereutectoid plain carbon steels at temperatures near and above the upper region of rapid transformation (Ar') when the austenite grains are increased in size. More recently, Griffiths. Pfeil and Allen3 investigated the effect of a series of different heating (austenitizing) temperatures upon the progress of isothermal transformation at 1245°F. (675°C.) and 745ºF. (395°C.) in a medium carbon, low-alloy steel; while they reported no measurements of the austenite grain size, their results suggest that increase in grain size retards austenite transformation at 1245ºF. (675°C), but has no appreciable effect at 745°F (395°C.). The present paper deals with the results of a study of the isothermal transformation of austenite in a single commercial alloy steel in which a fine-grained or a coarsegrained state was induced by appropriate selection of austenitizing temperature. The data are presented in the form of isothermal transformation diagrams, which clearly show that coarsening the grains lessens the rate of transformation of austenite to proeutectoid ferrite and pearlite—that is, at temperature levels above about 1000°F. (540°C.)—but is without significant effect at lower temperatures where the transformation product is bainite or martensite. It is to he presumed that the foregoing statement would be valid, at least in principle, for many other grades of steel; it confirms again that the mechanism of transformation to a pearlitic structure is fundamentally different from that to an acicular structure. A number of related observations were made, which seem to throw some light on the transformation process as it takes place in alloy steels, particularly at temperature levels in the vicinity of 1000ºF. (540°C.), where the transition from lamellar to acicular structures occurs. These data are discussed briefly in the belief that they may lead to a clearer understanding of this aspect of the subject. Material and Experimental Procedure The material investigated was a cornmercial grade of S.A.E. 4140 steel, the composition of which was as follows: 0.37 per cent C, 0.77 per cent Mn, 0.98 per cent Cr and 0.21 per cent Mo. It was hot-rolled to a 1 1/8-in. round bar and normalized by air-cooling from 1800°F. (980°C.).

Jan 1, 1941

By R. V. Ramani, G. W. Luxbacher

Computer simulation of mine ventilation system is rapidly becoming an essential tool in mine planning and design. This Paper examines the utilization of ventilation simulation techniques to evaluate the number, shape, size and layout of mine entries in a typical coal mining system. Since the mains and sub-mains serve primarily for transportation and ventilation and the ventilation system is critically important to the health and safety of the workers, there exists a great need for optimal designs in this area. Evaluation criteria could include, among others, minimization of power costs, shaft requirements and leakage. Constraints of this optimization problem include health and safety regulations and production and mine infrastructure requirements.

Jan 1, 1980

By Yap Chu-Phay

IN 1923, when the writer began his studies in metallurgy, he came upon an article by Professor Honda on the, Equilibrium Diagram of the Iron-carbon System, 1 which made a profound impression on him. What interested him most was this sentence: "In the recent diagram of the iron-carbon system, the solidus is usually shown as a curve bending considerably downward. But it can be shown by thermodynamics that if the liquidus is straight or slightly curved, the same must also be true for the solidus. Hence, in my constitutional diagram, the lower portion of the solidus is slightly bent upward." Ever since then the writer has been interested in thermodynamics, especially chemical thermodynamics. The applications of thermo-dynamics to the metallic systems have been, in the writer's opinion, sadly neglected, although we continually use the phase rule in our study of equilibria in the liquid and solid states of metallic alloys. Many investigators, among whom may be mentioned Heycock and Neville, and s Honda and his coworkers, have applied the simple Raoult-van't Hoff law of depression of freezing point, mainly to determine the heat of fusion, but no attempt has been made to investigate the applicability of the thermo-dynamic laws of solution (as opposed to the laws of solution derived from other sources) to metallic systems" showing either limited or complete solid solutions. Perhaps the reason for this neglect is that until recently there have been so few reliable data on the solidus, which is much more difficult to determine than the liquidus. The writer has under way at the present time an investigation of a number of systems, the solidi of which have been more or less reliably determined. Recently, the writer has not only shown the valid applicability of the thermodynamic laws of solution as applied to the system antimony-bismuth but has also suggested a method of attacking problems involving complete and incomplete equilibria.2 In the present paper, the same method of approach is employed. For convenience, we shall divide this paper into two parts:

Jan 1, 1931

By T. D. Tiemann

The chemical and mineralogical composition of Caribbean bauxite ores are described. Extraction of alumina by several processes from both Haiti and Jamaica bauxites is discussed and data presented. IMMENSE deposits of bauxite occur in the Caribbean islands of Hispaniola and Jamaica in the high plateau lands and have been excellently described by 0. C. Schmedeman.' The bauxite occurs as deposits in catchments or etched depressions in Tertiary limestone believed to have been deposited in the Eocene and Oligocene periods.' In appearance both the Haiti and Jamaica bauxites resemble a relatively high iron clay and have indeed been mistaken for such.' They are very soft and friable and disperse readily on vigorous agitation in water. The color range in general is light brown to red. Chemically, the outstanding characteristic of the bauxites is the low silica and high ferric oxide content. The extremely low silica makes them particularly valuable for the production of alumina in the Bayer plant since silica is responsible for the loss of both alumina and soda chemically combined as XNa,OYSiO2,ZAl2O2. The ferric oxide, only traces of ferrous iron are present, offers no interference in the production of high grade alumina. Typical oxide analyses of three types of ore are given in Table I2 and a list of the elements occurring in spectrographic quantities in Table 11." The size of the individual particles in the ore makes successful petrographic examination extremely difficult. The ores contain some relatively coarse grains of heavy minerals such as ilmenite, magnetite, and rutile, but other than occasional crystals of a few microns, the greater portion of the minerals are submicroscopic in size and approach colloidal dimensions. The mineralogic composition of the ores has been investigated by X-ray and differential thermal analysis.' These investigations indicate that the predominant mineral phases present are gibbsite (A1203.3H2O), boehmite (Al2O3.H2O), hematite (Fe2O3), and goethite (Fe2O3-H2O). There is no evidence of the occurrence of diaspore (Al2O3.H2O) in either the Haiti or Jamaica ores, but some type of "amorphous" alumina may be present in some of the bauxites of Jamaica." The temperature stability regions in the alumina-water system have been investigated and are given in recent literature. In the temperature range where the hydrated forms are stable, as determined by hydrothermal bomb methods," ibbsite is the stable phase to 155°C (311°F), boehmite from 155°C (311°F) to 280°C (536oF), and diaspore from 280°C (536°F) to 450°C (842°F). Although quite similar in many characteristics, the Haiti and Jamaica ore show a divergence in mineralogic composition that is reflected in the extractability of the alumina described in later paragraphs. Two principal differences occur in mineralogic composition. The iron-bearing mineral in the Haiti ores is predominantly hematite, while in the Jamaica ores goethite is predominant.4 Directly related to the extraction of alumina are the two minerals, gibbsite and boehmite. Boehmite is relatively high in the Haiti ores and in some of the less soluble Jamaica ores, while gibbsite predominates in the ores in Jamaica amenable to the American Bayer process of extraction. Pedersen and Related Processes In general, all processes for the extraction of alumina involving sintering or fusion of bauxite ores with limestone, soda ash, or a combination of limestone and soda ash followed by leaching, are based on the formation of alumina compounds that. yield alumina soluble in the subsequent leach. The principal idealized reactions in respect to alumina and silica for the three types of processes are as follows: Soda Ash Sinter: A12O3 + Na2CO3 = Na2O-Al2O, + CO2 SiO2 + Na2CO3 = Na2O . SiO2 + CO2 A12O2 + SiO2 + Na2CO3 = Na2O.Al2O8. SiO2 + CO2 Leach (with excess water): H2O + Na2O-A12O3 = 2 NaOH + A12O3 (insolution) H2O + Na2O-SiO2 = 2 NaOH + SiO2 (in solution) Soda Ash— Limestone Sinter: Na2CO2 + A12O3 = Na2O.A1203 + CO2 2CaCO3 + SiO2 = 2CaO . SiO2 + 2CO2 Leach (with excess water): Na2O' A1208 + H2O = 2NaOH + A13O3 (in solution) These latter reactions are the basis of the sinter process currently used for the recovery of soda and

Jan 1, 1952

By Ove Sandberg, Olav Bowitz

The operational characteristics of the Soderberg vertical spike anode are briefly discussed stressing the importance of the flow properties of paste in the fluid zone, the thermal shrinkage in the carbonizing zone, and the surface disintegration in the consumption zone. The requirements for paste recipe and binder quality are combined with design and operation of cell. A low temperature susceptibility of viscosity and low thermal shrinkage of paste together with a low microporosity of the binder coke are important properties. PRACTICAL application of Soderberg's idea of a selfbaking carbon electrode proved successful just before 1920. Shortly after, experimental work was started with the aim of developing a continuous electrode that could be adopted as anode in aluminium reduction cells. The intermittent operation of a large number of small prebaked anodes made the idea of developing a continuous anode for electrolytic production of aluminium especially tempting. Moreover, the electrode consumption in this process, even on a theoretical basis, is very high. Many installations were carried out in the 1930's and during the Second World War. During the tremendous post-war expansion of the aluminium industry, the Soderberg electrode has been steadily more widely adopted. Thus, today more than 60 pct of the Western World's output of aluminium is produced in cells with selfbaking anodes, see Big. 1. The quality of the anode paste of Sfiderberg elec- trodes is considered a major factor influencing the specific carbon consumption. The purpose of this paper is to survey the fundamental requirements which must be met in order to obtain good anode operation. We have limited this paper to a discussion of Elektrokemisk's research on the vertical spike type anode. I) FUNDAMEKI'TALS OF ANODE CARBON PERFORMANCE A) Brief Introduction. The only practical method for producing a conductive carbon anode of the size required is to form and carbonize a mixture of a carbonaceous binder and a precalcined dry aggregate coke. In the Soderberg electrode, the forming and carbonization take place in the electrolytic cell

Jan 1, 1962

By Jesse O. Betterton, Y. E. Lebedeff

AS a matter of the most widespread interest to lead-refining metallurgists, the process of desilverizing lead originated by Parkes is the most fundamental step in lead refining. While this basic operation, in addition to effecting a practically complete recovery of gold and silver, is also a great purifying operation and a governor on the purity and uniformity of the final refined lead, it has the important deficiency that no bismuth is removed in the operation. The problem of finding a satisfactory, inexpensive method for removal of bismuth that would fit in with the basic desilverization step has been one of enticing interest for lead-refinery metallurgists for many years. Of late it has become one of imperative interest, and while many attempts and much progress have been made, it is probably fair to say that metallurgical progress thus far is only catching up with commercial requirements. The Pattinson process, an original competitor of the Parkes process for desilverization, has received much attention for its possibilities for bismuth removal. Bismuth concentrations in the Pattinson process fall far short of the silver concentrations and as a result too many operations are required and a crawl in grade in the kettle units is experienced which requires periodic correction. Altogether, it has proved too expensive a remedy, from the cost standpoint of both installation and operation. The Betts electrolytic process is a fully satisfactory remedy but its present status in the field of lead refining is more a matter of bismuth removal than preference as a refining system, except, of course, in instances particularly favorable to the basic requirements of the process. The Betts process, of course, is essentially different from the Parkes process, and very difficult to associate therewith to any economy except in minor ways. Accordingly, where economy dictates the Parkes process, and this is true of far the greater portion of the world's tonnage, the adoption of the Betts process primarily for bismuth removal is apt to prove an expensive remedy on account of its normally higher cost of operation, inelasticity of the equipment for variable tonnages, and high per ton cost of installation.

Jan 1, 1937

By Charles Barrett

THE orientation of metal crystals and grains, both large and small,. can be determined conveniently and accurately without the use of X-ray apparatus. This seems to be appreciated by so few metallurgists that it may be useful to explain in detail the method we have found most satis-factory in the laboratory the reflection of light from crystallographic etch pits. This note includes a description of a suitable inexpensive instrument and instructions for etching various metals and for plotting the data. As the stereographic projection is used to facilitate handling the data, this note may be considered as an appendix to an earlier review of the metallurgical uses of the stereographic projection.1 Various methods involving etch pits have been used by other investi-gators, Bridgman's method2 consists of attaching the specimen to a sphere (a transparent sphere is convenient4), holding it at arm's length, and marking a spot on it when it has been turned so that the etch pits reflect light into the eye of the observer from a lamp standing behind him. It has an accuracy of about 2° and is extremely rapid. A greater accuracy can be obtained by having the reflected light fall on a screen, as has been done by Czoehralski, 5 Chalmers,6 and Schubnikov.7 All of these methods have been intended for undeformed single crystals. Tammann and his coworkers"' developed a method for estimating the number of grains in a polycrystalline aggregate having orientations in a given region of the stereographic triangle and thus obtained statistical information about deformation and recrystallization textures. While the method has had some use in recent years,9 it is not applicable to the majority of problems in physical metallurgy. Smith and Mehl10 determined orientations by plotting the directions of the sides of individual etch pits on a stereo-

Jan 1, 1940

By S. L. Hoyt

IN technological studies on steel considerable emphasis has been placed on the identification of the foreign inclusions, testimony of which is adequately given in the metallographic literature covering methods for their identification. The outstanding accomplishment in this field is the scheme devised by Campbell, Comstock and Wohrman for identi-fying various oxides, sulfides, silicates and other constituents by syste-matic etching tests and microscopic examination.1 The time involved in carrying out this procedure has led to attempts to secure quicker methods, or at least to shorten the time required to secure essential information. An example of this is the use of dark field illumination, but when this was tried out by the authors it was found that cavities and pits on the polished surface appeared bright on a dark field and could not be distinguished from small glassy inclusions. Still another means is the Leitz Ultropak, an instrument equipped with optical units for the illumination of the specimen by reflected light to secure an effect similar to dark field illumination. The structures are made visible in exceedingly sharp details by utilizing the inherent properties of the samples, such as refractive index, absorption coefficients and reflection powers. We have had no experience, with the Ultropak, but a recent paper by Benedicks and Löfquist3 describes methods for

Jan 1, 1934

By G. R. Heckman, H. J. Murphy, C. T. Sims

An incestigation has been made of the effects of heat treatment and alloy composition on the long-time stress-rupture properties and structural stability of the similar nickel-base alloys Udimet-500, Lrdimet-520, and Udimet-700. Rupture test data are presented at stresses ranging from 4 to 50 ksi at temperatures from 1450° to 1900°F for times up to 14,000 hr. Ductility response is emphasized. Optical and electron tnicroscopy were complemented by X-ray diffraction analyses of extracted phases to relate microstructural stability to the observed rupture properties. Particular attention is paid to Udimet-520 since structural characteristics of this alloy appear to vary somewhat from its sister alloys. Both cast and wrought performance of Lrdimet-500 are discussed. The computerized PHACOMP calculational technique, based on electron-vacuncy theory, is discussed and related to structural stability where appropriate. Electron microscopy and microprobe techniques were used to conduct evaluation of the oxidation characteristics of Udimet-500 exposed in air for 16,100 hr. The steady advance in strength and reliability of nickel-base superalloys continues to be one of the high points of modern metallurgy. The stress capability of these materials has increased steadily, allowing higher and higher operating temperatures in the highly sophisticated aircraft and industrial gas turbines now on the market. The attendant increase in efficiency, of course, means greatly improved power output. Gas turbines for industrial and marine use have long been designed with these objectives paramount the usual design requirements in terms of time of service being 100,000 hr. High-efficiency, long-life aircraft such as the supersonic transport require superalloy engine materials with high-strength and long-time structural stability. Thus, materials studied for and operating experience from industrial gas turbines provide a good reservoir from which technology of high value to the SST program can be drawn. This study is one such case. Three prominent nickel-base super alloys—Udimet 500, Udimet 520, and Udimet 700 were extensively evaluated for industrial gas turbine bucket use. Particular attention was directed toward structural stability as a requisite property. Within the present context, structural stability is defined as freedom from the propensity to form strength-robbing or embrittling phases such as u,p,x,or Laves, and the ability to maintain useful rupture strength and ductility throughout design life. MATERIALS The three alloys, cast Udimet 500 (U-500C), Udimet 520, and Udimet 700, were chosen for detailed evaluation based on preliminary studies which indicated that U-500C and U-520 possessed comparable rupture strength capabilities, and that U -700 had a greater strength capability but somewhat poorer ductility than wrought U-500. The nominal compositions of the three alloys, along with the compositions of the heats investigated, are presented in Table I. PROCEDURE Dimensionally rejected U-520 buckets from Special Metals Corp. heat 63370 were heat-treated using the four cycles delineated in Table 11. Cycle A was investigated to determine the effects of a shortened 1700°F primary age. Cycle B was considered a "standard" treatment. Cycle C investigated a higher solution temperature in combination with a shortened primary age, while cycle D assessed the effect of the higher solution temperature alone. These heat treatments were designed to produce optimum combinations of rupture strength and ductility through maximum y' development, the development of a y' grain boundary cushion, promotion of MC carbide degeneration reactions, and agglomeration of resultant M23CB. Since one of the premises of the evaluation of U-520 was that rupture strength would be equivalent to U-500, forged U-500 buckets from Special Metals Corp. heat 62916 were heat-treated with cycles A, B, and C to provide comparison. The heat-treated structures of U-520 and U-500 are illustrated in the 8700 times electron micrographs of Fig. l. The U-700 tested was all from 3-in.-diam hot-rolled and centerless-ground rod from Special Metals Corp. heat 2-1426. Two heat-treatment cycles were employed, E and F of Table 11. Cycle E is a standard four-step, triple-age treatment intended to provide an optimum match of strength and ductility through well-developed matrix and grain boundary y', as recommended by U-700 vendors. Treatment F is a shortened , single-age cycle which could provide a significant processing cost reduction should adequate strength and ductility be maintained. Following heat treatment, rupture specimens of U-500 and U-520 were machined from the buckets and tested. Standard rupture bars of U -700 were machined from the heat-treated rod and rupture-tested. Failed and withdrawn rupture bars were prepared and examined by optical and electron microscopy. Select specimens were electrolytically digested, and the residues analyzed for carbide and topologically close-packed phases using CrKa or CoKo radiation. Of the six different U-500C heats evaluated, five were cast by Misco Precision Casting Co. and one was cast by Haynes Stellite Co. Cast-to-size rupture bars

Jan 1, 1968

By M. L. Holzworth, Philip R. Sperry, Paul A. Beck

INTRODUCTION THE basic work of Z. Jeffries1,2,3 has long ago established the main features of grain growth in the presence of a dispersed second phase. Working with sintered specimens of initially fine grained tungsten, to which various amounts of thoria have been added, Jeffries found that grain growth was inhabited, that is, practically prevented, up to a certain annealing temperature. When this temperature, which increased with the thoria content, was exceeded, extremely large grains developed abruptly from the fine grained matrix. Such a "coarsening temperature" was later found by Gross mann13,14 in certain types of steel, while Bain showed" that in other steels grain growth was gradual, without inhibition and abrupt coarsening. Later work16,17,18,19,21 demonstrated the connection between coarsening and aluminum additions. The viewpoint that the direct cause of inhibition and coarsening in aluminum killed steels is a fine dispersion of aluminum oxide21 appears to be held quite generally, although some doubts have been voiced even very recently.20 In steels with Ti additions the titanium carbide phase is considered responsible for the inhibition effects found.20 The coarsening temperature increases, with the titanium content. That coarsening may occur, as a result of certain heat treatments, even in low carbon rimmed sheet steel, was shown by Samuels,22 He also detected coarsening in a steel ingot of similar composition, after giving it the same heat treatment as that used by him for the sheet material, In this instance the identity of the inhibiting phase has not been determined, However, Tangerding found 23 that even the few small carbide particles, which occur in carbonyl iron, have a very marked inhibitive effect. As a result of an oxidizing anneal at 850°C, large grains begin to form at the surface of the carbonyl iron specimen, and gradually grow inward as the subsurface oxidation of the carbide particles progresses and eliminates the obstruction, The carbide particles can be removed also by annealing in hydrogen, with similar results. But if the oxidizing anneal of 10 hr at 850°C in air, is followed by annealing in hydrogen for 75 hr at the same temperature, grain growth is more spectacular; usually the whole specimen is transformed into a single crystal (approx. 1,5 cm X 5 cm). The reversed procedure, that is, hydrogen annealing followed by oxidizing annealing leads to smaller grains. Tangerding arrived at the logical conclusion that there must have been in his specimens some additional obstruction to grain growth resulting from a minor impurity, other than carbon. It seems likely that this obstruction was caused by an oxide formed during the oxidizing anneal and gradually reduced during the subsequent hydrogen-annealing. Other instances of grain growth inhibition of varying severity, associated with a dispersed second phase, have been described by several authors. Notable examples: lead with 0.06 pct Cu or Ni,24 cartridge brass with 0.12 pct Cr,25 or with up to 0.15

Jan 1, 1948

By M. R. Geer

THE increase in the number of coal-cleaning plants employing dense-medium processes occurring since 1946 is especially interesting when viewed historically. Both sand and magnetite were introduced as material for heavy mediums at about the same time, sand in the Chance process in 1921 and magnetite in the Conklin process in 1922, but from that point on their records diverge. The Chance process enjoyed a steady growth from its inception, whereas no additional magnetite plants were built in the United States for over 20 years. Then, following the close of the World War 11, magnetite was again introduced, this time with marked success. During the following years some 47 plants employing magnetite medium were built.

Jan 7, 1953

By W. P. Sykes

THIS investigation was undertaken primarily to establish the relations existing between temperature and mechanical properties in molybdenum, nickel, and an aluminum-copper alloy. Molybdenum (m.p. 2500° C.) was chosen because it is partly similar to tungsten and partly similar to the common ductile metals. Also it is known to furnish, by proper treatment, a desirable material to use in studying relation of grain size and physical properties. The molybdenum used was of the quality that is drawn into wire 0.003 in. in diameter for use as filament supports in incandescent lamps; chemical analysis shows less than 0.1 per cent. of impurities. Nickel belongs to the same class as iron. Its melting point is 1450° C. and an allotropic change at about 370° C. results in a loss of magnetism above that temperature. This feature made nickel doubly valuable for the purposes of these tests. The nickel used was obtained from the Driver-Harris Co. as 0.090 in. (2.3-mm.) wire, annealed; analysis showed 99.8 per cent. nickel and 0.150 per cent. iron. Aluminum is one of the low melting-point metals. Some tensile tests at elevated temperatures have been reported by Bengough but the possibility of learning more with the low temperature and sensitive apparatus available recommended this metal. The samples marked Al are an aluminum-copper alloy; they contained 3 per cent. copper, 0.42 per cent. iron, and 0.21 per cent. silicon. The presence of the copper somewhat complicates the analysis of the results; but the action of copper in aluminum has been studied so that its influence might have been foretold, in part at least. The material and analyses were furnished by the Aluminum Castings Co. The nickel wire, which was deformed at 400° C., was drawn under a bath of molten lead and through a die, which also was immersed in the bath. A thermocouple was suspended in the molten metal to indicate

Jan 1, 1921

By H. J. Wasson, E. B. Hopkins

Throughout 1928, production of oil from Venezuela steadily increased, and at the close of the year, the output was at the rate of nearly 400,000 bbl. a day. The total for the year was approximately 106,500,000 bbl., representing an increase of about 66 per cent. over the 63,000,000 bbl. produced in 1927. Venezuela now stands next to the United States as the second largest oil-producing country in the world; and there is abundant evidence to suggest that this relationship will endure for a number of years. Reserves were notably increased in the Lake shore fields, and the potential output of the Maracaibo Basin is much greater than the current production. In spite of this, the percentage of production increase was comparatively moderate, and the rate of this increase continued to fall off slightly, as has been the case for the last three years. This does not suggest that further annual increases in Venezuelan output will not materialize; only that the rate of these increases appears to be on the decline, and that with every succeeding year the future tendency will be in the direction of a stabilized level of output. The following table shows the production trend of the country since 1925: 1925 increase over 1924, 132 per cent. 1926 increase over 1925, 80 per cent. 1927 increase over 1926, 75 per cent. 1928 increase over 1927, 66 per cent. Many factors will work to prevent a reversal of this trend, but the principal ones are strong ownership in large-acreage units, and the probable indisposition of the world market to absorb a more rapidly increasing Venezuelan output at prices profitable to the producers. The distress oil element is not a factor in Venezuela; also, any unforeseen jump, such as results in the United States from the discovery of a Seminole or a deep sand at Long Beach, or Santa Fe Springs, is impossible in Venezuela, on account of lack of means for transporting a sudden surplus of oil, and the slowness with which additional transportation equipment in the form of shallow-draft tankers can be obtained.

Jan 1, 1929

By Edward B. Durham

The refinery at the San Francisco Mint takes the bullion purchased by the receiving department, and carrying Illore than 200 parts of precious metals in 1,000, or, in mint parlance, over 200 fine, and separates and refines the various metals contained therein, using electrolytic processes exclusively. Bullion containing silver is treated in cells charged with a nitric electrolyte. These cells produce fine silver and leave a residue rich in gold. The residue from the silver-cells, together with crude gold-bullion, is treated in cells having a chloride electrolyte. These produce fine gold and leave a residue containing silver chloride. The latter is reduced to the metallic state with zinc and is then treated in the silver-cells. The various waste solutions and the wash-waters, after being freed from the bulk of their precious metals, still contain copper and other metals. These are removed by scrap-iron, and are then treated in the copper-cells, having a sulphate electrolyte. These cells produce pure copper, and collect a residue containing lead, some gold and silver, and all the metals of the platinum gronp that were in the bullion. This residue is relatively small, and is melted into bars and stored until suEcient accumulates to warrant treating it for platinum, etc. The refinery occupies three large and three small rooms. The large ones are, a melting-room, 30 by 34 ft.; a cell-room, 39 by 46 ft.; and a wash-room, 30 by 33 ft. The small rooms are used as foreman's osce, laboratory, and , re- spectively. The methods here described are those in use in December, 1909, when notes for the present paper were taken.

Jan 1, 1912