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By J. H. Wernick

IN temperature-gradient zone-melting1 a molten zone is moved through a solid or across a solid surface by the establishment of a temperature gradient. This technique has both practical and fundamental aspects. One practical application is to make p-n junctions for semiconductive devices, particularly for devices in which the junctions are desired within the semiconductor. From a fundamental point of view, the technique is being investigated as a method for determining diffusivities in liquid alloys, and preliminary diffusivity results have been reported by the writer." In this paper, the effects of crystal orientation, temperature, and molten zone thickness in temperature-gradient zone-melting, and the bearing of these effects on diffusivity measurements and n-p-n junction formation are discussed. Experimental Procedure An effect of crystal orientation was noted in early experiments. To facilitate its study, movements of wire zones across a surface, rather than through the body of a single crystal, were observed for various surface planes and travel directions. The experirr-entai setup is illustrated in Fig. 1. The graphite end-section for the high temperature heater has an apron about 1/16 in. above the upper surface of the crystal. This apron insures that the surface temperature of the block is equal to or greater than the temperature within the block at every point, Thus, the zone does not penetrate the block and convection in the liquid is minimized. The experi-through a block is shown in Fig. 2,

Jan 1, 1958

By D. R. Spink

In the preparation of zirconium and hafnium metals, there are many indications that impurity levels control the physical and chemical properties of the metal. The purpose of this work was to develop methods of producing pure raw materials that could be reduced to highly pure metals. Early work by the Carbomcndum Metals Co. and others indicated that certain fused salts were highly efficient in the removal of impurities from gaseous zirconium tetrachloride. We have developed workable fused salts along with a continuous and higly efficient scrubber design which can be used to produce very pure zirconium tetrachloride. Metal made from the purified tetrachloride has been shown to approach crystal bar metal in purity. Scrubber designs are discussed with recommended materials of construction. VARIOUS methods have been used to purify zirconium (and hafnium) tetrachloride. Most of these methods involve thermal degassing initially (the removal of more volatile compounds at temperatures below that where zirconium tetrachloride exhibits a significant vapor pressure) followed by a sublimation step (which conveniently leaves the nonvolatiles behind.) While these procedures effect definite purification, such processing is batchwise and does not result in optimum purification. Early work by The Carborundum Metals Co. and others indicated that fused salts were highly efficient in the removal of impurities from gaseous zirconium tetrachloride. The objective of this work was to develop a continuous fused-salt scrubbing process that would yield high-purity zirconium and hafnium tetrachlorides. The term "fused salt" refers to the molten state of ionic compounds and as used here, specifically refers to alkali metal and alkaline earth halides. Fused salts, because of their many valuable properties, are becoming increasingly im- portant industrially. These valuable properties of the fused salts are: 1) stability at elevated temperatures; 2)low vapor pressure; 3) low viscosity; 4) ability to dissolve many different materials; and 5) good elctctrical conductivity. All but the last property enhances the use of fused salts as scrubbing agents for zirconium and hafnium tetrachlorides. Fused-salt scrubbing may be defined for our purpose as the intimate contact between a gaseous compound and a molten salt with the purpose of removing impurities from the gaseous compound. In this case, the gaseous compound is zirconium tetrachloride which submlimes at 331°C. When this gas is contacted with a molten salt, impurities such as aluminum, iron, and titanium are removed and the resulting product is considered fused-salt scrubbed. Zirconium and hafnium are sold to a purity specification. Generally speaking, normal production without scrubbing is capable of meeting specifications. There are, however, several considerations That make the knowledge of methods of additional purification highly desirable. These are: 1) the control of product analysis; 2) the production of a pure product for special applications; 3) the salvaging of off-specification material; and 4) the use of raw materials with higher impurity levels than 1 he present raw materials. You will note that items 1 and 2 are somewhat complementary to each other and that item 4 assumes that The present process has impurity removal limitations. To better understand the part that fused-salt scrubbing of zirconium tetrachloride plays in the manufacture of zirconium, Fig. 1 contains an illustrated flow sheet of the industrial production of zirconium metal. In referring to Fig. 1, we can point out the specific benefits derived from our ability to purify zirconium tetrachloride. Purification of the crude (hafnium-containing) zirconium

Jan 1, 1962

By Neil Styler

This paper presents an analysis of measurements of inter-burden deformations above six longwall faces. An attempt is made to demonstrate some correlation between the movements at the various sites, and to examine their importance with respect to predicting caving height, disruption of overlying seams, and disruption of aquifers. This analysis demonstrates some significant differences between predicted surface subsidence, and inter-burden deformation. In addition it is shown that the caving height above a longwall face is equal to 8 to 12 times the extraction height, with a zone of fractured rock extending to approximately 50 times the extraction height above the seam.

Jan 1, 1984

By J. Chipman, N. J. Grant, H. L. Bishop, H. N. Lander

Data of several studies on the equilibrium between molten iron and open hearth-type slags have been combined to determine some of the chemical reactions involved in steel-making. Effects of slag composition and temperature on the iron oxide activity, distribution of sulfur between slag and metal, and the carbon content of the metal are discussed. Also, an overall reaction for the equilibrium between sulfur and oxygen is presented. DURING the past 15 years, a number of significant equilibrium studies have been carried out between liquid iron and simple basic and acid slags in an effort to throw light on the chemical reactions involved in steelmaking. This paper is a summary of the experimental reports on investigations which have been conducted at the Massachusetts Institute of Technology, and of related work in other laboratories. The investigations summarized in this paper include the works of Fetters and Chipman1 and Taylor and Chipman,' which dealt with simple slags that are similar to those found in the open hearth. The sulfur determinations of the slag-metal tests of Fetters and Chipman as reported by Grant and Chip-man" are included. Also, the investigations by Win-kler and Chipman' and Grant and ChipmanQ f more complex slag systems are included in this summary. The experimental procedure is described in detail in each of these papers and will not be discussed. Since the previous reports have been somewhat independent, it is desirable to review and combine the data of the various investigations to determine, as accurately as possible, the reactions in the slag-metal systems of the open hearth. It is the object of this report to present the combined data in such a way as to enhance their utility and applicability. Oxidizing Power of Slags of the System (CaO+MgO)-Si0,-FeO in Equilibrium with Carbon-Free lron The slags selected to determine the iron oxide activity in equilibrium with pure liquid iron were those containing less than 2 pct each of P,O,, MnO, or A1,0, on a weight percentage basis. The method used to calculate activities of iron oxide in liquid slags was that developed by Taylor and Chipman.' The solubility of oxygen in molten carbon-free iron under pure iron oxide slags can be expressed by the following eauation —6320 log (pctO)-------------— + 2.734 [1] where T is the absolute temperature. The oxygen solubility values as determined from Eq. 1 were used throughout this study to calculate the iron oxide activity. The iron oxide activities of slags of various iron oxide contents are plotted in Fig. 1 as a function of the basicity, which is defined as the ratio (pct CaO + pct MgO)/pct SiO,, and are based on molecular percentage values of the components. The percent (FeO), is the total iron content in the slag calculated to FeO. Fig. 1 shows that as the basicity increases at constant mol pct (FeO),, the iron oxide activity increases rapidly and reaches a plateau which extends on the basicity scale from about 1.3 to 2.3; the iron oxide activity then decreases rapidly until a basicity of about 3.0 is reached, where it tends to level off. The solid portions of the curves represent the experimental data of Fetters and Chipman and Win-kler and Chipman. Their experimental heats were made in magnesia crucibles, and hence the slags were saturated with magnesia. The broken lines on the left represent the experimental data of Taylor and Chipman, who used a rotating crucible. In general, these slags contained less than 3 pct MgO. The absence of data for slags containing less than about 40 mol pct (FeO), and basicity ratios greater than about 2.5 made it necessary to calculate curves using ionic concepts of slags. The broken lines on the right, which disregard the solubility limits of di and tricalcium silicate and lime, were obtained by following the treatment of Flood and Grjotheim,"

Jan 1, 1957

By J. C. Coughlin, M. C. Flemings, T. Z. Kattamis

Experiments on Al-4.5 pct Cu alloy shou the dendrite arnz spacing increases with time during isothermal holding in the liquid-solid region. This coarsening of the dendrite structure is then shown to occur at roughly the same rate during solidification as during isothermal holding. Final dendrite arm spacing in both types of experiments depends primarily on coarsening kinetics. It is concluded that driving force for the coarsening is reduction of liquid-solid sur/ace area. Calculations based on two simple models show qualitative apreement with experinzent. 1 HERE has been considerable interest in recent years in determining effects of solidification variables on dendrite arm spacing in cast alloys. The interest has resulted primarily from the clear evidence that 1) the degree of homogeneity which can be obtained in a cast alloy with commercially practical homogeni- zation treatments depends on dendrite arm spacing, and 2) mechanical properties of the heat-treated casting depend on the homogeneity obtained.'-' In wrought alloys, microsegregation from the original ingot is carried to some extent into the final wrought product, and affects mechanical properties in similar fashion Experimental evidence available indicates that dendrite arm spacing in cast aluminum alloys is influenced only by cooling rate (or "local solidification timev*) and alloy content.Fig. 1, for example,

Jan 1, 1968

By A. Y. Bethune, W. G. Woolf

THE hydrometallurgy of special high-grade zinc as practiced by the Sullivan Mining Co. at its electrolytic zinc plant, Kellogg, Idaho, involves an important filtration step immediately following the leaching process. By means of the filtration the heavy zinc sulphate solution is separated from the residual products which remain after the zinc calcine has been dissolved in the sulphuric acid electrolyte. Because this plant uses the so-called high-acid, high-density process' for the production of First, the strength of the electrolyte (270g H,SO, per liter) results in a saturated zinc sulphate solution, having a specific gravity of 1.510 to 1.540, which must be kept warm during filtration because of its property of "seeding out" small crystals if allowed to drop much below 60°C. Second, the action of the "high" acid on zinc calcine under the temperature conditions of the leach (80" to 102 "C), although favorable to good zinc extraction, causes a considerable quantity of iron to be dissolved (8 to 18. g per liter) along with variable quantities of alumina and silica, depending on the grade and type of original zinc concentrates roasted. These three, iron, alumina, and silica, are almost completely precipitated during the neutralization of the leach (only a few. milligrams per liter of each remain in solution), so that the resulting pulp, instead of being a granular, sand-like product having a particle-size distribution dependent on the fineness of the zinc calcines leached, is in reality a slimy, chemical precipitate whose filtration characteristics constantly change depending on the amounts of iron silica, and other impurities, which are dissolved and reprecipi-tated. Third, the combination of supersaturated solution of high specific gravity plus a dense, semi-gelatinous residue creates a difficult washing problem requiring a positive displacement wash to liberate the zinc sulphate entrapped in the pulp. In a closed-cycle hydrometallurgical operation, such as practiced in this plant, the extent of washing is determined by the volum,e limitations imposed on the intermediate wash waters by the amount of "fresh" (or process) water which may be added. The volume of fresh water used for makeup purposes is limited to the amount which is lost during the closed cycle by evaporation in the leach, sulphate content of the calcines leached, moisture content of the residue, and spillage. The Burt filter as modified and improved by the Sullivan Mining Co. has successfully met and overcome these difficulties under a variety of zinc plant operating conditions since 1928. It might have many interesting applications to metallurgical fields other than that of electrolytic zinc, and its possible usefulness to hydrometallurgists in general warrants its description and discussion. The Burt filter is so named from its inventor who originated it in Mexico for pulp filtration in the cyanide process for gold and silver ores. While retaining the basic principle of Burt's earlier revolving pressure-type filter with internal filtration media, a number of modifications and improvements have been made in Sullivan Mining Co.'s installation. The Burt filter may be classified as a batch-type pressure filter in contradistinction to either the conventional vacuum-type filter, which depends on atmospheric pressure to force solution through a cloth medium, or to the filter-press, which employs whatever pressure is imparted by the pump delivering the liquid being filtered. The Burt consists essentially of a hollow steel cylinder about 40 ft long, 5 ft in diameter, resting horizontally, and capable of rotation about its long axis. It is supported on one end by a hollow trunnion and near the other end by a riding-ring and roller combination. The cylinder is lined with filter units each fastened against the inside of the shell and parallel to the long axis so as to form a hollow cavity into which pulp may be charged. A specific amount of pulp is admitted to the filter and a unique valving arrangement prevents the loss of pulp while air pressure forces the solution through a canvas medium to the discharge port of each filter unit. The residue is left on the surface of the canvas inside the cavity. The remainder of the filter cycle is concerned with washing the residue free of zinc sulphate, discharging it from the Burt, and preparing the filter for the next charge. A more detailed description of Burt filter construction, a typical filter cycle, and its operating characteristics when employed on material encountered in this plant will be given in that order. Description of the Filter: Fig. 1 shows a side elevation view of a filter with riveted shell construction. Since this drawing was made shells have been fabricated by welding, instead of riveting, with complete success. Shells are lagged on the outside to retain heat. Fig. 1 shows a side elevation and plan view of a Burt filter in operating position. The 1/2-in. steel shells are lined with 3/16-in. copper sheet as protection against the corrosive action of the solution (containing about 500 mg Cu per liter) on iron, and the copper is given a thin protective coating of plastic-base paint. Fig. 2 is a view from the discharge end of the filter, with head removed, before filter units are fastened to the periphery. It shows

Jan 1, 1951

By W. G. Woolf, A. Y. Bethune

THE hydrometallurgy of special high-grade zinc as practiced by the Sullivan Mining Co. at its electrolytic zinc plant, Kellogg, Idaho, involves an important filtration step immediately following the leaching process. By means of the filtration the heavy zinc sulphate solution is separated from the residual products which remain after the zinc calcine has been dissolved in the sulphuric acid electrolyte. Because this plant uses the so-called high-acid, high-density process' for the production of First, the strength of the electrolyte (270g H,SO, per liter) results in a saturated zinc sulphate solution, having a specific gravity of 1.510 to 1.540, which must be kept warm during filtration because of its property of "seeding out" small crystals if allowed to drop much below 60°C. Second, the action of the "high" acid on zinc calcine under the temperature conditions of the leach (80" to 102 "C), although favorable to good zinc extraction, causes a considerable quantity of iron to be dissolved (8 to 18. g per liter) along with variable quantities of alumina and silica, depending on the grade and type of original zinc concentrates roasted. These three, iron, alumina, and silica, are almost completely precipitated during the neutralization of the leach (only a few. milligrams per liter of each remain in solution), so that the resulting pulp, instead of being a granular, sand-like product having a particle-size distribution dependent on the fineness of the zinc calcines leached, is in reality a slimy, chemical precipitate whose filtration characteristics constantly change depending on the amounts of iron silica, and other impurities, which are dissolved and reprecipi-tated. Third, the combination of supersaturated solution of high specific gravity plus a dense, semi-gelatinous residue creates a difficult washing problem requiring a positive displacement wash to liberate the zinc sulphate entrapped in the pulp. In a closed-cycle hydrometallurgical operation, such as practiced in this plant, the extent of washing is determined by the volum,e limitations imposed on the intermediate wash waters by the amount of "fresh" (or process) water which may be added. The volume of fresh water used for makeup purposes is limited to the amount which is lost during the closed cycle by evaporation in the leach, sulphate content of the calcines leached, moisture content of the residue, and spillage. The Burt filter as modified and improved by the Sullivan Mining Co. has successfully met and overcome these difficulties under a variety of zinc plant operating conditions since 1928. It might have many interesting applications to metallurgical fields other than that of electrolytic zinc, and its possible usefulness to hydrometallurgists in general warrants its description and discussion. The Burt filter is so named from its inventor who originated it in Mexico for pulp filtration in the cyanide process for gold and silver ores. While retaining the basic principle of Burt's earlier revolving pressure-type filter with internal filtration media, a number of modifications and improvements have been made in Sullivan Mining Co.'s installation. The Burt filter may be classified as a batch-type pressure filter in contradistinction to either the conventional vacuum-type filter, which depends on atmospheric pressure to force solution through a cloth medium, or to the filter-press, which employs whatever pressure is imparted by the pump delivering the liquid being filtered. The Burt consists essentially of a hollow steel cylinder about 40 ft long, 5 ft in diameter, resting horizontally, and capable of rotation about its long axis. It is supported on one end by a hollow trunnion and near the other end by a riding-ring and roller combination. The cylinder is lined with filter units each fastened against the inside of the shell and parallel to the long axis so as to form a hollow cavity into which pulp may be charged. A specific amount of pulp is admitted to the filter and a unique valving arrangement prevents the loss of pulp while air pressure forces the solution through a canvas medium to the discharge port of each filter unit. The residue is left on the surface of the canvas inside the cavity. The remainder of the filter cycle is concerned with washing the residue free of zinc sulphate, discharging it from the Burt, and preparing the filter for the next charge. A more detailed description of Burt filter construction, a typical filter cycle, and its operating characteristics when employed on material encountered in this plant will be given in that order. Description of the Filter: Fig. 1 shows a side elevation view of a filter with riveted shell construction. Since this drawing was made shells have been fabricated by welding, instead of riveting, with complete success. Shells are lagged on the outside to retain heat. Fig. 1 shows a side elevation and plan view of a Burt filter in operating position. The 1/2-in. steel shells are lined with 3/16-in. copper sheet as protection against the corrosive action of the solution (containing about 500 mg Cu per liter) on iron, and the copper is given a thin protective coating of plastic-base paint. Fig. 2 is a view from the discharge end of the filter, with head removed, before filter units are fastened to the periphery. It shows

Jan 1, 1951

By F. R. Morral, E. P. Miller

Hot-dipped heat-treated zinc coatings on sheet steel were examined with X-rays. The phases identified were compared with those listed in the modern literature 01 the zinc-iron system. The zeta (FeZn13) phase is shown to correspond to the phase found by Schueler (1925) in heat-treated zinc coatings. An investigation was undertaken to determine the phases present in hot-dipped heat-treated zinc coatings on steel sheets and wire. This kind of coating on wire was studied some years ago by Schuelerl by microscopic and chemical methods. He reported a new phase, FeZn10. Later, Clark and Stillwell,2 using X-ray crystal analysis, identified a new phase in ordinary galva. nized wire, which was assumed to be the FeZn10 phase. Since the extensive review of the iron-zinc alloys presented a few years ago,3 much new work has been published, some of which5-l6 was too late to be included in the recent edition (1939) of the American Society for Metals' Handbook.4 Figs. 1 and 2 are reproductions of the latest iron-zinc diagram proposed by Schramml1 as a result of his investigations by microscopic, thermal, magnetic susceptibility and X-ray methods. Table 1 summarizes all the known published X-ray data of the phases Present. The solubility of iron in zinc has been determined by x-ray methods.10 In the same manner the homogeneity range of the P phase was studiedlo using the principle that the parameter of an intermetallic compound changes while the concentration of One of the constituents changes. Schramm10 has found some 80 alpha lines in X-ray powder photograms of phase d1, and from these he believes that this phase is related to the P phase. Previous investi-

Jan 1, 1941

By E. P. Miller, F. R. Morral

Hot-dipped heat-treated zinc coatings on sheet steel were examined with X-rays. The phases identified were compared with those listed in the modern literature 01 the zinc-iron system. The zeta (FeZn13) phase is shown to correspond to the phase found by Schueler (1925) in heat-treated zinc coatings. An investigation was undertaken to determine the phases present in hot-dipped heat-treated zinc coatings on steel sheets and wire. This kind of coating on wire was studied some years ago by Schuelerl by microscopic and chemical methods. He reported a new phase, FeZn10. Later, Clark and Stillwell,2 using X-ray crystal analysis, identified a new phase in ordinary galva. nized wire, which was assumed to be the FeZn10 phase. Since the extensive review of the iron-zinc alloys presented a few years ago,3 much new work has been published, some of which5-l6 was too late to be included in the recent edition (1939) of the American Society for Metals' Handbook.4 Figs. 1 and 2 are reproductions of the latest iron-zinc diagram proposed by Schramml1 as a result of his investigations by microscopic, thermal, magnetic susceptibility and X-ray methods. Table 1 summarizes all the known published X-ray data of the phases Present. The solubility of iron in zinc has been determined by x-ray methods.10 In the same manner the homogeneity range of the P phase was studiedlo using the principle that the parameter of an intermetallic compound changes while the concentration of One of the constituents changes. Schramm10 has found some 80 alpha lines in X-ray powder photograms of phase d1, and from these he believes that this phase is related to the P phase. Previous investi-

Jan 1, 1941

By R. F. Mehl

Jan 1, 1961

By D. N. Seidman

In the course of a study of the electronic and thermodynamic properties of Pb-Se alloys it was found necessary to have an accurate knowledge of the phase diagram. However, the literature is in disagreement as to whether or not a monotectic reaction occurs in the lead rich portion of the phase diagram. Pelabonl reported only a two-phase region consisting of lead-rich liquid and solid PbSe extending from almost pure lead to the compound PbSe, and gave the melting point of PbSe as 1065°C. The data of Friedrich and Leroux2 are in general agreement with this type of diagram, with the melting point of the compound being 1088°C. However, Nozato and Igaki by inverse rate thermal analysis observed a monotectic reaction isotherm exlacing at 860°C with a monotectic composition of 20.5 at. pct Se. The miscibility gap in the liquid state extends from 7.5 to 20.5 at. pct Se. Hansen and Anderko4 accepted Nozato and Igaki's phase diagram in the region of the lead-rich monotectic. To reinvestigate this portion of the phase diagram, both thermal analysis and metallographic examination of various compositions were performed. The thermal analysis apparatus was constructed according to the specifications of the National Bureau of Standards. A t/t-l pct Rh thermocouple was calibrated against the melting point of copper (NBS), zinc (NBS), and antimony (A. D. Mackay), the emf being measured with a Rubicon Type B potentiometer sensitive to lpv. The absolute accuracy of the thermal analysis obtainable with this system is ± 0.5oC. Starting materials were semiconductor grade lead and selenium purchased from the American Smelting and Refining Co. Both elements were 99.999 pct pure with only trace impurities detected upon spectroscopic examination. One hundred galloys were sealed in quartz crucibles with a central thermocouple well under a vacuum of less than 1 p. This procedure prevented any composition change due to vaporization during the run. Cooling curves were obtained on the alloys listed in Table I. Data was taken by the direct method at cooling rates ranging between 1/2 to 2°C per min. The alloys were heated well above the liquidus and shaken vigorously to insure homogeneity. No evidence of an arrest indicative of the monotectic reaction was observed, and the two-phase region reported by Pelabonl and Friedrich and Leroux? was confirmed in general, although our data give higher liquidus temperatures than Friedrich and Leroux. The melting point of stoichiomet-ric PbSe determined for two different samples was 1080.7 0.5oC. The results of this investigation are compared with Nozato and Igaki's data in Fig. 1. To Complement the thermal analysis data, an 86 at. pct Pb specimen was examined microscopically. This composition was in the center of the miscibility gap reported by Nozato and Igaki.3 The alloy was heated to 1000°C, held for 1/2 hr, and water quenched. The specimen was polished using standard metallographic techniques for lead. The alloy was etched with an acetic-nitric acid etchant for 10 min at 45°C. Microscopic examination did not indicate the existence of two separate layers or solidified droplets imbedded in a matrix, as would be expected if a miscibility gap were present. The mi-crostructure shown in Fig. 2 consists of uniformly dispersed, dendritic PbSe in a lead-rich matrix.

Jan 1, 1962

By J. E. Tobey, David R. Mitchell, J. H. Kerrick

DETAILED knowledge of purchase specifications established by coal consumers is essential to the successful design and operation of a coal-preparation plant. ANTHRACITE Specifications should be considered by both the consumer and the producer as guide posts outlining a certain path for both to follow. Plants differ, therefore specifications must differ to meet the varied requirements. Specifications are not of themselves a "cure all" or an assurance of complete satisfaction in fuel utilization. Specifications should not be regarded as a license to engage in an orgy of buying any and all coals that may happen to fall within their limits. This would lead to the indiscriminate mixing of coals which may vary in their burning characteristics. Different coals of equal grade tend to be individualistic in their burning characteristics. Rather, specifications should be used to help simplify coal selection, to reduce the actual number of coals used over a given period; in other words, to have a stabilizing influence on coal or customer turnover. In the final analysis, the use of too many coals per year in a plant is costly to both the consumer and the producer. Too many sources usually result in higher operating and maintenance costs for the consumer and higher sales costs for the producer. Finally, the statement included in the report accompanying the com¬prehensive Coal Selection Charts prepared by the Coal Committee of the National Association of Purchasing Agents, and released in 1938, is significant. This Committee worked diligently for a period of 15 years seeking to find a scientific and reliable method for selecting coals. The two following paragraphs are quoted from its report: More important is the fact that no ready-made classification or set of specifications can possibly replace the judgment and resourcefulness of an experienced combustion engineer or fuel technologist, nor the usual need for full scale plant tests under the exact conditions of use before a final decision is made ...

Jan 1, 1943

By Harvey Cline, Donald P. Ferriss

THE violent outgassing of commercial tungsten and other refractory metals when melted in an electron beam zone refining apparatus1"3 is dealt with experimentally by one or both of two approaches. One is to provide a suitable emission current control1,2 the other is to purify the metal in the solid state before melting.4 The first of these is usually sufficient, but the authors chose also to investigate the source of the troublesome gases and to devise means of solid-state purification. Some further insights into the use of tungsten as a structural material at temperatures near its melting point were also revealed in the course of the work. One may speculate on the causes of gas formation in tungsten at high temperature by inferences from the literature and an examination of the impurities in commercial wire. Davenport5 observed microporosity in both tungsten and molybdenum filaments heated to several hundred degrees below their melting points. Studying the function of oxygen in molybdenum welds, Perry, Spacil, and wulff8 attributed similar porosity to the disproportionation of Moo2 to molybdenum metal and Moo3. Tungsten dioxide also disproportionates7 above 2000oC to yield WO3 vapor at considerable pressure. Commercial tungsten contains some 5 to 20 wt ppm O and a similar concentration of carbon depending on the details and precautions of processing. Therefore, evolution of CO is also a strong possibility as a source of gas at high temperatures. Furthermore, even for activities in the order of 0.01, it may be calculated that the pressure of CO at 3000°C would be over 4000 psi, which is in excess of the tensile strength of tungsten at this temperature.9,10 Powder metallurgy tungsten contains some 0.02 pet Fe and 0.002 to 0.005 pet of the elements Ni, Si, Al, Ca, Mn, Mg, and Mo; at temperatures over 2800°c, therefore, these elements will exhibit appreciable vapor pressure, though small compared to that of WO3 and CO. Some of these impurities may react to form high-pressure monoxides such as SiO and A10. Finally, dissolved and occluded nitrogen is an ever-present source of high-pressure gas. Commercial Type 218, General Electric filament wires, 0.025 in. diam, were heated by resistance in 10 -4 mm of Hg and in argon or hydrogen at pressures from 50 µ to atmospheric. For temperature determinations in vacuo, the Jones - Langmuir8 current-temperature relationship was employed. For gaseous atmospheres, the burn-out temperature was assumed to be the same as in vacuo so that a small, constant correction could be made for temperatures below burn-out conditions (i.e., local heating to failure). Several dozen experiments may be summarized by pointing out some structural observations. At 3050oC in 1 atm of A, porosity is very evident after 30 min, as shown in Fig. 1. For the section in Fig. 2, failure occurred 200°C below the melting point and many voids have grown in the grain bound-

Jan 1, 1962

By Stanley L. Lopata, Eric B. Kula

SEVERAL methods are available for determining pole figures by X-ray means.' The earlier film methods have been replaced by techniques in which the intensities are measured by Geiger counters on an X-ray diffractometerZm7. These methods utilize either flat transmission or reflection samples,214°8 cylindrical specimens,3 or spherical specimens.7 A single transmission or reflection sample will not yield information over the complete pole figure. The cylindrical specimens suggested by Nortod and the spherical specimen of Jetter and Borie7 have the advantage of allowing the whole pole figure to be obtained without any corrections to the intensity for absorption, There is a lower limit to the size of sheet which can be conveniently studied, however, and sample preparation can be rather tedious. Probably the most common method today for determining the complete pole figure is that developed by Schulz. A flat reflection sample is used for determining the pole figure from the center out to about 70". Because of the geometry of the system used, little or no correction for absorption or irradiated volume is necessary.4'6 A separate transmission sample is used for the region near the edge of the pole figure. This procedure requires two separate samples, one of which must be a thin carefully-prepared transmission sample. Furthermore, since the reflection and transmission data are in different arbitrary intensity units, a region of overlap must be obtained, and the intensity data from one set of measurements converted to units of the other. These are serious disadvantages of this method, and they point out the need for a simplified procedure. Since the reflection technique can be used for planes whose normals lie up to about 70° from the sample surface normal, it is apparent that a complete pole figure can be obtained by reflection alone if sample surfaces are cut at oblique angles to the rolling plane Specifically, if a rolled sample is cut so that the normal to the surface formed lies equidistant (54" 44') from the rolling plane normal, rolling direction, and transverse direction, then complete information for one quadrant of the pole figure can be obtained by reflection from the surface. Fig. 1 shows this oblique surface, as well as the position of the pole of this surface in the pole figure. When a surface has been cut oblique to the rolling plane, the standard polar stereographic net is inconvenient to use, and it would be more desirable to have the center of the net coincide with the pole of the oblique plane. Fig. 2 shows such a net, where the center has been offset 54' 44' to correspond to a specimen cut as in Fig. 1. This net was in effect obtained by rotating a standard polar stereographic net 54" 44' with the help of a Wulff net. With the experimental setup used. a sample can be cut from plate of 1/2-in. thickness or br Gen- erally thinner sheet is under investigation, and a composite specimen must be used. A convenient procedure has been to bond together, using epoxy resin, sufficient sheets to form a cube. These are clamped in a vise, and when dry, the whole vise is rotated and a flat surface ground at the required angle. The sample is then mounted inside a larger steel ring using Koldmount, the backside ground flat and parallel to the approximate desired thickness. The sample is then polished and etched to remove any effects of cold working during grinding. With this method only one quadrant of the pole figure is obtained. Often pole figures show symmetry around the rolling and transverse directions, and any slight asymmetry is due to scatter. Should the pole figure not be symmetrical, four oblique surfaces, corresponding to the four quadrants of the pole figure, would have to be examined. In most cases there is symmetry at least around the rolling direction, which reduces to two the number of quadrants to be investigated. For many purposes all that is required is an average polefigure for the four quadrants. This canreadilybe obtained with composite specimens of sheet material, where sheets Corresponding to each of the four quadrants can be intermixed. The four quadrants can be obtained by considering sheet in the normal position, and by rotatiolls of 180" around the sheet normal, the rolling direction, and the transverse direction. If desired, the whole thickness of the sheet can be used, yielding an average of the surface and interior textures; or the surface material can be removed from each sheet, resulting in a pole figure for the center alone. Eugene S. Meieran of the Massachusetts Institute of Technology has independently developed the same method. His results, adapted to a pole figure goniometer with a specimen spiraler, will be described in another publication.

Jan 1, 1962

THERE are two general classes of problems in connection with electric furnaces. First, those relating to the best utilization of the electrical power inside the furnace; second, those connected with the bringing of the electrical power to the point where it is to be utilized. Referring particularly to the latter class of problems, many calculations have been made, covering a wide variety of furnaces, to check the electrical capacity and power factor found from test. The following analysis, made for the purpose of determining the maximum capacity and approximate performance of a new furnace, to operate at 160 volts on a 60-cycle circuit, may be of interest. The first characteristic necessary to determine is the inductance, since this is the factor that limits the amount of power which can be put into the furnace. Inductance is calculated from the dimensions of the furnace, according to formulas of the U. S. Bureau of Standards,1 as

Jan 10, 1918

By Marcel Schlumberger

The electrical methods for surface-prospecting have been well developed in the last 20 years. The method involves, in the classic form, the sending of an electrical current into the soil, by means of two electrodes A and B, and studying the potential distribution at the surface, by measuring the difference of potential between pairs of points such as M and N. The points M and N are usually placed on a line between, and equidistant from, A and B. By increasing the distance AB, the current sent into the Earth, and likewise the distribution of surface-potentials, become influenced by regions of greater and greater depth below the surface. By varying the form and dimensions of the electrode-arrangements AMNB, called a "quadripole," one may make valuable deductions concerning the nature or thickness of beds, if one knows the electrical properties of these beds. On the other hand, if the form and dimensions of the electrodes AMNB remain fixed, the depth of penetration of currents in the Earth remains, so to speak, almost constant, although it tends to increase where the subsoil is more conductive, and conversely. Therefore, if one moves the constant-dimension quadripole over all the terrain to be Investigated, one achieves approximately a horizontal exploration. This permits a study of tilted beds or faulted horizon-tal beds. When the particular problem becomes deep, of the order of 2000 meters, or more, it is ne-cessary to Increase the distance between the current-sources AB to a length such that the work 'comes very troublesome, especially if the region is wooded. At the same time, the separation the points M and N must be likewise great (for example, one km) in order to obtain differences potential which are not too small; the measurement of potential differences across MN is then difficult because of the presence of parasitic potentials, due to a flow of telluric currents in fourth, and the order of greatness of these currents may exceed the quantities to be measured.

Jan 1, 1940

W. H. SHOCKLEY, Chairman, FRANK H.-PROBERT, :Vice-Chairman, T. A. RICKARD, Sec.-Treas.; 420 Market St.,. San Francisco, Cal. C. C. BRAYTON, J. F. NEWSOM. A Meeting of the San Francisco Section was held on May 7, 1917. Chairman Shockley was in the Chair. The Section was honored by the presence of President Moore and Secretary Stoughton of the Institute. C. W. Merrill introduced President Moore, who then spoke to the Section on the Aims of the Institute. He discussed the possibility of improving the standards of membership by introducing a classification of membership. The present rigid investigation of applicants was pointed out by him. He spoke of the important influence that the local Sections can exert on the Institute and of the importance of sociability and informality at the meetings. Secretary Stoughton, who was introduced by the Chairman, emphasized somewhat the same points. He mentioned the need for making the Bulletin of the Institute more, interesting than it is at present, this to be accomplished by raising the necessary funds by increased advertising. He asked for an expression of opinion on this point. He. said that the employment department of the Institute is now used extensively. At the request of Mrs. Mark L. Requa, Mr. Stoughton. announced that a San Francisco branch of the Woman's Auxiliary of the, Institute was being formed and asked that the ladies of the members' families send in their names to Mrs. Requa or to the Secretary of the Institute.

Jan 10, 1917

By B. Trafton, H. L. Hartman

An earlier paper1 introduced a rapid solution for mine ventilation network problems, employing the digital computer. In this paper, refinements and additions to the computer program which expand its scope of application and a solution to a ventilation network having a coal-mine configuration are presented. The revised program-written in FORTRAN for the IBM 7074 computer in Penn State's Computation Center-is applicable to any mine ventilation network employing natural splitting and having its fan located externally. It accomplishes the following: 1) Distributes an assumed total quantity of air flow among all airways of the network, performing iterations until an acceptable level of error is attained and the flow in each airway is known. 2) Computes the pressure drop (head loss) in all airways and the overall network and mine head losses. 3) Determines the operating point for the mine and a given fan, adjusting all air flows and head losses to the actual values. The basis of analysis used is the Hardy Cross method of successive approximation for solution of any fluid network, explained in detail in the earlier article. In brief, corrections to assumed air flows are computed for all the loops of a network; following distribution to the airways of each loop, the process is repeated until acceptable accuracy is attained. When a hand or desk-calculator solution is used, there is advantage to close approximation of the actual flows in the original assumption of air-flow distribution in the network. Since publication of the previous paper, in which assumption of initial quantities was also necessary in the computer solution, the program has been modified to make the first distribution itself, assigning the total quantity to one specified path in a split and then proceeding to correct the flows. The number of iterations required for a high-accuracy solution is little affected, at least in networks of few loops, 10 to 15 being sufficient to reduce the error to 1 pct or less. The principal limitation of the original program was that it contained no provision for handling a fan. Further, it did not determine the overall head loss in the network and was not designed for multiple parallel openings, such as occur in coal mines. The revised program was written to overcome these disadvantages and also to print out the adjusted flows for all airways, corrected for the system operating point. At the present time, the program can handle only an external fan. The procedure employed in solving a ventilation network is now as follows: 1) Input data consisting of airway characteristics and loop designation along with assumed direction of flow, for each branch of the network and any trunk airways, are fed into the computer. 2) Employing the resistance relationship, where R is resistance, K is friction factor, P is perimeter, L is length, A is area, and n is number of airways (where multiple intakes and returns are employed); values are computed for all airways. 3) An arbitrary, continuous route of flow through the circuit—from beginning to end—is selected and the path identified by airway numbers and read in. 4) Based on a total assumed quantity of flow Q (usually 100,000 cfm.) the computer employs the procedure described in the previous article in distributing quantities of flow among all the airways until a satisfactory level of accuracy has been attained (in the current program, the machine is turned off when the cumulative corrective error in cfm, is reduced to five times the number of airways). 5) Airway head losses H are calculated by the relation H = R Q2 and cumulated along the original designated flow route to find the overall head loss for the network. Trunk airways are then included to obtain the mine head.

Jan 1, 1964

By H. A. Buehler

The Ozark region occupies a large part of the southern half of Missouri, the northern portion of Arkansas and comparatively smalll areas in northeast Oklahoma, southwest Kansas, and southern Illinois. It is a roughly elliptical plateau which has been deeply dissected by stream erosion, and which slopes imperceptibly into the prairie regions to the north, east, and west, but which terminates rather abruptly along the Arkansas River on the south and Tertiary lowland to the southeast. The Boston Mountains extending for a distance of some 200 miles (321 km.) along the Arkansas River rise to an elevation of 2000 ft. (609 m.), forming the most prominent topographic feature of the region. The so-called St. Frangois Mountains in St. Frangois, Madison, and adjoining counties in southeast Missouri, form a prominent but more restricted topographic feature, the highest point rising to an elevation of 1800 ft. (548 m.). The remainder of the region is largely a plateau area varying from 800 to 1500 ft. (243 to 457 m.) in elevation. Stratigraphy The region is underlain chiefly by sedimentary formations, which outcrop in roughly concentric bands around a comparatively restricted area of igneous rocks in the St. Frangois Mountain district. Although located geographically near the eastern edge of the Osarks, the St. Frangois Mountains have apparently suffered the greatest orogenic movement and the lowest formations of the succession are exposed in their immediate vicinity. The various sedimentary formations of the region do not show any considerable metamorphism and have suffered little change since consolidation. With the exception of a few basic intrusions in Ste. Gene-vievg County and a pegmatite dike in Camden County, Missouri, there is no evidence of igneous action, since the first sedimentary beds were deposited.

Jan 1, 1918

By H. A. Buehler

LOCATION THE Ozark region occupies a large part of the southern half, of Missouri, the northern portion of Arkansas and comparatively small areas in northeast Oklahoma, southwest Kansas, and southern Illinois. . It is a roughly elliptical plateau which has been deeply dissected by stream erosion, and which slopes imperceptibly into the prairie regions to the north, east, and west, but which terminates rather abruptly along the Arkansas River on the south and Tertiary lowland to the southeast. The-Boston Mountains extending for a distance of some 200 miles (321 -km.) along the Arkansas River rise to an elevation of 2000 ft. (609 m.), forming the most prominent topographic feature of the region. The so-called St. Francois Mountains in St. Francois, Madison, and adjoining counties in southeast Missouri, form a prominent but more restricted topographic feature, the highest point rising to an elevation of 1800 ft. (548 m.).. The remainder of the region is largely a plateau area varying from 800 to 1500 ft. (243 to 457 m.) in elevation. STRATIGRAPHY The region is underlain chiefly by sedimentary formations, which outcrop in roughly concentric bands around a comparatively restricted area of igneous rocks in the St. Francois Mountain district. Although located geographically near the eastern edge of the Ozarks, the St. Francois Mountains have apparently suffered the greatest orogenic movement and the lowest formations of the succession are exposed in their immediate vicinity. The various sedimentary formations of the region do not show any considerable metamorphism and have suffered little change since consolidation. With the exception of a few basic intrusions in Ste. Genevieve County and a pegmatite dike in Camden County, Missouri, there is no evidence of igneous-action, since the first sedimentary beds were deposited.

Jan 10, 1917