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By C. N. Reid

Slip-line studies on deformed chromium single cvystals showed the usual bcc behavior. At room temperatuve, cross slip was prevalent—slip was not confined to a given plane, but the slip direction was (111). At -10O0K, slip occuvred on (110) planes, twins on(112) planes, and cleavage on (1001 planes. A single-crystal tensile specimen with an axis close to [011] showed a pronounced yield drop and high strain rate sensitivity which zclere used to derive relevant parame tevs in a dislocation dynamics treatment. Transmission electron microscope studies confirmed the existence of (110) slip planes and showed ecidence of loops punched out by precipitates and of grown-in dislocations promoting tangling. OF recent years experimental studies have been made of the deformation characteristics of single-crystal molybdenum and tungsten, but very little has been published on the behavior of single-crystal chromium. During a study of the mechanical properties of chromium, single-crystal studies were made which have already been partially described.&apos; However, additional information was generated which was not directly relevant to the main theme of Ref. 1, and, therefore, was not reported. In view of the need for complete documentation of deformation modes, the experimental observations made on the deformation of single-crystal chromium are summarized here, together with an electron-microscope study of the associated dislocation structures. It was found that, in terms of the deformation modes, chromium is a conventional bcc metal, showing a very pronounced yield-point phenomenon. Further, it was found that the flow strength of these crystals is very sensitive to the strain rate. Finally, the crystals were observed to contain many unidentified precipitates, which often were associated with prismatic dislocation loops. EXPERIMENTAL METHODS Single crystals were grown from rods of wrought chromium by the method of zone annealing. Rods of "1/4in.-diam were supported vertically in an argon atmosphere while an induction coil was moved up the rod at 1 in. per hr. The power was adjusted to just below that required for melting, and the process produced single crystals in about 30 pct of the rods used. The orientations of the crystals, in general, lay near [011] and are summarized in Fig. 1. Before this treatment, the wrought material contained 35 pprn C, 68 ppm O, and 12 ppm N.* An analyzed single crystal *Usual metallic impurities found in iodide chromium are: Al, 5 ppm; Ca, A ppm; Cu, 2 ppm; Fe, 75 ppm; Yg, 0.5 ppm; Yn, < 3 ppm; Mo, < 3 ppm; Ni, 4 ppm; Si, < 20 ppm; Ti, < 1 ppm; V, 4 ppm; Zr, < 3 ppm. contained 10 pprn C, 79 ppm O, and 50 pprn N. Tension and compression specimens were shaped from the crystals by mechanical grinding, followed by the electrolytic removal of about 0.010 in. from the surface in a perchloric/acetic acid bath. All specimens had a gage length of 0.75 in., and tension specimens had a diameter of 0.100 in., while that of the compression samples was 0.200 in. Mechanical tests were carried out at a rate of 1.3 pct per min, and temperatures below 0°C were attained by means of a nitrogen cryostat similar to that of Wessel.2 EXPERIMENTAL RESULTS Modes of Deformation. In addition to the tensile properties of these crystals, which are described in Ref. 1, deformation markings on the surface were studied. Crystals A and F, Fig. 1, were deformed in tension at 300°K to 10 and 16 pct strain, respectively. The surfaces contained visible slip lines, about 1 C( apart, composed of both straight and wavy segments. They did not define a single plane, and so determination of the slip plane was not possible. However, the slip direction was deduced by comparing the axial orientations of the crystals before and after deformation. Fig. 2 is representative, and shows that the axis ro-

Jan 1, 1968

By H. A. Tucker

This Bureau of Mines investigation was conducted to determine the appropriate quantities of rare-earth methals (REM) in the form of silicides to add to an alloy steel for the purpose of increasing toughness and ductility. The work was conducted in a vacuum induction furnace with the rare-earth additions required to deoxidize and desulfurize a simulated basic oxygen furnace (BOF) vacuum-degassed steel initially containing 0.013 to 0.016 percent sulfur. The product proved to be as good or better than the best basic electric furnace steel of the same composition made by the steel industry. Twenty-three experimental heats of 5 Ni-Cr-Mo-V steel were made, cast into 50-1b ingots, and hot-worked in a press and a rolling mill to ½ inch plates which were then heat-treated to 130/150 ksi4 yield strength. Impact and tension tests showed that the addition of 0.025 to 0.100 percent, or ½ to 2 lb per ton, respectively, of rare-earth metals when compounded with silicon were appropriate for increasing toughness and ductility. These quantities resulted in retained cerium contents between 0.014 to 0.025 percent, and increased the Charpy V-notch energy absorption and the percent reduction of area significantly as compared with base heats at the same sulfur content levels. All the test heats, including those with additions of REH of as much as 4 lb/ton, had greater Charpy V-notch energy absorption values than the base composition could have developed at the starting sulfur range of 0.013-0.016 wt pct.

Jan 1, 1968

By F. S. Thurner

This paper, a description of the new ore-unloading and stockpiling facilities at the Sydney Works of DOSCO Steel Limited, deals with a new approach to arrive at the most economical solution to combine ore unloading facilities for common bulk carriers and for different types of self-unloading vessels. Also discussed is the design and installation of a 1-mile-long steel-cord belt conveyor sys-tem with a most modern type of mobile belt conveyor stacker, along with automatic and semi-automatic controls for the entire ship-unloading and stockpiling operations.

Jan 1, 1968

By Thomas V. Falkie

4.3-1. Introduction. DEFINITION OF PRODUCTION SYSTEMS ENGINEERING. Surface mines, like most other mining and manufacturing operations, are usually organized along functional departmental lines. Frequently a mine manager will have his responsibilities divided among production, maintenance, administrative, and engineering functions. Often these are separate departments, but various combinations and variations of these functions can be found in mining companies throughout the world. The production function is responsible for physically removing the ore from the ground, processing it, and shipping the product to its market. The production manager supervises and is responsible for all man-machine systems necessary to extract and process the ore. The maintenance function, which is sometimes included within the framework of production, has the task of insuring the maximum availability and longevity of equipment needed to produce the ore. The administrative function is responsible for accounting, personnel, industrial relations, purchasing, public relations, property, and other related staff functions. For purposes of this chapter, engineering can be described as the function which plans, designs, and supervises construction of physical plant and equipment. In this context engineering includes mechanical, civil, chemical, electrical, and mining engineering. However, another phase of engineering is to prepare plans to insure that the various man-machine components function in an optimum way towards the single most important goal of any enterprise-the maximization of return on the investors&apos; money. Along with the planning, another duty of engineering is to audit all phases of the operation for the purpose of recommending improvements toward this same general goal. These latter two ideas form the basis for a discussion of production engineering and systems engineering. Production engineering is a catchall, problem-oriented function whose duties can include: 1) solution of day-to-day production problems, 2) short-

Jan 1, 1968

By J. C. Draper

This subject was introduced last April in a paper presented in Birmingham, Alabama, by James E. Elkin, General Superintendent of Duquesne&apos;s Coal Department. This paper will cover some of the same data and in addition it will update and further describe our experience. Our Portal No. 3 was started in June 1965 with battery tractor-trailer face haulage. This mine is operating in the Sewickley seam in Dunkard Township, Greene County, in Southwestern Pennsylvania as shown on Fig. 1. The Warwick group of mines fronts on the Monongahela River and extends westward for some ten miles as shown on Fig. 2.

Jan 1, 1968

By M. Boucraut

The authors investigate the influence of the basicity index CaO / Si02 on the sintering properties of hematite ore mixtures. The experimentation was performed with three different mixtures of ores from Tazadit, Nimba, Mano-River, Itabira, Marcona, Goa, Mapawa and Cassinga. Increasing the basicity index CaO / Si02 between 0.1 and 3, chiefly through limestone admixture makes possible to reduce the thermal consumption of sintering and to improve the physical and chemical properties of the sinter. In the case of a plant using hematite ores, it seems interesting to produce an hyperbasic sinter and to complete the blast furnace burden with calibrated ore or acid pellets.

Jan 1, 1968

Sphalerites from Devonian cassiterite-sulphide deposits and Pb-Zn-Ag fissure veins have similar ranges of Cd contents, but the average Cd and Fe contents could indicate a small initial difference in availability of Cd between the Zeehan-Renison Bell district and the Mt. Bischoff-Waratah district. Sphalerites from banded Pb-Zn deposits (Rosebery and Hercules) are characterized by low Cd content which is a world-wide feature of such deposits in exIrusive rocks, and may indicaIe a genetic relationship between ore deposition and vulcanism.

Jan 1, 1968

By G. R. St. Pierre, M. J. Pool, R. Speiser

The activities of chromium in solid Cr-Ti solulions contaitning from 10 to 90 at, pct Cr were measured over the temperatutre range 1250" to 1380°C. The Knzudsen effusion technique with direct weighing of the Knudsen cell was used. This was possible because the vapor pressure 0f chromium is about 600 times greater than the capor pressure of titanium so that the amount 0f titanium effusing could be neg-Lected. the activities of titanium were determined by g-raphical integration of the Gibbs-Duhertz equatiotz. The solutio~ls sllcdied exhibited positive deviations from Raoult&apos;s law, but they approached ideality as the temperature was raised from 125 to 138t C. The integral free energy of mixing was calclated from the activity values. AF has a maximum value of - 1.66 kcal a1 1390°C and a composition oj 55 at. pcl Cv. The free energy of formation of &apos;TiCr, is —0.76&apos; lzcal a1 1250°C. The heats and entropies of mixing usere determined using the second law and thus tile mlues could be in error by a considerable amount. The Cv-Ti system is not a regular solution. ThE increasing emphasis on application of various models to alloy formation and solution behavior has led to an intensified interest in the thermochemistry of alloys. In a majority of the cases where different models have been applied the alloy system used was a simple one. However, the amount of data available on more complicated systems is small and in order to fully understand the behavior of metallic solutions more experimental work has to be carried out on these systems. The Cr-Ti system is reasonably complex and even though this system was being investigated as early as 1937 by Kroll,&apos; no previous work has been done on the thermodynamic properties of either the liquid or solid state. This research was undertaken to determine the thermodynamic properties of solid Cr-Ti alloys. EXPERIMENTAL PROCEDURE The experiments on the Cr-Ti system were carried out in a water-cooled metal vacuum system. This system is composed of a brass vaporization chamber wound with copper tubing for cooling purposes, a brass liquid-nitrogen trap, an oil diffusion pump, and a Duo-Seal forepump. The pressure in the system is measured with an ionization gage. The interior of the vaporization chamber is shown schematically in Fig. 1. The Knudsen cell is supported by the molybdenum tripod, and a magnetically operated shutter is provided to protect the Pyrex sighting glass against deposition of metallic vapors in the intervals between temperature measurements. Heating is accomplished by means of a 20-kw 450-kc Westinghouse oscillator. The susceptor in this case is 10-mil tantalum seamless tubing which also forms the outside of the sample container. The remainder of the sample container consists Of an im~ervims re-crystallized alumina crucible and a 10-mil-thick tantalum lid. Two holes are drilled in the lid. The diameters of these holes were measured with the calibrated stage of a "Tukon" microhardness tester. The thicknesses were measured with a micrometer. A Leeds and Northrup disappear ing-filament optical pyrometer was used to measure the temperature. This is sighted through the smaller of the two holes in the lid and corrections for the emissivity of the sample were not necessary since the ratio bf cell length to hole diameter was large enough to insure a hohlraum. The pyrometer was calibrated at the ~~t~~~l Bureau of Standards, and the correction for the Pyrex sighting window was determined in the laboratory. The titanium used in this investigation was obtained from Mallory-Sharon and the chromium from The Union Carbide Metals Co. The reported purities were

Jan 1, 1968

By D. M. Blacknall, N. N. Winogradoff, E. W. Williams

Low-temperature measurements of photolumines-cence were used to evaluate the progvess in materials development. Variation of the impurity type, impurity concentration, and method of growth were used to clarify the chemical origin of defects in GaAs. Melt-g~ozun, epitaxial vapor-, and solution-grown samples were studied. A comparison of measurements at 77" and 20°K shows that more defects can be observed at the lower temperature. Th&apos;vee residual defects were identified in relatively pure GaAs. These were: silicon, copper, and a gallium vacancy-donor complex. Solution growth from a gallium solution inhibits the formation of the latter two. Eleven defects were studied and the "optical" activation energy of some of these, namely, silicon, cobalt, and chromium, has not been reported in the literature before. THE discovery of the injection laser in 1962 prompted extensive measurements of the photoluminescence of GaAs. The measurements were made at 77°K on GaAs doped with shallow impurities at various doping levels and compared with electroluminescence1&apos;2 and absorp- tion data.374 In addition, lower-temperature studies were made on relatively pure GaAS&apos; and on GaAs doped with oxygen,5&apos;" manganese,&apos; and copper.&apos; The observation of defects* in GaAs with photolu- *The word "defects" ~efers to both chemical impurities and native defects. minescence at low temperatures makes photolu mines-cence an invaluable tool in evaluating the progress in materials development. The only previous evaluation was done at 77°K when solution-grown and melt-grown GaAs were compared.O No identification of defects was made but it was shown that some of the deep-level luminescence seen in melt-grown GaAs was absent in solution-grown GaAs. The present work extends the comparison of preparation techniques to lower temperatures and to a study of epitaxial vapor-grown GaAs. It is particularly valuable for thin epitaxial layers since they cannot be analyzed by conventional analytical techniques. In addition, by varying the impurity type and impurity concentration the chemical origin and nature of defects in GaAs was demonstrated. Eleven defects were studied in all. Three of the defects were identified as residual defects which often contaminate GaAs prepared from the melt and the vapor. Only one such defect was observed in GaAs grown from a gallium solution and this was identified as silicon.

Jan 1, 1968

By Robert K. Linn

The New ldria Mining District is in the southern part of the Diablo mountains of the California Coast Range, 140 miles southeast of San Francisco. The district, noted primarily for quicksilver, also has become important recently as a producer of short-fiber chrysotile asbestos. Between 1853 and 1966, the New Idria district produced 568,092 flasks of quicksilver valued at about $55,600,000, 99 per cent of which was recovered from one deposit, the New Idria mine. In 1944, the district was ranked third in all-time production of North American quicksilver districts, and, since that time, the New Idria mine produced an additional 129,045 flasks, placing the district and the New Idria mine second in all-time production. The major structure of the region is the northwest-trending Coalinga anticline consisting of an asymmetric dome of sedimentary beds ranging in age from Jurassic to Quaternary and marked at its northwest end by an oval body of sheared serpentine 14 miles long by 4 miles wide. The serpentine core, rimmed by Franciscan sandstone of probable Jurassic age, was uplifted in stages between Jurassic and Quaternary time and was intruded along a ring of faults into beds of the Panoche Formation of upper Cretaceous age. The core of serpentine and Franciscan rocks is the locus of about 20 quicksilver mines that rim the faultbounded core and lie within the serpentine mass. The host rock of the most productive deposits is altered Panoche shale and sandstone that lies intermittently along the perimeter of the core. Deposits of the New Idria group of mines and those of a few other small mines lie along the northeast contact in the footwall of the New ldria thrust fault, and a few others occur on steep normal faults around the south and southwest. The chief ore mineral in all quicksilver mines is cinnabar, but minor amounts of metacinnabar and native mercury are found in some of the mines. Ore shoots were deposited in fracture zones and stockworks in altered Panoche shale and sandstone and in definite fissure veins in Franciscan sandstone. Rocks made highly amenable to fracturing by hydrothermal alteration were fractured extensively by late faults. The resulting fracture zones, located along the late faults and at changes in strike or dip of the hanging wall or footwall, are the principal controls of most ore shoots. The largest and richest ore shoots are those of the New Idria mine. The major ore bodies occur in fractured shale and sandstone beneath the New ldria thrust fault at its junction with major tear faults.

Jan 1, 1968

By R. L. Schmidt, J. D. Verhoeven

The diffusion coefficients and electrotralzsport mobilities of aluminum, gallium, and arsenic have been determined in molten germanium with the capillary reservoir technique. The diffusion coefficients are slightly higher than those determined by the solidification technique of Brirton et a1.1 It was found that aluminium and gallium migrate to the cathode in molten germanium) whereas arsenic migrates to the anode under an electric field. A possible technique for producing p-n junctions by means of electric field freezing is discussed in view of the experimental data. In the past decade or so the literature has abounded with articles concerning the solid-state properties of the semiconducting elements germanium and silicon. It is surprising by comparison how little has been published concerning the liquid-state properties of these materials. In the production of doped germanium or silicon the diffusion coefficient of the dopant in liquid germanium or silicon is an important quantity. Yet, to the best of our knowledge, no one has ever made a direct measurement of the diffusion coefficient of solutes in either molten germanium or silicon. A number of authors&apos;-4 have determined some diffusion coefficients by the indirect technique developed by Burton et al.1 This technique appears to give numbers of the correct order of magnitude but it does depend upon a number of assumptions in the analysis and also requires prior knowledge of the viscosity of the melt. In the present work a more direct measure of the diffusion coefficients of arsenic, gallium: and aluminum in molten germanium has been made. It has been shown independently by two groups of authors5, 6 that, when an electric current is passed through the interface of a solidifying metal containing an impurity, the resulting electrotransport in the liquid boundary layer at the interface offers a mechanism for control over the redistribution of the impurity accompanying the solidification. These authors show that the degree of control is proportional to the mobility, U of the impurity atoms in the liquid boundary layer, where the mobility is defined as the drift velocity relative to the solvent per unit electric field. In principle the results apply to the solidification of a doped semiconductor and offer an interesting technique for control of the doping of a semiconductor. In the present work the mobilities of aluminum, gallium, and arsenic were determined in molten germanium in order to evaluate the potential usefulness of electro-transport as a technique for solute control when applied to the solidification of doped germanium. EXPERIMENTAL PROCEDURE Both the diffusion coefficients and the mobilities were measured using high-purity alumina capillaries and a resistivity technique for analysis. A schematic diagram of the electrotransport apparatus is shown in Fig. 1 and the details of the cell design are shown in Fig. 2. For the mobility experiments electrical contact with the bottom of the capillary was made with graphite, as shown in Fig. 2. In order to prevent electrical contact with the melt the graphite was coated with a thin layer of alumina using a plasma spray torch. The cell assembly, a graphite electrode, and another assembly containing two blank capillaries were fastened to the lavite disk shown in Fig. 1. To make a run the system was evacuated and the doped germanium was outgassed at the operating temperature of 1030°C. The cell and blank capillaries were then submerged beneath the melt and a slightly positive pressure of helium was introduced to fill them. After passing current through the cell for a given time the cell and blank capillaries were raised from the melt and the furnace was shut off. The temperature of the cells dropped below the freezing point of germanium within 1 to 2 min after the furnace was shut off.

Jan 1, 1968

By Irving Wender

This report describes Bureau of Mines experiments and reviews the work of others on the exposure of coal and coal-derived products to gamma rays and some other types of radiation. Results are presented on tests of three bituminous coals and a lignite that had been pulverized to minus 200-mesh particles and exposed to 1,000 megaroentgens of gamma irradiation from spent-fuel elements of a nuclear reactor. Of about 20 chemical and physical tests in Bureau work, only mass spectrometry of gases evolved during vacuum pyrolysis of the coals to 450° C gave results indicating differences in the irradiated and unirradiated samples. Mass-spectral distribution curves for CO and CO2 evolution showed fewer irregularities (reversals of curvature) for irradiated coals; thus, mass spectrometry appears to be the most sensitive method for determining radio-induced changes in coal. It is concluded that coal is not significantly altered by gamma irradiation owing to the resistivity of its highly condensed ring structure. High-level gamma irradiation, therefore, is unlikely to prove advantageous in coal processing and utilization. Specially treated coals, because of resistivity of coal to radiation damage, may be useful as an absorbent in processing radioactive wastes.

Jan 1, 1968

"Developing markets for western metallurgical coal have continued to stimulate considerable exploration activity in the Rocky Mountain foothills and to influence major segments of a wide-ranging carbonization R&D pro-gram. Adjunct studies have included expanded petrographie investigations.Coal preparation has• been principally directed toward utilization of prepared small coal and was, like much of the year's combustion work, strongly influenced by concern over atmospheric pollution. Particular attention has been given to desulphurization and to the suppression of pollutants in combustion systems.In the area of non-fuel utilization of coal, interest has centered on plant nutrients and on a series of coal-based carbons which, inter alia, possess utility as filtration media.Other projects included the development of improved sampling and analytical methods, investigations into the effect of storage on coal proper-ties and R&D in solids pipelining. In addition, a significant volume of basic 'uncommitted' research has been maintained."

Jan 1, 1968

Jan 1, 1968

By M. R. Geer

The ever-increasing need to guard against stream pollution has intensified interest in the problems of handling and disposing of flotation tailing. Therefore, the Bureau of Mines investigated the possibility of using crushed washery refuse to adsorb the free water in thickened flotation tailings on a bench scale and then in a pilot plant because the conventional methods of disposing of coal flotation tailings--impounding them or filtering them so they are dry enough to be conveyed to the refuse dump--are sometimes either impractical because of space limitations or costly because of low filter capacity. Most of the refuse samples tested were of similar mineralogical composition and exhibited similar water retention capability. The amount of crushed refuse required to adsorb the water in a particular tailing was influenced greatly by the fineness of the solids in the tailing and hence the percentage of solids to which it could be thickened. The ratio of crushed refuse to tailing solids required to provide a mixture dry enough to be carried on an inclined conveyor belt varied from 2.4 to 6.4. Several chemical agents that were tested were very effective in turning the free water in tailings into a stable gel. Fly ash also was very effective in adsorbing water.

Jan 1, 1968

By Harold D. Palmer

The marine geologist and coastal engineer have at their disposal a wide variety of geophysical tools with which to investi¬gate sea floor topography and structure. Such devices include towed magnetometers, shipboard gravimeters and a variety of acoustical systems for recording the relief of the sea floor and buried structural features. The versatility of this latter group of systems lends itself to a variety of applications essential to those projects where excava¬tion of the sea floor is required. This paper describes the use of several acoustic devices and their Limitations and presents a case history in which a rapid survey from a small vessel provided detailed information critical to the planning stage of a specific coastal project. In this discussion, shallow water is defined as depths less than 150 feet. At present, this limit includes the maximum depth of economic dredging and most other offshore activities. To be sure, the maximum depth at which routine useful work can be accomplished is rapidly increasing, but the majority of current marine activities are located in water depths here defined as shallow.

Jan 1, 1968

By Thomas M. Larimer

Prior to April, 1961, the coal charge to Clairtonts coke oven batteries was 3" x 0" mine waslied coal having approximately 6.0% to 7.0% moisture. Even at this size and moisture content, the arching, rat-holing and hang-up was excessive and the effective live storage of coal was only 60% to 70% of the rated capacity of the coal bunkers, depending upon the moisture of the coal. In addition, many production delays were encountered in the time and methods required to fill the larry cars. The need for an improved metallurgical coke led to the introduction of pulverized coal to a portion of the plant in 196 1. When the full potential of the pulverizing equipment was realized, we were able to serve seven batteries in our second unit of batteries with pulverized coal through two coal bunkers. The discharge hoppers of these bunkers were equipped with air vibrators to assist the flow of pulverized coal into the larry cars. The vibrators were helpful in this respect but required considerable maintenance and caused damage to the bin plates.

Jan 1, 1968

By Y. Baskin

Solid-solubility relationships in the Pseudobinary systems UAS-UP, UAs-US. UAS-UC, aid UAs-UN were investigated. The first two systems exhibit complete mutual solubility, whereas the component compounds in the other two systenzs are immiscible. The above information, together with solid-solubility data joy six additional pseudobinary systems , were analyzed for compliance wilh the Hurrze-Rothery rules for rnetallic systems. The relative size difference of the component nonmetal atoms was found to be the dopainant jactor determining the extent of solid solubility between the NaC1-type uranium compounds. The anionic and covalent radii of the nonmetal atoms appear to be inadequate for these systems, but compuled radii based on rare earth compounds yield consistent results for the uranium compounds. THE actinide elements, like metallic elements of the transition and rare earth series, readily form binary compounds with nonmetallic elements of groups IV, V, and VI of the periodic table. Of particular importance are the NaC1-type equiatomic compounds with carbon, nitrogen, sulfur, phosphorus, and arsenic. The uranium members of this family of compounds have high melting points, are essentially stoichiometric, and exhibit various amounts of mutual solubility. Thus, they are of interest for investigating the factors governing the extent of solid solubility. Previous investigators have determined the solid-solubility limits in the pseudobinary systems between the compounds UC, UN, US, and UP. Anselin et a1 .&apos; reported complete miscibility in the system UC-UN. Baskin and shalek 2 and Allbutt et a1.3 reported that UP and US exhibit complete mutual solubility. Shalek and white4 reported partial miscibility in the system US-UC. At 1800°C the maximum solubility of UC in US is 40 mol pct, but that of US in UC is 4 rnol pct. shalek5 found limited solubility in the system US-UN; the maximum solubility of UN in US is 11 rnol pct at 1800°C, while that of US in UN is only 0.3 mol pct. White and askin 6 found very limited miscibility in the system UP-UC at 1800°C. Approximately 7 mol pct UC is soluble in UP, but there is no solubility of UP in the monocarbide. Phase relations in the pseudo-binary system UN-UP were investigated by askin.&apos; Approximately 0.7 mol pct UN is soluble in UP at 1800°C, while UP is immiscible in UN. The present study was carried out to explore the extent of terminal solubility in the systems UAs-UC, UAs-UN, UAs-US, and UAs-UP. This information, combined with existing data, provided a sufficient basis on which to determine the factors governing solid solubility in pseudobinary systems containing NaC1-type uranium conpounds. I) EXPERIMENTAL 1) Materials. The compounds UC and UN were obtained from the Kerr-McGee Corp. and United Nuclear Co., respectively. The US, UP, and UAs were synthesized by reacting finely divided uranium with H2 S, pH3, or AsH3 gas at low temperature (300° to 500°C), followed by homogenization in a vacuum at moderately high temperatures (1400° to 1700°c).8-10 The materials were essentially stoichiometric, with the exception of UC, which exhibited a C/U ratio of 1.05. Oxygen was the major contaminant in these compounds, ranging from 0.05 wt pct in US to 0.30 wt pct in UC, and it was generally combined with uranium to form UO2. The UO2 content in these materials was usually of the order of 1 wt pct, and did not exceed 2 wt pct. Furthermore, no evidence was found for a high-temperature reaction between uranium dioxide and any of the compounds. Chemical analyses of equilibrated compositions in the systems UAs-UP and UAs-US showed that the non-metal atom to uranium ratios averaged about 1.01, and that the oxygen contents ranged from 0.06 to 0.22 pct. However, the small deviations from stoichiome-try or the presence of minor oxygen impurities do not invalidate the conclusions to be drawn from this study. 2) Experimental Procedures. The component compounds in powdered from were blended in the desired proportions for 5 hr in the ball mill that consisted of stainless-steel balls in a plastic container. Chemical analyses indicated very little metallic pickup from the blending operation and virtually no increase in oxygen content. The pellets were pressed in a 0.270-in.-diam steel die under 40,000 psi pressure. One wt pct of stearic acid dissolved in CCl 4 served both as a binder and as a die lubricant. Chemical analyses revealed that the stearic acid left no carbon residue in the sintered samples. The pellets were sintered in vacuum in an unsealed tantalum crucible. The temperature, measured with a calibrated optical pyrometer, was maintained at 1800" + 30°C for 3 hr. This was sufficient time for attaining equilibrium as no change occurred in either the lattice parameters or the sharpness of the X-ray patterns when samples were annealed for longer periods of time. The pellets were cooled with the furnace. Debye-Scherrer powder patterns were taken at room temperature with a 114.59-mm-diam Norelco powder camera and CuKor radiation (CuGI = 1.5405A). Unit cell dimensions were determined from a Nelson-Riley extrapolation to the high-angle reflections. The values for were precise to k 0.001A. 11) RESULTS X-ray and met allographic investigation revealed that complete mutual solid solubility exists in the pseudobinary systems UAs-UP and UAs-US. The lattice parameter vs composition plots, Fig. 1, show a

Jan 1, 1968

Jan 1, 1968

By H. L. Luo

SYSTEMATIC investigations of the Fe-Ga system have been reported only very recently."&apos; The maximum solid solubility of gallium in a-Fe is nearly 50 at. pet at 900°C. However, from Ref. 1, it was not evident that the a-Fe solid solution could be retained successfully beyond 17.38 at. pet Ga by solid-state quenching. The present investigation reports the retention of a-Fe solid solution at 50 at. pet Ga by quenching from the liquid. An ordered phase of CsC1-type B2) structure was observed between 34 - 50 at. pet Ga. Since it was considered very probable that the CsCl structure would occur at high temperatures, alloy filings were also quenched by the conventional quenching technique. In addition to the CsCl phase, a second ordered phase of BiF3-type (DO3) structure was found in the range 25 - 30 at. pet Ga. Alloys were prepared from elements of 99.99 pet purity or better, induction-melted in alumina crucibles under hydrogen. After reweighing, the alloy ingots were cast into wires under argon. From the weight losses and the reproducibility of the lattice parameters, compositions were estimated to be within ± 0.3 at. pet. The techniques of quenching from the liquid state were reported before.3-5 Prior to quenching, a small section of cast alloy wire (30 - 50 mg) was melted in an alumina insert under an argon flow. The quenched specimens were in the form of flakes, typically 1 sq mm in area. For solid-state quenching, alloy filings passing 200 mesh were sealed under a reduced helium atmosphere in a thin-bottom silica tube. After heating for -30 min at the desired temperature in a vertical furnace, the sealed tube was rapidly dropped into ice water so that the thin bottom of the tube broke on impact. The quenched alloy filings were always ferromagnetic and could be collected by a magnet. X-ray diffraction patterns were taken with iron-filtered cobalt radiation in a 114.6-mm-diam Debye-Scherrer camera. High-angle lines were always resolved and spacings were computed relative to ? (CoKa1) = 1.78890Å. Lattice parameters were obtained from extrapolation against the Nelson-Riley function. The variation of lattice parameter with composition is shown in Fig. 1, together with the data of Dasarathy and Hume-Rothery.1 Uncertainties in the present measurements are within the dimensions of the symbols or indicated by error bars. X-ray diffraction lines indicative of CsC1-type ordering could be clearly identified for alloys of 34 - 50 at. pet Ga quenched from the liquid and alloys of 35 - 41 at. pet Ga quenched from -975°C. Within experimental error, no difference in

Jan 1, 1968