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By H. R. Ogden, E. S. Bartlett, A. G. Imgram

THE tensile and notch tensile ductile-to-brittle transition characteristics of several refractory metals and alloys have been well documented.1-3 Electron-beam melted tantalum and columbium have been shown to retain excellent ductility at very low temperatures. Some indications of brittle behavior (low ductility and cleavage fracture) were observed with columbium tested at -253oC, but no similar effects were noticed with tantalum. Increasing the interstitial oxygen content in these two materials resulted in the detection of indications of brittle behavior at higher temperatures, although good ductility was retained in both bases at -196°C when they contained about 1 at. pet 0. Detailed descriptions of the impact transition behavior of these two materials at various purity levels have not been available. This technical note describes the effect of interstitial oxygen on the impact properties of wrought, fibered tantalum and columbium and compares the transition behavior to the previously determined tensile transition characteristics. Tantalum and columbium impact specimens with three different interstitial oxygen levels indicated in Table I were tested at temperatures ranging from -196o to 300°C. Oxygen additions were made to 1/2-in.-diam bars of electron-beam melted material in a Seiverts Apparatus. The oxygenated bars were then homogenization-annealed to obtain uniform cross-section hardnesses and swaged to

Jan 1, 1964

By Frank Firmstone

When in charge of the Glen don Iron Works, the importance of good methods of filling was forcibly brought to my attention, and it occurred to me that the first step toward the discovery of the best plans was the accumulation of exact information as to the distribution actually effected by various chargers; also, that something could be done in this direction by careful measurements in the furnace, to be afterwards recorded for comparison on drawings. The figures shown herewith have been prepared from such measurements, and nearly all of them refer to Glendon, where the fuel used was anthracite and the ore-mixture about threequarters of New Jersey magnetic ores and one-quarter of brown-ores from the vicinity of the works. Every occasion furnished by the blowing-in of furnaces was utilized, but the data accumulated rather slowly in this way; and, opportunity oEering to make special trials at no great expense, the figures from 2 to 7 were thus obtained. The trials were made by dumping a hopperful (6 barrows) of material at once into the furnace, and, when all the fuel of a round (12 barrows) had been put in, the profile of the upper surface was obtained by stretching a steel tape across the top on a diameter and at a known height. By measuring down from this with a graduated rod, the profile was easily obtained with sufficient accuracy, especial pains being taken to get correctly the crests of the ridges and the bottoms of the hollows, as many intermediate points being included as seemed necessary. This was repeated on another diameter when there was occasion. The same course was followed for the limestone and ore.

Jan 1, 1899

By Thomas E. Ban, Charles D. Thompson, Charles A. Czako

Continuous sintering-a metallurgical process for more than 50 years-has broadened from its origin in nonferrous metallurgy to present-day applications in ferrous, chemical, and nonmetallic fields. During the past year, self-fluxing sinter production has been a subject of active interest to iron metallurgists in North America. Accomplishments however, have come predominantly from Europe and proper interpretation of these reports requires an understanding of European raw materials and European economics. The technology, of course, can be applied universally.

Jan 10, 1959

By C. S. Brooks

Several of the commonly used methods for deter-mination of effective grain densities of minerals have been evaluated for accuracy and precision, and their applicability to various types of petroleum reservoir minerals tested. Consideration was given to the effect of consolidation, swelling clay, and wettability on these grain-density determinations. Procedures with helium displacement, a modified low-pressure Boyle's law porosimeter, and liquid displacement (water, n-decane, and n-octanol) were tested. The helium-displacement procedure was used primarily as an independent reference for which the effects of fluid-solid interaction, e.g., adsorption and wettability, were negligible. The procedures with the Boyle's law porosimeter and with liquid displacement are the methods in common use. Minerals investigated included calcite, West Texas limestone core samples, California sandstone core samples, and Wyoming bentonite. The number of samples tested, while not large, was adequate to permit application of statistical methods. Grain-density measurements on calcite (Iceland spar) provided a basis of comparison for the accuracy and precision of the procedures under investigation for a material with a high degree of chemical and physical homogeneity and for which fluid-solid interactions were at a minimum. Liquid-displacement procedures (water or n-decane) provided the greatest reliability and precision for measurement of the grain densities of the limestone tested. Gas-displacement procedures (helium or Boyle's law porosimeter) provided the greatest reliability and experimental convenience, if not the greatest precision, for the measurement of the grain densities of the swell- ing clay, Wyoming bentonite, and the shah sandstones which -contained appreciable amounts of swelling, in-terstitial clays. These experiments were designed to evaluate the applicability of the grain-density procedures in common we to some of the less tractable minerals—tight limestones, shaly sandstones, and swelling clays. The results should provide a useful basis for a selection of the method most suitable for application to the various petroleum reservoir minerals encountered and especially for use in the estimation of formation porosity. INTRODUCTION These experiments were undertaken to evaluate the accuracy and precision of several commonly used methods for determination of effective grain densities of minerals, and to test their applicability to various types of petroleum reservoir minerals. Consideration was also given to the effect of consolidation, clay, and wettability on these grain-density determinations. Procedures used included measurements with helium displacement, with a modified low-pressure Boyle's law porosimeter, and with liquid displacement (water, n-decane, and n-octanol). The minerals investigated included calcite, West Texas limestone core samples, California sandstone core samples, and Wyoming bentonite. The accurate determination of the porosity of petroleum reservoir formations, in particular those of low porosity, has received much attention. Both bulk-volume and grain-volume measurements necessary in the evaluation of porosity have been examined by many investigators with the objectives of improving both the accuracy and the precision of these determinations. In this investigation statistical criteria for selection of the most reliable and suitable procedure for use with a given type of mineral are demonstrated. The grain-volume measurement procedures appear to be the most susceptible to improvement.

Jan 1, 1958

By B. R. Eichbaum, J. E. Murphy, J. A. Eisele

The US Bureau of Mines demonstrated ferric chloride leaching of galena concentrate on a continuous bench scale basis. Leaching was performed at 95°C (200°F) and with a contact time of 15 minutes. The ferric chloride leaching solution was continuously fed to a leaching tank at a constant rate for periods up to 45 hours. In each test, a constant redox potential was maintained in the slurry exiting the leaching tank by controlling the concentrate feed rate. In the 45 hour test, lead extraction exceeded 99.5%, and the lead chloride produced was 99.97% pure.

Jan 1, 1986

By Robert Lowrie

Nine intermetallic compounds were tested in tension at various temperatures. Seven exhibited extensive plastic deformation at elevated temperatures. Correlations of tensile strength and elongation are attempted with melting (decomposition) temperature, valence electron configurations of the component elements, heat of formation, crystal structure, density, and volume decrease accompanying compound formation. A LTHOUGH intermetallic compounds have been -tX known for many years, the study of their mechanical properties, particularly in tension, is just beginning. The problem has been unattractive because of the well-known, erratic behavior of brittle materials tested in tension. The strong influence of surface or internal flaws as stress raisers in non-ductile materials and the effect of eccentricity of loading in superimposing bending stresses on the state of tension in the specimen are extremely difficult to mitigate and impossible to completely eliminate. Thus, tensile properties determined for brittle materials, such as intermetallic compounds at temperatures low in comparison to their melting points, are at best only general guides to the values to be expected in an ideal test of a perfect specimen of the material. It is, nevertheless, surprising that apparently no attempt was made to follow up the pioneer work of Tammann and Dahl1 in this field. Working with crude apparatus, these investigators succeeded in showing unequivocally that at temperatures sufficiently close to their melting points (from 75" to 400°C for the compounds tested) intermetallic compounds did exhibit plasticity. This was indicated by the appearance of slip lines on the surface of the specimen. No observations of strength were made in these tests, which were of a compressive or indentation type. Rossi2 in 1932 attempted to study the physical and mechanical properties of single crystals of a group of intermetallic compounds. However, he was able to prepare only one material, Cu2Z8,, in the form of large, defect-free, single crystals. Thus, he was able to report only the relative fragility of the compounds at room temperature. He reported one compound, Ag,Zn,, to be somewhat plastic at room temperature and Cu,Si to be friable, the latter in agreement with results reported herein. Although test results are available only in classified literature, it has also been announced that MoSi, possesses some ductility at elevated temperatures." In 1948 and 1949 Savitskii and Savitskii and Baron -ublished their work on the hot extrusion of Mg-Zn, Al-Mg, and Cu-Zn compounds. Under the favorable state of stress existing for this process MgZn, MgZn,, MgZn,, ß (Al-Mg), ? (Al-Mg) and 0 (Cu-Zn) could be reduced by amounts up to 90 pct at elevated temperatures. These authors also report that hardnesses of Mg-Zn compounds decrease from room temperature values of about 300 kg per sq mm to 30 to 50 kg per sq mm at 325°C. They found that alloys consisting solely of one Mg-Zn compound were most resistant to softening on heating, mixtures of a compound and eutectic less resistant, and mixtures of two compounds least resistant. The more rapid softening of mixtures of

Jan 1, 1953

By C. T. Young, J. L. Lytton

In recent investigations,1,2 the strength and thermal stability of dislocation substructures prepared by 5 to 25 pct room temperature tensile straining and recovery annealing at 120°, 160°, and 200°C have been studied in randomly oriented polycrystalline high purity aluminum. The techniques of transmission electron microscopy revealed that a major source of the strength and stability of dislocation substructures was the formation, during room temperature straining, of well-defined cells bounded by dislocation tangles which rearranged into nearly perfect dislocation networks during recovery, forming the boundaries of subgrains. The strength of such substructures increases with decreasing cell or subgrain size,2"6 and the formation of fine subgrain structures can provide thermally metastable strength at low temperatures and can favorably alter the course of primary creep at elevated temperatures.7'8 For maximum benefit, however, sub-grain growth should be reduced or eliminated. It was, therefore, decided to investigate the use of heterogeneous precipitation on dislocation networks as a means of imparting increased strength and thermal stability to subgrain structures through effective pinning. C.T. YOUNG, STUDENT MEMBER AIME, and J. L. LYTTON, Member

Jan 1, 1970

By C. M. Schwartz, J. R. Bridge, D. A. Vaughan

THERMAL expansion coefficients of a uranium were originally reported' on the basis of X-ray diffraction measurement of lattice constants at 25°, 300°, and 650°C. These data have been reproduced by Katz and Rabinowitch.' CuK radiation had been used in this work, with consequent crowding of the patterns. Considerable overlap of the back-reflection lines was observed as the temperature was raised. Subsequent reexamination of the data led to the conclusion that errors had resulted from failure to obtain unequivocal indexing of the high angle reflections at elevated temperatures. The measurements have been repeated, using FeK radiation, which provided sufficient dispersion to assure proper indexing of the reflections, at each temperature level. The unit cell dimensions were re-determined at ten temperatures, from 25" to 650°C. Schuch and Laquer easured the macroscopic contraction from room temperature down to —253°C, and reported a negative value from —210" to —253°C; they suggested the possibility of the occurrence of a phase change. In the present work, the lattice constants of uranium have been measured down to —253°C, to test this hypothesis. Filings were prepared from a single piece of pure uranium bar stock. They were carefully cleaned with a magnet and pickled in nitric acid to remove traces of iron from the file. They were then annealed at 600°C in a sealed evacuated silica tube. The annealed filings were pickled in strong nitric acid to remove any oxide layer, washed in water and alcohol, quickly dried, and sealed in evacuated thin-walled silica capillary tubes. If properly sealed, the sample could be heated to the a-ß transforination temperature without significant buildup of the diffraction pattern of oxide. The high temperature X-ray diffraction camera was modified from the design of Hume-Rothery and Reynolds.' The thermocouple used to record the specimen temperature was calibrated from lattice-constant measurements of a standard silver specimen, using the Hume-Rothery and Reynolds values for silver over the temperature range from 25" to 700°C. Temperatures were reproducible to 210°C. Temperatures to —210°C were attained by passing precooled gas over the sample. The gas from the cooling train was directed over the sample capillary tube and thermocouple by means of a chimney of 1-mil polystyrene. The 36-gage Cu-constantan thermocouple had been calibrated by

Jan 1, 1957

By R. W. Nash, A. E. Schwaneke, V. R. Miller

The Bureau of Mines developed a detector for controlling sorting devices to separate the copper-bearing fragments from the barren portion of Michigan native copper and western prophyry copper ores. A successful sorter could be used to preconcentrate the ore and eliminate costly hoisting or hauling of waste. An induction balance unit was developed and used in sorting tests on crushed sized - 2.5 + 1.3-cm (- 1 + 112- in.) ores from the Kingston (0.9% Cu) and Centennial (1.6% Cu) mines of Upper Michigan. Concentrates of 4.0% and 7.5% Cu, respectively, were obtained at recoveries of 85 and 80% of the copper in the feed. Eighty percent of the sorted ore was rejected as tailing. Sorting larger fragments improved the separation efficiency. Tests on - 10+ 5-cm (- 4 +2-in.) sized Kingston (1.6% Cu) and Centennial (2.1 % Cu) ore samples yielded concentrates of 4.3 and 4.5% Cu, respectively, with corresponding recoveries of 92 and 91 %. A bout 60% of the sorted ore was discarded as tailing. Porphyry copper sulfide ores also responded to electronic sorting but at a lower separation efficiency. Sorting response was affected by the degree of segregation.

Jan 1, 1979

By K. P. Gupta, P. A. Beck, N. S. Rajan

By determining the a phase boundaries in the following ternary systems: V-Fe-Si (at 1175oC), V-Co-Si (at 1175°C), V-Ni-Si (at 1175oC), Cr-Mn-Si (at 1000°C), Cr-Co-Si (at 1175°C), Cr-Ni-Si (at 1175°C), V-Fe-A1 (at 1175°C) and Cr-Co-A1 (at 1175°C), it was found that Si exerts a stabilizing effect on these a phases, while A1 tends to destabilize them. Si atoms in solid solution occupy sites D in the a structure, The co/ao ratio increases with increasing Si-, Mn- or Fe-content. The volume of the unit cell decreases with increasing Si-content. THE stabilization of certain metal silicides (the Nowotny phases) by the addition of relatively small

Jan 1, 1961

By R. C. Nelson, T. L. Weaver, A. I. Michals

This paper describes the design and performance of an apparatus for making continuous nondestructive resistance measurements throughout a spool of fine wire. Highly reproducible results on clean and graphite coated tungsten and rnolybdenum wires from 1 to 9.5 mil are presented. A linear relation between resistance and wire weight (per standard length) was obtained on clean wires, but only on those coated wires with very uniform coatings. Results indicating a correlation between tensile strength, hardness, and resistivity are reported. THE increasing demand for greater uniformity in fine tungsten and molybdenum wires destined for use as mandrels, grids, and coils in radio tubes and as filaments in light bulbs has rendered inadequate the standard (sampling) approach to the control of wire diameter and other physical properties. This ap-

Jan 1, 1961

By Andrew E. Nevin, Sidney A. Williams, James N. Lukanuski

Three porphyry copper districts in southern Arizona are partly overlain by post-ore fanglomerates with certain physical and petrologic characteristics which define a distinct and significant class of rock. These units are the Locomotive fanglomerate at Ajo, the Helmet fanglomerate at Twin Buttes-Mission-Pima, and the Cloudburst formation at San Manuel- Kalamazoo, herein termed “Locomotive-type fanglomerates.” Post-ore units at Poston Butte and Lakeshore, Ariz., and Sar Chesmeh, Iran, also appear to fit this class. Locomotive-type fanglomerates may be genetically related to porphyry copper deposits as subsequent products of differentiation, volcanism, uplift, and sedimentation in short-lived basins of limited areal extent. These units are sufficiently distinct to be utilized as exploration guides for porphyry copper deposits in the Southwestern U.S., northern Mexico, and elsewhere.

Jan 1, 1977

By John W. Lane, Richard A. Ronzio, Frederick N. Bender

Climax Molybdenum Co. operated a hydrometallurgical plant at Climax, Colo., from August 1966 to August 1968 to recover molybdenum from an oxidized ore. The feed, tailings from sulfide flotation, was first upgraded by cycloning. The concentration plant handled 6000 tpd of feed and produced 2000 tpd of slime concentrate. The concentrate was leached by a sulfuric-sulfurous acid solution at 65°C. The molybdenum was solubilized in the form of "molybdenum blue." Activated charcoal was added to the leach tailings in a resin-in-pulp type circuit. Molybdenum was adsorbed on the charcoal. The charcoal was screened from the pulp and washed. The washed charcoal was pumped to columns where it was ammoniated and air-blown. The oxidized molybdate then was washed from the charcoal. The eluate was evaporated until ammonium dimolybdate crystallized out. The ammonium dimolybdate was calcined to molybdenum trioxide.

Jan 1, 1973

By J. A. Herbst, J. L. Sepulveda, J. D. Miller

Abstract-Lead cake, a zinc smelter flue dust residue, consists primarily of lead sulfate. Characteristic properties of lead cake were determined in order to aid the understanding of reaction mechanisms involved in bismuth removal from lead cake by sulfuric acid digestion. Sp gr (specific gravity) measurements, surface area measurements, and photomicrographs revealed that the particles of lead cake are quite porous and seem to consist of an agglomeration of submicron grains (0.4 pm) fused together in a manner similar to cement clinker. Analysis of experimental rate data, which was independent of particle size, indicates that the dissolution reaction involves two distinct, rate limiting steps. The initial stage of reaction appears to be limited mainly by intergranular diffusion of the reactant, hydrogen ion, while the latter stage of reaction appears to be controlled by diffusion of soluble reaction products through the reaction product layer of the individual grains.

Jan 4, 1978

By F. J. Deadrick, A. L. Ramirez, R. J. Lytle

This article describes the evaluation of a new geophysical technique used to map fractures between boreholes: electromagnetic geotomography used in conjunction with salt water tracers. An experiment has been performed in a granitic rock mass. Geotomographic images have been generated and compared with borehole geophysical data: neutron logs, acoustic velocity logs, caliper logs and acoustic televiewer records. Comparisons between the images and the geophysical logs indicate that clusters of fractures were detected but single fractures were not.

Jan 1, 1982

By P. D. Merica, A. N. Finn, R. G. Waltenberg

CeRtain compositions of the light, i.e., aluminum-rich, alloys of aluminum with magnesium and copper have become quite well known within the past ten years under the name of duralumin. These alloys are used for rolling and forging and can be so treated as to develop quite remarkable mechanical properties. Thus a properly heat-treated alloy containing about 4 per cent. of copper and about 0.5 per cent. of magnesium, rolled into sheet or rod, will have a tensile strength of approximately 55,000 1b. per sq. in. (3866 kg. per sq. cm.) with an elongation in 2 in. (50.8 mm.) of about 15 per cent. This alloy, duralumin, was developed by Wilm,1 and its properties more fully described by Cohn.2, The authors considered it worth while to investigate the mechanical possibilities of the light alloys of two somewhat analogous ternary series; namely, of aluminum-magnesium-nickel and aluminum-magnesium-manganese, to study the effect of variation of composition upon mechanical properties within the alumimum-rich group of the aluminum-magne-

Jan 1, 1921

By E. Buehler

THE floating zone refining technique'-4 has provided a new experimental approach to the purification of many reactive materials especially those with high melting points. The method avoids the use of a crucible and at the same time it provides a favorable environment at the freezing interface for the growth of single crystals. The physical properties of refractory metals such as molybdenum and tungsten have long been of interest from a fundamental point of view and because of their widespread use in vacuum electronics. Single crystals are often desirable for study. Prior to the introduction of zone melting, single crystals of these metals were usually grown in the solid state at temperatures slightly below the melting point by strain annealing3 or by the application of a moving temperature gradient. Such techniques were mostly successful on wires, ribbons, or rods having small cross-sectional areas. Recently, larger samples of tungsten, molydbenum, tantalum, columbium, and rhenium were melted by a floating zone process which employed electron bombardment heating.10 Single crystals were obtained in many instances

Jan 1, 1959

By G. F. Bolling

HE high mobility of grain boundaries in zone-refined metals has been particularly demonstrated for lead above 150°C in grain growth studies1 and in the extensive work by Aust and Rutter.1 In these investigations, no elaborate precautions were taken to eliminate oxygen from the zone-refined lead; however the alteration of creep characteristics by oxygen concentrations of less than 5 x 10 -5 wt pet

Jan 1, 1962

George Otis Smith, Washington, D. C. (communication to the Secretary) : The somewhat exceptional features discussed by Dr. Jenncy in his paper on " The Mineral Crest" mere recognized and described by Mr. Tower in our report on the Tintic district. The general absence of surface-outcrops of important ore-bodies, and their occurrence, when present, at relatively low points, are noticeable characteristics of this district, and the statements made by Dr. Jenncy agree in general with our observations. The approximately horizontal upper limit of the Silver Gem ore-body in the Bullion-Beck mine is figured in this report, and mention made also of the horizontal pipes of ore found in several mines." In only one case," however, was any hypothesis

Jan 1, 1903

By D. M. Lewis, R. C. Emmett, B. C. Wojcik, F. A. Baczek

The ElectroSlurry™ electrowinning concept has been incorporated into a process flowsheet for recovering copper from smelter flue dusts. The process has averaged 96% recovery of the copper as high-grade electrowon cathode, while at the same time removing a majority of the impurities that degrade drawn copper as a result of recycling flue dust and liberator cathodes. The dust is processed through several stages consisting of leaching, copper precipitation, ElectroSlurry electrowinning, and waste liquor treatment. The process may be integrated into a smelter operation and become an effective and feasible means of maintaining good product purity.

Jan 1, 1981