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By Herbert R. Babitzke

As part of a project to develop refractory metal alloys suitable for high-temperature structural applications, the Bureau of Mines applied solid solution and precipitation-hardening techniques to columbium and tantalum alloys. Thirty-three alloys were evaluated to determine their formability, strength, and oxidation resistance. Three alloys had tensile strengths near 40,000 psi at 1,200° C: Cb-1N-5W-5V-10Hf (No.4), Cb-15Hf-5W-0.5B (No. 31), and Cb-15Hf-SW-IB (No. 32). Oxidation resistance of the high-strength alloys was good. Alloy4 gained only 34 mg/cm2 at 1,200° C, and 21 mg/cm2 at 1,000° C in 2 hours. Hot forming was done without any protection from oxidation.

Jan 1, 1968

By E. L. Singleton

The electrochemical reduction of aluminum chloride to aluminum was investigated in a closed, two-compartment cell utilizing a molten chloride electrolyte. The externally heated cell was divided into a reduction compartment and a combination AICl3 feed and metal removal compartment. Aluminum was deposited at 700° C on a molten aluminum catbode from a KCI-NaCI-AICI3 electrolyte. The AICl3 content of the electrolyte was replenished by either vapor or solid additions. The chlorine evolved was collected and measured to give a quantitative evaluation of AICl3 reduction. The effects of anode and cathode current densities and AIC13 concentration on anode current efficiencies were studiedo A range of 64 to 84 percent anode current efficiency was obtained with the 25-pound electrolyte capacity cell and related auxiliary equipment.

Jan 1, 1968

By Philip C. Good

Preliminary studies showed that direct hydrolysis of H2SiF6 to SiO2 and HF at elevated temperatures was subject to many mechanical difficulties, and that corrosion of construction materials was a serious problem. Elimination of SiO2 from the HF product was generally poor. An alternative procedure, hydrolysis of lime-neutralized H2SiF6 by steam at 950° to 1,100° C, yielded a product very low in SiO2. Condensates containing up to 300 g/1 HF were prepared.

Jan 1, 1968

By M. E. Tyrrell

Research objectives were to determine the reasons for erratic behavior of semisilica horizontal zinc retorts in service; to investigate potential corrective measures including the possible utilization of more refractory materials in the retort body; and to delineate laboratory tests suitable for process control in the manufacture of retorts. Correlation of laboratory test results and data supplied by the cooperating smelters indicated that structural failures due to thermal shock and laminations in the retort body are largely responsible for the erratic behavior of horizontal zinc retorts in service. The most promising modifications made in the retort body and evaluated on a laboratory scale included finer grinding of the plastic clay fraction, substitution of mullite grog for calcined fire clay and grain alumina for silica, plus the use of an organic binder. Lamination-free extrusions having excellent thermal shock resistance were prepared from a mixture composed of 50 percent low-silica Missouri plastic clay through 100 mesh, 25 percent mullite grog through 6 mesh, and 25 percent alumina through 100 mesh. The mix was pugged under 28-inch vacuum with 1 percent ligno sulfonate binder in 12 percent tempering water. Laboratory tests suitable for process control in the manufacture of retorts are described.

Jan 1, 1969

By J. E. Zeilinger

This Bureau of Mines report describes the preparation characteristics of the significant coalbeds of Clay, Gilmer, and Lewis Counties, W. Va. In 1966, almost 1.3 million tons of coal was mined in these counties, of which more than one-half was from the Pittsburgh coalbed. Washability analyses were made of 16 coalbed samples. Of these, only 11 samples could be upgraded to metallurgical quality. For steam or power generation five of the coals were of low sulfur content as received. The remaining samples were generally of medium sulfur content even after upgrading.

Jan 1, 1969

By Alla D. Mah

The heats of combustion of three chromium carbides, Cr23C6, Cr7C3, and Cr3C2, were determined by combustion calorimetry. Heats of formation calculated from the results follow: ?Hf°298 (Cr23C6) = -94.7 ± 5.0 kcal/mole, ?Hf°298 (Cr7C3) = -43.3 ± 1.7 kcal/mole, and ?Hf°298 (Cr3C2) = -22.5 ± 0.8 kcal/mole.

Jan 1, 1969

By R. R. Brown

The Bureau of Mines undertook a limited feasibility study to determine the practicality of removing copper from automobile scrap by thermal treatment. Test specimens, prepared by wrapping bare and insulated copper wire around small steel coupons, were heated at 600° to 1,150° C in various atmospheres for different lengths of time under both static and dynamic conditions. The tests indicated that adequate removal of copper cannot be effected by thermal treatment of scrap above the melting point of copper. Tests showed that copper present in scrap as insulated wire is embrittled by thermal treatment at 800° to 900° C if the insulation contains lead, and that the embrittled copper is almost completely removed by a mechanical action such as tumbling. Also chemical pretreatment of specimens to effect embrittlement of copper and the magnetic separation of oxide scale were studied. Tests showed that bare copper can be embrittled by depositing waterglass (Na, Si409) on copper prior to thermal treatment.

Jan 1, 1968

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instruction3 issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor; if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1969

By Edward W. Parsons

To determine in what part and to what extent creep or movement exists in an installed rock-bolt anchor and the effect of the creep or bleedoff on the tension load on a rock bolt, as well as the effect of normal mining activity on the rock-bolt load and anchor, the Bureau of Mines conducted tests in the laboratory and in two mines using four types of expansion-shell anchors, the wedge bolt, and in one mine, explosive-anchored rock bolts. Specially mounted heavy-duty springs, calibrated to obtain load readings from spring movement, were installed on the test bolts to prevent a drastic reduction in tension load caused by slipping or seating of the anchor. A dial gage, reading to 0.0001 inch, measured movement of the anchor shell against the rock and seating of the anchor wedge plug in the shell. While all bolts had electrical resistance strain gages for load reading, only readings from the laboratory tests were used because those from the field tests were erratic. The tests revealed that most load loss resulting from static loading is due to the slippage and seating of the serrations on the anchor shell into the drill-hole wall. Dynamic loading, primarily from sudden shocks from nearby blasting, and possibly from ground movement or mining activity, will cause the anchor wedge plug to seat in the anchor shell.

Jan 1, 1969

By C. C. Merrill

The Bureau of Mines beneficiated the wastes generated by commercial titanium chlorination operations to reclaim metal values and reduce the problem of disposing of solid wastes. A water leach solubilized about 40 percent of the dry weight and over 75 percent of the metallic impurities. The residue from the water leach was rich in titanium dioxide and carbon; it was combined with rutile and recycled to a laboratory chlorinator. The contained carbon was used in lieu of part of the coke requirement.

Jan 1, 1969

By G. H. Keith

Oxygen and nitrogen cause strain aging in electrorefined vanadium, as evidenced by maxima in yield and tensile strengths and by Snoek internal friction peaks. Alloys containing up to 0.22 percent oxygen and 0.11 percent nitrogen were investigated. Tensile strengths of oxygen-and nitrogen-containing alloys were 66,000 and 68,000 psi at 300° to 400° C, compared with 53,000 and 62,000 psi, respectively, at room temperature. Total elongation decreases to about 7 percent at the temperature of maximum strength. At 600° C, strain aging is not evident. Based on interstitial contents calculated from internal friction measurement, the increases in strength caused by nitrogen and oxygen were 440,000 psi per weight-percent nitrogen and 260,000 psi per weight-percent oxygen. Application of the Schoeck and Seeger treatment to the Snoek effect in these systems results in a calculated lattice distortion of 0.24 and 0.15 caused by the presence of an interstitial nitrogen or oxygen atom, respectively. Alloys containing boron or carbon were also investigated. Both elements refine the grain size but have no other effect because of their low solubility in vanadium.

Jan 1, 1969

By Verne E. Hooker

In situ stresses, based on isotropic and anisotropic relations, were evaluated using computer techniques from overcoring data obtained in dimension stone quarries along the Appalachian Piedmont, the Ozark Uplift, and the Ouachita Tectonic Belt. Stresses in the horizontal plane near the surface are compressive and range from 100 to 4,500 psi. The direction of maximum compressive stress seems to be alined with the general tectonic structure for most of the determinations. The ratio of the maximum to minimum elastic parameters in the horizontal plane ranges from 1.05 to 2.46 for these competent rocks. Isotropic versus anisotropic stress determinations show differences only as great as 25 percent in stress magnitude and 25° in orientation.

Jan 1, 1969

By John E. Kelley

The Bureau of Mines conducted a study to determine the feasibility of joining refractory metal compounds to each other and to oxide ceramics by a vacuum hot press-diffusion bonding method. Very satisfactory joins were made of ZrC to ZrB2, ZrN to ZrB2, ZrC to ZrN, and of ZrC, ZrN, and ZrB2 to Al203. Each of these join assemblies contained a mixture layer comprising 50 weight-percent each of the two end compounds. The mixture layer, sandwiched between each end compound, enhanced bonding and smoothed out the thermal expansion gradient between the two end members. Strength and thermal shock tests showed that the join areas of the ZrC, ZrN, and ZrB2 joins were stronger and more shock resistant than the parent materials. Also included in the joining tests was one each of TiC to TiB2, TiC to TiN, TiB2 to TIN, and TiC to ZrB2 joins. Each of these was well bonded, showing that the vacuum-hot-press method can be used for a variety of systems.

Jan 1, 1969

By F. R. Cattoir

This Bureau of Mines study investigated molten salt electrorefining for beneficiating low-grade, high-carbon ferrochromium products which can be readily produced from domestic chromite concentrates. A second objective was to refine commercial ferrochromium into low-iron chromium products. Electrorefining of both types of ferrochromium in molten CaC12-NaCl-CrC12, CaCl2-MgC12-CrCl2, or KC1-LiCl-CrCl2 electrolytes produced chromium-iron products with virtual elimination of other impurity elements and some lowering of the iron content, Over 90 percent of the chromium present in the feed materials was recovered. The electrodeposited products were upgraded further by magnetic separation techniques into chromium containing less than 5 percent iron. The technical feasibility of preparing a premium chromium product from a low-grade, high-carbon ferrochromium made from domestic chromite was demonstrated. Chromium virtually free of carbon, oxygen, and silicon from high-carbon ferrochromiums was produced. In addition, the amenability of three commercial grades of ferrochromium to electrorefining and magnetic separation for preparing chromium metal containing less than 5 percent iron was determined.

Jan 1, 1969

By D. H. Desy

The Bureau of Mines studied the properties of copper that had been oxide dispersion-strengthened with 2 vol pct of either yttria or alumina. Compounds of copper and aluminum or yttrium, coprecipitated from aqueous solution, were converted to oxides; the copper was reduced, compacted, sintered, and extruded. For the resulting copper-dispersoid composites, room temperature tensile properties after annealing in hydrogen, elevated temperature tensile and stress-rupture properties, and electrical conductivity were determined. Compared with oxygen-free copper, copper-2 vol pct alumina or yttria had improved strength after annealing between 400° and 1,000° C, and improved elevated temperature strength, with little loss in electrical conductivity.

Jan 1, 1969

By L. A. Neumeier

The Bureau of Mines evaluated the properties of a Zn-0.75 pct Cu-0.12 pct Ti alloy extruded at temperatures between 400° and 720° F. The extrusions were made with a reduction ratio of 28-to-l and at relatively slow speed. Rod was also extruded at 560° and 640° F with a reduction of 255-to-l. With increased extrusion, temperature, extrusion pressures decreased substantially and creep resistance of the rod improved significantly. Coefficients of thermal expansion were low in the long rod dimension. Microstructures, hardness, and tensile properties were also evaluated, and a limited evaluation was made of bend ductility at 32° F for the rod extruded with the 255-to-1 reduction.

Jan 1, 1969

By Thys B. Johnson

Operations Research techniques for determining optimal shipping schedules and production and product allocation are discussed. A hypothetical mining operation model is formulated by the Bureau of Mines, and optimal production and product allocation are determined. The technique of sensitivity analysis is discussed and is used to illustrate the effect of the variability in a mining operation on the optimal production and product market plan.

Jan 1, 1969

By J. T. McCartney

In an effort to correlate the size of pyrite particles in coal and coal-particle association with the removal of pyrite before burning, the Bureau of Mines conducted a study of 61 coals presently being used for electric power production. The results were obtained by visual microscopic studies of polished briquets of minus l4-mesh samples. Mean pyrite particle sizes ranged from 20 to 400 microns and proportions of pyrite contained in coal particles to an extent greater than 50 percent by volume (estimated) ranged from 20 to 95 percent. These parameters were correlated with reductions in pyrite accomplished by float-sink tests at 1.60 sp gr on 14-mesh, 3/8-inch, and 1-1/2-inch samples. The correlation coefficients between pyrite removal and mean pyrite particle size were 0.89, 0.84, and 0.79, respectively, for these samples. Correlation coefficients between pyrite removal and coal-pyrite association parameter were 0.92, 0090, and 0.85, respectively. It is apparent that extent of pyrite removal can be fairly well predicted from microscopic analysis.

Jan 1, 1969

By Wesley T. Holmes

In this final stage of a three-part investigation of the smelting of titania-bearing iron materials, the Bureau of Mines conducted semicontinuous smelting tests in a laboratory electric arc furnace on four concentrates and one are. The objective was to substantiate the significance of liquidus temperature measurements in predicting satisfactory slag compositions in electric furnace smelting of titaniferous magnetites to produce pig iron. Previously obtained liquidus temperature data were used in determining flux requirements. Self-fluxing pellets of either ore or concentrate plus fluxes and reductants were made to produce pig iron and slags containing 0.2 to 0.6 percent titanium. Individual constituents of the slags generally agreed within 5 percent with the value of the corresponding constituent of target composition. Liquidus temperature of furnace slags generally agreed within 50° C of the value obtained from corresponding nominal synthetic slag. The results of the three phases of the investigation may serve as guide-lines for determining flux requirements in smelting a wide variety of titaniferous magnetites and other titania and iron-bearing materials.

Jan 1, 1969

By G. W. Weems

The Bureau of Mines used the Burnett method and apparatus to determine the compressibility factors for helium and carbon dioxide mixtures at 0°, 10°, 20°, 23°, and 35° C and to pressures of 900 psia. Tables of compressibility factors and approximations of the virial coefficients are presented for seven binary mixtures as well as for helium and carbon dioxide. The results compare favorably with existing data.

Jan 1, 1969