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By K. R. Dorman

To develop the potential of precast concrete sets as a support medium in underground mines, a three-piece precast concrete drift set was designed for a small opening and tested to destruction in an underground straining frame. Thirty-six tests were made with three sizes of members using three different loading conditions. In addition, 14 members were tested individually in the laboratory. Test results are compared with theoretical calculations. A cost comparison shows the use of concrete sets would be advantageous where conventional wooden timber requires excessive replacement.

Jan 1, 1968

By A. G. Starliper

Laboratory studies were made to produce whiskers of tungsten over a wide range of operating temperatures. Hydrogen reduction of tungsten hexachloride in a vacuum furnace at temperatures from 2,7000 to 3,3000 C yielded a small quantity of tungsten whiskers, provided a low degree of supersaturation was maintained. Direct measurements of 3,000,000 to 4,000,000 psi were obtained for the ultimate tensile strengths of individual whiskers averaging 3 to 4 microns in diameter with average aspect ratios of 1,000. This compares with strengths of 300,000 to 400,000 psi for 13-micron-diameter commercial filaments.

Jan 1, 1968

By Hillary W. St. Clair

Reaction rate coefficients were determined from analyses of the effluent gas for the reduction of granular ferrous oxide to metallic iron by passing carbon monoxide through a packed bed of oxide at a controlled rate in the temperature range 1,000° to 1,300° C. Coefficients were determined by the comparison of observed analyses and calculated analyses using a mathematical model that takes into account the nonuniform composition of both the solid oxide and the gas. A method is also given for finding the value of the rate coefficient that best fits the observed data.

Jan 1, 1968

By F. W. Wood

The use of consumable.-electrode arc melting as a production technology is growing. One advantageous feature of this process is that it avoids ingot contamination by soluble crucible materials by employing a chilled metal crucible. Because the thermal balance under these conditions is rather delicate and does not necessarily provide a favorable environment for solidification, catastrophic imbalances can occur. The effectiveness and mechanistic roles of various factors are mostly unknown, and more intelligent insight regarding the distribution of temperature and heat is needed. Experience has provided several pertinent observations, some of which are quite superficial. The most meaningful data have resulted from studies of molten pool shapes and sizes and from measurements of heat flow through crucible walls. Overall experience, intuitively interpreted and supplemented, is sufficient nevertheless as a basis for a boundary-value treatment of the problem. A mathematical analysis based on a separation of variables, using conventional differential equation methods, provides a useful solution. For a cylindrical ingot, the temperature varies as a Bessel function of an argument proportional to the radius and as an exponential function of longitudinal position. Trial calculations using the problem solution seem to verify the general correctness of the result as compared with experience. The role and nature of solution parameters are also clarified, though not entirely resolved. It is revealed that the barrier to heat flow at the ingot-crucible surface has a prominent influence. Utility of the model embodied in the problem solution is readily demonstrated by considering a variety of contemporary questions about arc melting, and it is hoped that utility can be enhanced by improvement of the model.

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 Andrew J. Fergus

The purpose of this study was to provide basic information to aid further research on beryllium mineral flotation. Contact-angle and microflotation (Hallimond tube) methods were used to study collector action and flotation response of beryllium minerals and associated gangue minerals with representative commercial surfactants. Chrysoberyl received prime attention. Results indicated that selective flotation of beryl and chrysoberyl from fluorite and quartz is possible with sodium isooctyl phosphate below pH 2, and fluorite and topaz are readily collected by both anionic and cationic surfactants. Several modifying reagents were studied at one pH and one level of collector concentration. Aluminum sulfate, starch, and sodium silicate proved to be depressants in chrysoberyl flotation.

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 Edwin M. Murphy

Methods are described for filling underground cavities remotely with dry material pneumatically injected through a borehole to seal openings, prevent air movement, and reduce subsidence; this often brings underground fires under control by limiting the access of air. Large-scale tests were made in the Bureau of Mines Experimental Coal Mine, Bruceton, Pa., in an operating mine, and in an abandoned Pennsylvania mine. Supplemental trials were made aboveground in galleries and in the laboratory. The parameters studied include horizontal and inclined passageways, obstructions in the entry, water leakage into the borehole, dry material, and grout and slurry mixes. The materials studied were fly ash, crushed and pulverized limestone, and sand. Best results were obtained with dry fly ash, though satisfactory seals were obtained with the other materials. When a borehole is dry and ends at an open void, casing is not necessary. If more than 5 gpm of water flows in the borehole, if the void contains loose debris, or if coarse material is injected, a material feedpipe should be inserted through the borehole. Fly ash was most suitable for remote filling because of its low angle of repose (8°) and its good flow characteristics. The depth of borehole through which the fly ash is injected has no appreciable effect on the filling operation.

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 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 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