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By David R. Flinn

This Bureau of Mines report describes methods to electrodeposit erosion-resistant titanium diboride coatings from molten alkali metal borate baths at 900° C. These coatings have been shown to be highly resistant to material loss during impingement with high-velocity alumina and silicon carbide powders, and they show promise as protective coatings to reduce metal loss in erosive chemical environments, such as coal gasification systems. The most erosion-resistant coatings were prepared on nickel, Inconel, and molybdenum from an electrolyte containing LiBO2, NaBO2, Na2Ti03, and TiO2. The best coatings were deposited at current densities of [~]20 ma/cm2, using titanium or titanium diboride anodes. Erosion-resistant coatings were shown to exhibit (1) a high degree of crystallographic orientation along the (100) or (110) planes, (2) a chromium impurity level of less than 3 pct, and (3) a uniform, smooth, consolidated surface appearance when viewed under a microscope or by scanning electron microscopy. Optical spectroscopic studies of the molten electrolyte suggest that the lower valent (+3) titanium ion predominates in the baths.

Jan 1, 1979

By J. S. Hansen

In support of its objective to conserve mineral resources by minimizing premature failure of materials, the Bureau of Mines conducted a cooperative study with the U.S. Department of Energy on the erosion and abrasion resistance of hard materials for valves in coal conversion systems. This report describes a newly developed erosion-testing apparatus and presents data on the erosion resistance of over 200 materials. Erosion resistance of most metals was comparatively low. In contrast, ceramics and cermets such as B4C, WC, SiC, Si3N4, and TiB2, when fabricated to minimize porosity, displayed greater than five times the erosion resistance of metals. Coatings such as boron diffused into Mo and WC, chemical-vapor-deposited TiCN, and electrodeposited TiB2 were highly erosion resistant if applied in thicknesses ranging from 60 to 75 µm. Erosion resistance of cemented carbides was inversely related to metal binder content.

Jan 1, 1979

By A. Visnapuu

The Bureau of Mines, as a part of its goal to minimize occupational hazards associated with mining and mineral processing operations, has developed and field tested a compact exhaust air muffler for mechanized, jumbo-mounted pneumatic rock drills. The muffler is constructed of 1/8-inch sheet steel and has nominal dimensions of 1-3/4 by 9 by 13 inches. A directed air passage, flexible neoprene baffles, and an expandable slit-type outlet are incorporated to reduce drill exhaust air noise and eliminate muffler icing. Field tests in actual mining operations showed a l5-dbA reduction in exhaust noise and an 8-to 12-dbA reduction in overall drilling noise with no icing problems or decrease in drill performance. Data are presented on muffler construction, laboratory, and field test results.

Jan 1, 1979

By James R. Aggson

This Bureau of Mines report presents a finite element analysis of roof stresses associated with a 4-foot-high by 18-foot-wide underground coal mine entry. This analysis starts with known loading conditions determined in an underground coal mine in West Virginia and is extended to other possible underground loading conditions. The roof failures predicted by the finite element analysis under known loading conditions correlate well with the roof failures observed underground. The most probable failure modes are identified for the various loading conditions considered. Various failure preventive measures are discussed.

Jan 1, 1979

By P. C. Good

This Bureau of Mines report describes the preparation of phosphoric acid directly from phosphate ore, without prior beneficiation, in a small-scale, continuous process research unit, as part of an effort to improve minerals and metals recovery from domestic resources while minimizing environmental effects. Three phosphate-matrix samples, ranging in grade from 18.2 pct P20S5to 11.9 pct P205, were dry-fed at a rate of 1.82 kg/hr (4 lb/hr) to a continuous-circuit, 12-liter, single-tank digester to yield phosphoric acid and byproduct gypsum filter cake. Comparison with earlier data shows that a significantly improved filtration rate was attained in a single-tank reactor compared with that attained in a five-tank reactor train processing the same ore. Iron and aluminum impurities in the product phosphoric acid averaged about 60 pct higher than amounts reported in commercially prepared, concentrate-derived acid. All gypsum filter cakes prepared had a firm, sandy texture, rendering them physically suitable for stacking or landfill use. Introduction of dry attritioning and air classification approximately doubled the attainable filtration rate when the dry-beneficiated product was digested. In air classification, there was a 12-to 14-pct P205 loss. Depending on the technique used and the matrix grade, overall P205 recovery ranged from about 72 to 89 pct.

Jan 1, 1979

By L. A. Haas

The U.S. Department of the Interior, Bureau of Mines, is conducting laboratory-scale research to determine the leaching conditions required with sulfuric acid for extracting base metal from a matte with a copper-to-nicke1 ratio of 6 to 1. The matte (61.2 pct Cu, 9.7 pct Ni, 3.3 pct Fe, 21 pct S, and about 5 oz of precious metals per ton) was prepared from Duluth Complex (Minnesota) ore by smelting a bulk sulfide flotation concentrate. The matte was pre leached at atmospheric pressure to selectively extract 20 pct of the nickel, and the undissolved solids were referred to as the matte residue. Autoclave leaching of the matte residue extracted over 95 pct of the nickel, copper, and iron. The remaining leach residue in the autoclave contained over 100 oz of precious metals per ton. The leaching conditions required were matte grind of greater than 98 pct minus 325 mesh, pulp concentration of 50 g/1, total pressure of 100 psig with oxygen at 150° C or 400 psig with air at 180° C, 50 g/1 H2S04, 700 rpm agitator speed, and 6 hours of leaching time. The leaching time was decreased to 2 hours by increasing the agitator speed to 1,300 rpm. Sulfuric acid concentration greater than 50 g/1 did not appreciably enhance the base metal extraction, but with less acid, residues with higher iron concentrations were obtained. Supersaturation of the liquor was prevented at 150° C by using a 1ixiviant that contained 30 g/l Ni and 20 g/1 Cu.

Jan 1, 1979

By T. E. Bernard

The CO2-absorbent canisters used in four approved rescue breathing apparatus were investigated. A breathing machine was used to simulate human expiration with gas flow rates of 26, 37, and 48 1/min of 3.5% CO2 in air. The exit gas CO2 concentration, the pressure drop across the canister, and the exit-gas temperature were monitored. The absorbent capacities of the packed-bed canister designs were found to be dependent on flow rate within the range studied, while the capacities of the other designs were less affected. The radial canister had the least resistance to breathing while the complex bed design proved to be the most effective in utilization of the chemical. The overall results indicated that LiOH (lithium hydroxide) has the highest capacity for CO2 absorption among the absorbents tested. It can be used in a simple packed-bed design while maintaining acceptable levels of resistance and exit-gas temperature. Examination of oxygen supply with respect to CO2-absorption capacity suggested that it is desirable to closely match CO2-absorption capacity with the avail-able O2 supply to minimize the size and weight of rescue breathing apparatus.

Jan 1, 1979

By D. E. Shanks

As part of its goal to help maintain an adequate supply of minerals to meet national economic and strategic needs, the Bureau of Mines, U.S. Department of the Interior, is investigating a fused-salt electrolytic procedure for producing zinc metal. A previous report described preliminary, small-scale work on the fused-salt electrolysis of ZnC12. The present report covers a more detailed investigation of the properties of ZnC12-alkali metal chloride electrolyte systems in relation to the production of zinc metal and also discusses electrolysis in largescale, internally heated cells. The effect of composition on bath stability, current efficiency, cell voltage, and liquidus temperature was determined for the ZnCla-NaC1-KC1, ZnC12-NaC1-LiC1, and ZnC12-KC1-LiC1 electrolyte systems. An electrolyte com-posed of 38 mole-pct ZnC12, 31 mole-pct NaC1, and 31 mole-pct KC1 gave the best overall results. Sludge (ZnO) formation in the ZnC12-NaC1-KC1, ZnC12-KC1-LiC1, and ZnC12-KC1 systems was investigated during prolonged electrolysis. The ZnC12-KC1-NaC1 electrolyte showed the least sludge formation. A 1,500-amp cell was operated using the ZnC12-NaC1-KC1 electrolyte at 500° C. Zinc metal was produced at the rate of 4.0 lb/hr with a current efficiency of 95 pct.

Jan 1, 1979

By E. R. Cole

The Bureau of Mines developed a procedure that enables substitution of zinc cathodes for the aluminum cathodes normally used in commercial zinc electro-winning. Using zinc cathodes eliminates the necessity for stripping and makes it possible to electrowin zinc from solutions derived from material containing excessive amounts of soluble fluorides; for example, zinc concentrates obtained as a byproduct of fluorspar mining in Kentucky and Illinois. To demonstrate the viability of using zinc cathodes, fluoride-containing zinc concentrate was roasted, leached, and purified according to current commercial practice. Electrolysis was carried out in 0.8-, 1-, 5, and 10-liter cells at 35° to 40° C with a cathode-current density of 8 amp/dm2 in a solution containing 65 g/l Zn++ and 200 g/l H2S04 using PbO2 anodes. Zinc deposits were produced on zinc cathodes with good morphology and excellent current efficiency (90 to 94 pct) in solutions containing enough fluoride (~0.5 g/l, F+) to cause sticking of zinc to aluminum cathodes. The approach described has failed previously because of severe solution-level corrosion of the zinc cathodes. The present investigation found that the use of a simple mechanical barrier to prevent oxygen migration from the anode was sufficient to prevent solution-level corrosion of the zinc cathode starting sheet.

Jan 1, 1979

By William C. McBee

Specialized sulfur concretes were developed by the Federal Bureau of Mines as a result of research for the beneficial utilization of sulfur in construction materials. Materials were developed for use in acid and salt corrosive environments where portland cement concrete has been found to deteriorate. Because the mineral aggregates also come into contact with the corrosive media, concretes were developed utilizing both limestone and quartz aggregates. The sulfur binder used with both aggregates was modified by reaction with 5 pct dicyclopentadiene to improve product durability. Sulfur quartz aggregate concrete was found to have moderately high strength characteristics (6,000 psi compressive) and was extremely resistant to chemical attack by both acid and salt solutions. Sulfur limestone aggregate concrete exhibited very high strength characteristics (9,000 psi compressive) and was extremely resistant to chemical attack of salt solutions. Both types of concretes maintained their strength and integrity after long-term testing in acid and salt solutions and exhibited considerable resistance to damage by the action of freezing and thawing. Potential uses include leach tanks, electrolytic cells, thickeners, bridge decking, industrial flooring, pipe, and tile.

Jan 1, 1979

By A. E. Raddatz

The Federal Bureau of Mines, as part of its goal to minimize undesirable environmental impacts associated with mineral processing, has investigated a soda-smelting technique for processing ilmenite into pig iron and a titanium slag that is suitable for a feed to a sulfate-process titania pigment plant. By this procedure, the generation of ferrous sulfate waste and its associated disposal problem is obviated. Molten titania slag was quenched, water leached, and filtered to yield a sodium titanate intermediate product containing about 70 wt-pct Ti02, 1 wt-pct Fe, and 20 wt-pct Na20. This intermediate product, high-soda titanate (HST), was mixed with H2S04, calcined, quenched, and water leached to produce a low-soda titanate (LST) product that contained only 2 wt-pct Na20. Both the HST and LST were evaluated as feed materials for preparing titania by the sulfate process. About 95 pct of the Ti02 was extracted from HST and LST by digestion in concentrated or 50-wt-pct-H2S204 solutions. About 95 pct of the solubilized Ti02 was subsequently recovered from the titanyl sulfate solutions by hydrolysis. Barren solutions from hydrolysis, containing about 26-wt-pct H2S04, were upgraded by vacuum-thermal evaporation or electrodialysis. The regenerated acid solutions were used to digest additional HST and LST.

Jan 1, 1979

By J. B. Stephenson

The Bureau of Mines, under an interagency agreement with the Department of Energy (DOE), investigated the feasibility of hardfacing the critical surfaces of valves and similar devices by chemical vapor deposition. The purpose of this research was to increase the wear resistance of these components for use in the abrasive and erosive environment of coal gasification units. Tungsten and molybdenum coatings were produced on nickel-plated carbon steels and stain-less steels by hydrogen reduction of the metal hexafluoride at 325° to 600° C. Titanium nitride coatings were produced on low-carbon steels by the reaction of titanium tetrachloride, hydrogen, and nitrogen at 1,000° C. Titanium carbonitride coatings were produced on low-carbon steels by the reaction of nitrogen, hydrogen, and methane at 900° C. Tungsten, molybdenum and titanium nitride coatings were formed on 6-, 10-, and l2-inch (0.15-, 0.25-, and 0.30-meter) ball valve seats for evaluation in the low-Btu coal gasification pilot plant at the Morgantown Energy Research Center, Morgantown, W. Va.

Jan 1, 1979

Toward the goal of maximizing minerals and metals recovery from domestic resources, the Bureau of Mines, U.S. Department of the Interior, has conducted in situ corrosion studies at the Salton Sea Known Geothermal Resources Area (KGRA) in the Imperial Valley, Calif., to evaluate and characterize materials of construction for geothermal resources recovery plants. General-, pitting, and crevice-corrosion characteristics of 13 commercially available alloys were investigated for periods of 15 and 30 days in seven process environments expected to be found in typical geothermal resources plants. Stainless steel alloy 29.4, Inconel 625, and the Hastelloys G, S, and C-276 were the most resistant to general corrosion, did not pit, and exhibited little susceptibility to crevice corrosion. Stainless steel alloys 430, E-Brite 26-1, and 6X had low general corrosion rates, but pitted and were susceptible to crevice corrosion. Stainless steel alloy 316 L had a low corrosion rate, but corroded intergranularly, pitted, and was susceptible to crevice corrosion and to stress-corrosion cracking. Titanium-1.5 nickel and TiCode-12 had low corrosion rates, did not pit, and were not susceptible to crevice corrosion. Carbon and 4130 steels had high corrosion rates, pitted, and had high susceptibilities to crevice corrosion. The major scale-forming mineral on the corrosion samples in most of the process environments studied was galena mixed with lesser amounts of other minerals.

Jan 1, 1979

By Max L. Glenn

As part of its goal to minimize requirements for mineral commodities through conservation and substitution, the Bureau of Mines conducted research to develop molybdenum as a potential substitute for superalloys containing the strategic and critical materials, nickel, chromium, and cobalt. Since molybdenum requires protection from oxidation at high temperatures, several complex oxides of the spinel and perovskite structure were investigated to determine which possessed the greatest potential for use as oxidation-barrier coatings. Two spinels (MgCr204 and MgA1204) and five perovskites (BaHfO3, YCrO3, NdCrO3, BaZrO3, and LaCrO3) were selected for testing. Various high-temperature prop¬erties that are important for oxidation-resistant coatings were examined, including diffusion rates of oxygen and molybdenum, recession (vaporization) rates, hardness, erosion resistance, sinterability, reactivity with molybdenum, and ease of application. From the evaluation of high-temperature properties, two spinels (MgCr204 and MgA1204) stand above the other oxides as possible coatings for molybdenum. However, laboratory coatings of MgCr204 at 1,360° C (2,480° F) are equivalent or inferior to currently available MoSi2 coatings; laboratory coatings of MgA1204 may be comparable under limited conditions to currently available MoSi2 coatings at the same temperature.

Jan 1, 1979

By T. H. Jeffers

To help maintain an adequate supply of minerals to meet national, economic, and strategic needs, the Bureau of Mines investigated the feasibility of extracting copper from coarse native copper ore with ammoniacal ammonium carbonate solution by a simulated in situ leaching procedure. A 5.9-metric-ton (6.5-ton) sample of minus 30.5-centimeter (12-inch) conglomerate-type ore analyzing 1.96 percent copper was leached in a column for 556 days with a solu-tion that contained, in grams per liter, 2.2 NBs and 1.9 CO[3=]. The copper extraction was 71.4 percent, and reagent consumptions were, in kilograms per metric ton of ore, 1.1 NBs and 0.85 CO[3=] (in pounds per ton of ore, 2.2 NH3 and 1.7 CO[3=]). The pregnant leach solutions contained about 1.4 grams per liter copper, which was readily extracted from these low-tenor liquors with a 1:19 mixture of an organic extractant and kerosine. Copper was stripped from the loaded organic with depleted electrolyte containing 150 grams per liter H2S04, and the copper was recovered by electrowinning with antimonial lead anodes. Conditions also were established for minimal lead transfer to the cathode copper.

Jan 1, 1979

By L. E. Schultze

As part of the Bureau of Mines research program on recovering alumina from domestic resources, methods for extracting iron from aluminum sulfate solutions (obtained by leaching kaolinitic clay with dilute sulfuric ,acid) were investigated. In countercurrent extraction experiments at a l-gal/hr flow rate of aluminum sulfate leach liquor, the iron concentration 'was decreased from 1.4 g/l to 0.01 g/l after four stages of using a primary amine extractant. The iron-loaded amine solution was regenerated in five stages using 3[N] sulfuric acid or in four stages using 6[N] sulfuric acid. The aluminum sulfate solution obtained was suitable for the preparation of alumina meeting cell-grade standards of less than 0.01 pct iron.

Jan 1, 1979

By A. T. Iannacchione, D. G. Puglio

The Bureau of Mines established geologic factors affecting the mining of the Lower Kittanning coalbed to aid in coalbed minability studies and examined the occurrence of "wants" (places where coal is missing) and types of unstable roof rock strata. Trends established from mapping, including prediction of areas of high methane emissions, were extrapolated to unmined areas. "Wants" in the coalbed are of two types: Erosional and depositional. Erosional features occur where north-south-trending sand-filled channels cut into the coalbed. Variations in depositional environments have caused the coalbed to "split" into several thinner units. Slickensides, commonly indicative of unstable roof, are adjacent to and on the underside of sandstone channels; they were caused by differential compaction and by soft sediment sliding along the contact between the sandstone and adjacent shale. The frequency of unstable roof also increases where the interval between the Middle and Lower Kittanning coalbed is less than 30 feet. The zones of weakness at the contacts above and below the Middle Kittanning coalbed are the controlling factors for unstable roof in these strata. Methane emissions from the coalbed are controlled primarily by depth, fracture permeability, and rank of coal. Local geologic factors are coalbed thickness, associated rock strata, structure, and proximity to outcrop.

Jan 1, 1979

By A. T. Iannacchione

The Bureau of Mines established geologic factors affecting the mining of the Lower Kittanning coalbed to aid in coalbed minability studies and examined the occurrence of "wants" (places where coal is missing) and types of unstable roof rock strata. Trends established from mapping, including prediction of areas of high methane emissions, were extrapolated to unmined areas. 'Wants' in the coalbed are of two types: Erosional and depositional. Erosional features occur where north-south-trending sand-filled channels cut into the coalbed. Variations in depositional environments have caused the coalbed to "split" into several thinner units. Slickensides, commonly indicative of unstable roof, are adjacent to and on the underside of sandstone channels; they were caused by differential compaction and by soft sediment sliding along the contact between the sandstone and adjacent shale. The frequency of unstable roof also increases where the interval between the Middle and Lower Kittanning coalbed is less than 30 feet. The zones of weakness at the contacts above and below the Middle Kittanning coalbed are the controlling factors for unstable roof in these strata. Methane emissions from the coalbed are controlled primarily by depth, fracture permeability, and rank of coal. Local geologic factors are coalbed thickness, associated rock strata, structure, and proximity to outcrop.

Jan 1, 1979

By Robert F. Chaiken

The Bureau of Mines is using model ducts lined with coal to study the nature of coal mine fires, their rate of propagation, their influence on ventilation airflows, and their response to sealing and other fire suppression measures. For scale-modeling purposes these studies are being carried out in various size ducts; eventually they will include a full-size mine entry in the Bruceton multiple-entry Experimental Mine. To date, work has been carried out in an insulated 9.l-m-long duct with a 5-cm thickness of coal leaving a 23-by 23-cm square opening for air ventilation. Fire propagation processes in this duct were mainly transient in nature owing to the relatively small length-to-diameter ratio. This report describes the experimental equipment employed and the results obtained to date.

Jan 1, 1979

By B. J. Scheiner

As part of the goal to maximize minerals and metals recovery from primary domestic resources, design factors associated with minimizing current leakage in bipolar cell configurations were studied by the Bureau of Mines as a means of improving the efficiency of bipolar e1ectrooxidation cells. Initial studies that were conducted in a small bipolar cell operating at 140 to 145 volts and 15.4 amp indicated how design factors could be employed to minimize cur-rent leakage around adjacent electrodes during cell operation. Based on these results, a 40-electrode, 108-kva prototype of an industrial-sized cell was constructed and tested for extracting metal values from offgrade molybdenite concentrates. The feasibility of recovering molybdenum and rhenium from the oxidized pulp also was determined. Feed to the process sequence consisted of flotation concentrates containing 16 to 35 pet Mo as molybdenite and 6 to 15 pct Cu. E1ectrooxidation in the prototype cell resulted in 84 to 97 pct Mo and Re extraction with a corresponding energy consumption of 9 to 13 kwhr/1b Mo extracted.

Jan 1, 1979