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By H. R. Babitzke, H. Kato, R. E. Siemens, G. Asai

The purpose of this investigation was to develop a wide variety of columbium and tantalum alloys and to determine their suitability for use at elevated temperatures . Sixty - nine columbium and tantalum alloys were investigated . For this study , columbium was alloyed with two or more of the following : nium, tungsten , vanadium , titanium, and zirconium . Tantalum was alloyed with vanadium or hafnium, or hafnium and carbon . The fabricability was determined by an arbitrary procedure . Hardness measurements , elevated - temperature tensile properties , and oxidation- resistance studies were made . Of the alloys studied , Cb - 15 Hf - 5W, Cb - 15Hf - 5W- 10Ti , Cb - 15Hf - 10W- 10Ti , Cb - 10V - 5W, Ta - 30V , and Ta - 20 to 33Hf exhibited excellent high - temperature properties . These alloys were not only easy to fabricate , but they also had good oxidation resistance and excellent high- temperature strength .

Jan 1, 1964

By Thomas C. Miller, Rudolph Sporcic

A relatively simple and inexpensive encapsulated hydraulic device has been developed by the Bureau of Mines to facilitate study of coal bumps , and to measure pressure changes in a coalbed as it is subjected to roof loading during mining . Construction of the device and application techniques are described . Preliminary feasibility tests in the laboratory and field indicate that the device responds satisfactorily to pressure changes in coal created by roof loading .

Jan 1, 1964

By George H. Holmes

Beryllium deposits in the northern Virgin Mountains , Clark County , Nev . , and Mohave County , Ariz . , about 70 miles northeast of Las Vegas , were investigated by the Bureau of Mines . The investigation indicated a widespread occurrence of beryllium- bearing pegmatites within an extensive belt of mica - schist . Several deposits with significant beryllium mineral concentrations were encountered . Only a few of the samples analyzed contained more than 1 percent beryllium oxide ( BeO ) ; in many of the samples , no beryllium was reported . The average tenor of samples from the more important occurrences was 0.25 percent BeO . Chrysoberyl is the predominant beryllium mineral in the pegmatite sills ; beryl predominates in the more massive bodies . Minute quantities of cesium and lithium minerals also occur , but no columbium , tantalum , or other rare minerals were found . Ore dressing tests on a composite sample containing 0.28 percent BeO which was representative of the pegmatite sills , indicated an 85 percent recovery of the chrysoberyl ( 70 percent recovery of total BeO ) by gravity concentration in a concentrate containing 17.6 percent BeO .

Jan 1, 1964

By John K. Alley, Robert C. Johnson

The primary objective of the research was to grow aluminum borate whiskers or fibers and to determine their properties . Molten salt bath and vapor deposition methods were used for synthesis . Whiskers exceeding 25 mm in length were grown . The best results were obtained by vapor deposition and most of the data presented were determined on whiskers produced by this method of synthesis . Three different aluminum borate compositions ( 4.8A1203 B₂03 , 3.8A1203 B203 , and 2.5A120, B203 ) were identified by X- ray and chemical analyses . The aluminum borates 4.8A1203 B20, X- ray diffraction pattern was indexed . Optical data were obtained on the three aluminum borates . In addition the following whisker properties and growth factors were determined : ideal atmospheric dewpoint for vapor deposition method , near 65 ° F ; temperature range of whisker formation , 1,000 ° to 1,400 ° C for the molten bath method of synthesis , > 1,000 ° to < 1,400 ° C for the vapor deposition method ; whisker growth rates by the vapor deposition method , maximum 12 mm per hour ; raw material vaporization , 50 to 60 percent of the fluoride lost in 1 hour ; tensile strength , maximum obtained 174,162 psi ; melting points , ranged from 1,675 ° to 1,795 ° C.

Jan 1, 1965

By Van E. Shaw, D. J. Bauer

Conversion of euxenite concentrate to sulfates with sulfuric acid and solvent extraction of the yttrium- rare - earth mixture with EHPA were studied to determine extraction and separation characteristics . Digestion with 3.5 pounds of 96 percent sulfuric acid per pound of concentrate at 336 ° C for 4 hours resulted in an easily handled product with a yield in excess of 98 per- A thorium- free product was obtained by calcining the sulfated material for 3.5 hours at 650 ° C prior to leaching with water . Di ( 2 - ethylhexyl ) phosphoric acid solvent is an effective extractant with preference for cerium ( IV ) and heavy - group rare - earth elements including yttrium . Separation of complex rare - earth mixtures into light- and heavy - group fractions is feasible , and these fractions can be further processed to isolate ytterbium , neodymium , and dysprosium by changing processing conditions to obtain separation factors greater than two between these and adjacent elements .

Jan 1, 1965

By S. J. Gasior

A method for destroying the caking properties of bituminous coal was developed by the Bureau of Mines. Coal is treated in a fixed bed by heating through its plastic range under controlled temperatures in mildly oxidative atmospheres composed of inert gas and/or steam containing about 1 volume-percent oxygen. High-volatile A (hvab) and high-volatile B (hvbb) and low-volatile bituminous (lvb) coals in the size range 1/8 to 1-1/2 inches were successfully treated at 0 (atmospheric pressure) to 300 psig in static beds 6 to 18 inches deep. Conditions of treatment depended on the coal and ranged from 80 to 200 minutes at 350° to 510° C. Char produced in this manner from hvab coal was gasified with steam at 800° C and 100 psig in a fixed bed in one series of tests and in other tests was exposed to hydrogen in a dilute co current free-falling-bed system at 750° C and 3,000 psig without agglomerating.

Jan 1, 1965

By Manuel Gomez

The heat contents of thermally dried lignite, subbituminous B coal, and their corresponding low-temperature chars were determined at various temperatures below the highest temperature to which these materials had been exposed before testing. Similar studies were made on high-temperature char and coke, spent shale, and ash prepared from both coal and spent shale. Heat content of the carbonaceous materials tested correlated well with temperature. Heat con-tent results for spent shale compared well with the published results. Statistical analysis of experimental data together with published information showed moisture, volatile matter, carbon content, and temperature to be the principal variables influencing the specific heat of coal. The specific heat of devolatilized carbonaceous substances, char and coke, approached that of graphite as the carbonization temperature was increased. The elemental specific heats of coal constituents, estimated from the ultimate analysis and the specific heat of coal, compared favorably with published elemental specific heats.

Jan 1, 1965

By C. C. Popoff

This report reviews the phosphate deposits, mines, and industry, and prospects in 10 districts covering most of the Montana phosphate field. These districts are discussed individually, and an evaluation of the resources and potential of each is presented. Phosphate rock produced from underground mines in the Garrison district is shipped to Canada for processing to fertilizers, utilized locally for production of animal feed supplement, and pulverized and sold for direct application to the soil. Production from the Melrose district is shipped to Silver Bow and processed to elemental phosphorus. The Maxville-Philipsburg district is destined to become a major producer with the development of the Douglas Creek mine and beneficiation plant by Montana Phosphate Products Co. Montana ranks fourth after Florida, Tennessee, and Idaho in total annual production in the United States. Production him increased from about 60,000 long tons of acid-grade phosphate rock in 1940 to more than 660,000 tons of acid-, beneficiation-, and furnace-grade ore in 1961. Montana has the second largest potential resources in the Western field; in the area south of Butte there are approximately 1.2 billion tons of phosphate rock (+18 to +31 pct P2O5) available above and within 100 feet below entry level; and in the northern part of the field there are about 67.6 million tons available above entry level. In contrast to Idaho, most of the phosphate deposits in Montana are best suited to underground mining.

Jan 1, 1965

By Jr. Oitto

A polyester-type resin and deformed-steel reinforcing bars (rebars) were used in to strengthen and to stabilize bolted, fractured wall rock along pas 1:&apos;y. in a western gold mine. Reinforcing bars were placed in boreholes drilled into fractured rock and then were surrounded by resin pumped under pressure into the holes and intersecting fractures until the wall rock was thoroughly impregnated. Pumping and injection equipment and infusion procedures are described. Visual examinations for movement in bonded and adjacent unbonded rock were made for 3 years. Fractured walls containing resin-rebar installations were strengthened. The results suggest that resin-rebar support can be used advantageously and economically in repairing fractured or broken rock when compared with rock bolting or timbering.

Jan 1, 1965

By Jr. Norman

Thermoelectric properties of depleted uranium selenides and tellurides were investigated from room temperature to 700 C. Several depleted uranium monoselenides and monotellurides were doped with selected cationic and anionic materials to determine the effect of impurity additions on the thermoelectric properties. The undoped uranium selenides and tellurides were semimetallic conductors exhibiting low Seebeck coefficients and electrical resistivities. Partial or complete degeneracy was in evidence, indicating a charge carrier energy distribution similar to that in a metal. Doping increased the Seebeck coefficients of the uranium monoselenides and monotellurides; however, the corresponding change in the power factor in the figure of merit was small because of the increase in electrical resistivity.

Jan 1, 1965

By Foster Fraas

The Bureau of Mines investigated a method for calculating values of adsorption energy; the goal was to devise an equation consistent with experimental data accumulated in the investigation of adsorption as related to ore separation processes. Numerical identification of the constants of a previously formulated equation provided an equation by which values of adsorption energy could be calculated. Values thus calculated checked with those obtained by calorimetric measurement.

Jan 1, 1965

By R. R. Nothdurft

The internal friction of eight single crystals of magnesium with orienta-tion ranging from 10° to 84° was measured at 33.5 kc and 272° C, and the results were interpreted in terms of the pinned-dislocation model proposed by Granato and Lucke. Results show that the strain-amplitude-dependent decrement varies with orientation in a manner predictable by the G-L model. Different values of strain-amplitude-independent decrement were observed at different orientation angles, but correlation with the theory was not conclusive. Problems and steps for further study are discussed.

Jan 1, 1965

By K. C. Dean

This report is the first of a series concerned with processes for producing magnesium. These reports will evaluate metallothermic, carbothermic , and electrolytic production methods, and will furnish a cost basis for comparing the processes. Areas deemed most promising for future research will be delineated for each procedure. This report presents briefly the history of the metallothermic process, and describes the operations of the Defense Plant Corp. (DPC) plants that employed the process. A hypothetical plant designed to produce 12,000 tons of magnesium per year, using ferrosilicon as a reductant, is described, and raw materials, energy, and major equipment requirements are estimated. Several process modifications are suggested for future research.

Jan 1, 1965

By Albert W. Deurbrouck

This report describes the preparation characteristics of 23 coal samples collected from nine of the more significant coalbeds of Fayette County, W. Va. In 1963 almost 5.4 million tons of medium to high volatile B coals of excellent quality for metallurgical and steam markets were produced in Fayette County. Of the 23 coal samples collected 11 would require some upgrading to pro-vide metallurgical quality products, 11 were acceptable as received, and 1 was a noncaking coal. Cleaning these coals to metallurgical standards would require only the removal of the sink 1.58 specific gravity material which would be quite easy as very little near-separating-gravity material was present at this gravity.

Jan 1, 1965

By Robert C. Johnson

Single crystal whiskers of ZrO2 and TiO2 were grown by solution and crystallization of these oxides in molten baths. Mixtures of Na2B407 and LiC1 were the most suitable growth media for zirconia. Sodium borate alone and Na2CO3 plus SiO2 were best suited for titania. The solubilities of zirconia and titania in molten sodium borate were determined, Whether zirconia whiskers were dendritic or nondendritic depended on the temperature used. The best single crystal whiskers were grown below 1,100° C. Titania whiskers always grew as single crystals. The tensile strengths of zirconia and titania whiskers were about 15,000 psi and 50,000 psi, respectively. Modulus of rupture was about 49,000 psi for zirconia whiskers and 75,000 psi for titania whiskers. Chemical analyses showed the zirconia and titania whiskers to be pure. The zirconia and titania whiskers were shown by X-ray analysis to be, respectively, baddeleyite and rutile.

Jan 1, 1965

By James S. Browning

The Bureau of Mines conducted laboratory batch and pilot plant flotation tests to determine the technical feasibility of recovering commercial-grade mica from a California micaceous schist. Best results in the laboratory batch tests were obtained using sodium carbonate and sodium silicate for pH control and quartz depression, and a combination of fatty acid and cationic reagents as the mica collector. In continuous pilot plant flotation tests, an alkaline fatty acid-cationic method recovered about 70 percent of the mica in a concentrate analyzing 95.6 percent mica.

Jan 1, 1965

By J. L. Eakin

A method was developed by the Bureau of Mines in the laboratory and in the field to relieve capillary waterblocks in gas wells. Impaired gas permeability was improved by this inexpensive chemical treatment which lowers the surface tension of the water held in the capillaries of the formation. Effectiveness of the alcohol-surfactant treatment was tested with a variety of chemicals and with sandstone cores cut from rocks having relatively low permeability. Field tests on 20 gas-producing and storage wells demonstrated the effectiveness and limitations of the method. The productive capacity of some wells was doubled by the treatment. The final test was evaluated by the neutron logging technique for measuring changes in apparent liquid saturation. Maximum apparent liquid saturation was reduced by 52 percent; gas production rate increased from 2.3 to 3.5 MMcfd (million cubic feet per day).

Jan 1, 1965

By J. G. Donaldson

Cobalt-tungsten binary deposits were formed in laboratory experiments by hydrogen reduction of the anhydrous mixed vapors of cobaltous chloride and tungsten hexachloride. The materials were sublimed in seperately heated zones of reaction tube and were transported in a stream of purified helium into the deposition section of the tube where the chloride gases were reduced to metal by a countercurrent flow of hydrogen. Heattreating of the near stoichiometric binary metallic deposits converted nearly all to the intermetallic compound Co3W, however, small quantities of both cobalt and tungsten remained. Mechanical tests showed that the tensile strength of heat-treated 75 percent cobalt-25 percent tungsten deposits was twice as high as that of similarly treated deposits of cobalt.

Jan 1, 1965

By W. L. Acherman

Molybdenum, tungsten, and vanadium were found by the Bureau of Mines to possess generally superior chemical and galvanic corrosion properties in many aqueous corrosive media at temperatures up to the boiling point. The corrosion resistance of vanadium in certain solutions was further improved by alloying it with such metals as columbium, tantalum, and titanium. was susceptible to a type of crevice corrosion in mercuric chloride solutions, but no other instances of crevice corrosion were encountered. With few exceptions, molybdenum, tungsten, and vanadium were not adversely affected when coupled with dissimilar metals in galvanic corrosion experiments; in some cases one or both members of a couple were protected by contact. When exposed to aqueous ammonia spray at 60° C, all three metals were attacked, but they were moderately resistant in spray environments of substitute ocean water and ammonium dihydrogen phosphate.

Jan 1, 1966

By Louis A. Panek

Determining the change of stress in rock based on measurements of the deformation of a drill hole is a procedure that is increasing in popularity. A closely related procedure involves the applicat10n of this principle to determine the existing stresses in a rock medium, by cutting free (core drilling) an annulus containing the drill hole. In this Bureau of Mines report, expressions are derived from which one can calculate the stress ellipsoid--the three-dimensional change of stress, or the existing three-dimensional stress field, as the case may be. Study of these equations shows that the stress components in three dimensions can be determined by measurements in only two drill holes, and yields general principles that are useful in planning an efficient program of drilling and measurement. Procedures are given for calculating the least squares estimates of the stress components and their standard errors, and for evaluating or comparing calculated values by means of standard statistical inferences.

Jan 1, 1966