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By H. R. Shell, Robert C. Johnson, Wilbur H. Warwick

Alpha silicon nitride fibers , Si3N4 , were successfully grown in graphite crucibles by a new method utilizing silicates and silicon ( S in equations below) as sources of silicon and using carbon , aluminum , and silicon as reducing agents (R in equations below ) . The basic reaction mechanism is believed to be generally as follows : 1,300 - 1,500 ° C S + R + N₂ SiO + RO + N₂ › 3Si0 + R + 2N₂ _1,300 - 1,500° C 3RO + Si¸N • ( 1 ) ( 2 ) A build - up of coatings on the solid raw- material particles hindered the evolution of silicon or silicon monoxide vapor and thereby slowed down further formation of silicon nitride fibers . Free oxygen in the crucible caused the formation of amorphous silicon dioxide ( SiO2 ) fibers . This problem was solved by passing , entering , and exiting gases through layers of lump graphite inside the reaction vessel . The silicon nitride fibers grew best around 1,400 ° C. Nitrogen flow rates from 4 to 6 liters per minute were adequate . The fiber widths were generally only a few microns whereas their lengths sometimes reached one - quarter inch or more . Chemical and X- ray analyses indicated that bulk fiber samples were usually 80 to 90 percent Si3N4 . The fibers had good oxidation resistance to about 1,260 ° C. Thermal shock resistance was excellent . Electrical resistance was determined .

Jan 1, 1964

By H. D. Hess, C. P. Mabie

This report describes in detail the results of petrographic research conducted on 21 phosphate ores representing important deposits in southwestern Montana , southeastern Idaho , and northeastern Utah . The ores are described and categorized by mineralogical and chemical composition , thermal behavior of organic carbon , and textural constitution . Descriptive and genetic classification schemes applicable to western phosphate ores are discussed ; results from related studies made of the collophane mineralogy are also presented . The latter studies were centered on determining unit - cell dimensions and CO₂ , P2O5 , and fluorine content of collophane concentrates of 11 high - grade phosphate- rock hand specimens selected solely for this purpose . On the basis of this investigation , operational methods have been developed for quantitatively describing textural and compositional features that are likely to be significant in determining the response of phosphate ores to conventional beneficiation treatments ; systems for classifying the ores in relation to these features have been proposed . Studies to date point out distinct textural and compositional variations in the western phosphates and illustrate their importance in determining optimum beneficiation procedure .

Jan 1, 1964

By M. E. Kundick, W. E. Dieter, L. Cohen

The major details of design and maintenance of a seamless stainless steel fume hood system , developed by the Bureau of Mines , are described and illustrated . Operating and housekeeping routines are outlined .

Jan 1, 1964

By William R. Wayment, David E. Nicholson

The Bureau of Mines studied some physical properties of hydraulic backfills and their paramount characteristics , and made preliminary attempts to compact this type of material . The in- place density of hydraulic backfills affects the properties of strength , consolidation , and water percolation . Dense fills give better support than loose fills . In - place density properties themselves are affected by grain size , grain size distribution , and the particular conditions of sedimentation in a stope ( the amount of work the slurry water does to compact the material ) . Field sampling of in - place densities of fills presently used in four different mines and laboratory and underground compaction tests using a standard concrete vibrator show that the initial in - place density of the cohesionless fill material tested can be significantly increased by vibratory compaction .

Jan 1, 1964

By Henry M. Harris, Hal J. Kelly

Electrical dewatering tests are described in which the laboratory cells were designed for continuous operation using an endless metal belt as the anode . The test slurries were dilute , containing from 2.5 to 14.4 percent solids (specific gravity of 1.02 to 1.10 ) that were all minus 8 microns in size . Recovery of the solids of low water content was the practical objective of the investigation . Process variables evaluated and reported are : The effect of feed rate , amount of electrolyte , samples from different sources , and the use of two cells in series . These variables are evaluated on the basis of yield of clay per kilowatt - hour , recovery , and the amount of solids in the deposited clay . Recovery , yield , and solid content of the belt anode product are interdependent , and changes that will improve one of these characteristics often are accomplished at the expense of the others . Tests in which recoveries range from 50 to 60 percent usually result in yields of 8 to 9 kilograms (kg ) of dry clay per kilowatt- hour (kwhr ) . Under these conditions , the solid content of the deposited clay approximates 50 percent . One test sample , composed of kaolinite , showed very high yield , 13 to 16 kg per kwhr ; high recovery , 53 to 58 percent ; and 52 to 54 percent solids in the cake .

Jan 1, 1964

By Richard F. Hewlett

This Bureau of Mines report presents the computer programing methods and mathematics required to generate either random numbers or normal random numbers to be used for the construction of statistical probability models for simulating mineral deposits by Monte Carlo techniques . Theoretical frequency functions are evaluated as an illustration of simulation applications . Numerical and analytical methods of simulating and dissecting some complex frequency distributions are described .

Jan 1, 1964

By Charles H. Atkinson, Robert T. Johansen

Tremendous volumes of petroleum ( crude oil and natural gas ) at present cannot be recovered economically . The feasibility of using nuclear explosions for production stimulation therefore has been investigated . Data from underground nuclear tests conducted by the Atomic Energy Commission were reviewed , and the physical effects were evaluated for stimulating petroleum production . Calculations of the effect on ultimate recovery of increasing reservoir temperature with nuclear explosives showed disappointingly small increases . Production increases caused by fracturing of massive low- permeability reservoirs appear technically and economically promising . Petroleum reservoirs that might be converted from submarginal to commercial production are being located and evaluated as to potential reserves and as a location for a field test .

Jan 1, 1964

By L. H. Adami, E. G. King

The heats of formation of four sulfides --MnS ( alabandite ) , FeS ( hexagonal pyrrhotite ) , ZnS ( wurtzite ) , and CdS ( greenockite ) -- were determined by hydrochloric acid solution calorimetry . The heats of formation from the metals and rhombic sulfur at 298.15 ° K are , respectively , -51.01 ± 0.19 , -23.81 ± 0.24 , -45.86 ± 0.20 , and -35.70 ± 0.30 kcal /mole . The corresponding free energies of formation were calculated from the heats of formation and the pertinent entropy values .

Jan 1, 1964

By R. L. Crosby, L. W. Higley

Magnesium- rich magnesium- aluminum- zirconium alloys in the cast and in the extruded and heat- treated condition were studied to identify the phases present and to determine phase distribution . In cast alloys , two intermetallic compounds were identified : ZrAla by X- ray diffraction ; and Mg₁ Al₁₂ by microscopical observation . Based on microscopical comparisons between the known phases in the cast structures and the phases in the structures of extruded and heat - treated rods , ZrAl₂ and Mg1 , Al12 were identified in the structure of the latter . The presence of these intermetallic compounds in rod specimens could not be confirmed by X- ray diffraction . ZrAl₂ was observed in the structure of extruded and heat - treated rod specimens containing as little as 0.01 weight - percent zirconium . The presence of aluminum restricts the solubility of zirconium in magnesium because of the strong tendency to form ZrAla . This intermetallic compound segregated in clusters of small particles in the matrix of cast alloys , and only slight improvement in distribution was noted when the alloying techniques were varied .

Jan 1, 1964

By Richard F. Hewlett

Numerous populations of assays have been simulated for a range of assay values representative of low-grade mineral deposits to facilitate the study of problems encountered in evaluating these deposits. Analysis of these simulated populations of assays (obtained by using statistical probability models for the simulation) makes possible the quantification of the effects of (1) various composite assay intervals, (2) ore reserve computational methods, (3) uneven assay intervals, and (4) various cutoff grades on both the precision and the accuracy of the estimated average grade and tonnage of ore.

Jan 1, 1964

By F. R. Cattoir, R. E. Cumings

Columbium metal was electrorefined in a fused - salt electrolyte . Excellent results were obtained in lowering the impurity content in a 94 - percent columbium anode feed material to produce a 99.8- percent - pure metal . The reductions of the major impurities follow : Oxygen from 19,800 to 500 ppm , carbon from 9,700 to 25 ppm , iron from 9,200 to 630 ppm , nitrogen from 2,100 to 90 ppm , and silicon from 750 ppm to not detected . Columbium with a purity of 99.9 percent was produced from 99.5- and 99.8 - percent grades of columbium. The investigation was devoted to the evaluation of a fused - fluoride - salt electrolyte ( KF - NaF- K₂ CbF, ) for electrorefining columbium. The effects of the columbium concentration and the voltage upon the product's purity were investigated . The effect on the cathode current efficiency of ampere - hours of deposition and the formation of a dual valence state of the columbium was also investigated .

Jan 1, 1964

By R. A. Beall, S. L. Ausmus

The development of a completely water - free expendable graphite mold material , useful for reactive metal castings , has been detailed . Mixing and curing variables have been evaluated both by physical testing of the material itself and by castings of titanium , zirconium , and hafnium . The blend of powdered graphite , cornstarch , dextrin , cereal binder , linseed oil , and Carbowax -4000 is a successful mix when mulled in a carbon dioxide atmosphere , and properly cured and fired . The primary advantage of this material is its adaptability to standard foundry techniques ; i . e . , core blowing and hand ramming . Temperatures in the curing and firing cycles do not exceed 960 ° C , and no vacuum firing is required .

Jan 1, 1964

By D. Bienstock, J. H. Field, M. J. Lempel

A computer program is presented to perform the detailed and numerous calculations required for determining the interface temperatures and steady - state heat flow through a furnace wall composed of several refractories in layers . A method is developed that will allow the designer to determine the various thicknesses for each refractory layer to minimize either the total wall thickness or the cost of the wall per unit of area . A sample problem is presented and analyzed to illustrate the techniques involved .

Jan 1, 1964

By Richard F. Hewlett

An attempt has been made to fit assay data from an underground copper deposit to a three-dimensional polynomial surface as a means of expressing assay points in terms of their mine coordinates by a mathematical equation. The resulting equation was evaluated to predict the grade trend of the deposit. Although the fit obtained by this initial experiment is not considered accurate enough to provide good predictions about the deposit, the methodology is presented in this preliminary report to show the potential usefulness of the technique in mineral deposit evaluation. The technique also should be useful in determining the grade of blocks of ore for production scheduling and blending problems in open pit operations. Further experimentation is needed to increase the reliability of the computer program, to increase the precision of the method, and to make the solution more flexible for use on other mineral deposits.

Jan 1, 1964

By P. L. Woolf, N. Bernstein, M. M. Fine

Continuous experimentation utilizing a 3- by 36 - foot rotary kiln was conducted to demonstrate the feasibility of simultaneous induration and reduction of magnetic taconite concentrate . Lignite , or lignite - anthracite mixtures , and green magnetite pellets (64.2 percent Fe , dry basis ) were heated in a rotary kiln to about 2,100 ° F. After separation from excess reductant , the product pellets were found to be highly reduced and acceptably hard . A total of 140 tons of prereduced pellets with an average Fe content of 79.0 percent was produced at Minneapolis and smelted in the Bureau's experimental blast furnace at Bruceton , Pa . Two additional supplies of prereduced pellets were obtained from The Steel Company of Canada , Ltd. , Hamilton , Ontario , which contained 83.8 and 91.3 percent Fe , respectively . Smelting of prereduced pellets was compared with that of unreduced pellets obtained from The Hilton Mines , Shawville , Quebec , and from the Erie Mining Co. , Hoyt Lakes , Minn . Blast furnace tests established that a substantial decrease in coke rates and higher production result from the use of prereduced pellets .

Jan 1, 1964

By Robert K. Koch, Henry E. Blake

Laboratory tests were made to determine if aluminum fluoride of commercial grade could be synthesized by reacting alumina hydrate with dilute ( 25 to 75 grams per liter of fluorine ) aqueous fluoride solutions . • Products containing up to 90 percent aluminum fluoride ( A1F ) were synthesized by reaction of alumina trihydrate ( A120 3H2O) with either dilute hydrofluoric acid ( HF ) or ammonium fluoride ( NHF) solutions , the ammonium fluoride solution resulting from ammonia ( NH ) desilication of a hydrofluoricfluosilicic acid ( HF - H₂ SiF ) solution . Fluorine recoveries of over 80 percent were obtained with either type of solution . The hydrated precipitates of AlF, and ( NH4 ) , A1F ( ammonium aluminum fluoride ) obtained by reacting hydrated alumina with these solutions were subsequently converted to anhydrous AlF, by controlled heating .

Jan 1, 1964

By Gus Pantages, Bernard D. Blaustein, Charles Zahn, Irving Wender

Oils from coal hydrogenation have been examined at the Bureau of Mines to learn whether any centers of the optical activity reported in coal would survive catalytic hydrogenation at 450-525 ° C and about 8,000 psig pressure , and , if so , to obtain information about the nature of the active products . Oils from carbonization tars also were examined . Optical activity was found in the majority of the distillate fractions of the hydrogenation oils and in almost all distillates from the carbonization tars . No activity was observed in the tar - acid and tar - base fractions examined . Methods for isolating optically active concentrates included distillation through a packed column , liquid chromatography on silica gel , and adduction with urea . For the materials so processed , the optical activity segregated mainly in the paraffin - naphthenic and the hydroaromatic fractions . Although the specific compounds responsible for the optical activity were not isolated , experimental and spectrometric findings indicate that alkylsubstituted cycloalkane , cycloalkene , and hydroaromatic structures are most likely responsible for the optical activity of the concentrates . The optically active centers probably derived mainly from the steroids and terpenes in the biological materials that participated in the formation of coal .

Jan 1, 1964

By R. D. Berkenkotter

This report describes a weighted method for evaluating the mean and variance of assay data from samples of different length . The method , which produces unbiased estimates from which valid confidence limits can be computed , is appropriate for bedded deposits of variable bed thickness and for vein deposits of variable vein width . Assay data from the bedded Florida phosphate deposit is used to illustrate the procedure .

Jan 1, 1964

By Louis A. Panek, John A. Stock

A flat slot is created in rock to cause stress relief effects in a pair of hydraulic borehole pressure cells (previously installed in drill holes above and below the slot ) , which act as sensing devices . This relief is annulled by repressuring the slot by means of a flat hydraulic cell . The slot pressure at annulment is taken to be the existing ground stress at right angles to the plane of the slot . A number of trial installations in the rib of a mine drift showed that for a valid determination of ground stress the sensing devices that respond to relief and repressuring must be within a specified zone close to the pressure transmitter ; otherwise the indicated ground stress may be excessive . By using an additional pair of borehole pressure cells , installed a few feet away , the existing rock stress can be redetermined at intervals , irrespective of a change of stress intensity subsequent to the initial installation . Based on these findings , equipment and procedures have been developed that make possible the installation and operation of a permanent rock stress monitoring station for observing mining - induced stress changes . The station consists of a 12 - in - wide hydraulic pressure cell cemented in a flat slot and four 2- by 8 - in flat hydraulic pressure cells in nearby drill holes . All drilling for the installation can be done with an air leg drill and conventional bits . Once the installation is completed , all required information is obtained by Bourdon pressure gage readings . The apparatus is simple , relatively inexpensive , and reliable under operating conditions in a wet mine . Unlike most methods of rock stress determination , this scheme permits periodic remeasurement of absolute rock pressure over several years , without additional drilling or instrumentation . Similar to other flat slot procedures , stress measurements are obtained without making auxiliary tests to determine elastic

Jan 1, 1964

By H. Kato, G. Asai, R. Blickensderfer, R. Siemens

Some relationships were established among crystallographic orientation , rollability , deformation texture , annealing behavior , slip planes , and ductile- brittle bend transition temperature of molybdenum single crystals . Six large molybdenum single crystals obtained from an ingot melted by electron beam were oriented by X - ray diffraction and rolled on crystallographic planes of low indices in a known direction . During room temperature rolling , cleavage occurred on 100 type planes . At 300 ° C the crystals were rolled to 95- percent reduction in thickness . The crystals ( 001 ) [ 110 ] and ( 011 ) [ 100 ] were most easily rolled . Pole figures were used to correlate the deformation textures of the rolled crystals with the initial crystallographic orientation . Several of the textures which developed could be explained as a rotation about a < 110 > axis of symmetry . The cube crystal ( 001 ) [ 100 ] retained much of its " cubic " orientation . The (001 ) [ 110 ] crystal developed the simplest texture , whereas the ( 211 ) [ 113 ] and ( 211 ) [ 120 ] crystals developed the most complex textures . The 1 - hour recrystallization temperature of the crystal ( 211 ) [ 113 ] was 700 ° C , which is about 300 ° C lower than that of commercial polycrystalline molybdenum . The poles of the slip planes ( as determined from gross slip lines at relatively low magnification ) tended to lie within 20 to 60 degrees of the pole of the rolling plane . The Knoop hardness was slightly dependent upon crystallographic orientation but more dependent upon rolling direction . The ductile- brittle bend transition temperature was dependent upon the rolling orientation and the dislocation density .

Jan 1, 1964