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By S. J. Rothman, L. T. Lloyd

S. J. Rothman and L. T. Lloyd (Argonne National Laboratory)— Hagel's paperz0 discusses the question of the mechanism for self-diffusion in bcc transition metals. Recent work21"23 has led us to agree with him in reabandoning the ring mechanism in favor of a defect mechanism, most likely vacancies. On the other hand, we think that Hagel's attempt to group together all self-diffusion in bcc transition metals is wrong. We prefer the scheme of Peart, Graham, and omlin," who separate them into two groups. One group contains the anomalously behaved metals P titanium,', y uranium, and perhaps zirconim.' The other group contains a iron," this alloy was held at 1800°C for 2 hr before quenching, its structure was all a. B. C. Giessen, I. Rump, and N. J. Grant (Authors' reply)—We very much appreciate the discussion by Deardorff and Kato regarding the a to /3 transformation temperature of hafnium. In the W-Hf program, as well as in a current study of the system Cr-Hf, standard precautions were exercised against contamination, including vacua of less than 10"5 mm Hg and a weight control check of all specimens to insure an impurity rise of less than 100 ppm. Following receipt of the above discussion, a revision was made in the annealing process. Arc-cast specimens were etched with a 10 pct HF-90 pct HNO solution until 1 mm of surface, including a possible oxide film, was removed. Annealing was done in a hafnium container which provided a long diffusion path for gaseous contaminants. Finally, the heat treating time was shortened. Structural changes were noted to occur quite slowly. A 99.5 at. pct Hf alloy showed 70 pct /3 after 30 min at 1700°C and was 100 pct /3 after 10 min at 1715°C. After 24 hr at 1740C, the alloy was found to be 10 pct/3. This change is due to contamination; it was estimated that it corresponds to an increase of 60°C in the transformation temperature over a 24 hr period. The corresponding change in 30 rnin would be slight. Using the same hafnium as in the above publication, and three new alloys at 98, 99, and 99.5 at. pct Hf, the transformation temperature was indicated to be 1715" 15°C. Since this hafnium contained 4.4 at. pct Zr, a correction of 40 5C, based on an assumed approximately linear transformation temperature curve, must be made for pure hafnium. This yields a value of 1755 20°C in good agreement with Deardorff and Kato's value. Because the slope of the boundary is small, this permits a good extrapolation, and we regard the W-Hf alloys as well suited to check the Hf transformation temperature. niobirn,'' and molybdenum,22 whose activation energies correlate with the melting temperature and whose Do values follow Zener's predictions.28 We have no quarrel with Hagel's placing chromium into the second group; we disagree with his interpreting our data to make uranium fit into that group. Hagel considers that the measurements of self-diffusion in uranium below about 950°C represent combined volume and grain boundary diffusion. This contention is based on the curvature of the penetration plot for our 891°C run,4 which also has a nearly straight line plot of log c vs x. Hagel has extrapolated these characteristics to our 803.5C run and fitted his Arrhenius plot for self-diffusion in y uranium to our four highest temperature points only. We think this is wrong for the following reasons.

Jan 1, 1963

By C. M. Mason

Bureau of Mines studies were made on the sensitivity of several ammonium nitrate-fuel oil (AN-FO) mixtures to bullet impact. The experimental work was done with one military rifle and two high-velocity sporting rifles with a variety of ammunition. For the three rifles used, the order of efficiency in initiating detonation in AN-FO mixtures was 220 Swift >300 Weatherby Magnum >30-&apos;06. The velocity of the bullet was found to be a decisive factor in the initiation. The sensitivity of various materials studied increased as follows: Clay-coated prills with 4 percent oil <fresh surfactant-coated prills with 4 or 6 percent oil <surfactant-coated prills with 4 or 6 percent oil and aged 270 days <crushed prills with 6 percent oil <very low-density, surfactant-coated prills (micronized), with 4 percent oil.

Jan 1, 1963

By John C. Sawyer

The mechanism of catastrophic oxidation of chromium and 446 stainless steel is examined. Data are presented to show that accelerated oxidation of these two materials, as caused by lead oxide, can occur in the absence of a liquid layer contrary to presently accepted theory. An alternate theory is proposed in which the rate of accelerated oxidation is a function of the rate at which lead oxide destroys the protective oxide formed on the base metal. An example of the application of the theory is given for the catastrophic oxidation of chromium in the presence of lead oxide. WHEN stainless iron-, nickel-, or cobalt-base alloys are heated in air to moderate temperatures in the presence of certain metallic oxides, oxidation will proceed at an accelerated rate. This phenomenon, often called "catastrophic oxidation", is most pronounced for the stainless steels. With these alloys the condition is so severe that large masses of oxide will form on the surface of the alloy in 1 hr or less at temperatures of 1200o to 1700oF. While a number of oxides are known to cause this effect, PbO, V2O5, and Moo3 are the most familiar, having been the subject of one or more investigations which have appeared in the literature.1-7 In presenting the results of these investigations, many of the authors have offered possible explanations to account for the more rapid rate of oxidation observed; however, the liquid layer theory as proposed by Rathenau and Meijering 2 has been the most commonly accepted mechanism. The liquid layer theory proposes that a low-melting oxide layer is formed on the surface of the alloy as the result of the interaction of the alloy oxide and the contaminating oxide. When the temperature of oxidation is above the melting point of the oxide on the surface, a liquid layer will form and oxidation will proceed at an accelerated rate. At temperatures below the melting point of the surface oxide, oxidation will proceed more slowly in the normal manner. It is argued that the rates of diffusion of oxygen and metal ions through the liquid layer are extremely rapid thereby accounting for the high rate of oxidation. Various experimental data have been presented to show that the temperature at which accelerated oxidation first becomes apparent coincides with the melting point of the eutectic oxide which would be present on the surface. Some exceptions have been observed, e.g., silver will oxidize in the presence of Moo3 at temperatures below the lowest melting eutectic; on the other hand, stainless steel will not be catastrophically oxidized at 1500oF in a molten bath of PbO and SiO2. In reviewing the various theories which have been used to explain catastrophic oxidation, Kubaschewski and Hopkins 8 favor the liquid layer theory, but note that, ".. .as experimental observations are not altogether in agreement with this theory (liquid layer theory), one should consider it a necessary but not a sufficient condition." In contemplating the liquid layer theory, it appears that sufficient evidence has not been presented to establish the theory beyond question. As a means of further clarification, a program of research was undertaken to determine in greater detail the mechanism of accelerated oxidation as caused by lead oxide. The first part of the program deals with a comparison of the oxidation of both AISI 446 stainless steel and chromium metal in the presence of lead oxide, vs the oxidation of these two materials in air alone. These comparisons are made at a number of different temperatures, most of which are below the melting point of the surface oxides. The second part of the program is concerned with a presentation of an alternate theory of accelerated oxidation exemplified by the system Cr-PbO-Air. PROCEDURE AND RESULTS Several experimental methods are commonly used to follow the progress of oxidation. One of these, the weight-gain method, was chosen for this work. This procedure requires that a specimen of the alloy be weighed, oxidized for a given period of time at an elevated temperature, and reweighed—the difference between the two weights being noted. The weight gain of the specimen represents the amount of oxygen acquired from the atmosphere to transform a portion of the specimen to oxide. In those cases where there is a tendency for the specimen or oxide to volatilize at the testing temperature, additional data must be collected so that a correction factor can be determined. This factor must be applied to the weight change in order to ascertain the actual amount of oxidation which has taken place. The specimens used for this work were 1 1/2 in.

Jan 1, 1963

By W. S. Owen, A. R. Rosenfield

The measured changes in the yield stress of a poly crystalline Ta-O alloy after strain aging at 100°C have been separated into two components; the change inflow stress and the change in dislocation locking parameter. These two components vary independently indicating that at least two separate recovery processes take place during strain-aging. Variations in the locking parameter can be accounted for by segregation of oxygen atoms to dislocations, but variations inflow stress cannot be explained by current theories. STRAIN-AGING in Fe-C and Fe-N alloys has been studied extensively.&apos; The kinetics of the removal of the interstitial solute from solution appear to agree with the predictions of the cottrell-bilby2 model or a variation of it proposed by harper.3 Solute segregates to the dislocations under the influence of the elastic strain field of the dislocation and the rate of depletion of the solute can be measured by following the change in electrical resistivity4 or internal friction.5 On reloading a prestrained specimen, plastic flow starts at Fig. 1, but after aging the reloaded specimen yields discontinuously at a higher stress The aging index reflects the extent to which the yield has returned. Until recently it was usual to assume that ? is a result solely of the pinning of dislocations by the segregated solute atoms, that is, that op and oj coincide and the strain hardening curves AB and CD are continuous. Thomas

Jan 1, 1963

By F. B. Petermann

Two-stage electric smelting tests, using small submerged arc furnaces, were made on high-iron manganiferous materials from the Pioche District, Nev., and the Cuyuna Range, Minn. The object was to reduce sufficient iron in the first stage to give a slag with a favorable Mn to Fe ratio for smelting to ferromanganese in the second stage. The nodulized flotation concentrate from the Pioche District contained 29.2 percent Mn and had a Mn to Fe ratio of 2.3:l. When smelted with coke and silica or alumina as flux, more than 90 percent of the manganese was recovered in slags with Mn to Fe ratios of 10: :24:1. The Pioche slag was smelted to ferromanganese using coke and lime- stone or dolomite as flux. The ferromanganese was high in silicon but other- wise met specifications. Recovery of manganese to ferromanganese in this step was 73 to 78 percent. Overall recovery of manganese was about 70 percent. The sintered flotation concentrate from the Cuyuna Range material contained 12.9 percent Mn and had a Mn to Fe ratio of 0.3:1. When smelted with limestone as flux, about 83 percent of the manganese was recovered in a slag with a Mn to Fe ratio of about 6:1. The Cuyuna slag was smelted to ferromanganese with coke and limestone for flux. Recovery in this step was 61 percent of the manganese in a high silicon ferromanganese. Overall recovery of manganese was about 50 percent.

Jan 1, 1963

By A. R. Taylor

The Bureau of Mines has determined the heat capacity and enthalpy values for beryllium sulfate (BeS04) throughout the temperature ranges of 10° to 300° K in an adiabatic calorimeter, and 350° to 860° K in a Bunsen-type ice calorimter, The heat-capacity data were extrapolated to 0° K, and smooth values of heat capacity, entropy, enthalpy function, and free-energy function were reported at 10-degree intervals between 0° and 300° K. The method of least squares was used to fit the enthalpy data with an algebraic equation. The equation also was used to calculate values of heat capacity, entropy, enthalpy function, and free-energy function at 50-degree intervals between 300° and 900° K.

Jan 1, 1963

By César Alvarado Olivares

El presente trabajo describe la solución planteada al problema de renovar el equipo de celdas de flotación que por el tiempo de uso (19 años) y por su tipo de diseño, ya no ofrecfa el rendimiento que hoy en día se puede conseguir en esta clase de tratamiento. La solución consiste en

Jan 1, 1963

By E. J. Rapperport, E. D. Levine

The boundaries of the (a +ß) field in the Al-Li system were determined between 150°and 550°C utilizing quantitative metallography and lattice-parameter measurements. The solubility of lithium in aluminum decreases from 12.0at. pct Li at 550°C to 5.5 at. pct Li at 150°C. P Al-Li is saturated with aluminum at 45.8 at. pct Li and has this boundary value constant over the temperature range 150°to 550°C. THE solid solubility of lithium in aluminum has been determined by several investigators, 1-6 but, as shown in Fig. 1, there is little agreement among the various determinations. The earliest investiga-tions&apos;-&apos; are suspect because of the use of impure materials. Although high-purity materials were employed in more recent work,4&apos;5 the experimental techniques may have led to contamination of the specimens. Probably the best work has been that of Costas and Marshall,6 who obtained close agreement between results obtained by two independent phase-boundary techniques: electrical resistivity and mi-crohardness. No detailed studies of the solubility of aluminum in the bcc ß phase, Al-Li, have been reported. Cursory investigations1,2,6 have indicated only that the (a+ß) -p boundary lies between 40 and 50 at. pct Li and is relatively independent of temperature. The present work was undertaken in order to provide an independent check on Costas and Marshall&apos;s determination of the solubility of lithium in aluminum, to extend knowledge of this solubility limit to temperatures below 225°C, and to make an accurate determination of the solubility of aluminum in Al-Li. EXPEFUMENTAL Alloy Preparation. In view of the difficulties encountered in previous investigations of the A1-Li system, close attention was paid to the use of methods of alloy preparation and treatment that would minimize contamination. Aluminum sheet (99.99 + pct Al) was vacuum-induction melted in a beryllia crucible to remove hydrogen. Lithium (99.9 pct Li) was charged with pre-melted aluminum into a beryllia crucible, in a helium-filled drybox. The crucible was sealed in a Vycor tube and transferred from the drybox to an induction furnace. Melting of alloys was performed by induction heating in a helium atmosphere. Solidification was accomplished by means of a suction apparatus, shown in Fig. 2, in which the alloy was forced by changes of pressure into a 3/16-in. inside diam closed-end beryllia tube. This technique produced rapid solidification of a small portion of the melt, resulting in alloys with a high degree of homogeneity. Typical lithium distributions are presented in Table I. Transverse sections 1/8 in. long were cut from the alloy rods, and each section was split in half longitudinally. One half of each section was analyzed for lithium, and the opposing halves were employed for phase-boundary determinations. Lithium contents were determined by flame photometry with an accuracy of 1 pct of the amount of lithium present. Thermal Treatments. Homogenization and equilibration heat treatments were performed in electrical-resistance furnaces with temperatures controlled to ± 2OC. Calibrated chromel-alumel thermocouples were employed to measure temperature. Homogenization was performed in helium-filled l?yrex tubes for 1 hr at 565°C. The encapsulated specimens were then transferred directly to furnaces maintained at lower temperatures for equilibration. Equilibration times were 2 hr at 550°C, 8 hr at 450°C, 27 hr at 350°c, 90 hr at 250°c, and 285 hr at 150"~. These times were chosen on the basis of conditions employed by previous investigators. Alloys were quenched from the equilibration temperatures by breaking the capsules into a silicone oil bath. By performing all possible operations either in sealed capsules or in a helium-filled drybox, the specimens were given minimum exposure to the atmosphere. Quantitative Metallography. Metallography of Al-Li alloys is difficult because of the atmospheric reactivity of the ß phase. It was found possible, however, to prepare surfaces of good metallographic quality by preventing contact with moisture during preparation. Grinding through 4/0 paper was performed in the drybox. The specimens were then transferred under kerosene to the polishing wheel. Three polishing stages were employed: 25-p alundum with kerosene lubricant on billiard cloth, 1-µ diamond paste on Microcloth, and 1/4-p diamond paste on Microcloth. Between stages the samples were cleaned by rinsing in trichloroethylene and buffing

Jan 1, 1963

By George Simkovich

It was hypothesized that solid-state point defects should alter the flotation properties of solids. Tests conducted on pure AgCl and AgCl doped with CdC12 show that atomic point defects exhibit an important role in the floatability of AgC1. Tests conducted on PbS doped with Ag2s or Bi2S3, also show that the defect structures resulting from these dope additions, i.e., a combination of electronic and atomic point defects, contribute significantly to the flotation of PbS. IT has been established that flotation occurs only when a finite contact angle exists between a solid and a gaseous bubble.&apos; This angle, measured through the liquid phase, is expressed by the equation where the are inter facial free energies and the subscripts S, G, and L represent solid, gas, and liquid phases, respectively. As is seen in Eq. [I] three interface free energies, sG, sl, and GL, enter into the contact angle equation. Therefore, any variation in these energies which sufficiently varies the contact angle will, in turn, vary flotation processes. Changes made in any of the phases concerned, i.e., gas, liquid, or solid phase, are reflected through the changes occurring in two of the surface energy terms. Thus, a change in the liquid composition would be noted in sL and GL, and it is this phase, the liquid, which is most frequently altered in flotation studies., Changes in the solid phase must be reflected through the changes occurring in the sG and sL terms. In particular, it is hypothesized that changes in the surface concentrations of point defects in the solid-phase will alter the sG and sL terms which, in turn, will be reflected by flotation results. As an illustration of this hypothesis one may consider the defect structure and the flotation of AgC1. The bulk defect structure of AgCl is essentially one involving equal number of cation vacancies and interstitial cations.3 Upon adding CdC1, to AgC1, a greater number of silver ion vacancies are created in the bulk of the crystal.4 On the surface of the crystal the smaller binding forces and the free space accomodations may also allow for the creation of "surface interstitial anions", which will be designated as ad-anions. Thus, the point defect structure of the surface of AgCl doped with CdCl, will consist of cation vacancies and/or adanions. If the molecular forces responsible for the surface energies, ?SG and ?sL, are significantly altered by the presence of these surface point defects, then differences in flotation results will be noted as the concentration of these defects is varied. The defects present in AgCl are predominantly atomic in nature. In the case of PbS both electronic and atomic defects are present.5 This compound conducts electrically by either electrons or electron holes depending upon whether excess lead or excess sulfur is present. Upon disolving BiS3 in stoichio-metric PbS, one increases the concentration of cation vacancies and the number of electron carriers in the bulk of the crystal.5" At the surface, the possibility of ad-anions must also be considered. Conversely, upon dissolving AgS in stoichiometric PbS one increases the concentration of interstitial cations and the number of electronhole carriers in the bulk of the crystal.5,6&apos; At the surface the interstitial cations will be designated as ad-cations. Thus, the point defect structure of the surface of a PbS crystal doped with Bi2S3 will consist of a number of cation vacancies and/or ad-anions and an excess of electrons. Conversely the point defects on the surface of a PbS crystal doped with Ag2S will consist of a number of ad-cations and an excess of electron holes. Again, as in the case of AgC1, should the molecular forces responsible for the magnitude of the interface free energies, ?sG and ?sL, be significantly altered by the presence of these surface defects then significant differences in flotation results will be noted as the concentration of these defects is varied. EXPERIMENTAL To test this hypothesis flotation tests were conducted on pure and doped AgCl and on PbS doped with either Bi2S3 or Ag2S. Preparation of the AgCl samples was performed as follows: AgCl and weighed amounts of CdC1, were melted in a porcelain crucible. The melt was then forced through a capillary tube and the particles emitted solidified in air as they fell about 1.5 meters. Spherical particles, -0.50 + 0.25 mm, were separated from the remaining solidified material

Jan 1, 1963

By Leonard F. Heising

At the Groveland mine iron ore is mined by open-pit methods and concentrated by means of spirals and flotation. A brief history of the mine and its early development is given. The ore deposit is described, with emphasis on those physical characteristics that affect the choice of mining and milling methods. Development and mining, which include breaking ground, loading, transportation, engineering, and operating control, are explained, and the milling method is described Mining and milling costs are given in percent of total cost.

Jan 1, 1963

By C. O. Hawk

As an exploratory effort to produce useful products from coal by a new path, the Bureau has made a few experiments on the fast heating of finely ground coal particles by irradiation with a flash of high intensity light. The flash was produced by an electrical discharge at high voltage through a xenon-filled tube. The flashes lasted from 2 to 3 milliseconds. The reaction took place in small sample tubes, ½ inch-dimeter by 4 inches long, and with small amounts of coal (total amount charged 0.1 gram, probable effective amount not more than 20 milligrams). Average particle size of the coal, estimated on a numerical basis, was 20 microns. Temperatures reached were evidently quite high, because all products obtained in quantity were characteristic of high temperature pyrolysis. Apparently, conversion of the coal was extensive where isolated particles received the full benefit of a flash. It seems particularly significant that acetylene was present in appreciable amounts--comprising almost 3 percent of the total gaseous product in one case. This is good evidence of a short heating period to very high temperature (well above 1,000° C) followed by rapid quenching. Although the results are interesting, they do not suggest any immediate practical application.

Jan 1, 1963

By R. E. Mussier

This investigation was made to study new methods to prepare high-purity yttrium metal, Various methods were used to prepare pure intermediate compounds, primarily chlorides, bromides, and iodides, which were subsequently reduced to metal. The process found most suitable for the preparation of pure anhydrous yttrium chloride involved thermal dehydration of a mixture of hydrated yttrium chloride and ammonium chloride while under vacuum. Yttrium bromide and iodide were prepared most effectively by the direct halogenation of yttrim carbide. Yttrim carbide was obtained by reacting and melting yttrium oxide-carbon mixtures in a carbon-arc furnace. Yttrium halides were purified by vacuum distillation and reduced by alkali or alkaline-earth metals. Lithium and sodium proved to be the best reductants from the standpoint of yield (>95 pct) and purity (>99.8 pct) of the yttrium. The product of the reduction step was sponge metal, which was consolidated readily by conventional cold-mold, arc-melting procedure. The purest yttrium obtained in laboratory scale work was prepared by sodium reduction of yttrium chloride and contained only 125 pp oxygen; other impurities did not exceed 1,000 ppm. In larger scale tests yttrium containing only 800 to 1,000 ppm total impurities was obtained by lithium reduction of yttrium chloride. The tensile properties of high-purity yttrium were determined. Mechanical tests showed that yttrium can be forged, extruded, rolled, spot welded, and deep drawn.

Jan 1, 1963

By E. P. Pfleider, D. H. Yardley

Layers of magnetic taconite of above average magnetic iron content extend down dip on the Mesabi Range to depths beyond the reach of open pit mining. A selected layer with thickness of 75 to 100 ft underlies many square miles. Such a selected layer can provide over 50 million tons of recoverable concentratc per square mile, at lower concentration ratios than in the present open pit taconite operations. The system contemplated would consist of large scale underground quarrying by a lane and pillar method. Working heights would be 60 to 100 ft; room widths, 50 to 75 ft; and productivity targets, about 40 tons per man-shift. The most critical problems would he roof control and blasthole drilling. The successful operation of large open pits and concentrating plants for treatment of magnetic taconites indicates that the basic techniques and economic problems of pellet production have been solved. The open pit reserves are large, but they are not necessarily available in sufficient quantity or quality to provide an adequate raw materials base for all potential producers. Furthermore, as the more easily available open pit crudes are used up, the pits will become deeper, stripping costs per ton of concentrate will increase, and recoveries will decrease as leaner crudes are utilized. The time will come when supplementary and replacement reserves of magnetic taconite will be required. One way these can be obtained is by underground mining of the down-dip extension of the Mesabi magnetic taconites, especially those layers averaging well over 25% recoverable iron. A key point in such a proposal is the possibility of realizing substantial savings by beneficiating an ore of 30% magnetic iron at 2.5 to 1 ratio of concentration. This contrasts with current practice in Mesabi commercial taconite plants, where the ore averages 22 to 25% magnetic Fe, with concentration ratios of about 3.0 when producing 61% Fe pellets. Two factors which favor the eventual development of underground taconite mining are: 1) the desirable physical structure and high grade of taconite pellets in general and 2) the improved engineering techniques in underground mining. Experience in large scale room and pillar mines demonstrates that, given strong rock strata immediately above a high grade mining

Jan 1, 1963

By Gilbert Santoro

In this study tantalum carbide filaments of various compositions in the fcc region were prepared by heating a tantalum wire in a measured amount of hydrocarbon vapor. Such properties as tensile strength, transverse-rupture strength, microhard-ness, lattice parameter, electrical resistivity, and magnetic susceptibility were measured as a function of carbon content. Some of these properties showed a maximum or a minimum between a carbon-to-tantalum molar ratio of 0.80 and 0.85, the composition range at which the color changes from metallic gray to gold. The recent literature has shown that in the large homogeneity range for the fcc phase of the Ta-C system there is a marked variation for such properties as microhardness,&apos; electrical resistivity, &apos; thermodynamic properties,z&apos;3 lattice parameter and superconductivity. In addition to the technological interest of these variations within a single phase, important theoretical benefits may ensue from a continuous investigation of properties vs stoichiometry in tantalum carbide and other refractory defect compounds, for example the effect of the metal-metal distance and crystal structure upon bond formation and electronic structure. Whether there is a similar variation of the tensile strength is of practical importance. Of theoretical interest would be the knowledge of how the magnetic susceptibility varies with carbon composition. Both of these properties, as well as the transverse-rupture strength, were determined for tantalum carbide filaments in the fcc phase region. The lattice parameter, the electrical resistivity, and the microhardness were also investigated and compared with values appearing in the literature. EXPERIMENTAL PROCEDURE Material Preparation. Tantalum carbide specimens of various carbon content were prepared by statically carburizing high-purity tantalum filaments in measured quantities of pure hydrocarbon gas. The filaments, which were 10 mil in diameter and 20 or 40 cm long, were heated by their own resistance at temperatures from 1800" to 2200°C using alternating current in some cases and direct current in others. Tantalum wire from two sources was used. One had a reported purity of 99.96 wt pct Ta. The ingot from which this wire was drawn had been electron beam-melted as the final step in its purification. The reported purity of the other wire, which was prepared by a powder metallurgical process, was 99.88 wt pct Ta. The impurities of both tantalum sources are listed in Table I. Spec-trographic-grade toluene or research-grade propane was used as the source of carbon. The apparatus for the carburization of the filaments is shown schematically in Fig. 1. The system was evacuated to 1 x l0-&apos; mm of Hg when using the electron beam-melted tantalum and to less than 1 p when using the less-pure tantalum. Neither the difference in the base vacuum, nor in the hydrocarbon gas, nor in the tantalum filaments resulted in any detectable difference in the properties studied in this work. However, only the carbides prepared from the higher-purity tantalum were used in the magnetic-susceptibility determinations. Once the base vacuum had been reached, the system was flushed with the hydrocarbon and re-evacuated. For any desired composition of the carbide, hydrocarbon gas was allowed to leak into a constant-volume flask to a predetermined pressure. These pressures were measured by a Cartesian diver-type mercury gage with a range from 0 to 20 mm and with a scale expanded to nine times. The hydrocarbon gas was allowed into the reaction tube and the filament was quickly raised to the reaction temperature. The slack in the filament due to thermal expansion was taken up by drawing out the movable electrode with a screw mechanism. The filaments were kept at temperature from a few minutes to 200 hr. In the majority of cases the heating time was 6 hr. The reaction tube was cooled by cascading water on its outer surface. By means of an ammeter and a voltmeter the electrical resistance at the reaction

Jan 1, 1963

By Nicholas J. Grant, W. Michael Yim

The creep-rupture properties of nickel, in as-prestrained or prestrain-polygonized condition, were studied at 1300°F and 4000 psi, and also at 700°F and 26,000 psi. An improvement of strength was noted in both the as -prestrained and the prestrain-polygonized tests at each temperature. The as-prestrained tests, however, showed superior creep resistance to the prestrain-polygonized ones. From the results of X-ray and etch-pit studies, the strengthc gain was interpreted in terms of dislocation density and the stability of preformed substructures. COLD work is known to improve the strength properties of metals at low temperatures. At high temperatures, however, the strength improvement is often lost if gross structural changes, such as re-crystallization, take place prior to or during the test. Even in the absence of recrystallization, a prestrained metal may undergo structural changes— polygonization and the formation of well-defined subgrains—which importantly effect the resultant properties. The relationship between substructure and creep properties has received considerable attention in recent years. The work of wood1 indicated that the creep strength of aluminum and its alloys was closely related to the subgrain size. Hazlett and Hansen,2 and Ancker, Hazlett, and parker,3 working with nickel and nickel alloys, had shown that small amounts of prestrain at room temperature followed by a recovery anneal at 800°C (1470°F) improved the strength at both low and high temperatures. The strength gain was attributed to an increase in the number of subgrain boundaries as a result of the prestrain-polygonization treatment. More recently Coldren and Freeman4 studied the effect of substructures on the creep rate of nickel at 1550°F. Their conclusions indicated that the substructure size as measured by the number of boundaries was the factor that controlled the creep rate. In addition, the perfection of the subgrain boundary has been indicated to have an important role on the strength.&apos; On the other hand, there are data which disagree with the above observations. Grant, Chaudhuri, Silver, and Ganow6 found no creep strength improvement by a prestraining treatment. In reviewing the role of subgrains on high-temperature creep, Shepard and Dorn7 concluded that the contribution of the subgrains to high-temperature creep strength was a minor one. Guard,8 in a recent study on poly-gonized nickel, has cast doubt on the validity of the postulate that subgrain size controls the creep rate. In the majority of the previous studies, the subgrain boundaries have been singled out as the most important factor in determining creep strength; however, there is no firm theoretical ground for the postulate that the subgrain boundaries act as effective barriers to dislocation motion.B910 Little effort has been directed toward the study of the relationship between creep strength and other structural variables, such as dislocation density, lattice strain,

Jan 1, 1963

By V. D. Hanson

When maintenance of a plant or operation is under discussion immediately three "M&apos;s", all in short supply, are brought to mind - money, men and markets. This paper will present what currently is being done at our plants and its effect on the 3 "M&apos;s". Examination of coal realization figures (F.O.B. Mine) from 1945 to the present reveals the fact that open and free competition can and will meet market conditions. The industry, without benefit of advantages afforded tax and transportation wise to oil and gas, remains the backbone of the energy market of United States. Figure No. 1 shows the realization figures from 1945 through 1962 compared to the hourly earnings. Note that through 1945 to 1948 F.O.B. prices increased $1.93 per ton while hourly earnings increased $.66 per hour. Since 1948 (with the ex¬ception of 1957) F.O.B. prices have declined $.45/ton, while hourly earnings have increased $1.23 per hour. Basically the maintenance men possibly represent the highest increment rate in the overall hourly earning.

Jan 1, 1963

By L. D. Clark

Pay-out, the ratio of capital expenditure to annual cash return can be very revealing when employed to gage the merits of a proposed mining venture. It is a quantity, numerically but not physically equal to a factor, by which cash return may be discounted to equal required investment. The fewer the pay-out years, the greater the average annual earning power of the project. Considerable material has been written in the past about the most important and difficult problem mining management faces in evaluation of a property: the optimum production rate for the venture. What daily capacity should be adopted for the proposed operation that it may be the most rewarding to those underwriting it? H.C. Hoover has said, "The most important objective is the least cost per ton mined; and minimum working costs can only be gained by the most intensive production." Theoretically and practically, the quicker the ore is removed, the more profitable should be the venture because of the saving in fixed charges, the consequent lower unit costs and the interest unearned by the profit from the unmined ore. Yet, such performance will be tempered by policy and a restraint imposed by the ratio of capital expenditure to annual cash return. * The &apos;Annual net profit after taxes but including depreciation and depletion allowances. former will be based upon an analysis of the economic climate anticipated, with its many ramifications including the demand for the product, prices, tax laws, the conduct of labor and related wage scales. The variables and intangibles involved in estimating the optimum production rate for a mine do not readily lend themselves to mathematical relationships or equations and the problem can become complex indeed. The more readily applicable and relatively faster appraisal method will be used which, in addition to being reasonably adequate in most cases, will serve as a guide, should a more expanded and detailed estimate be desired. The first question is what is company policy with respect to the rate of investment return? This will depend on that significant period of time referred to as the pay-out, which can be defined as the estimated interval during which capital investment is returned through application of annual cash return to its recovery. Expressed another way, it is the ratio of capital expenditure to the annual cash return. For example, if the capital investment is $C and the annual cash return is $A (after Federal tax), then $C/$A = the pay-out period in years. That is to say, if $C = $1,500,000 and $A = $214,000, then which is the mathematical expression for the period of time it takes to recover the funds originally invested in a mining enterprise. The relationship yp = $C/$A can be useful — an expression which requires only the significant tern yp to be fixed; in other words, the long range investment policy. For what is the pay-out period but an expression of that policy in terms of the speed, within practical limits, with which an individual or company may want to recover capital expenditure? A policy by which pay-out will be fixed is imperative. This ratio must lie within relatively narrow limits governed by what is economically feasible. It cannot be too low, rendering the ratio impractical or absurd, nor too great, delaying the return of capital for reinvestment beyond a commensurate interval. What pay-out will govern this policy? Federal corporate taxes would seem to present the best measure. Consider mining in Canada where new mines are exempt from Federal income tax for 3½ yr from date of first production. This exemption expressly allows The Act states: "A corporation . . . i s not required to include the profits . . . for the period of 36 months commencing with the day on which the mine came into production in reasonable commercial quantites." a company to recover capital expenditure during the early stages of production. With such an incentive, it is logical to strive for as much capital redemption as possible during this period. Thus, 3½ yr would be a major contribution to the pay-out in Canada. Furthermore, it generally takes from 1½ to 3 yr to develop

Jan 1, 1963

By Floyd B. Bowen

Pumping methods are used, almost exclusively, to transport materials in the mining, beneficiation and chemical processing of phosphate rock in the Florida phosphate pebble field. Matrix pumping systems capable of pumping 15,000 g.p.m., transporting 15,000 long tons (dry) per hour, are now in use. They utilize 16-by 48 Yz -in. pumps, driven by 1.250-h.p. motors, discharging into pipelines 20 inches .in diameter .and sometimes several miles in length. As an average, it is necessary to pump 3 tons of matrix to the beneficiation plants, and to dispose of 2 tons of sand tailings and clay as waste, in order to produce 1 ton of shipping-grade rock. The washers and flotation plants, where the clay and phosphate and silica particles are separated, require the movement of large volumes of slurries with densities ranging from 2-3 per cent to 45 per cent solids, by weight. Extensive waste disposal systems require the pumping of dilute clay slurries in quantities of up to 50,000 g.p.m.,

Jan 1, 1963

By R. D. Berkenkotter

Titanium and iron assays obtained from cores of three diamond-drill holes from the Cebolla Creek titaniferous iron deposit were evaluated by statistical techniques to obtain information concerning the mineral characteristics of the deposit and to make a preliminary determination of sampling requirements for the deposit. A range of sample volumes representing sizes from one-sixth NX core 2 feet in length through full NX core 10 feet in length were prepared by split-ting the NX core with a diamond saw and combining pulverized splits. Results indicate the existence of at least two statistical populations having different average grades of iron and titanium. Each has an assay frequency distribution that is not normal but is highly peaked (leptokurtic). Frequency distributions of assays from specific altered zones of the drill holes appear to be normally distributed. Increasing the cross-sectional area of the sample unit to change assay volume did not result in significant changes either in assay values or the resulting frequency distributions of assays. However, when assay volume is increased by increasing sample interval, the shape of the assay frequency distribution changes, and a normal distribution of assays is approached. Positive correlation exists between titanium and iron assays. The degree of correlation, although very significant, is too low to use for prediction purposes. Although the amount of data from three widely separated drill holes is not sufficient to establish an average grade for this large deposit, it indicates a range of expected assay values and provides some information for determining requirements of future sampling for evaluation purposes.

Jan 1, 1963

By C. A. Komar

The Bureau of Mines is investigating possible applications of acoustic energy at sonic and ultrasonic frequencies in petroleum production. A phase of this work involves measuring sound velocity through petroleum reservoir rocks. References and abstracts were prepared as a bibliography to make available to others some of the material obtained from a literature search covering the past applications and the present uses of sound. Laboratory and theoretical studies of the various parameters that influence the velocity of sound in porous media account for the wealth of information now available. Velocity of propagation of sound waves in porous sediments as a function of depth is a quantity frequently measured. Velocity logging systems, capable of measuring speed of sound waves in underground formations penetrated by wells, have been developed for interpretative studies. The close relation between acoustic velocity and porosity makes it possible to determine porosity from velocity logs. Most velocity log interpretation in terms of porosity is based on a formula developed by Wyllie and others known as the time-average relation.

Jan 1, 1963