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By E. F. Adkins, R. W. Douglas

The variation of the spectral emissivity of osmium and ruthenium with temperature can be expressed by the following relations: DURING a study of the sintering characteristics of osmium and ruthenium, discrepancies in the previously accepted melting points of the metals were noted. The melting temperatures had not been measured at the time of the work, but were estimated in the literature as 2700°C for osmium and 2450°C for ruthenium.' A recent investigation by Baird2 has shown the melting temperatures of osmium and ruthenium are 3000" and 2250° C, respectively. In the present work, osmium bars sintered at temperatures as high as 2900° C showed no evidence of melting, whereas ruthenium showed definite evidence of melting at temperatures as low as 2250°C. In view of the apparent discrepancies, the melting temperatures of both metals were determined. The spectral emissivities of both metals were determined as an aid to studies of the sintering characteristics of these metals. MATERIALS AND PROCEDURES The materials used in these studies were metal powders supplied by Englehard Industries, Inc., through the courtesy of The International Nickel Co. Analytical data from three laboratories, although not in complete agreement as to the purity of the material or the major impurity elements, indicated that the maximum impurity levels were 0.5 and 1.0 wt pct in osmium and ruthenium, respectively. The metal powders were pressed to 1/4 by 1/4 by 6-in. bars at 20Tsi using carbon tetrachloride as a lubricant. The pressed bars were presintered 1 hr at 1200°C after heating 1 hr at 400°C. The presintered densities of the several bars of the metals ranged from 65 to 80 pct of ideal density. Specimens were self-resistance heated in a vacuum sintering bell. Temperatures were measured with an L&N, disappearing filament optical pyrometer. True temperatures were read at the base of an 0.30-in.-diam, 0.150-in. deep hole drilled into the center of a presintered bar. Apparent temperatures were read from the surface of the bar adjacent to the hole. MELTING POINT DETERMINATION The melting temperature of the metals was determined as the temperature at which a slight additional increase in current through the specimen resulted in a reduced temperature at the base of the hole. The apparent reduction in temperature is a result of the liquid metal filling the hole, thus altering the black-body conditions. The melting points of osmium and ruthenium, based on three deter-

Jan 1, 1962

By F. V. Lenel, G. S. Ansell

The creep behavior of an aluminum -aluminum oxide alloy, A T 400, fabricated by compacting an atomized aluminum powder, extruding the compact, cold working, and recrystallizing the extrusion, was investigated. This alloy has a dispersion spacing of 1 . Previously Ansell and Weertman determined the steady-state creep rate of a recrystallized aluminum-aluminum oxide SAP-type alloy, MD 2100, with a 0.48-p dispersion. This alloy was found to have a steady-state creep rate of less than 10-6 min-1, too small to be measured accurately. By employing a more sensitive method of measuring creep rate, it was possible to determine the steady-state creep rate of AT 400 alloy, which is somewhat faster than that of MD 2100, at a series of temperature and applied stresses. Above a stress of Burger's vector, A = dispersion spacing, u = is a shear modulus) the rate follms an equation of the type: Steady-state creep rate K = A exp. where A is a constant, Q is the activation energy for sey-diffusion, and is the applied stress. At stresses lower than the steady-state creep rate drops off sharply and is no longer in agreement with this equation. This behavior is in good agreement with that predicted by the model for dispersion strengthened alloys in the stress and temperature range investigated. The absolute value of the creep rate is, however, four orders of magnitude lower than that predicted if the normal number of active dislocation sources are assumed to be present. It is concluded that in this SAP-type alloy the usual three-dimensional dislocation network is not present. Instead, short dislocation segments extending from one dispersed particle and terminating at a neighboring particle may act as dislocation sources. With this provision the creep model proposed by Ansell and Weertman reasonably accounts for the creep behavior which was observed. RECENTLY, Ansell and Weertman1 proposed a dislocation model from which they derived creep equations to describe the steady-state creep behavior of dispersion - strengthened alloys. Following Schoeck,2 they assumed that the rate controlling process for steady-state creep is the climb of dislocations over the dispersed particles. In order to verify their creep model, Ansell and Weertman determined the steady-state creep behavior of an aluminum-aluminum oxide SAP-type alloy, MD-2100, in both the fine-grained as-extruded, and coarse-grained recrystallized conditions. Since the grain size was the order of the dispersion-spacing, their model was not applicable for the as-ex- truded alloy. It should, however, be applicable to the coarse-grained recrystallized alloy. The results they obtained were rather unexpected. No meas-ureable steady-state creep was observed for the recrystallized MD-2100 alloy. If their model is correct, and if the second-phase particles act solely to hinder dislocation motion, then some measureable steady-state creep would have been expected. On this basis, they postulated that, in this SAP-type alloy, the main effect of the fine dispersion was to inactivate dislocation sources rather than to hinder the movement of dislocations. In order to understand more fully this unusual creep behavior, and to determine the validity of the model proposed,' the steady-state creep behavior of an aluminum-aluminum oxide recrystallized SAP-type alloy, with a somewhat coarser dispersion spacing, was investigated. The results of this study are presented in this paper.

Jan 1, 1962

By Harold M. Feder, Irving Johnson

Tkermodynamic functions for dilute solutions of uranium in liquid cadmium were obtained from galvanic cell measurements. Deviations from Henvy's law were observed at concentvations down to 2 x 10-3 atom fraction. Unusually large negative values of the pavtial molal relative enthalpy and excess entvopy of uranium, suggestive of the occu,vvenctwe of partial ovdering of cadmium around uranium in these solutions, were found. The negative relative partial molal enthalpy of uranium at the liquidus accounts for the observed retrogvade solubility of metallic uranium between 473" and about 630°C. The standard free enevgy of formation of UCd,, from a-uranium and liquid cadmium is given by F,° THE constitutional diagram of the U-Cd system,' Fig. 1, is unusual in several respects. The near equality of the Goldschmidt atomic radii2 (Cd, 1.52A U, 1.56A) might be expected to give rise to extensive mutual solubility of the elements except for the restrictions imposed by differences in valence and electronegativity.3 The latter factors must be strongly influential because mutual solubilities in the terminal solid phases are probably negligible, and the solubility of uranium in liquid cadmium in the readily accessible range is only about 1 at. pct. Interestingly, the solubility of uranium in liquid cadmium actually decveases slightly with increasing temperature from 473" to about 630°C. Such a retrograde solubility in a liquid phase is a rare phenomenon in metallic systems; no other authenticated examples were found among the nearly 700 binary phase diagrams compiled by Hansen and Anderko.2 These observations suggested the existence of some unusual interaction between uranium and cadmium. Greater insight into the nature of this interaction was sought by measurement of the thermodynamic properties of the system. EXPERIMENTAL PROCEDURE The emf of cells denoted by the scheme was measured. Each cell consisted of two uranium and two alloy electrodes immersed in a molten lithium chloride-potassium chloride eutectic mixture containing uranium trichloride. The physical arrangement is shown in Fig. 2. The potential between any pair of electrodes could be measured with a Leeds and Northrup Type K-3 potentiometer. The measurements were made at points marked in Fig. 1. It should be noted that points on the phase boundaries represent the concentrations of uranium in the saturated liquid phases of heterogeneous alloys. Uranium Electrodes. Uranium, which is not a particularly soft metal, is capable of retaining residual stresses, and its potential may depend upon its physical condition. Electrodes were prepared from 3-mm diam rods of hot-rolled high-purity4

Jan 1, 1962

By H. A. Hoffman

Competition from an all-flotation plant, with demonstrated economies and efficiencies, plus a change in smelting contract and introduction of improved cyclones lead to conversion from gravity-flotation. Detailed descriptions are given of equipment installed and procedures used at St. Joseph Lead's Federal mill. Future plans include further quality control by instrumentation in all aspects of the mill operation. Also planned are improvements in materials handling systems. Competitive conditions will continue to dictate improvements and changes in the mill flowsheet. The advent of all-flotation mills in the Lead Belt was introduced by the Indian Creek mill in late 1953. This modern and efficient plant then became a pattern for the other mills in this area to re-evaluate their circuits in an effort to develop flowsheets that would improve operating conditions and metallurgy. The Indian Creek mill demonstrated that all-flotation would require considerably less operating and maintenance labor than the combination of tabling and flotation that was common in the Lead Belt at that time. Two significant changes occurred in recent years to allow all-flotation to be seriously considered in other Lead Belt mills. One was a change in the smelting contract which did not require gravity concentrate. Another was the development of cyclones which provided classification of the flotation feed in a very small space. Since the Federal mill was the largest concentrating plant in the Lead Belt it was felt that the greatest savings could be made by investigating the all-flotation possibilities at this mill. Interest was stimulated by the milling and ore dressing Depts. to determine if this mill would be converted without undue cost, provided the metallurgy could be improved. Accordingly, laboratory tests were initiated to learn what metallurgical benefit could be derived. Numerous tests were run which indicated that grinding to all-flotation would improve the tailing by as much as 0.02 pct Pb. This was quite significant when multiplied by the tonnage of ore treated. Projecting the added cost of power for extra grinding and flotation, and the additional flotation reagents required, plus additional new equipment that would have to be purchased, it would still add up to a considerable saving. The all-flotation mill would reduce man power by some 30 pct, and make a metallurgical improvement. Operating costs could be reduced bv 2$ per ton. The metallurgical improvement would amount to 4$ per ton, for a total of 6$ per ton of ore milled. An estimate of the cost of the conversion was set at $250,000. With the savings as estimated this could be paid off in about two years. On paper it therefore seemed attractive enough to justify a mill test. MILL TESTING One section of the Federal mill was made available for use as a separate test circuit. Cyclones and density controllers were borrowed from the Viburnum and Indian Creek mills. Denver flotation cells were obtained from the Desloge mill that was then shut down. Two 10-cell groups of Fagergren flotation machines, consisting of eight roughers and two cleaners in each bank, were segregated from the remainder of the plant. The 9x12-ft rod mill was continued as a primary grinding mill. The two 6%x12-ft mills on this section were converted from rods to balls, and the speed increased to 22.0 rpm. Cyclones were installed to close the circuit of these ball mills. The ground pulp from each of the ball mills was fed separately to its own bank of flotation cells so that two completely separated test circuits could be run in parallel. This test circuit operated on a three-shift basis from Dec. 22, 1959 to Mar. 21, 1960. The first few weeks were occupied in developing conditions for proper metallurgy and trouble-free operations. Results were rather erratic but as the ore dressing laboratory and the mill operators became more familiar with conditions they were able to obtain expected results, which could be duplicated day after day. The last five weeks of testing indicated the best results and are tabulated in Table I. During the first two weeks a Denver unit cell was used on No. 1 flotation circuit. Even though it recovered almost one half of

Jan 1, 1962

By R. C. Corey

Anticipating the need for convenient, economical, and safe means for disposing of combustible wastes contaminated with low-level activity, in connection with private and institutional uses of radioisotopes, the Atomic Energy Commission (AEC) has provided the Bureau of Mines with funds to develop an incinerator for this purpose. A prototype incinerator, designated hereafter as BOMAEC-30, was designed, constructed, and tested, based on fundamental and applied research investigations of the combustion characteristics of rubbish and sawdust, which will comprise the bulk of contaminated wastes. No radioisotopes were used in the tests; the objective was to remove as much particulate matter from the products of combustion as possible. The prototype unit was designed to burn 30 pounds per hour, using 100 percent over fire air admitted tangentially in an all-metal, cylindrical combustion chamber. The gas-cleaning system consisted of special fabric bags and absolute filters.

Jan 1, 1962

By D. L. Albright, R. W. Kraft

A technique is described whereby the study of crystal perfection through the use of conventional X-ray rockite curves is extended to three dimerzsions. Specinzens of unidirectionally solidified eutec-tic alloy which consist of a nearly perfect parallel arrangement of alternating Platelets of Al and CuAl2, but which contain lamellar faults have been analyzed by this technique in conjunction with X-ray microscopy. Analysis of the data has shown that some rotational symmetry about the growth direction occurs, that small groups of lamellae between faults diffract as a unit, and that the misorientation caused by a fault is on the order of a degree of arc. A eutectic-grain can be defined as that portion of a eutectic specimen in which the crystallographic orientation of each phase AND the microscopic or met-allographic orientation of the phase particles have fixed angular relationships one to another. Eutectic-grains of the A1-CuA12 eutectic, which is a normal lamellar eutectic, have been grown by unidirectional solidification and identified as such.1-3 To a first approximation, a eutectic-grain in this system consists of two interpenetrating single crystals which are related to each other and to the lamellae themselves as follows:

Jan 1, 1962

By S. R. Borrowman

This investigation by the Bureau of Mines was undertaken to develop information on the extractive metallurgy of thorite ores because potential ore bodies of this mineral have been found recently in Colorado, Idaho, and Montana. Basic information on thorite ore treatment that would be useful in appraising the potential of these and other domestic thorium resources was developed. The work was done mainly on thorite ore containing 3.87 percent ThO2 from the Powderhorn district, Colo., and on a composite sample containing 0.52 percent ThO2 from the Wet Mountains district, Colo. Limited tests of d corroborative nature subsequently were made on a sample containing 2.30 percent ThO2 from the Lemhi Pass area on the Idaho-Montana border.

Jan 1, 1962

By A. M. Gaudin

A new method of measuring the viscosity of unstable suspensions has been developed, using a Heinz viscometer. The technique was applied to kaolin-water suspensions. Spreads in viscosity with lime additive were measured.

Jan 1, 1962

By J. D. Brown

The electron optics, vacuum system, and sample stage assembly for the Bureau of Mines? electron probe X-ray spectrograph were purchased. Four scanning curved-crystal spectrometers, two reflection- and two transmission-type, were designed and constructed by the authors. The reflection spectrometers are placed in a vacuum chamber for measurement of long-wave-length X-radiation. Detection, pulse-amplitude discrimination, and recording circuits are provided for the simultaneous measurement of four X-ray spectral lines. Minimum spot size is approximately 2 microns in diameter at 30 kilovolts and a sample-to-ground current of 5 x 10-8 ampere. At this voltage and current the limit of detection with reflection spectrometers is less than 0.05 weight-percent for most elements. The limit of detection for elements determined by transmission-type spectrometers, evaluated at 35 kilovolts and 5 x 10-8 ampere, is approximately 0.1 weight--percent for all elements having excitation voltages below 20 kilovolts. In general, reflection spectrometers exhibited satisfactory but poorer resolution than the transmission type, resolution of the spectrometers being limited primarily by crystal imperfections, with greater mosaic structure being introduced by the grinding process for the reflection crystals. Several applications of the electron probe X-ray spectrograph are described. Analysis of a uranium-steel is discussed in detail to illustrate calculation of composition from measured X-ray intensities.

Jan 1, 1962

By C. H. G. Bushell, James E. Lawver, William Barbarowicz

Proper use of automatic controls in the process industries is a combination of art and science. Although many phases of automatic control theory can be expressed by precise mathematical relationships, the final control arrangement usually requires considerable effort by trial and error before the optimum control circuit is found. The failure of flotation operators to recognize that control circuits require study and plant experimentation before satisfactory operation occurs has led to a popular misconception that flotation plants simply do not lend themselves to automation. This widespread belief has been overcome to some degree in recent years by the numerous installations of automatic controls that have paid their way by increasing profits in terms of increased recoveries, lowered costs, or higher grade concentrates. WHY CONTROL ? Any form of automation must be justified in terms of ultimate return on in- vestment by improving quality, by increasing plant throughput, or by reducing the total operating costs. Generally speaking, automatic controls rarely re- place a mill operator. They assist the operator in holding important variables within predetermined limits. Large tonnage operations usually can justify a great deal of automation because an increase in one or two units of recovery results in enormous savings compared to the capital and operating costs of controls. DETERMINATION OF CONTROL The first questions in considering plant automation are: 1) What variables must be controlled? 2) What are the optimum levels of the variables? The optimum operating conditions for any process are those which maximize profits. Many of the variables active in flotation processing can be determined by experimentation in the laboratory or pilot plant 10. Although laboratory experiments can pinpoint variables, the true optimum conditions existing at plant level usually must be determined by plant scale experiments. In recent years, the concepts of detailed experimental designs in the laboratory, followed by plant experiments, have reached the stage of maturity where

Jan 1, 1962

By W. A. Tiller, W. C. Johnston

A theoretical analysis of alloy solidification in which the effective partition coefficient, k, of the solute is allowed to vary as a function of interface position is performed. A variety of solute distm'butions in the solid is predicted depending upon the functional dependence of k with interface position. Conversely, the variation of k with interface position required to produce a particular solute distributzon in the solid can be calculated. These preciictions have been tested by controlling the width of the momentum boundary layer in the liquid as a function of interface position with a rotating mugnetic field. One of the objects of controlled solidification is to utilize the freezing process for the preparation of crystals of specific materials containing a predetermined distribution of solutes. For example, a thermoelectric power generation material may exhibit a figure of merit, 2,' as a function of temperature, T, and solute concentration, C, as illustrated in Fig. 1. If we wish to use this material in a device between the temperature limits T1 to T2 a significantly greater efficiency will result from the device if the thermoelectric element illustrated in Fig. 1 consists of a range of solute concentrations appropriately located with respect to the temperature distribution rather than using a sample of constant solute concentration. For this reason and many others2 we are interested in programming and controlling the solute distribution in a single crystal

Jan 1, 1962

By C. R. Masson, M. L. Pearce

The nitrogen contents of seven specimens of iron and steel were determined by the three methods. Good agreement won generally observed between the results of the isotope -dilution and Kjeldahl determinations, tltzts establishing the reliability of the isotope -dilutzon technique. For some specimens, the vacuum-fusion values at 1650 °C were lower than the corresponding Kjeldahl values by up to 0.0015 pct absolute. These differences were eliminated for a specimen of "pure" iron by performing the vacuum-fusion analyses at 2100 ° to 2240 °C. The reason for this relatively high temperature required m the vaczium-fusion analyses is discussed. ThE determination of nitrogen in iron and steel has been the subject of numerous investigations and a concise review of the extensive literature in this field has recently appeared.' Two methods of analysis are most commonly employed, the vacuum -fusion and the chemical or Kjeldahl method. Except in special cases where the presence of certain alloying elements may present difficulties, both methods are generally regarded as applicable, although the vacuum-fusion method is more sensitive and is often preferred for samples of very low-nitrogen content. The method of isotope dilution, first employed for the determination of gases in metals by Kirshenbaum and Grosse,2 has recently been applied to the determination of nitrogen in iron and steel.3,4 The method is attractive in that it does not require the quantitative extraction of gas from the metal specimen. Staley and Svec3 modified the standard Kjeldahlpro-cedure by introducing, along with the steel sample, a measured amount of ammonium sulfate enriched in the isotope 15N. The nitrogen content was obtained by measuring the isotopic ratio 15N/14N in the resultant solution. The technique involved the distillation of nitrogen as ammonia from alkaline solution and subsequent oxidation of NH4+ in the distillate to gaseous nitrogen. The results for iron and steel samples of commercial origin were often in reasonable agreement with values quoted by the suppliers, although occasional marked discrepancies were observed, particularly with the results of vacuum-fusion analyses. Preliminary work in this laboratory4 on the determination of nitrogen by isotope-dilution in the gas phase yielded results for three samples which were significantly higher than the values obtained by vacuum-fusion. The present paper describes an extension of this work to a wider variety of samples. Analytical results by the Kjeldahl method are also reported. EXPERIMENTAL The technique employed for the isotope-dilution determinations was similar to that described elsewhere.4 Several minor modifications were made to the apparatus. These included the use of molybdenum instead of platinum-rhodium suspending wires when crucibles were degassed at temperatures above 1600°C. The circulatory system used previously for converting CO to CO2 was replaced by a single chamber, the walls of which were cooled directly in liquid nitrogen. Temperatures were measured with an optical pyrometer which had been recently calibrated and, as in the previous study, were minimum values obtained by sighting on the center bottom of the crucible. Temperatures obtained by sighting on the interior walls were always higher by 100' to 130°C with the design of crucible employed. Flat-bottomed crucibles exhibited an even larger temperature difference. To check the efficiency with which crucibles were degassed in the isotope-dilution apparatus, several experiments were done in the vacuum-fusion apparatus, suitably modified4 for isotope-dilution studies. Faster pumping speeds and higher degassing temperatures were possible, the latter due to the use of a generator with a higher power output (10 Kva at 398 kc per sec). In these experiments the combustion of CO was omitted and a correction4 was made for the contribution of CO to the ion current at m/e 28, used in determining the isotopic ratio R = l5NP4N. This correction did not seriously influence the re-

Jan 1, 1962

By Louis A. Panek

Tests of mine-roof models in a centrifuge show that the suspension effect due to bolting a horizontally bedded mine roof with frictionless surfaces of contact between beds depends principally on the number of bolted beds and their relative flexural rigidities, provided that sufficient bolt tension is exerted to prevent strata separations at the bolt locations. Strata separations tend to occur in the unbolted roof mainly because the beds have unequal thicknesses. "Suspension effect" refers to the transfer of part of the weight of weaker or thinner beds to the flexurally more rigid beds by roof bolts or by any other means. The factors investigated were number of beds in the bolted unit, bed thickness, modulus of elasticity of beds, length of bolts, spacing of bolts across and along the opening, bolt load, and intensity of roof load. The general principles of behavior of the bolted roof beds are explained by an approximate theory. Model test data are used to validate the theory and to obtain an expression for the "suspension efficiency". As the suspension effect actually observed in the models is smaller than that predicted by the approximate theory, the suspension efficiency in general is less than unity. Mathematical expressions are obtained for (1) the change in roof bending stress due to the suspension effect, which is needed for design of a roof-bolting system, (2) the change of roof deflection due to the suspension effect, which may be useful for evaluating the effectiveness of a roof-bolting system, and (3) the bolt load or pre-load that is required to achieve the desired reinforcing effect.

Jan 1, 1962

By R. O. Dannenberg

This report describes aperiments by the Bureau of Mines and reviews theoretical aspects of the use of organophosphate solvent extraction for recovering beryllium from sulfate leach liquors. The leach liquors were prepared by sulfuric acid leaching of lime-sintered low-tenor beryl flotation concentrates. The experimental work on sulfate leach liquors showed that the acidic esters of organophosphates extracted beryllium slowly but in preference to aluminum. Three common alkylphosphoric acids, di- (2-ethylhexyl) (EHPA), heptadecyl (HDPA), and dodecyl (DDPA), in order of decrmsing selectivity, yielded a partial separation of beryllium from aluminum.

Jan 1, 1962

By George Krauss, M. Cohen

The reverse martensitic transfomzation (i.e., the conversion of martensite to austenite on heating) was investigated in Fe-Ni alloys containing 30.5 to 33.5 wt pct Ni. The reversed austenite was found to be sufficiently distorted to exhibit marked differences in mechanical properties and to undergo recovery and re crystallization on further heating. In particular, the yield strength of the reversed austenite was as much as 2.5 times higher than that of the virgin austenite: with five cycles of the direct and reverse martensitic transformation, the yield strength was 2.6 times higher. There was an accompanying decrease in strain-hardening capacity and in stable ductility or uniform elongation. The recrystallization was observed to follow sigmoidal kinetics, but was characterized by an abnormal1y large temperature dependence which was evidently due to carbon segregation at the migrating grain boundaries. Upon recrystallization, the strength Properties reverted to those of the virgin austenite, but the ductility did not fully recover until the annealing temperature was further raised to dissipate the carbon segregation at the grain boundaries. The transformation of reversed austenite to produce second-generation martensite resulted in an unusually imperfect structure, thereby leaditg to additional strengthening. Horlleuer, the martensitic phase was much less responsive in this respect than was the austenite. MOST martensitic transformations are capable of undergoing a reverse transformation back to the austenitic phase on heating.&apos; This reaction, like the direct transformation to martensite on cooling, is usually athermal. In analogy with the Ms andMf temperatures for the martensitic transformation (where M, > Mf), the reverse transformation is characterized by the As andAf temperatures (where As<Af). It is well-known that the finish (Af) of the martensite-to-austenite reaction on heating may occur at a temperature where austenite is not stable relative to other phases in the equilibrium diagram.&apos; Reverse martensitic transformations have been found to influence the properties of the parent austenitic phase in a number of ferrous alloys. The austenite thus produced after one or more reversals is significantly altered in strength, microstruc-ture, diffusivity, and annealing characteristics compared to well-annealed, virgin austenite. The first detailed observations of such phenomena were made by Wasserman3 on an Fe-30 wt pct alloy. He found that the reversed austenite (i.e., austenite formed by the reverse martensitic transformation) was much stronger than the original austenite, and the second-generation martensite (i.e., martensite produced from the reversed austenite) was somewhat stronger than the first-generation martensite. On heating the reversed austenite, recrystallization occurred in a manner similar to that of a cold-worked metal; the Laue spots sharpened and the strength decreased.4 In recent years, Russian workers have shown considerable interest in these reverse martensitic transformations. Most of such investigations5-10 have been concerned with the stabilization of reversed austenite relative to subsequent martensitic transformation, and because of its unusual nature, this phenomenon will be discussed in detail elsewhere." On the other hand, the annealing behavior of reversed austenite and the attendant variation in properties have received little attention beyond the experiments of Wasserman.3,4 Gridnev eta1.,8 in one of the few such studies. followed the hardness change of reversed austenite as a function of time at three annealing temperatures. The marked strengthening of austenite achieved by the reverse martensitic transformation has been referred to as "transformation strengthening" by Wasserman3,4 and as "phase hardening" by Malyshev et a1.7,9,10 to differentiate it from hardening produced by cold working. Both groups of investigators noted that further strengthening of the austenite could be attained by repeated or cyclic transformations, but the first cycle resulted in the most pronounced effect. Evidence of the altered microstructure of reversed austenite has been reported by Maximova and Nikonorova6 and by Edmonson and KO.12 The former found that reversed austenite was much more sensitive to etching than the original austenite, and the latter authors observed a (&apos;ghost" structure resembling martensite in certain areas of the reversed austenite. Enhancement of the self-diffusion rate in reversed

Jan 1, 1962

By C. J. Bechtoldt, H. C. Vacher

Quenched alloys, prepared by powder metallurgical techniques, were examined by microscopic and X-ray diffraction methods. The compositions and heat treatments were chosen so that the chromium and nickel solvuses could be determined and a range of composition and temperature, in which a eutectoid had been reported, could be explored in small intervals. The results showed no evidence of eutectoid reactions having taken place. ALLOYS containing iron, chromium, molybdenum, and nickel are extensively used in high-temperature applications. In order to provide basic information on the solid-state reactions that occur in such alloys, the National Bureau of Standards is engaged in an extensive study of the equilibrium phases in the binary, ternary, and quaternary systems involving these four metals. Attention was directed to the chromium-nickel system because a review of the literature showed conflicting data. A recent compendium1 of the constitution of binary alloys gives two diagrams for the chromium-nickel system, one a simple eutectic and the second a diagram showing a eutectoid and a eutectic. The eutectoid was the result of an allotropic transformation in a high-temperature solid-solution form of a chromium-rich phase called 0. The approximate temperature and composition of the eutectoid was 1200°C and 30 at. pct Ni. In the preliminary study, at the Bureau, no transformation was indicated in the chromium-rich phase of ternary and quaternary alloys in which chromium and nickel were major components. Similar results have been reported from time to time in the literature,2-8 In consequence of this situation, a systematic study was made of the constitution of heat-treated chromium-nickel alloys using metallographic and X-ray diffraction methods. The compositions of the alloys were selected so as to determine the boundaries of the chromium-rich and the nickel-rich phases and to explore in small intervals the ranges in composition and temperature in which the eutectoid had been reported. The results of this study are reported and discussed in the present paper. EXPERIMENTAL PROCEDURES Materials, Alloys, and Heat Treatments—The alloys were prepared by a powder metallurgy technique similar to that used in earlier work.9 Analyses of the materials used are given in Table I. Powders were mixed using a vibrator in 30-g batches of predetermined composition; 2-g pellets were made from the mixture by compacting at room temperature in a 1/2-in. diam mold under 60,000 lb per sq in. pressure. The pellets were sintered in dry hydrogen for 10 days at 1300°C. At the end of the sintering treatment the specimens were quenched in water, which caused a pale green film to form on the chromium-rich alloys and thin black scale to form on the nickel-rich alloys. The pellets after sintering were approximately 1/2 in. diam by 3/32 in. thick. The purification train9 was modified by inserting a tube of titanium turnings, heated at 700°C to increase the efficiency of the removal of oxgen and nitrogen. It was found in the earlier work that the sintering treatment lowered the carbon, oxygen, and nitrogen contents of chromium-rich alloys to 0.01, 0.01, and 0.004 wt pct, respectively, and that there was a loss of chromium. In order to ascertain the extent of this loss, the chromium contents of certain alloys were determined chemically. They included those alloys used to determine the parameter-composition curves and those of critical composition, used to determine the chromium-solvus microscopically; these analyses were made on samples after the final heat treatments. The mixed powder values for the chromium content of those alloys that were not analyzed were adjusted to conform to a smooth curve based on the chemically analyzed values for

Jan 1, 1962

By Shiou-Chuan Sun

This paper is to be presented at the Annual Meeting of the American Institute of Mining, Metallurgical and Petroleum Engineers, New York, New York, February 18-22, 1962. Permission is hereby given to publish with appropriate acknowledgments, excerpts or summaries not to exceed one-fourth of the entire text of the paper. Permission to print in more extended form subsequent to publication by the Institute must be obtained from the Secretary of the Institute. If and when this paper is published by the Institute, it may embody certain changes made by agreement between the Technical Publications Committee and the author, so that the form in which it appears here is not necessarily that in which it may be published later.

Jan 1, 1962

By M. J. Ginsberg, N. A. Gokcen

THE preliminary study of electrochemical desul-furization performed by Ohtani and Gokcen1 left a number of points concerning the process to be investigated. Two of these were i) the determination of the effect of greater current and voltage on the desulfurizing Flower of acid slags (% CaO/% SiO2- 1) and ii) the possibility of the loss of silica in slag by the reactions 2C (in metal) + SiO2 (slag) = Si (in metal) + 2CO(g) and C + SiO2 (in slag) = SiO(g) + cO(g) proceeding to a point at which the composition of the slag was sufficiently altered toward the basic side so a1.s to noticeably affect the rate of de-sulfurization. The apparatus and the procedure used in the present investigation were the same as those used by Ohtani and Gokcen, except the control circuit was connected to 120 v dc instead of 24 v dc and thereby allowed greater freedom in choosing the values of both current and voltage. The graphite crucible containing the melt and serving as the cathode was 3-in. high, and was of 1 1/2-in. ID with a graphite bar of 3/8-in. diam and 8-in. length threaded into the bottom for electrical connection. This was placed into a magnesja outer crucible with a hole in the bottom and alumina insulation was packed between the two crucibles. A charge consisting of 180 g of

Jan 1, 1962

By J. R. Ross

A reconnaissance for sources of scandium and a metallurgical investigation of recovery methods for byproduct scandium from uranium mill solutions were conducted by the Bureau of Mines. The work on scandium was undertaken to obtain information on domestic resources and to explore and develop recovery procedures in consonance with the Bureau&apos;s long-range program for conservation and wise utilization of mineral resources. The element scandium is widely distributed in the earth&apos;s crust in trace amounts, but it seldom occurs as an important constituent in any mineral. An exception is thortveitite, (Sc,Y)2 Si207) a rare mineral that contains various amounts of scandium and yttrium and may contain up to 42 percent scandium oxide (SC203). Knowledge of the chemistry of scandium has expanded rapidly in recent years (1, 4, 9)4 but only fragmentary information is available about the metal because it is still largely a laboratory curiosity without established uses (2, 3). A recent study shows some of the physical proper-ties of the metal are (1) density of 3.05 grams per cubic centimeter) (2) melting point of 1,540° C, (3) hexagonal close-packed structure) (4) hardness of about 50 Brinell (500-kilogram load), and (5) an alloy behavior similar to yttrium and rare-earth metals (2). The price of $2,850 a pound for scandium oxide of 99.9 percent purity and $2,700 a pound for oxide of 99 percent purity reflects the scarcity and complex chemistry of the element.

Jan 1, 1962

By M. A. Klugman

[This paper represents a portion of a lager study, concerning dispersion patterns of major, minor and trace elements in wall-rock about ore-bodies in part of the Colorado Mineral Belt. This phase of the work pertains to the Mg/Ca ratio variations in wall-rock adjacent to ore-bodies in two mines of the Alma-Horseshoe Mining District of Central Colorado. The mining district is located 80 miles southwest of Denver (Figure 1) on the east flank of the Mosquito Range. The area is typified by rugged relief with altitudes from 10,500 to 14,000 feet.]

Jan 1, 1962