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By Nicholas J. Grant

It is the purpose of this paper to examine a number of the recent developments in powder metallurgy, being most concerned with those which are yet to prove themselves rather than those which have achieved commercial maturity. Such developments include the production of very much coarser and very much finer powders, down to the near-micron size range. Also considered are activated sintering, direct powder rolling and extrusion (both hot and cold), brazing and welding, hydrides of reactive metals, oxide dispersion strengthened alloys and theoretical evaluations. Introduction T HERE surely can't be very much argument with the fact that powder metallurgy has made large advances on many fronts during the past ten or more years (1). These advances have taken place in raw materials, in processing, in product development and in a better understanding of many of the phenomena which occur in the various steps involved in powder metallurgy. It should be clear, in view of such growth, that it will not be possible to highlight all of the new developments in the present paper. Many of these developments,

Jan 1, 1965

By I. Iwasaki

The interaction of starch and calcium ions in soap flotation of activated silica from iron ores was investigated using the response surface method. The results were correlated with adsorption studies and into pilot plant tests. It was reported previously1,2 that in soap flotation of activated silica from iron ores there existed an optimum combination of the amounts of starch and calcium chloride addition, and that corn starch as a depressant for iron oxides became effective when a critical amount of starch was added, beyond which excess starch appeared in measurable quantities in the aqueous phase. Further, adsorption studies2,3 with various starch products on hematite or quartz showed that the adsorption of starch at a given pH was markedly enhanced by the presence of calcium ion in solution. From these observations it becomes of interest to investigate the interaction of starch and calcium added to the ore pulp, and their influence on the selectivity of flotation separations. This paper describes an empirical relation between such dependent variables as the grade and recovery of iron in the concentrate and the residual concentrations of starch and calcium ion in solution as a function of two independent variables, namely the amounts of starch and calcium chloride addition, as determined by using the general technique of response surface methodology. The results thus obtained are correlated with the adsorption studies on hematite and quartz, and with a typical pilot plant operation. MATERIALS AND METHODS The ore sample used in the batch flotation studies was the fine fraction of a Mesabi gravity concentrate produced by pilot plant grinding and classification. The sample analyzed 55.21% iron and 14.70% insol, and consisted of 85.81% minus 325 mesh (corresponding to Ore C). 2

Jan 1, 1965

By R. C. Gifkins

R. C. Gifkins (CSIRO)—In this paper evidence is put forward to support the idea of grain boundary shearing in aluminum at 4.2°K and the phenomenon is explained in terms of a low-temperature "equicohesive temperature". It is stated that these findings show that grain boundary shear cannot be ruled out in any situation by temperature arguments alone. We believe, from our own recent study of "apparent grain boundary sliding'' at temperatures below 0.45 Tm, that it can be ruled out on temperature arguments alone.45 Our experiments were made principally with magnesium and a Ms-A1 alloy ("Magnox A12"). Careful examination of offsets of marker lines or steps at grain boundaries produced by deformation at room temperature (-0.3 Tm) showed many of these to result from curvature over narrow zones along the grain boundaries. A significant residuum did, however, appear as a sharp offset or step. It was found that the mean value of this step rose to a small value during the first 0.5 to 1 pct strain and then remained at this level with further strain. Moreover, exactly the same values were obtained (at the same stress) at 75°C instead of 21°C. That is, in this range of temperature the "apparent sliding" was not temperature-sensitive. At 125°C and above there was sliding which increased with strain and which was temperature-dependent. When this temperature-dependent sliding was used to calculate the sliding to be expected at room temperature, this underestimated the "apparent sliding" by a factor of 104. The conclusion drawn is that the "apparent sliding" consists of shear localized in a zone of a width measured perhaps in microns, whereas it seems that true sliding occurs on the boundary surface.46 A model for such localized shear has been developed in general terms, following a similar model of Urie and Wain.47 Other strong evidence for low-temper- ature sliding has been based on the offsets of marker lines consisting of a substructure seen using the electron microscope to resolve these.48 We have repeated this work and found that the effects can be accounted for in terms of cracks in an oxide film which is produced when the substructure is etched up; these cracks form over zones of shear rather than at actual interfaces. However, in aluminum at room temperature (-0.3 Tm) there is no "apparent sliding" which is optically detectable. We suggest that, when the temperature is much lower (and possibly the rate of strain higher, too), as in the experiments of Chin et al., then aluminum behaves like magnesium at room temperature, and a narrow zone of shear develops to accommodate differences in strain across the grain boundary. Such a zone could well give rise to triple-point cracks. It is hoped to investigate these suggestions further. B. Y. Chin, W. F. Hosford, Jr., and W. A. Backofen (authors' reply)—It is interesting to have Dr. Gif-kin's comments, although it is somewhat difficult to reply in detail without the reference containing the work that he describes. Apparently though, he does find a low-temperature temperature-independent sliding that would seem to be related to the observations reported here. Perhaps some of the difficulty has semantic origins, growing out of the distinction between ('true sliding" and "apparent sliding".

Jan 1, 1965

By D. J. Pye

Certain high molecular weight synthetic polymers in very dilute solutions decrease water mobility in porous media 5 to 20 times more than would be expected from the solution viscosity. This indicates that increasing water viscosity to reduce adverse mobility ratios in water floods is economically feasible in many situations. Laboratory results are consistent with accepted theory with respect to improved areal sweep, permeability distribution and displacement efficiencies as would be predicted from the solution mobility measured in the core. The laboratory results have been confirmed by field pilot floods which recovered 80 per cent and 100 per cent more oil than comparative water-flood pilots in fields containing 16 cp and 130 cp oil respectively. Economic analyses based on pilot data indicate the method to be profitable. INTRODUCTION The desirability of improving the water-oil mobility ratio in waterflood-ing operations has long been appreciated, especially for high viscosity crudes. Methods of reducing the oil viscosity by application of heat, gas resaturation and miscible drives have met with some success. Conversely, it has been generally conceded that increasing the water viscosity would also be effective, but the amount of thickening agent required to effect an appreciable increase in viscosity is discouragingly high. The use of such materials as glycerin, sugar, or glycols is completely out of the question economically, so that considerable attention has been given to the use of the much more efficient synthetic water-soluble polymers as viscosity improvers; but even these materials are not economically attractive. If increased water viscosity could be economically realized, marked improvements in areal sweep efficiency, as discussed by Caudle and Wittel and others, would be realized in field operations. Similarly, the improved mobility ratio would bring about increased recoveries by correcting permeability distribution problems as discussed by Stiles2 and Dykstra and Parsons,' and improvements in displacement efficiency would be obtained as recognized by Buckley and Leverett4 and Welge.5 LABORATORY STUDIES THE RESISTANCE EFFECT In the course of research to develop a more efficient water-soluble polymer viscosity builder, we discovered that a very few types of water-soluble polymers exhibited a most unusual and very interesting property not previously observed. Among the earliest materials showing such activity were polymers containing acry-lamide. Fig. 1 shows a typical plot of the solution viscosity vs concentration for one of these polymer solutions as determined in an Ostwald viscometer. As usual, such a plot is an approximate straight line on semi-logarithmic paper. Now, an inspection of Darcy's law, shows that a viscosity value can also be determined in a formation sample if the pressure, flow rate and permeability are known. If the core permeability is previously determined with wa- ter or brine, then the viscosity of another aqueous fluid may be determined from the equation. The viscosities so determined for glycerin (glycol or polyvinyl alcohol solutions, for example) agree with the viscometer determinations. However, in the case of the water-soluble polymer solutions in which we are interested, the viscosities measured in the formation sample depart very markedly from the viscometer values. A typical relationship for a polymer solution is also shown in Fig. 1. This unusual departure from the expected response is referred to as a resistance property of the polymer and is quantified as "resistance factor". Since the resistance factor R can best be determined in a core under study, the term has been defined on the basis of the ratio of the brine mobility to the polymer solution mobility at residual oil saturation so that:

Jan 1, 1965

By Jr. Oitto

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

Jan 1, 1965

By R. V. Lundquist

The specific conductance of solutions of sodium hydroxide and of sodium aluminate was directly proportional to the temperature. The specific conductance of sodium aluminate solutions with identical sodium ion concentration and at constant temperature decreased with increase in aluminum concentration. The aluminate ion population in solution was shown to consist of a mixture of monovalent and polyvalent ions. Aluminate ions did not influence the temperature dependence of pH in caustic solutions containing sodium aluminate. The density and viscosity of a solution was inversely proportional to the temperature and directly proportional to the concentrations of sodium and aluminate ions.

Jan 1, 1965

By J. R. Johanson

With the continuing development of automatic operations, it is important that reliable discharge rates through hoppers and bins be obtained for bulk solids. In most applications a feeder is used to control the feed rate. The selection of this feeder size is usually based on the rated ability of the feeder to move material without regard to the capability of the material to flow through the opening in the hopper onto the feeder. The dis charge rate through a given hopper opening may vary from zero to a theoretical maximum depending on the flow properties of the material. This paper presents an equation for the maximum discharge rate for a bulk material as a function of the hopper shape, the opening size and the flow properties of the material. Discharge-rate tests on various materials indicate good agreement with calculated values for opening sizes from a fraction of an inch to several feet. As part of a program to develop improved design criteria for bulk storage and handling facilities, a specific study of the methods involved in calculating the rate of discharge of bulk solids from hoppers and bins has been made. This study is closely related to earlier work done on the prevention of flow problems through the choice of proper design geometry of hoppers and bins1. The present paper is an extension of this earlier work, and therefore many of the concepts previously derived and explained will be used without explanation. Two types of flow will be considered: plane-strain flow in a wedge-shaped hopper and axial-symmetry flow in a conical hopper. The literature contains many studies on discharge rate for regular-shaped dry particles2*3 such as glass beads, lead shot and coarse dry sand. However, the work is empirical in nature, and it is difficult to extrapolate the given information to apply to moist, sticky materials typical of many industries. Some studies4 have shown a decrease in discharge rate with an increased moisture content of the material. However, no attempt was made to correlate the discharge rate with moisture. The method of calculating discharge rate presented in this paper was derived analytically from the basic knowledge of the flow of frictional, cohesive, granular solids, The equation includes the effect of material cohesion (stickiness), hopper configuration, opening size and bulk density of the material. THEORETICAL WORK The basic assumptions made in deriving the discharge rate equation are as follows: 1) The material is a frictional, cohesive, granular solid. 2) The flow is considered continuous and without significant density change. 3) The material at the hopper opening forms a continuously failing arch that is in dynamic equilibrium. 4) The strength of the material in the arch, which must be overcome for the arch to fail, is caused by the pressure in the flowing mass near the hopper opening. 5) This pressure at the hopper opening can be calculated5. If we consider the dynamic equilibrium of an arch of uniform thickness such as that shown in Fig. 1,

Jan 1, 1965

By Robin O. Williams

Robin 0. Williams (Oak Ridge National Laboratory)— The authors have questioned the degree to which the coherency strains between the iron-rich and chromium-rich phases are isotropic as proposed in Ref. 5 on the basis of the difference between the elastic properties of the two phases. The relative magnitude of the stresses is determined by the moduli as shown by Eqs. [2], [3], and [4] of Ref. 34. However, the moduli of the two phases have no direct bearing on the uniformity of either the stress or strain within either phase. The idea that the strains are isotropic within each phase (but normally of different magnitude and always of different sign) is based entirely upon the experimental observation that X-ray line broadening has not been detected even when the particles become rather large. It has not proven possible to grow the particles sufficiently large that they lose coherency. Based upon this lack of line broadening one can estimate an upper limit for the nonuniformity of the strains within each phase as follows. It is considered possible to detect line broadening if it is as great as 10 pct of the separation of the K, doublet for the (211) line using chromium radiation. The doublet separation would correspond to a total strain of 0.0017 such that the total variation of lattice parameter relative to the average lattice is now k0.05x0.0017 or something less than ± * For the present case the strain in each phase is roughly 0.002 such that the variation of strain within a phase will not exceed 5 pct. It is stated that the expression derived for strengthening for the hydrostatic straining as observed in this system would substantially overestimate the magnitude due to dislocation flexure. This is contrary to the conclusion reached in the original paper34 for the present range of particle sizes. What is the lowest temperature at which a has been observed to form in this alloy? M. J. Marcinkowski, R. M. Fisher, and A. Szirmae (nutlzors' reply)— -Williams' arguments based on X-ray findings for a chromium-rich precipitate and an iron-rich matrix strained to a common lattice parameter are certainly convincing. This being the case, there are no shear components of strain associated with the precipitate-matrix aggregate to interact with the shear components of the dislocation stress fields, contrary to the opinion expressed by the present authors. On the other hand, the present authors, in spite of this error, did not expect the shear interactions to be significant. The chief objection to Williams' model in the present case is that the various segments of the dislocation line are assumed to pass from one potential valley to the next independently of neighboring segments. This is only true for a highly flexible dislocation line, i.e., one whose radius of curvature is something less than the center to center distance between precipitate particles which amounts to about 90A in the present alloy. In order to maintain this curvature, an externally applied shear stress of at least 230,000 lb per sq in. would be required or about four times the observed stress. It is therefore concluded that the dislocation lines move rather rigidly through the lattice. This being the case, the forces on the dislocation resulting from the hydrostatic interaction between the stress fields of the edge-dislocation components and the precipitate particles should average out to zero; that is particles above the below the slip plane produce forces on the dislocation of opposite sign and therefore will cancel when averaged over the entire length of the dislocation. On the other hand, since the dislocation is not perfectly rigid, Williams' model may lead to some strengthening, but far less than that predicted. A second and equally serious objective to using Williams' strengthening model for the present alloys is that profuse wavy slip due to the motion of screw dislocations played a predominant role not only in the unaged alloys but in the fully aged ones as well. Since the screw dislocation has associated with it only shear components of stress the hydrostatic strengthening model no longer applies. In view of these arguments the present authors must reject Williams' model of strengthening as being pertinent to the present alloy system. The present authors have made no detailed study of the lowest temperature at which a forms in the quenched ferritic alloys. None was ever observed n the alloys aged at 500°C so that forma-tion must occur at temperatures higher than this and was therefore not a factor in the present study.

Jan 1, 1965

By T. P. Papazoglou, N. A. D. Parlee, W. C. Phelps

PRACTICAL designs for good "home made" molybdenum furnaces are hard to find in the literature. The one described briefly below left something to be desired but was good enough to operate as a rather long (30 in.) two-zone furnace for periods of over 2 months at temperature (1400° to 1600°C) without shutdown. The principal problem in our application was to establish a temperature profile with two distinct constant-temperature zones and no dip between the zones. This and other problems mentioned below would not arise, however, if both zones were operated at the same temperature and if a shorter furnace were acceptable. Since molybdenum windings oxidize very rapidly when heated in air, impervious refractory tubes were used for both the furnace core and the outer jacket tube shown in the accompanying figures. A protective atmosphere of forming gas (10 pct H2, 90 pct N2) was continuously passed through the gas-tight annular volume between the core and outer jacket. The water-cooled copper ends shown in Figs. 1 to 3 sealed the ends of the tubes. Annealed molybdenum wire (40 mil) was wound on the recrys-tallized alumina core (35.5 mm OD by 28.5 mm ID by 30 in.) at a spacing of 0.36 in. The spacing was reduced to 0.29 in. close to the ends to partially compensate for end heat losses. Fig. 2 shows two molybdenum-ground lead taps off the center of the winding to produce the two independect temperature zones. The ground lead was insulated with 1/4-in. alumina tubing and connected to the grounded copper end by passing the wires through the gas port tube and crimping each wire into notches cut at the mouth. To prevent sagging of the core at high temperatures, refractory "troughs" were cut from alumina and mullite tubing to cradle the core. The support "troughs" which were 6 in. long and located about 5 in. from each end of the annular volume also served as radiation shields. In view of the different expansion coefficients and operating temperatures of the core and outer jacket (3.5 in. OD by 3 in. ID by 30 in.), the ends of the tubes were smoothed and squared to produce good sealing surfaces, and the core was ground 1/32 in. shorter than the outer tube. The power terminals were passed through their respective conductor ports which were internally lined with alumina tubing and sealed with Armstrong adhesive A-6 leaving about 1 in. of protruding lead wire for external connections. (Adhesive A-6 is a two-component system consisting of an epoxy-type resin with a mineral fibrous filler and an amine catalyst.) Figs. 1 and 3 show the entire assembly of concentric refractory tubes, copper ends, and sealing o rings, held together with two brass flanges and 3/8-in. bolts with heavy springs for dimensional flexibility. The furnace shell (19 by 19 by 30 in.) consisted of a steel frame with sheets of transite forming a box. The copper ends protruded through two 3.75-in. circular holes cut at the center of each transite square end. Thermal insulation next to the transite exterior was effected by K-23 B&W bricks alld in a central volume of approximately 9 by 9 by 30 in. a row of K-30 bricks was lined up to support the hot assembly. The rest of the volume around the outer

Jan 1, 1965

By T. S. Lundy, F. R. Winslow

DIFFUSION coefficients of Hf181 in the high-tem-perature bcc phase of reactor-grade hafnium were determined at temperatures of 1795° to 1995°C by standard lathe-sectioning techniques. The temperature dependence of the data may be described by an Arrhenius-type expression for this limited temperature interval. However, hafnium is classed with the "anomalous" bcc metals zirconium, titanium, and y uranium by the low values of Do and Q observed in this study. The hafnium metal was received as 1/2-in.-diameter crystal bar. Analyses by the Analytical Chemistry Division of Oak Ridge National Laboratory showed the major impurity to be zirconium— about 2.1 pct. The total interstitial content was about 225 ppm with 190 ppm of this oxygen. The Hf"' was supplied as HfC12 in HC1 solution by the Isotopes Division of Oak Ridge National Laboratory. The hafnium bar was cut into disk-shaped specimens 3/8 in. long. One of the flat faces of each specimen was metallographically treated and then the isotope was deposited by vacuum evaporation from a tungsten filament. A 3 by 3 in. NaI (Tl) crystal with a single-channel analyzer was used for counting y rays with energies of 0.3 to 0.7 Mev. The as-deposited layers of isotope had counting rates of about 200 counts per sec. Specimens were annealed in argon in a tantalum resistance furnace. Temperatures were measured with a microoptical pyrometer calibrated for the particular furnace sighting conditions. All sectioning was done by standard lathe techniques. Section weights were determined on a semimicrobalance. A density of 12.5 g per cu cm was used in determinations of section thicknesses. Activities associated with the various sections were measured and the penetration data were treated using the computer code by winslow.' In all cases, except for specimens annealed at temperatures below 1795°C, normal Gaussian penetration behavior resulted. At lower temperatures, plots of In A(x) vs x2 were nonlinear [~(x) = relative activity at a distance x from the

Jan 1, 1965

By C. R. Johnson, R. A. Greenkorn, L. K. Shallenbarger

This paper describes a study, based on core data, of the directional permeability of a sandstone reservoir. Directional air permeabilities are explained and correlated with lithology by the tensor theory of permeability, which is extended to the more general case of heterogeneous anisotzopic porous media. In this case, the permeability tensor is made up of two components: (I) anisotropy (variation around a point) which correlates with bedding, and (21 heterogeneity (variation from point-to-point) which correlates with grain size. INTRODUCTION Previous studies of directional permeabilityl.5-8 have concerned themselves only with anisotropy at a point, rather than with both point-to-point differences and local anisotropies. In this paper, we present the existing tensor theory of permeability for anisotropic porous media and then extend it to the more general case of heterogeneous anisotropic porous media. The laboratory measurements of directional permeability are explained in view of this extended theory and the data are discussed in terms of the lithologic factors that correlate with it. The results show what the heterogeneity and anisotropy of the reservoir element are, and that the directional permeability correlates with lithology. Data used in this paper are measurements of air permeability in eight directions, spaced at 45° intervals, on 142 2-in. vertical plugs from 30 cores. The core data are meaningful in terms of directional permeability because the cores were oriented to within 45O during drilling and coring.3 Although we initially thought that only 60 per cent of the core material was reliable, subsequent study showed that almost all of it was reliably oriented. After determining the air permeabilities, the data were reduced to three independent variables for each plug: the major and minor permeability axes, and the direction of the major axis. These were obtained by converting the permeability data to the reciprocal square root of permeability and fitting the transformed data with ellipses according to the tensor theory of permeability.8 The point-to-point areal variation of the minimum permeability axis is related to grain size. The direction of the permeability axes, where the major axis exceeds the minor axis by at least 5 per cent (measured variation is about 4 per cent), correlates with the bedding. The permeability tensor used in this study must be considered as the sum of a scalar and a tensor, with the scalar being the minor axis permeability as a function of position, and the tensor the directional effect, which is additive permeability over the minor axis. In this case, the point-to-point variation or heterogeneity (minor axis) is substantially larger than the variation at a point or anisotropy. It may be important that this separation of "directional permeabilities" be recognized when considering migration of fluids due to permeability variation. Local migration may be due to anisotropy and point-to-point migration may be due to heterogeneity, but the direction and magnitude of these may not be the same. Furthermore, in truly heterogeneous systems, one would expect that anisotropy would be the smaller of the two effects. THEORY TENSOR THEORY OF PERMEABILITY FOR ANISOTROPIC POROUS MEDIA8 Darcy's law for flow in porous media in its usual form is where qis the flow rate vector, k is the permeability, is the viscosity, is the vector differential operator, and P is the Pressure. Consider flow, q, through a unit area in the direction of the unit vector n from elementary flow tubes parallel

Jan 1, 1965

By W. V. Green

Creep of tantalum was measured at temperatures from 0.6 to 0.89 of the absolute melting temperature. The creep curves include first, second, and third stages. Steady-state creep rate depends on the fourth power of stress. The activation energy for creep throughout this temperature range is approximately 114 kcal per mole, measured by the aT technique. Subgrain formation occurs as a result of creep strain, and pile-up dislocation arrays are observed in etch-pit patterns. BECAUSE of its high melting point-which is exceeded only by those of rhenium and tungsten—and its high room-temperature ductility compared to most of the other high-melting-point metals, tantalum will undoubtedly be utilized in an increasing number of high-temperature applications. Alloying studies directed toward increased high-temperature strength must use data on tantalum itself as a base line in order to evaluate the effectiveness of the alloying additions. However, to date, no systematic study of creep of tantalum at temperatures above one-half of its melting point has been reported in the literature. Conway, Salyards, McCullough, and Flagella1 have measured linear creep rate of tantalum sheet as a function of stress, but at only one temperature, 2600°C. This paper describes a relatively thorough study of the high-temperature creep of tantalum. METHOD Material Tested. The commercially supplied, l/2-innch-diameter tantalum rod used for this work was electron-beam-melted, cold-forged, rolled, swaged, cleaned chemically, and vacuum-annealed for 1 hr at 1000°C, all by its manufacturer. The vendor's analysis included 60 to 170 ppm C, 3.4 to 4.2 ppm H, 60 to 80 ppm 0, 15 ppm N, and a hardness ranging from 66 to 81 Bhn and averaging 76 Bhn. Creep eimens Used. Two creep-tested specimens are shown in Fig. 1. The 1/4 in.-diameter gage section was 3/4 to 1 in. long, and terminated either at shoulders 5 mils high or at 20-mil-diameter tantalum wires spot-welded to the circumference of the gage section. Both kinds of shoulders served equally well as fiducial marks for optical strain measurements. The spot welding did not alter the creep behavior in any detectable way; the 5-mil- high sharp shoulders did not result in any detectable localized effect on the strain. Before testing, each tensile bar was first mechanically polished -id then electrochemically polished according to the method referred to by Forgeng2 as the "Thompson Ramo Woolridge" method, which was suitable for tantalum after small adjustments of technique were made. Two tensile bars tested at low stresses had 1/8-in.-diameter gage sections and utilized only the weight of the bottom grip for the applied load. Although these diameters were smaller than were desired for other reasons, applied loads were known with high precision in the tests in which they were used. Testing Procedure. Two different constant-load creep-testing machines were employed, one of which has been described by Smith, Olson, and Brown.3 In both, the tensile bar is held vertically on the axis of a cylindrical tungsten tube or screen heater by threaded tungsten grips. The tensile bars and associated grips are heated by radiation from the incandescent heaters, which are heated by their own electrical resistance. Both testing machines use pins to hold the bottom grips in place. The load is applied to a tensile bar through hanging weights, a constant force-multiplication lever, a pull rod sealed to the chamber lid, and a top grip threaded to the pull rod at one end and to the tensile bar at the other. In one machine, the vacuum seal is a bellows with a low spring constant; in the other, the seal involves a rotating "0 ring". With the latter, rotation is converted to translation with a crank shaft, so that elongation of the tensile bar is accommodated with no change of tensile load. The incandescent tensile bar is viewed by an external optical system through slots in the radiation shields and heater, and an enlarged image is projected on a ground-glass screen. Gage-length measurements are made on this image with cathetometers on traveling microscopes. With regard to creep-test results, the two machines were identical. Thorium oxide coatings were applied to the threaded ends of the tensile bars, to prevent diffusion welding of the tensile bars to the grips during testing. Specimen temperatures were measured with an L. & N. optical pyrometer which had been calibrated against a standard carbon arc, and were corrected fir window absorption by calculation from the measured spectral transmittance of the quartz observation windows. Longitudinal temperature gradients in the tensile-bar gage length and temperature drifts during testing were detectable but small, and were estimated to be 10°C or less. Accuracy of temperature measurement was confirmed by comparing the temperature measured on the surface of a special

Jan 1, 1965

By T. S. Lovering

Jan 1, 1965

By Thomas P. Meloy

There is much interest in the automation of entire comminution circuits, At the present technological level it is possible to automate a circuit but to date it has not been done, To successfully automate a circuit, a number of problems must be solved. Not all of them are engineering problems. The purpose of this paper is to discuss some of these problems, as certain the implications of these problems and indicate solutions to them. In this paper the term "automation" is used loosely but in the popular sense. Namely, that a plant is automated if a computer is used to control the basic flow of the materials as well as setting the critical parameters in the process. Specifically, the discussion will concern itself with the control of comminution circuits from the dumping of the ore into the primary crusher until the final interface between the comminution circuit and say, the flotation mill in the case of a sulfide ore.

Jan 1, 1965

By H. Biloni, B. Chalmers

Metallographic studies of the segregation of solute in and near the surfaces of chill-cast alloys have shown that, under sufficiently severe conditions, nucleation on the cold mold surface is followed by the formation of a disc of solid of the same composition as the liquid. This disc is surrounded by two concentric rings in which the concentration first decreases and then increases. The discs and rings are surrounded by a region in which arms of low solute concentration separate regions of high concentration. These arms start at the periphery of the outer ring and are initially radial; they make a gradual curved transition from the radial direction to a crystallographic direction. A normal dendritic substrcture is established beyond the position at which the arms have become crystallographically aligned. When the cooling is less severe, the disc becomes less irregular in shape and has a concentration minimum at the center. The term "Predendritic" is proposed for these transitions. A qualitative explanation is outlined for the phenomena observed at the surface and in the equiaxed region of the ingots. It is well-established1-' that the normal mode of solidification for alloys under most conditions is dendritic. A characteristic of dendritic solidification is the growth of rods or plates in specific crys-tallographic directions. The remaining liquid solidifies later, usually with a higher concentration of solute than the original liquid. Very little is known, however, about the transition from a crystal nucleus until the dendritic pattern is established. It is clear that there must be a transition because the nucleus is much smaller than the characteristic spacings found in the "steady-state" structure. And it also seems clear that the initial conditions must be important since the undercooling existing during the nucleation of the grains has a remarkable influence upon the grain size4 and the segregation pattern. The present paper reports a study of the micro-segregation in regions where crystals have nucleated, and the conclusions that can be drawn regarding the early stages of growth, in connection with the details of the solidification process. Aluminum of 99.993 purity, A1-Cu alloys containing 0.5 to 20 wt pct Cu, and Pb-Sn alloys with 5 wt pct Sn were cast and examined metallographically at the as-cast surface, close to the surface, and in the interior after casting. The alloys were cast from controlled temperatures against surfaces at different temperatures ranging from room temperature to approximately the liquidus temperature of the alloy. The surfaces were, in various experiments, graphite, stainless steel, copper, and aluminum. The methods used for metallographic examination were as follows. 1) The Nomarski phase contrast interferometer6 was used to obtain information on the topography of the as-cast surface. 2) The distribution of any solute present in A1 99.993 pct and copper in the A1-Cu alloys was studied by the anodic film technique originated by Lacombe and Mouflard7 and previously applied in the study of the solidification of aluminum by Biloni.8 The electropolished surface of the specimen is anodized under controlled conditions so that the thickness of the oxide film and therefore the interference colors under white light are sensitive to the local composition. This technique was applied to the as-cast surfaces and to metallographically prepared surfaces from the interior. 3) If in Al-Cu alloys, the surface is anodically oxidized for several minutes, instead of seconds as in the color-film technique, the copper segregation is outlined by a different level with respect to the matrix. This method is less sensitive but complementary to that for the color films. 4) The distribution of copper revealed and mapped by the metallographic techniques was confirmed by electron probe. 5) In samples with high concentration of copper, evidence for the copper distribution could be seen optically after electropolishing.

Jan 1, 1965

By F. X. Tartaron

This report describes work done by the Bureau of Mines to simplify the design and operation of the vortex cone, a new device for prerefining blast furnace iron. Three new apparatus arrangements were tested. Results with one of these arrangements average 74.2 pct silicon removal and 61 pet oxygen efficiency (disregarding removal of carbon and manganese).

Jan 1, 1965

By C. K. Eilerts

Finite difference equations were programmed and used to integrate the second-order, second-degree, partial differential equation with variable coefficients that represents the transient linear flow of gas-condensate fluids. Effect was given to the change with pressure of the compressibility factor, the viscosity, and the effective permeability and to change of the absolute permeability with distance. Integrations used as illustrations include recovery of fluid from a reservoir at a constant production rate followed by recovery at a declining rate calculated to maintain a constant pressure at the producing boundary. The time required to attain such a limiting pressure and the fraction of the reserve recovered in that time vary markedly with properties of the fluid represented by the coefficients. Fluid also is returned to the reservoir at a constant rate, until initial formation pressure is attained at the input boundary, and then at a calculated rate that will maintain but not exceed the limiting pressure. The computing programs were used to calculate the results that would be obtained in a series of back-pressure tests made at selected intervals of reservoir depletion. If effect is given to the variations in properties of the fluid that actually occur, then a series of back- pressure curves — one for each stage of reserve depletion — is required to indicate open-flow capacity and related flow characteristics dependably. The isochronal performnce method for determining flow characteristics of a well was simulated by computation. INTRODUCTION The back-pressure test procedurel is based on a derivation of the equation for steady-state radial flow of a gas, the properties of which are of necessity assumed to remain unchanged in applying the test results. The properties of most natural gases being recovered from reservoirs change as the reserve is depleted and pressures decline, and the results of an early back-pressure test may not be dependable for estimating the future delivery capacity of a well. The compressibility factor of a fluid under an initial pressure of 10,000 psia can change 45 per cent and the viscosity can change 70 per cent during the productive life of the reservoir. There are indications that the effective permeability to the flowing fluid can become 50 per cent of the original absolute permeability before enough liquid collects in the structure about a well as pressure declines to permit flow of liquid into the well. The advent of programmed electronic computing made practicable the integration of nonlinear, second-order, partial differentia1 equations2.3 pertaining to flow in reservoirs. Aronofsky and Porter4 represented the compressibility factor and the viscosity by a linear relationship, and integrated the equation for radial flow of gas for pressures up to 1,200 psi. Bruce, Peaceman, Rachford and Rice5 integrated the partial differential equations for both linear and radial unsteady-state flow of ideal gas in porous media. Their published results were a substantial guide in this study of integration of the partial differential equation of linear flow with coefficients of the equation variable. The computing program was developed to treat effective permeability as being both distance-dependent and pressure-dependent. In this study all examples of effective permeability are assumptions designed primarily to aid in developing programs for giving effect to this and other variable coefficients. The accumulation of data for expressing the pressure dependency of the effective permeability is the objective of a concurrent investigation. FUNDAMENTAL DIFFERENTIAL EQUATIONS DIFFERENTIAL EQUATION OF FLOW Linear transient fluid flow is represented by the partial differential equation,

Jan 1, 1965

By H. W. Winkler, Discussion, V. L. Forsyth

The development of a new gar lift valve has removed many of the obstacles limiting over-all gas lift efficiency. The valve is pressure charged in place in a well, and operating pressure can be changed without pulling. Temperature and gas gradient compensation have been eliminated. Intermitting and constant flow installations, using conventional pressure-charged valves, are compared with designs incorporating the new automatic stabilizer controlled valve. Specific well performance data are presented. The means of obtaining and controlling multiple-point injection of gas are explained and contrasted with single point injection. The effect on small diameter strings and multiple string installations is discussed. The effect of flowing temperature gradient on a design using conventional pressure-charged valves, the limitations imposed by such temperature, and the obvious benefits which result from the use of automatic stabilizer controlled valves are shown. Reduction of gas requirements is stated mathematically and demonstrated with specific examples which are identified as to oil company and well. Increased fluid recovery resulting from greater drawdown is illustrated. The economic advantages are mentioned with emphasis on reduction of capital expenditures, as well as reduction in operating expenses. INTRODUCTION Much of the engineering and research work performed with gas lift has been based upon the supposition that under producing conditions gas would be injected at a single point in a well. Many tests were performed in determining the optimum size of the opening through which gas would be passed and the exact placement of the valve equipment. The objectives in a gas lift installation are to unload the well and to efficiently produce the well after it is unloaded. Until recently, the function of upper valves was simply to unload the well. An operating valve located at a proper place in a well served as a single injection point for lifting liquid to the surface. The basic problem in using such equipment is to arrive at operating depth with sufficient operating pressure to efficiently lift the liquid. Few gas lift installations are designed with all required well data available. However, regardless of the quality and availability of data, and regardless of the accuracy of the design, there is the practical problem of preparing and placing gas lift equipment in the well in exact accordance with the plans and intentions of the engineer. In recognition of these and many other problems, attention was directed toward a means of removing the need for temperature and gas gradient compensation, a way to change the gas lift installation to meet the changing requirements of the well itself, and a manner of compensating for changes in oil-water content, fluid volumes, PI, and bottom-hole pressure resulting from flood or repres-suring activity. A device which could actually set and change the operating pressure of gas lift valves in the well would meet most of these needs. There now exists a new gas lift valve which fulfills the original objectives and in so doing actually accomplishes much more. With this device, called an Automatic Stabilizer Controlled valve, there is an exact matching of valve operating pressure and well conditions. Gas is injected at more than one point in the well, thereby making controlled multiple-point injection of gas a reality. Installation calculations are materially simplified and the need for basic temperature and gas gradient data no longer exists. Section I—The Automatic Stabilizer Controlled Valve The operation of the ASC valve is more easily understood by first studying a conventional pressure-charged valve and then inserting the stabilizer element to observe the changes which result. Fig. 1 is a schematic of a conventional precharged pressure-operated valve. The pressure in the dome pd, acts downward, against the area of the bellows A,, to hold the valve closed. The resulting force Bf plus the spring effect of the bellows Sf represents the total force acting to close the valve. Correspondingly, the tubing pressure ptbg works upward against the port area Atbg and the casing pressure pc works upward against a portion of the area of the bellows

Jan 1, 1965

By P. E. Rider, K. A. Gschneidner, O. D. McMasters

The solid solubilities for thirteen rare-earth metals in gold were determined by using the X-ray parametric method. Solubilities ranged from 0.1 at. pct for lanthanum in gold up to 8.8 at. pct for scandium in gold. The solubilities from lanthanum to gadolinium were very small and essentially constant, but a sharp increase occurred from gadolinium to scandium. The large solubilities for the heavy rare-earth metals were not expected because of the large size and electrochemical differences between rare-earth atoms and the gold atom. Contributions from first- and second-order elasticity theory plus an electronic contribution were found to reasonably account for a more favorable size factor. Electron transfer from the rare-earth metal to the gold Is thought to occur such that the resultant rare-earth and gold electronegativities are favorable for solid-solution formation. It was also found that this mutual adjustment of size and electronegutivity does not occur if the pure-metal size factors are greater than a critical value of 25 pet. The eutectic temperatures for ten systems were determined and these remained fairly constant at approximately 809 "C for the lighter lanthanide metal-gold systems until the Er-Au system was reached, at which Point the eutectic temperature successively increased reaching a maximum of 1040°C in the Sc-Au system. This rise was correlated to the size factor becoming more favorable for solid-solution formation at erbium. The valence state of ytterbium was found to change from two in the pure metal to three when ytterbium is dissolved in the gold matrix. RECENT results1 reported concerning the solubility of holmium in copper, silver, and gold, showed that the solubility of holmium in gold was quite large, 4.0 at. pct, compared with 1.6 in silver and 0.02 in copper. The small solubilities of holmium in silver and copper are quite reasonable in view of the large size difference (22.2 and 38.2 pct, respectively), large electronegativity difference (0.59 for both systems), and possible unfavorable valency factor (assuming one for silver and copper and three for holmium). The large solubility in gold, however, is unexpected because these same factors are also unfavorable for holmium and gold (22.5 pct size difference and 0.69 electronegativity difference), and because the light rare-earth metals, lanthanum, cerium, and praseodymium, have negligible solid solubilities in gold.2 In view of this unexpected behavior, it was felt that a study of the solid solubilities of most of the rare-earth metals in gold would be desirable to better understand the factors involved in the formation of solid solutions. Of the rare-earth metals added to gold in this study, only ytterbium is divalent in the pure metallic state (the other rare-earth metals are all trivalent) and many of its physical properties (such as the metallic radius, electronegativity, and so forth) are much different from those of the normal trivalent rare-earth metals.' The properties of ytterbium are such that one would expect solid-solution formation to be less favorable for ytterbium in gold than for any of the normal trivalent rare-earth metals. But chemically ytterbium is known to possess a stable trivalent state, and it is quite possible that ytterbium may alloy as a trivalent metal under certain conditions rather than as a divalent metal. Because of the dual valency nature and because so little is known about the alloying behavior of ytterbium, the gold-rich ytterbium-gold alloys are of special interest. EXPERIMENTAL PROCEDURE Materials. The gold used in this investigation had a purity of 99.99 pct with respect to nongaseous impurities. In general the rare-earth metals were prepared by reduction of the corresponding fluoride by calcium metal.3 The impurity contents of the metals used in this study are given in Table I. Preparation of Alloys. Two- or 3-g alloy samples were prepared by arc melting. The samples, with the exception of some of the Er-Au alloys, had weight losses of 0.5 pct or less. All alloy concentrations noted in this paper are nominal compositions. After arc melting, the alloys were wrapped in tantalum foil, sealed off in quartz tubing under a partial atmosphere of argon, homogenized for approximately 200 hr at 780°C, and then quenched in cold water. X-Ray Methods. The X-ray parametric method was used in determining the solubility of the rare-earth metals in gold. filings were sealed in small tantalum tubes by welding under a helium atmosphere. The tantalum tubes were then sealed in quartz tubing under a partial argon atmosphere, and annealed for times ranging from 1/2 to 3 hr (the length of time was inversely proportional to the an-

Jan 1, 1965

By L. B. Pankratz

Heat content measurements were conducted for GaPo.996 and InPo.986 over the temperature range from 298° to 1,100° K, and for In2S2.897 over the range from 298° to 1,200° K. Both the actual experimental data and values adjusted to conform with the stoichiometric compositions (GaP, InP, and In2S3) were reported. Entropy increments above 298.15° K were calculated for the stoichiometric compounds, and heat content and heat capacity equations were derived.

Jan 1, 1965