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By J. W. Whalen

The design, operation and evaluation of an instrumental method for the determination of fluid saturation in porous materials during multiphase flow studies is described. The presence of a magnetic tracer comprising approximately 20 per cent by weight of the aqueous phase is necessary in the utilization of this method. The results of two-phase relative permeability studies on two samples of porous media are presented. The realizable accuracy of the magnetic susceptibility apparatus in fluid saturation determination is estimated to be 2 saturation per cent. The response characteristics of the instrument, together with its simplicity of operation and maintenance are sufficient to recommend its use in routine laboratory studies. INTRODUCTION The problem of fluid saturation determination in laboratory multiphase flow studies characterizing oil recovery processes is one which has been given exhaustive study. Briefly the requirements which are considered essential for a method sewing this purpose are: (1) that the measurement be made external to the porous rock sample under study with no interruption of the fluid flow pattern, (2) the saturation indication must be independent of fluid distribution in the volume scanned by the measuring device, (3) the sensing element should have a small field of definition enabling several independent measurements to be made along the length of a core sample, and (4) the properties of the fluid phases should not be too greatly influenced by required tracer substances. Several methods of saturation determination have found acceptance as meeting most of the above requirements. These include resistivity,1 X-Ray absorption,2,3,4 radiotracers,5,6,7 and neutron8 diffraction The merits of these techniques have been discussed elsewhere in detail and will not be considered here. It may, however. be pointed out that the elaborate instrumentation required by the methods mentioned above, with the exception of the resistivity method (which is undesirable from other standpoints) encourages the development of methods of saturation determination which, while meeting the requirements listed, are simple to operate and maintain. It is the purpose of this paper to describe the instrumentation and evaluation of a technique for the determination of fluid saturation which combines relative simplicity with an accuracy and applicability comparable with methods now in practice. DESCRIPTION OF THE METHOD If the magnetic susceptibility of one of the fluid phases contained within a porous material is sufficiently greater than that of the remaining phases, the fluid content of the material with respect to that phase may be determined by an induction measurement. This may be accomplished by measuring the induced voltage in the secondary of a transformer which contains the porous sample and its interstitial fluids as a portion of the magnetic flux path. Since the fluids used in multiphase flow studies involving petroleum reservoir samples possess uniformly low magnetic susceptibilities, the use of a magnetic tracer in one of the fluid phases is required. In view of the relatively high paramagnetic susceptibility of salts of the transition elements, together with their high water solubility. these compounds become logical choices as tracer materials. Cobaltous chloride, having a specific magnetic susceptibility of 17.5 x 106 cgs electromagnetic units, was used as the tracer material throughout this work, in a concentration of approximately 20 per cent by weight in the aqueous phase. MAGNETIC SUSCEPTIBILITY APPARATUS Basically, the magnetic susceptibility apparatus consists of a transformer serving as the detecting head, a

Jan 1, 1955

By R. W. Armstrong, P. C. Jindal

WE should like to point out that Hu and cline.1 in their study of the recrystallization of titanium, have obtained data which appear very important for accurately determining the dependence of hardness on grain size for this material. It has been proposed2,3 that the macrohardness. H. of a poly crystalline material should depend on its average grain diameter, l. in accordance with the relationship: H =H0 + kHl-1/2 [1] where Ho and kH are experimental constants. This relationship follows from the hardness dependence on yield stress or flow stress4 and. thence. the Hall-Petch stress-grain size relations.5'6 Fig. 1 shows the Diamond Pyramid Hardness. Dph. values vs the reciprocal square root of the average diameter of the recrystallized grains, taken from the titanium data reported by Hu and Cline. The data in this figure give a linear relationship for the hardness over a wider range of grain diameters than anyone has previously measured. The data are not linear, for example. on an I-1 or l-1/3 scale. At the very large grain sizes the data are in reasonable agreement with measurements earlier reported by Holden, Ogden, and Jaffee.7 For the grain sizes smaller than 1 µ, which correspond in Fig. 1 to hardness values greater than 150, the material was reported as not being completely recrystallized and, therefore, these data appear less meaningful as far as the hardness dependence on grain size is concerned. However. it has been suggested by other investigators that deformed materials exhibit strengthening due to an effective grain size refinement even in the unrecrys-tallized condition.8-10 Also. Hu and Cline have shown that a change in texture occurs for titanium during the recrystallization process and. especially. following it. The influence of this texture change on the hardness-grain size relation would be expected to be less than that reflected in the unidirectional stress-strain behavior, even for an hcp material. because of the actual combined stress system which applies for the hardness test. For, at least, certain combined stresses, average values of the orientation factors should still occur in the stress-grain size analysis of a material exhibiting a preferred orientation.' We previously suggested3 that the experimental constants. H0 and kH. from the Meyer hardness-grain size relation should be correlated with the Hall-Petch constants, uoy and ky.5,6 Our recent study" of the Hall-Petch relation and the hardness-grain size results which obtain for a number of polycrystalline materials shows that: The inequality [2] is explained by noting that the hardness should be correlated. perhaps, with the flow stress at some value of strain, as suggested by Dugdale,12 and. also, that the influence of strain on the Hall-Petch relation is to increase uo and not change k very much." Normally. Dph values and Brinell hardness values are nearly equivalent to each other and to the Meyer hardness number. For the case of titanium, then. the inequality [2] may be evaluated using the experimental values of ao = 8.0 kg per sq mm and ky = 1.3 kg per mm3/2 obtained from the experiment of Guard.6,13 Thus, (Ho/uo) = 12 and (kH/k3) = 1.3. This research has been supported at the University of Maryland through the Center of Materials Research by the Advanced Research Projects Agency of the U.S. Government.

Jan 1, 1969

By B. H. Kear, S. M. Copley

Stress-stvain curves are presented for Ni3Al (y') cvystals in several ovientations, deformed in tension and compression at constant displacement rate, at temperatures from 70° to 2000°F. Both the yield stress and wovk havdening increase with temperature, with the magnilude of the effect dependent on ovientation. The yield stress maximum occurs at 1500°F in [001], at 1400°F in [011], and at 1200°F in [111]. The suppression of the yield stress peak in [011] and [111] orientatiorzs is due to the onset of cube slip, rather than octahedval slip, a1 elerated temperatures. The temperature and orientalion dependence of work hardening in nominal single slip orientations corvelates with changes in the CRSS ratio for octahedral slip and cube slip, in agreement with a model for work hardening based on pinning of screw dislocalions by cross slip from an octahedral plane into a cube plane. It is concluded that the unique plastic properties of y' have a decisive influence on both ductility and strength characleristics of y +y' nickel-base superalloys. It has long been recognized that the strength of y + y' nickel-base superalloys depends on the precipitation of the y' phase [basically Ni3(Al,Ti)]. This paper presents new data on the strength characteristics of single crystals of simple y' (Ni3Al), and forms the first step in a systematic program aimed at elucidating the mechanisms of hardening in the complex commercial alloys. 1) EXPERIMENTAL PROCEDURE Single crystals of off-stoichiometric NiA1 were grown from the melt under vacuum by a modified Bridgman method. The melt was poured into a preheated alumina mold and crystal growth was promoted from one end by gradient cooling. The crystals were homogenized by annealing in hydrogen at 2400° F for 72 hr followed by furnace cooling. Chemical analysis of samples taken from several crystals gave an average composition of 88.2 wt pct Ni. Spectrographic analysis gave as the principal impurities in weight percent— Si (0.02), Mg (0.01), Fe (0.02), Ti (0.002), Cu (0.008), and Co (0.03). Tensile specimens with specifications as in Fig. 1 were prepared by a series of operations involving electrical discharge machining, precision grinding, and electropolishing. Compression specimens with dimensions 1/4 by 1/4 by -3/4 in. were prepared in a similar manner, except for the initial shaping operation using a precision cut-off wheel/two-circle goniometer unit to give selected crystal orientations. Specimens were deformed in a Baldwin-Wiedemann testing machine with furnace attachment, using a strain rate of 5 x 10-4 sec-1. The strain measuring device consisted of extension arms attached to the tensile grips (or compression plattens) at one end and leading out of the furnace to an LVDT at the other. Temperature was controlled by a thermocouple placed in contact with the specimen. According to the known phase diagram for the Ni/A1 system,' when an alloy of the specified composition is cooled from the melt, primary y (nickel solid solution) dendrites grow at the expense of the liquid phase, which becomes enriched in aluminum. At the eutectic composition the remaining liquid freezes as a two-phase mixture of y + y' (Ni3Al). Upon further cooling, a solid state transformation occurs, involving the precipitation of y' in the primary dendrites, and the complete transformation of the eutectic mixture to massive y'. The as-cast structure consists, therefore, of y + y' dendrites with interdendritic regions of massive y', i.e., transformed eutectic, Fig. 2. 2) DISCUSSION OF RESULTS 2.1) Stress-Strain Curves. Fig. 3 shows tensile stress-strain curves for crystals in orientations close to [001] deformed at temperatures from 70° to 2000°F. Both the yield stress and total elongation are strongly temperature-dependent. At 70°F, easy glide is absent, and the work hardening coefficient BIT - G/300. At T > 1500°F, the negative slope of the stress-strain curves is due to pronounced necking in the crystals. The yield stress maximum at 1500° F corresponds with a minimum in the ductility, Fig. 4. The extensive duc-

Jan 1, 1968

By W. L. Phillips

Stress-train curves were obtained for single crystals of silver, Ag-5 pct Zn, Ag-10 pct Zn, and Ag-20 pct Zn tested in tension and shear at 78°, 195°, and 297°K. At room temperature the critical resolced shear stress gC increased, the length of' the easy-glide region increased, and the rate of' work hardening dwving easy glide decreased with increasixg zinc concentration. The change in the ratio of uc at room temperature to that at lower temperatures was significantly greater for the alloys than for pure silver. It was found that an increment in stress was necessary to continue slip when the slip direction was rotated 60 deg. The magnitude of this increment increased with strain for all alloys, increased with zinc concentration for a given strain, and for a given strain increased with decreasing -temperature. DESPITE its practical importance in improving the mechanical properties, alloying is not fully understood. Except for copper alloys few sets of systematic data are available. Von Goler and Sachs' studied the deformation of Cu-Zn alloys of increasing zinc content and found that, for dilute alloys, the critical resolved shear stress increases linearly with concentration. The range of easy glide was found to increase with increasing zinc content. Schmid and seliger,2 Sachs and Weerts,3 and Osswald4 have shown that with Mg-A1, Au-Ag, and Cu-Ni crystals, respectively, the critical resolved shear stress also varies linearly with concentration. More recently, Linde and his coworkers have investigated the variation of the critical shear stress of copper alloyed with tin , antimony, indium, germanium, silicon, nickel, and gold. They found that the slope of the critical resolved shear stress is related to the change of lattice parameter with composition, and also to the difference in Goldschmidt's atomic diameter between solvent and solute atoms. Garstone, Honey-combe, and creetham6 have shown that similar relationships can be found for small additions of silver, gold, and germanium to pure copper. They found that, with increasing silver or gold concentration, the critical shear stress for glide is increased by alloying, and so is the range of easy glide, which reaches as much as 60 pct for 0.50 pct Ag alloy and 0.62 pct Au alloy, as compared to 6 pct for pure copper of similar initial orientation. They also found that the alloying additions had little effect on the rate of hardening during easy glide, the slope scarcely changing with increasing alloy content. General secondary slip was detected only when the crystals began to harden rapidly. Although the slip appeared to be very fine in the early stages of deformation, coarser slip bands were formed towards the end of the extensive easy-glide range. The present investigation describes the deformation characteristics of single crystals of Ag-Zn containing different concentrations of zinc. Tension and shear testing were used for this study. EXPERIMENTAL PROCEDURE The method of growing the single crystals, sample preparation, and method of testing have been described in detail previously.' EXPERIMENTAL RESULTS A) Tension-Room Temperature. The initial orientations and stress-strain curves of single crystals of silver, Ag-10.0 pct Zn, and Ag-20.0 pct Zn are shown in Fig. 1. It is evident that there is considerable change in the stress-strain characteristics as a function of zinc concentration. The effects of zinc concentration on the critical resolved shear stress for both CU-zn8 and Ag-Zn alloys are summarized in Fig. 2. At all concentrations the resolved shear stress of the Cu-Zn alloys is higher than that of the Ag-Zn alloys. The resolved shear stress increases parabolically as a function of composition for both alloy systems. The length of easy-glide region increased with increasing zinc concentration, Fig. 3b). As the length increased the slope (do/de) decreased slightly, Fig. 3(b). Metallographic investigations demonstrated two significant effects of increasing zinc concentration. First, the amount of clustering increased, compare Figs. 4(a) and (b). The slip lines changed from uniform in pure silver to clustered in the Ag-20 pct Zn and Ag-30 pct Zn alloys. Second, the amount of cross slip decreased as the amount of clustering decreased.

Jan 1, 1968

By W. R. Foster, J. M. McMillen, A. S. Odeh

The complete equations of average linear momentum balance for a single-phase fluid in an incompreisible, homogeneous, porous medium are derived. The derivation begins with Euler's equation of motion for a continuum and uses an integral transform recently developed by Slattery. 7 For steady flow of a compressible, Newtonian fluid, the usual equations of motion result. For transient flow, the space-time description of the pressure is determined in the lowest approximation by the telegrapher's equation. From the analysis a new phenomenological coefficient results which connects the viscous traction to the deriv ative of the linear momentum density. The magnitude of this coefficient determines the velocity of sound through the pore structure in this approximation to the pressure field. INTRODUCTION The modification of Darcy's law of momentum balance for steady, single-phase flow through porous media has been discussed for many years. The first modification was suggested by Forcheimerl who added terms of higher order in the velocity. These can be expected to appear because the underlying microscopic equations of momentum balance are themselves nonlinear in the point velocity field. The Reynolds tensor pvv, which represents the convective flux of momentum density, appears in the momentum balance equation. Only in rectilinear flow (parallel stream lines) does the divergence of this tensor vanish. Since the steady flow stream lines in most porous media are not parallel, nonlinear dependence of the pressure gradient on the velocity should naturally appear. This nonlinearity has nothing to do with turbulence in the ordinary sense of random fluctuations in the pressure and velocity fields. It arises simply because the stream lines converge and diverge, even for steady flows. Klinkenberg2 demonstrated that the permeability coefficient in Darcy's law depends on the absolute pressure or, alternatively, on the density field. However, because he neglected inertial terms of the Forcheimer type, his correction coefficient could not be represented by a constant but tended toward a constant as the velocity decreased. Forcheimer's and Klinkenberg's modifications can be combined in a rigorous way to account for both inertia and slip during steady flow. This will be shown in a future paper. The transient change of pressure in porous media has been described by the diffusion equation.3 This form results from eliminating the velocity and density fields from a combination of the equations of motion in the form of Darcy's law, the continuity equation and an equation of state. Fatt4 suggested that the cause of deviations from the prediction of the diffusion equation for pressure transients lies not in the choice of Darcy's law as the equation of motion but on the existence of dead-end pores which might invalidate the averaged equation of continuity. On the other hand, Oroveanu and Pascal5 noted chat the time derivative of the momentum density must be included in the equations of motion since this measures the local rate of change of momentum density. Their differential equation for pressure is the telegrapher's equation (neglecting gravity). However, their form of this equation predicts that the speed of pressure propagation through the pore structure is the same as that through the bulk fluid. M. K. Hubbert6 attempted a derivation of Darcy's law by volume averaging the Navier-Stokes equations. Since these equations represent momentum balance at a point within an open set of points containing the fluid itself, Hubbert's volume averaging cannot lead to tenns involving transfer of momentum between the fluid and the walls of the pores. Once these viscous tractions are lost by choosing a control volume containing only fluid, they cannot

By H. Dykstra

Calculated wellbore pressures were obtained for parameters of radilcs ratio and permeability. In all cases bur two, after-production was allowed to occur for one day. The calculated pressure build-up data were compared with actual pressure build-up data from a condensate well. The paper discusses the comparison, gives reasons for, inability to match calculated (2nd actual data, and presents conc1usions derived from the comparison. INTRODUCTION Considerable information has been published on the decline in wellbore pressure for oil and gas fields resulting from production of fluids. Considerable information also has been published on pressure build-up for oil fields, but relatively little has been published for gas and condensate fields. Perrine' summarized the equations derived for pressure build-up in oil wells and showed how the different methods could be applied. On the other hand, very little theoretical information has been published on pressure build-up in gas or gas-condensate wells.2-4 Tracy,' by pointing out the similarity between the equation describing oil wellbore pressure decline and the equation describing gas wellbore pressure decline, showed how methods of pressure build-up analysis could be applied to a gas well. In analyzing pressure build-up data for gas or gas-condensate wells, it would be very desirable to compare actual pressure build-up data with calculated pressure build-up data. Such a comparison would lead to a better feeling for the quantitative picture of gas-well build-up curves and would help to establish a degree of confidence in a given build-up curve. This paper discusses the comparison and presents conclusions made from it. Calculated wellbore pressures are given for parameters of radius ratio and permeability. In all cases but two, after-production was allowed to occur for one day. The work was done in an attempt to evaluate the reserves of a gas-condensate field. As will be discussed later, it was not possible to make an evaluation. METHOD OF CALCULATION The method used for solving the depletion and pressure build-up behavior for a gas-condensate well was that developed by West, Garvin and Sheldon.5 or the IBM 704 computer program used, it was assumed that liquid condensing out of solution would have only a minor effect on the flow behavior. Therefore, the field was treated as having single-phase flow, with the gas saturation S, remaining constant at unity minus the connate-water saturation Sw. As will be discussed later, this may not have been a good assumption. It also was assumed that oil production could be considered as equivalent gas production by using a conversion factor based on an analysis of the liquid produced. An outer boundary condition of no-flow was assumed. BASIC DATA The data required for the study were reservoir properties, fluid properties and production data. Reservoir properties included the following: thickness h, 179 ft; porosity, 0.194; connate-water saturation, 0.43; gas saturation, 0.57; permeabilities k, 1.0, 0.5, 0.25 and 0.15 md; radius ratios re/rw, 800, 1,000 and 2,000; wellbore radius rw, 5 in.; initial reservoir pressure P, 6,529 psia; and reservoir temperature, 272°F. The selection of permeabilities was based on core-analysis data showing an average air permeability of about 2 md. With a relatively high connate-water saturation, the average effective gas permeability would be about one-half, or less, of the air permeability. The selection of radius ratios was based partly on the observed rapid decline in wellbore pressure during production and partly on the fact that the well was believed to be located in a relatively small fault block. Reservoir fluid properties were obtained from a reservoir fluid study on a recombined sample of gas and condensate. Gas formation-volume factors were calculated from pressure-volume measurements made at reservoir temperature. Gas viscosities were calculated by the method of Carr, et al,G from an analysis of the re-combined sample. These data are shown as a function of pressure in Table 1. The production schedule from the gas-condensate

By F. W. Warnaars

The Los Bronces copper deposit is located on the west side of the Andes Mountains in central Chile about 54 km (34 miles) northeast of Santiago. The deposit consists of a hydrothermal breccia complex that was emplaced in the western part of an earlier porphyry copper mineral system. This system exhibits propylitic, sericitic, silicic to potassic hydrothermal alteration with disseminated and stockwork copper-molybdenum sulfide mineralization over an area of about 12 km2 (5 sq. miles). The Rio Blanco Mine, about 800 m (0.5 miles) east of Los Bronces, is an underground block caving mine located in the central part of this system. The mineralization at Rio Blanco is characterized by one of the highest primary copper grades known for porphyry copper systems. Present mining at Los Bronces is from an open pit located in the northern part of a hydrothermal complex that is composed of at least seven different copper-bearing tourmaline breccia pipes. Together these pipe form one large contiguous body about 2 km (1.2 miles) long and 0.7 km (0.4 miles) wide at the surface. This body crops out at elevations of between 3.5 and 4.1 km (2 and 2.5 miles) above sea level. Each breccia pipe has a characteristic shape, matrix, type and degree of mineralization and alteration. Quartz, tourmaline, specularite, anhydrite, pyrite, chalcopyrite, sericite, chlorite, and rock flour are present in significant quantities in most breccia matrices. The clasts consist mainly of quartz monzonite, andesite, and minor amounts of quartz latite porphyry. The seven different breccia pipes are identified, from oldest to youngest, as Ghost, Central, Western, Infiernillo, Fine Gray, Anhydrite, and Donoso. The breccias coalesce, interfinger, or display gradational contacts. In places they form sharp contacts with each other and with the surrounding intrusive or volcanic host rocks. Early breccias are disrupted or cut by subsequent breccia events. Explosive emplacement was followed by collapse after the release of hydrothermal pressures. The Los Bronces breccia complex has sharp contacts with the surrounding intrusive stock and andesites. These contacts dip inward on the north, west, and south margins. The eastern contact is nearly vertical and/or dips slightly outward and suggests a westward tilting of the body of about 15° after emplacement. The breccia complex is not fully explored at depth, but is known to extend at least below the 3 km (2 mile) elevation in its central eastern part, about 1 km (0.6 miles) below the highest breccia outcrop. Primary copper sulfide minerals are most abundant in the Donoso and Infiernillo breccias where the matrix consists mostly of tourmaline, quartz, sulfides, specularite, and/or chlorite with minor amounts of rock flour, sericite, and clay. The volume of the matrix material is mostly smaller than in the other breccias. Secondary enrichment enhanced the primary copper grade in the southern two-thirds of the Los Bronces breccia complex and in much of the surrounding porphyry system. Primary grades of 0.3% to 0.5% copper have been enriched to approximately 0.9%. This enrichment may extend from surface outcrops to a depth of more than 500 m (1, 640 ft) in more permeable parts of the breccia complex. A leached and oxidized capping of variable thickness covers a large part of the enriched layer and exceeds 300 m (984 ft) at one location. The shape and depth of the enrichment blanket and the capping suggest that the enrichment process is still active.

Jan 1, 1983

By J. M. Karpinski, R. O. Tervo

A method and equipment have been developed for measuring the impact strength of grains of brittle materials. It is shown that brittle materials develop a characteristic particle size distribution when fractured by impact. A simple mathematical model has been found to describe this distribution, and one of the parameters of the model has been designated the r value. The r value is directly proportional to impact energy and, for fixed impact energy, it becomes a useful criterion of grain strength. Data are presented on the variation of the r value as a function of sample history, initial size, energy input and number of impacts. The results are interpreted in terms of the flaw theory of brittle fracture. The view is now widely held that brittle materials comprise a strong matrix, throughout which flaws or points of weakness are scattered at random. Failure always starts at one or more of these imperfections, and planes of fracture are established by the geometry of the flaw distribution. This view has been developed extensively by Weibull 1,2 and experiments of a confirmatory nature have been reported.3,4 Thus the process of fracture or size reduction of brittle materials can be regarded as a process of elimination or creation of flaws, and the concept of strength is intimately connected with the size and history of the specimen tested. One consequence of the point of view described above is that brittle materials will fracture to yield similar size distributions, although the impact energy to produce a given amount of fracture may vary greatly from one material to another. Generally speaking, experimental investigations of brittle fracture in solids have been confined to two extreme experimental situations. On one hand, we have tests on single specimens of well-defined, but artificial, geometry and, on the other, empirical data have been obtained on the feed-product relation in a variety of mills. The first situation necessitates specimen preparation, which in the case of brittle materials is equivalent to a priori size reduction, while the second one suffers from the disadvantage that little knowledge is gained about individual fracture events. Also, the statistical significance of single specimen tests may be questioned. Our approach lies somewhere between these two extremes. We test a large population of sized specimens and yet subject each specimen to a single fracture event. In 1956 G.H. Fetterley of Norton Co., Chippawa, Ont., made the empirical observation that product size distributions obtained from impacting sized grits can be described by the following equation where R is the proportion by weight of the grain that remains on a screen having an opening x on a side, x, is a parameter having the dimensions of length, and r is a number. This equation has since been derived on a theoretical basis by Gaudin and Meloy.5 They identify x, with the initial size of the test piece and r with the number of flaws per unit length. As will be shown below, our experiments indicate that both x, and r are functions of energy and hence they should more properly be called the effective initial size and the effective number of flaws respectively. Also, our empirical data give us no basis for assuming that r represents the effective number of flaws per unit length, rather than per unit volume. METHOD AND MATERIALS The impact test machine has been designed to feed specimens, essentially one at a time, into an evacuated chamber, where they fall freely and are struck with random orientation by one or the other of a pair of flat steel vanes. The vanes are mounted at opposite ends of a steel bar, which rotates at a closely controlled angular velocity about a vertical axis. Fig. 1 shows the flat circular vacuum chamber with the cover removed, and the horizontal steel bar with the steel vanes at the ends. The cylindrical pot in which the grains are collected after impact appears at the left. Fig. 2 shows the equipment assembled for a test. The vacuum chamber occupies the central position with the variable speed drive below the table surface, the vacuum pump at the extreme left

Jan 1, 1964

By R. Taggart, D. H. Polonis, W. C. Gallaugher

In the Ti-Cu system, the a' phase can be produced over a wide range of alloy composition witJwut the retention of measurable amounts of the ß or ? phases. This paper reports on the decomposition of this hexagonal martensite phase front the standpoint of solute corzcentratiorz, tempering temperature, and coherency strain condition. The mechanism of precipitation during tempering comprises localized precipitation which is followed by discontinuous precipitation if sufficient coherency strains are present. The localized precipitation process in hypoeutectoid alloys is described by the generalized Johnson-hiehl equation and an activation energy of 46,000 cal per mole. In hypereutectoid alloys the corresponcEing activation energy is 51,000 cal per mole. The rate-controlling process has been proposed as the difision of copper along a' platelet interfnces. SEVERAL investigations have been reported concerning the kinetics of decomposition of the mar-tensitic a' phase in titanium binary alloys.' In the Ti-Mo system,' two modes of a' decomposition have been observed in the presence of /3 phase; one of these involves the precipitation of fine a from a', and the other involves diffusion across the a'-ß interface. In studies of the Ti-Cr system, Rostoker2 did not detect the formation of TiCr2 during tempering. In Ti-Ni alloys,3 the intermediate phase Ti2Ni has been found to precipitate directly from a' along the interfaces between plates. With the exception of the study of Ti-Ni alloys the previous investigations of tempering phenomena in substitutional martensites are mainly qualitative and do not present a detailed description of the precipitation processes. The following limitations restrict the correlation of the microstruc-tural processes and reaction kinetics during tempering in most binary-alloy systems. 1) A mixture of at least two phases characterizes the constitution of quenched alloys. 2) Difficulties have been encountered in obtaining uniform structures throughout quenched samples. 3) The reaction products, and in particular their morphology. have not been clearly resolved. 4) The martensitic a' phase forms over only a limited composition range for most titanium-base binary alloys. Gomez and polonis4 showed that the Ti-Cu system provides an excellent basis for investigating the tempering of a' over a range of composition without the complication of retained P or the transition w phase. In the present work the effects of solute concentration, tempering temperature, and coherency strain conditions are considered with reference to the over-all precipitation process in quenched alloys of the Ti-Cu system. Both microstructural observations and kinetic data are correlated to define the rate-controlling processes which govern the observed localized and discontinuous precipitation reactions. An earlier paper5 was devoted to a discussion of the modes of heterogeneous nucleation of Ti2Cu from the martensitic a' structure. The present paper will therefore emphasize the progress of the tempering reaction beyond the initial stages. EXPERIMENTAL METHODS The Ti-Cu alloys for this study were prepared by conventional arc-melting procedures. Chemical analysis revealed that the alloy buttons contained approximately 0.02 wt pct 0, 0.04 wt pct N, and within 0.1 wt pct of the intended copper concentration. The progress of the tempering reaction was followed by means of electrical-resistance measurements utilizing a Kelvin double bridge, microhard-ness readings with a 400-g load, and X-ray dif-fractometry patterns to reveal line-broadening effects. Metallographic specimens examined at magnifications greater than X1000 were shadowed with germanium to reveal fine structural details. Direct carbon replicas were prepared for the electron-microscopy studies. EXPERIMENTAL RESULTS Property Changes. The changes of microhardness that accompany the precipitation of Ti2Cu from a' are shown in Figs. 1 and 2. As the solute concentration increases the peak hardness, for a given tempering temperature, increases. In alloys of given composition the time to reach the peak hardness agreed with the time to attain maximum X-ray diffraction peak breadth, as shown in Fig. 3. The maximum hardness and the maximum line breadth increased with lower tempering temperatures, and the time to reach the maximum also increased. The a' peaks broadened during the initial stages of tem-

Jan 1, 1965

By R. Bakish, C. S. Barnett

IN experiments on tantalum strained in tension, Bechtold did not observe deformation-twinning even at a temperature as low as that of liquid air.' This is an unexpected behavior for a metal of body-centered-cubic structure. Therefore, it is desirable to determine whether the lack of twinning is an inherent characteristic of this particular metal, or whether the reluctance to twin can be overcome under suitable conditions. The following experiments were performed under conditions favorable to twinning and cleavage in their competition with slip, namely, with impact loading on large-grained sheet at low temperatures. The crystallography of cleavage in tantalum sheet was also investigated carefully because of the remarkable ductility of tantalum at low temperatures and because recent tests on oxygen-embrittled tantalum had disclosed unusual cleavage behavior for a metal of this structure: cleavage primarily on (110) planes and only occasionally on {100}.2 The tantalum, supplied by Fansteel, was of 99.9 pet purity, with the chief impurities being iron (0.03 pet) and carbon (0.03 pet). Coarse grains were produced by the strain-anneal method, the anneal being 4 hr at 2000°C in a vacuum of 10-3 mm Hg, followed by furnace cooling. Impact deformation was applied in various ways: a) by hammer blows on an anvil, the specimen and anvil being immersed in liquid nitrogen ( —196°C), b) by driving a precooled center-punch into the sheet, and c) by bending around a crystallographically determined axis with a hammer blow. The impact-deformation produced bands and slip lines on the surface, Fig. 1. The bands have every appearance of being deformation twins, a) They are tilted with respect to the untwinned surface. b) They have the appearance of Neumann bands in iron, thin lens shape, some having serrated edges. c) The orientation in each is different from that of the surrounding matrix and uniform within a given band, see slip lines within them in Fig. 1. d) Upon repolishing and etching, the difference in orientation and the resemblance to Neumann bands is again evident, Fig. 2. (In this micrograph the slight bend in the bands as they cross grain boundaries was noted frequently and results from the high degree of preferred orientation in the sheet.) e) The bands persist after annealing treatments that would have removed them had they been a low-temperature martensitic phase, e.g., after an anneal of 1/2 hr at 900°C. When back-reflection Laue data were plotted for single-surface analysis of several grains, every trace of the bands in each grain could be explained by (112) planes. In addition, two of the bands were located in space by traces on two surfaces, and these also were found to lie on (112) planes within the error of the stereographic plot. Since (1 12) is the anticipated composition plane for deformation twins in body-centered-cubic metals it is felt that the observations listed above are conclusive evidence for the identification of the bands as twins. Similar tests with impact at —77° and at 25°C produced no twinning. It is concluded that the critical shear stress for slip at the rates of straining used was always low enough to prevent the applied stress from reaching the value required for twinning at these temperatures. It was noted that the serrations along the edges of the twin bands exhibited parallel crystal facets. Several similarly oriented notches are visible in Fig. 1, and a remarkable set is shown in Fig. 3. It appears from Fig. 1 and similar areas that notches are frequently associated with the intersection of a slip line with a twin, although not all such intersections are at notches. In some instances a slip line appears to enter the twin, cross it, reflect from the opposite side and recross it, producing a pattern resembling a notch but without producing the notch itself, see Fig. 1. It is suggested that the stress concentration at the end of a slip line is responsible for these details. The strain energy associated with the pile-up of dislocations at a twin boundary may be lessened by untwin-ning or failing to twin a portion of the twin band, or

Jan 1, 1959

By J. T. Norton, H. Blumenthal, S. J. Sindeband

The interstitial phases formed by the transition elements with carbon, nitrogen and boron constitute a unique class of substances which are of considerable technical interest because of their well developed metallic properties and their high hardness and melting points. They are also of interest from the point of view of structure. It was pointed out by Hagg1 some years ago that the principal factor determining these structures was the relative sizes of metal and metalloid atoms. He predicted that if the ratio of the radii of metalloid to metal atoms was less than 0.59, the metal atoms would be arranged in a close-packed fashion of relatively simple type. This prediction has been amply confirmed. It appears, however, that this specification applies most generally to those structures in which the metalloid atoms occupy isolated positions in the lattice and there is no tendency for strong binding between the metalloid atoms themselves. The series of borides of the type MeB2 formed from the transition elements of the fourth (Ti, Zr) and fifth (V, Cb, Ta) groups of the periodic table provide an opportunity to investigate this situation further. If one takes as a basis the radius of 0.87 A for the boron radius and the Goldschmidt values for the metal atoms in 12 coordination, then the radius ratio varies from 0.54 for zirconium to 0.64 for vanadium, which latter is considerably greater than Hagg's limit of 0.59. It was of interest, therefore, to see if these five elements would form borides of the MeB2 type and have simple isomorphous structures. When this investigation was initiated, relatively little information had been published on the structure of this group of borides. McKenna2 reported the preparation of ZrB2 by a carbon reduction process. Its structure was hexagonal and the approximate lattice constants were given as a = 3.15 A, c = 3.53 A. Ehrlich3 reported the structure of TiB2 as being of the C 32 type with a = 3.02, c = 3.21 and c/a = 1.06 A. Recently, Kiessling4 published the results on ZrB2, showing it to be one in which the metal atoms are arranged in a simple hexagonal lattice with the boron atoms in flat sheets, midway between the layers of metal atoms. The structure is C 32 type with a = 3.169, c = 3.530 and an axial ratio =1.11 A. He also states that CbB2 and TaB2 are isomorphous with ZrB2. Preparation of Borides The borides of titanium, zirconium, columbium and tantalum were made by the electrolysis of fused salt baths after the method described by Andrieux.5 The bath, totalling about 6500 g in each case had the following general composition: Metal Oxide + B2O3 + CaO + CaF2. The actual proportions of the ingredients were determined for each individual case. Although Andrieux reports the preparation of vanadium boride by the same electrolytic method, several attempts proved unsuccessful. However, it was possible to prepare VB2 by the carbon reduction method used by McKenna to produce ZrB2. The mixture consisted of V2O5 + 6B2O3 + 11C and the reduction was carried out in an induction heated graphite crucible. This method proved satisfactory for ZrB2 and TiB2 and undoubtedly the others could be made in the same way. The borides, which were all in the form of fine gray metallic crystals from the electrolytic bath or gray powders from the reduction process, were carefully separated from other constituents and analyzed chemically for metal and boron content. The densities of the boride powders were measured using a standard 10 cc pyenometer at 18°C and ethyl benzene proved to be the most satisfactory liquid for this purpose. X Ray Technique The boride crystals, as prepared, were too small for single crystal examination so that powder techniques were employed. Patterns of the finely ground borides were prepared, using the Norelco recording X ray spectrometer. The lines on these patterns were indexed with the aid of Hull-Davy charts and the approximate dimensions

Jan 1, 1950

By R. R. Goddard

By use of the frequency response method with a radioactive tracer, it was possible to determine fluid dispersion and distribution in a natural consolidated and an unconsolidated medium. Measurements were made in a linear flow system at oleic saturations of 69 per cent in the consolidated medium, and 100 per cent in both media. Dispersion and distribution were obtained by measuring the amplitude attenuation and the phase velocity of sinusoidal waves with a dual monitor apparatus. The gamma ray emissions permitted in situ measurements at any distance along the porous samples. One result of importance was that the effective diffusivity increased as the wave length increased. As a consequence, a dispersion coefficient appropriate for the injection of large slugs might exceed the value measured by use of small slugs. Since flow models based solely on fluid velocity and an effective diffusivity coefficient imply that the diffusivity should be independent of frequency, such representations were not adequate for the data of this study. A comparison was made with a capacitance model of porous media with deadend PVs, but even this model was not completely adequate. By using attenuation and phase velocity data, fluid dispersion can be predicted without postulating a differential equation satisfied by the tracer concentration, thereby eliminating the need of a complicated model to represent dispersion. INTRODUCTION The flow of similar miscible fluids through a porous medium can be fairly adequately described by two parameters: the average fluid velocity and the effective diffusivity.1-3 It has been pointed out recently, however, that significant discrepancies exist between this representation and the experimental data.4-7 An improved agreement can be obtained by introducing additional parameters based on the concept of dead-end pores. The purpose of the present investigation was to find out whether the frequency response method could be used to measure the relevant parameters. The method was used in the following form. A stream of fluid was flowed at a constant rate through a sample of porous material and the concentration of a radioactive tracer in the fluid was varied sinusoidally at a fixed frequency. The effects of flow through a porous medium are a decrease in the amplitude of the concentration wave and an increase in the velocity of the peaks of the waves above the average velocity. Attenuation and phase veIocity of the waves were measured as a function of frequency and fluid velocity. The simple two-parameter model implies that the diffusivity should be independent of frequency. Data reported in this paper show that the diffusivity decreases as the frequency increases. Hence, as shown also by many others, the two-parameter model is not completely adequate. Coats and Smith 5 used two additional parameters in their model: the volume of the dead-end pores and the rate of mass transfer between dead-end pores and the flowing stream. Their capacitance model of a porous medium containing some stagnant fluid, to which transfer occurs by molecular diffusion, did not explain the dispersion results of either the present study or of theirs. Instead, the capacitance effect can be better described as the result of extreme velocity variations within the pores of the medium, with transfer between the velocity zones by convection. EXPERIMENTAL PREPARATION OF POROUS MEDIA Data reported here were obtained with a natural Berea sandstone, and with two packings of 20/25 mesh sand. Pertinent information about these media is listed in Table 1. The sandstone core was first sealed with a non-

Jan 1, 1967

By R. W. Olson, A. L. Benham

Viscous fingering was studied as it occurred in an open Hele-Shaw model (1 ft x 4 ft x 1/16 in.); it was also studied in the same model packed with 80-mesh glass beads during miscible displacements under unfavorable viscosity ratio conditions. It was determined that the lengths of 20 elements of the front were distributed normally around the average position of the combined elements under all conditions. Represented by the normal distribution, the length of the viscous fingers grew linearly with the distance traveled from the point of finger formation, increased with displacement velocity, and increased with increasing mobility ratio. Results obtained during the first few inches of displacement were of little or no use in predicting finger growth and/or finger length throughout the 4-ft model since the point of finger initiation cannot be predicted and would often occur several inches from the point of injection with either positive or apparent negative coordinates. The fingering occurring during a miscible slug displacement was much greater than would be predicted based upon the actual mobility ratios between in-place fluid and slug and between slug and following fluid, using the results described above for miscible displacement in the absence of a slug. Many of the experiments in the packed model showed that the rate of growth of the viscous fingers was diminishing toward the end of the displacement in the 4-ft long model, indicating that microscopic mixing, such as diffusion or dispersion, was decreasing the viscous fingering effect. INTRODUCTION Viscous fingering is a manifestation of a finger-shaped interface between displaced and displacing fluids occurring during typical miscible displacement projects for oil recovery. Its cause may be traced to the instability of a viscous fluid being displaced by a more mobile fluid. Viscous fingering takes on important significance in the miscible slug process 1.2 where it may be a dominant factor in determining minimum slug size. Experimental1-3 and theoretical4-7 studies of viscous fingering have been made by other investi- gators. However, an exhaustive study of the variables affecting viscous fingering had not been made. The present study was undertaken in an effort to determine the effects of some of the more obvious variables—such as mobility ratio, displacement velocity, distance displaced, and packing—upon viscous finger length and growth in a small laboratory model. It does not necessarily follow that conclusions reached by studying the results of this model study may be applied to the field. Future studies would have to evaluate the effect of model size on extension of these results. EQUIPMENT AND EXPERIMENTAL PROCEDURES A flow diagram for the equipment used in this study is shown in Fig. 1. Basically, it consisted of (1) a constant-rate pump for the injection of displacing fluid into (2) a model made up of two flat transparent plates spaced a small distance apart and (3) provisions for the production of fluid into a calibrated graduate. The displacing fluid contained a dye which allowed visual observation of finger spacing and length. The pump performed at rates from 2.5 cc/hr to 480 cc/hr, while pumping a light mineral oil into a bladder in a closed glass container holding the displacing fluid. The model was made up of two plates of 1-in. Plexiglass with dimensions 1-ft wide by 4-ft long. These were spaced 1/16 in. apart so that the internal model dimensions were 1-ft wide x 4-ft long x 1/16

By L. A. Roe, John Jan

Iodine is a soft, lustrous, grayish-black nonmetallic element with a density of 4.9. It is the least active of the four members of the halogen family. The other members are, in order of increasing activity, bromine, chlorine, and fluorine. Iodine is a solid at ordinary temperatures, while bromine is a liquid and chlorine and fluorine are gases. Iodine melts at 113°C and volatilizes at 184.4°C to a blue-violet gas with an irritating odor. It occurs in nature only as iodates and iodides or other combined forms. It was discovered by Bernard Courtois in France in 1811, who noticed its presence as an unknown substance in crude soda ash obtained from burning seaweed. Gay-Lussac recognized it as a new element and named it iode, from the Greek word "ioeides or iodes" for violet color (MacMillan, 1970). The world production is not known with any great certainty, but it is probably between 25 and 35 million lb per year, of which about 30% is consumed in the United States. Geology and Mineralogy Iodine compounds occur as a minor constituent as a mineral in the Chilean nitrate deposits and in solution in brines and seawater. According to the US Geological Survey, it is the 47th most abundant element in the earth's crust. The minerals lautarite, Ca (I03)3 (calcium iodate), and dietzeite, Cat (103)2 (CrO4), (calcium iodate-chromate) are found in Chilean nitrate deposits which are located in Antofagasta and Tarapaca provinces on the eastern slope of the coast range in a desert area. Various brines contain iodine compounds. Seawater contains about 0.05 ppm of iodine and some seaweeds will extract and accumulate it up to 0.45% on a dry basis. Some coals in West Germany also contain iodine compounds. The known and potential sources of iodine reported in 1968 are given in Table 1. Table 2 lists estimated world iodine reserves. Iodine has been recovered from brines in Java, Indonesia, France, England, and the USSR. Iodine has also been recovered from seaweed in Ireland, Scotland, France, Japan, Norway, and the USSR. The indicated reserves and future resources of iodine are large but have never been adequately measured. Analysis Iodine as the free element can be detected by the characteristic blue color it gives to a starch solution. Quantitatively it is determined as the free element by titration with standard thiosulfate solutions using starch as an indicator. Colorimetric methods are also applicable. Markets and Prices Iodine and its compounds are generally marketed in the form of: iodine, crude; iodine, resublimed; calcium iodates; calcium iodide; potassium iodide, sodium iodide, and numerous organic compounds. Product Specifications Crude iodine, World market: 99-99.5% 12. Crude iodine, US produced, average: 99.8% 12. Crude iodine, USP XVII Specs: not less than 99.8% percent I2. Resublimed iodine is usually 99.9% and ACS specifications call for not over 0.005% total bromine and 0.020% nonvolatile materials (Anon., 1971). Prices, c.i.f. United States, for iodine have been steadily increasing from $1.18 per lb of crude in 1967 to $6.37-7.27 in January 1981 (Anon., 1981). In 1980 the price of iodine increased by 50%.

Jan 1, 1983

By E. J. Dulis, R. M. Fisher, K. G. Carroll

IT is well known that ferritic steels containing more than 15 pct Cr when subjected to temperatures in the range of 700" to 1000°F exhibit increasing hardness and decreasing ductility. The phenomenon has been widely termed the "885 °F embrittlement," after the temperature of most marked effect.'.' In view of the excellent review articles available in the literature3-6 only a brief account of experimentally established facts need be given here. The extent of changes in physical characteristics during embrittlement depends on chromium concentration and time at temperature, higher alloy content and longer time both promoting more rapid and extensive changes. In a 27 pct Cr steel, changes in impact strength and in angle of fracture in bending can be detected after only a 1 hr exposure at 885°F; after 50 hr this steel becomes quite brittle. Hardness increases slowly with time during thousands of hours exposure and may attain a maximum hardness number twice as large as that of the unexposed steel. Microstructural changes accompanying embrittlement have been described as an initial widening of grain boundaries followed by eventual darkening of ferrite grains. Embrittled steels etch more readily, e.g., the weight loss of a 27 pct Cr steel in acid solution may occur at a rate one hundred fold greater following exposure at 885 OF. Marked changes which accompany embrittlement have been observed in electrical resistivity, specific gravity, and magnetic coercive force. Changes in physical properties may be readily removed by heating at temperatures above the embrittling range, such as a treatment at 1100°F for 1 hr. It has frequently been noted that the 885 °F embrittlement suggests precipitation on a submicro-scopic scale of a chromium-rich constituent, the nature of which has not been revealed by X-ray diffraction. Progressive broadening of the body-centered cubic diffraction lines during embrittlement has been observed," and recent observations by Lena and Hawkes' upon single crystals have shown early asterism in X-ray photographs, disappearing within an hour at 900 °F. Many workers have ascribed8-13 the phenomenon to a precipitation of a phase (FeCr), which is known to cause embrittling effects at temperatures much higher than 885°F. Two general observations, however. suggest that a precipitation cannot be responsible for the 885°F phenomenon: 1—prior cold work greatly enhances a formation, whereas it scarcely affects the 885 °F embrittlement, and 2—the presence of an alloying element such as nickel or manganese may have an effect on the 885 °F embrittlement which is opposed to its effect upon a formation. The slight enhancement of a formation and 885°F embrittlement observed in the presence of elements with strong carbide and nitride forming tendencies' is probably a consequence of lessened chromium depletion of the matrix. The bar graph in Fig. 1 shows a typical example, taken from two 27 pct Cr steels used in this work, of the hardness after exposure for 10,000 hr at 900°, 1050°, and 1200°F. Steel A (0.03 pct C, 3.13 pct Mn) showed marked hardening at 900" and 1200°F, whereas steel B (0.12 pct C, 0.63 pct Mn) exhibited only the 900°F hardening. The cr phase was found in steel A at the higher temperatures but not in steel B. Presumably a formation is enhanced by the low-carbon and high-manganese concentrations in A," Thus there are two distinctly different hardening phenomena present which cannot both be ascribed to v precipitation without invoking a transition phase possessing remarkable properties. Materials A number of chromium steels exposed for long periods (5000 to 34,000 hr) at 900°F, as well as unexposed samples of one of the steels, were available for this investigation. Table I gives the chemical compositions and aging treatments of these steels. In addition to these steels exposed in the elevated temperature test furnaces of the National Tube Division, a number of high-chromium steels were heated for short periods in small laboratory air furnaces and lead baths. Supplementing these commercial steels, a sample of high-purity (0.018 pct C, 0.002 pct N) 28 pct Cr iron, exposed 1000 hr at 887°F. was furnished by the Union Carbide and Carbon Corp. In addition, an alloy of iron and chromium of high purity containing 46 pct Cr was used. This

Jan 1, 1954

By Joseph E. Worthington

The present-day Northumberland gold mine is one of the deposits generally characterized as a Carlin-type occurrence. It lies at the crest of the Toquima Range in Nye County near the center of Nevada. Gold mineralization occurs in two modes, in argillaceous and in silicified limestones, and is generally very fine-grained or micron gold. The Northumberland district has had a history that is typical of many western gold districts: minor production prior to World War II and intermittent exploration thereafter until a combination of geological insight, improved economics, and the advent of heap leach technology created the Northumberland gold mine. Nye County, Nevada, was sparsely populated and little explored in the early years of the settlement of the west; the Northumberland district was not established until 1866. Initial interest was in silver and the district operated as a very small producer for the next seventy years. The disseminated gold occurrences in silicified limestones were recognized and Northumberland Mining Co. was organized to develop the property in the late 1930s. Northumberland Mining Co. actually conducted drilling operations (over 200 drill holes) and mined from small open pits in the silicified limestones. They ultimately produced almost 936 kg (33,000 oz) gold before being shut down by War Production Board Order L-208 in 1942. After World War II gold mining activities were essentially nil for over a decade due to the poor economics of gold production. The property was, however, a known gold producer and attracted recurrent exploration attention. About 45 holes were drilled under the direction of Peter Joralemon for private interests between 1959 and 1963. Next Kerr McGee drilled about 25 holes during 1963 and 1964. Some- what later, in 1968, Homestake drilled 20 holes. The property was then acquired by Idaho Mining Co. which drilled about 30 more holes between 1972 and 1974. By this time the Northumberland mine was becoming somewhat shopworn with over 300 holes drilled. Interest in gold prospects was increasing substantially in Nevada, how- ever, due to rising gold prices in late 1974, and several companies were interested in continuing exploration at Northumberland. In 1975 Cyprus Mines Corp. was successful in obtaining a joint venture arrangement with Idaho Mining Co. for further exploration and development of the property. The overall Cyprus exploration program was under the direction of James G. Hansen, Vice President Exploration. The geologist recommending acquisition of Northumberland was Peter E. Chapman who reported to Joseph E. Worthington, Manager of U.S. Exploration for Cyprus. The basis for selection of the Northumberland mine as an exploration target for Cyprus by Chapman was essentially prior knowledge of regional and 16cal geology and of the mine. Exploration for the next few years was directed by Chapman under the supervision of Worthington. During 1975 and 1976 rotary and check core drilling were conducted that indicated that a substantial Carlin-type or disseminated, low-grade gold deposit occurred in two separate bodies. Drilling was based on geologic mapping and rock chip geochemical sampling. Both ore zones were reflected at the surface as gold and arsenic anomalies in rock chips. Heap leach tests attempted in 1977 were aborted by a flash flood, but were completed in 1978. Engineering studies occupied the next couple of years until the property achieved production in the fall of 1981. It is now producing by open-pit mining with gold recovery by heap leaching and cyanide extraction at a rated capacity of approximately 2722 t/d (3000 stpd) ore. Metal recovery has been projected (probably conservatively) at 5 10 kg/a (18,000 oz per year) gold and 1.6 Mg/a (59,000 oz per year) silver. Reserves are reported to be adequate for ten to fifteen years of production. REFERENCES Anon., 1981, "Gold in Nevada," Span Magazine, Vol. 21, No. 3, Standard Oil Co., pp. 6-9. Koschman, A.H. and Bergendahl, M.H., 1968, "Principal Gold- producing Districts of the United States, Professional Paper 610, US Geological Survey, p. 193. Kral, V.E., 195 1, "Minerals Resources of Nye County, Nevada, Bulletin, Vol. 45, No. 3, Geology and Mining Series 50, Nevada University.

Jan 1, 1985

By M. Kaufman, A. E. Palty

The phase structure and aging characteristics of two nickel-base alloys, Inconel 718 and 702, were investigated. Wrought and cast Inconel 718 showed ArisCb as the major hardening phase, as well as ture was positively identified. Inconel 702 had Ni3Al as the major hardening phase, as well as Cr7C3-of the phase amounts with temperature was determined. 1 HE value of phase structure and aging rate information in the utilization of alloys has been well established. As part of a continuing program, the results obtained on two nickel-base alloys, hconel 718 and Inconel 702, are presented here. Inconel 718 is a relatively new alloy considered for application in both sheet and cast form. Its novelty lies in the use of high columbium tantalum levels in a Ni-Cr-Fe base. No previous work on this type of alloy has been reported in the literature. Inconel 702 is being used now as an oxidation-resistant sheet alloy. Occasional fabrication problems spurred work on its basic structural behavior. The composition of 702 is essentially nichrome plus aluminum and titanium for strengthening and added oxidation resistance. This puts it in the basic class of other nickel-base alloys which have already been studied. The two alloys will be treated separately. INCONEL 718 Phase Study Methods. The phases present after the various conditions investigated were determined by X-ray diffraction analysis of two different elec-trolytically extracted residues and microscopic examination. The extraction methods, using 10 pct HC1 in alcohol and 10 pct H3PO, in water and the X-ray technique have been described previously.' The effect of temperature on the phase behavior was studied on sheet material using the following heat treatments: 2250°F, 2 hr, ice brine quench 1300 100 hr, water quench 2250°F, 2 hr, ice brine quench 1400°, 100 hr, water quench 2250°F, 2 hr, ice brine quench 1500°F, 100 hr, water quench 2250o 2 hr, ice brine quench 1700°F, 48 hr, water quench 2250°F, 2 hr, ice brine quench 1850°, 24 hr, water quench 2250°, 2 hr, ice brine quench 2000°F, 6 hr, water quench The high solution temperature was an attempt to dissolve as many phases as possible without causing melting. Aging exposures were made longer than normal heat treating times in order to approach equilibrium conditions more closely. Cast material was examined only in the as-cast condition and with the normal heat treatment (1700°F, 1 hr, air cool 1325oF, 16 hr,air cool). Materials. The full phase study was performed on sheet specimens approximately 1/2 in. by 2 in. by 1/16 in. The cast pieces were cut from the gating system of a vacuum-cast test piece. An all weld-metal specimen was made by running many weld beads on the sheet using filler made from the sheared edges of the sheet. All external contamination was removed by belt-sanding followed by an electro-polishing treatment. The typical composition of wrought Inco 718 is as follows: The alloy is air-melted. Cast hco 718 may have higher molybdenum. Due to the expectation of finding a Ni-Cb phase (Ni, Cb) for which no X-ray diffraction pattern was available in the ASTM Index, a special 5 Ib heat to the stoichiometric composition of this intermetallic

Jan 1, 1962

By O. N. Carlson, W. M. Paulson

A phase diagram is proposed for the Y-C system based on the vesults of thermal analyses, microscopic obsevvations, and X-ray diffraction studies. Three intermediate phases occur in the system: a congru-ently melting fcc phase with a wide range of homogeneity about the composition Y2C, an intermediate solid-solution region between 55 and 58 at. pct C, and a bct dicarbide melting congruently at 2415°C. All three compounds undergo a phase transformation at elezlated temperatures. A continuous serzes of solzd solutions exists between the fcc phase and the high-temperature form of YC2 with a maximum in the solidus at 2000°C and 30 at. pct C and a minimum at 1805°C and 54 at. pct C. THIS investigation of the Y-C system was undertaken as part of a nuclear materials development program. Yttrium-base alloys are of interest as possible containers for liquid metals, and carbides are currently receiving increased attention as high-temperature materials for advanced reactors and other applications. Previous work on this system was limited in scope, and the results were somewhat inconclusive and at times contradictory. Spedding et al.&apos; reported the existence of a triyttrium carbide having an fcc structure with a wide range of homogeneity and Dean et a1.2 reported the existence of a rhombohedra1 phase having the stoichiometry of Y2C. Bachella et a1.3 observed that the latter was the result of ordering of carbon atoms in the fcc solid solution. The ordering range was placed at 800" to 1000°C. Vickery et a1.4 reported a high-melting compound which they identified as yttrium dicarbide, and Spedding and coworkers1 determined the structure of this phase as bct with lattice parameters a = 3.66 and c = 6.17A. Samsonov et al.5 reported the melting point of YC2 as 2300" * 50°C. Recently Bowman et a1.6 found a transformation in the dicarbide from the tetragonal to an fcc form at 1320 20°C. Samsonov and coworkers7 reported a monocarbide of yttrium melting at 1950" * 20°C and also a sesqui-carbide melting at 1800" * 50°C. The existence of the latter has also been indicated by others,1&apos;8 but neither compound has been definitely established. The Y-C phase diagram shown in Fig. 1 was proposed by Chubb and Keller8 in 1964 based on the data available at that time. The tentative nature of this diagram together with the uncertain status of the compounds indicated that additional work on this system was needed. EXPERIMENTAL PROCEDURE Yttrium metal of 99.9 pct purity was prepared for use in this study by the reduction of YCl, with calcium to form a sponge product.9 The major impurities in this material were as follows: 100 ppm C, 150 pprn H, 20 ppm N, 300 to 1000 ppm O, <20 ppm Ca, <100 ppm Cr, <80 ppm Cu, 150 ppm Fe, <30 pprn Mg, <400 ppm Ta, and <100 ppm Ti. Alloys were prepared by arc melting yttrium sponge together with pieces of high-purity graphite rod in a purified argon atmosphere. Homogeneity was insured by repeated melting, inverting the ingot between melts.

Jan 1, 1969

By A. K. Mukherjee, J. E. Dorn, J. D. Mole

Investigations were carried out on the effect of polyslip on the strain hardening of aluminum single crystals. The orientations investigated were those lor which the tensile axis was in the [001], [111], [112], and [012] directions plus another for which the Schmid angles for {111}(110) slip were 1 deg. The experimental data were analyzed on a model based on the intersection of dislocations with particular emphasis on the effect of polyslip on the activation volume for inter-section. It is shown that the rate of strain hardening inreases for those orientations wherein attractive dislocation intersections occur and that those orientations which produce the greater number of such intersections exhibit the greater strain hardening. Good correlation of the data is obtained with the concept that attractive junctions, as proposed by Saada, Play an important role in accounting for the rate of strain hardening. EXISTING concepts on the nature and cause of strain hardening in fcc metals have been deduced principally from experiments on the deformation of single crystals under single slip. The effect of crystal orientation on the shapes of the stress-strain curves for single slip have been summarized by seegerl and more recently by Clarebrough and Hargreaves.2 Tensile specimens whose axes fall near the center of the [001]-[011] line of the standard triangle of the stereographic projection exhibit the longest range of easy glide (Stage I) and the lowest rates of linear hardening (Stage 11) whereas specimens whose axes lie near fie [001]-[111] line of the standard triangle have limited or no easy-glide range and exhibit somewhat higher linear strain-hardening rates. Specimens whose axes lie near the [001] or the [ill] poles do not exhibit easy glide and have the highest rates of linear hardening. Kocks3 has shown that the highest rates of linear hardening Occur under Polyslip when the tensile axis coincides with the [111] or the [ 001] pole. Since the rate of strain hardening is sensitive to specimen orientation and the incidence of polyslip, these relationships might help to discriminate between various dislocation models for strain hardening in fcc metals. Previous attempts to analyze the effect of orientation on strain hardening,1"3 however, did not provide a unique answer to this problem. Consequently the present investigation was undertaken wherein additional data, particularly that for the effect of polyslip on the activation volume for intersection, was also determined in order to provide more complete information on the details of strain hardening. Whereas analyses of these data reveal that several recommended models for strain hardening are at variance with the facts, good correlation of the data is obtained with the concept that attractive junctions4 play an important role in accounting for the rate of strain hardening. I) EXPERIMENTAL APPROACH seegerl demonstrated that slip in fcc crystals at low temperatures is dependent on thermally activated intersection of glide dislocations with forest dislocations. This has been confirmed by tests on single crystals of aluminum by Mitra, Osborne and Dorn5 and on polycrystalline aluminum by Mitra and Darn.&apos; Thus in accord with Seeger&apos;s theory, the shear strain rate, ?, below a critical temperature, T, is where .V is the number of points of contact per unit volume between forest dislocations and glide dislocations, A is the area swept out per successful intersection, b is the Burgers vector, v is the frequency of vibration of the segment of the glide dislocation undertaking intersection, U is the activation energy for intersection, k is Boltzmann&apos;s constant, and T is the absolute temperature. For aluminum, which has an extremely high staeking-fault energy, the constriction energy is negligibly small and therefore the activation energy decreases practically linearly with the stress according to as will be recomfirmed later, where Uo is jog energy at the absolute zero, G and Go are the shear moduli at the test temperature T and O°K, respectively, L is the spacing of the forest dislocations, t is the applied shear stress for slip, and tGo is the stress field that must be surmounted athermally.

Jan 1, 1965

By Ralph E. Esarey, Robert G. Reno

DriLLing activity and prospecting for oil and gas increascd in Indiana in 1941 over the previous year. The greater part of the drilling and development continued to centralize in the Indiana portion of the Interior Coal Basin, in the southwestern part of the state, but other parts of the state were not neglected. Many wildcat wells were drilled, including a series of core tests through the mantle of drift on the southern flank of the Michigan Basin. These core tests have been followed by several unsuccessful production tests. Production tests were made also along the axis of the Logansport-Kankakec branch of the Cincinnati Arch. In all, 411 field locations and 141 wildcat wells were completed in Indiana during 1941; that is, a total of 552 wells, an increase of 3 2 wells over the previous year. The field tests resulted in 260 oil wells, 57 gas wells, and 94 dry holes; wildcats included 16 oil wells, 3 gas wells and 122 dry holes. At the end of the year, 53 field wells and 34 wildcats were drilling. Gibson and Posey Counties led the state, with 154 and 155 wells drilled, respectively. However, 125 wells produced oil in Gibson County, while 98 produced oil in Posey County. Twenty-five per cent of all wells drilled were wildcat; II per cent of these produced oil and 5 per cent produced gas. Grifin field continued to lead in drilling activity, with 157 successful wells and 20 dry holes (including important wells defining the field). Production is found in five pay zones (Tar Springs, Waltersburg, Elwren, Aux Vases and McClosky). It produced a major part of Indiana&apos;s estimated 7,200,000 bbl. of oil during the year. Heusler field, Posey County, expanded with 11 oil ells and 4 dry holes in the Waltersburg and Tar Springs. Vienna field, Posey County, completed four oil producers in the Mansfield sandstone, between 1200 and 1250 ft. The College field, discovered late in 1940, received three oil producers and two dry holes in the Aux Vases. Two new fields were discovered in Posey County during the year: Lamott pool, in the Tar Springs, at 1950 ft., had initial production of 55 bbl. on discovery. One producer and one dry hole have been drilled since. Mt. Vernon pool found saturation in both the Waltersburg and Cypress formations. The discovery well tested about 1000 bbl. per day; it tested the McClosky at 2764 ft. Seven producers have been drilled since the October discovery. Welborne-Switch pool found oil in the Cypress sand at approximately 2500 ft., with an initial production of 33 bbl. One more well in the area proved a dry hole. Gibson County had the following discoveries in 1941: The Patoka field was opened by a McClosky producer of 300 bbl. Another producing well has been drilled. An attempt was made to extend the Illinois Mt. Carmel field into Gibson County, Ind., and one producer of 24 bbl, was completed on the Indiana side. A dry hole has since been drilled, one location south. One small well was completed in the Mans. field at 1105 ft. in sec. 31, T.2 S., R.12 W., Gibson County promising a new field

Jan 1, 1942