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By Ivan Simon, R. K. McConnell

Anticipating the availability of tiltmeters suitable for use in boreholes, this article proposes a method of using one or more of these meters to determine in situ stress distribution before and after mining operations. Several ways of using relief techniques to measure in situ stresses in rocks have been developed. These techniques, summarized by Merrill,1 involve measuring deformations which take place when a specimen of rock is wholly or partially isolated from the stress field in the surrounding rock. Measurements of rock deformation caused by stress relief from mining operations can, in principle, also be used to estimate in situ stress distributions. Müller2 has mentioned experiments being carried on in Austria with a "deformation indicator" to determine the tilting of holes drilled before a mine opening is made. Similar work using borehole extensometers has been reported by Potts? and Duvall4 has called attention to the possible use of tiltmeters in making these measurements. Considerable attention is now being paid to the use of tiltmeters in detecting rock deformation associated with fault movements, earthquakes, earth tides, etc. The instruments used for these measurements have usually been of the mercury tube, water tube, or quartz fiber type, but because of their large size, and/or fragile nature, such instruments would not be suitable for use in mining stress measurements. Recent instrumentation developments, however, give promise that rugged, sensitive tiltmeters small enough for use in boreholes may soon be available.' In anticipation of these developments, this article presents a number of calculations of the possibility of using one or more tiltmeters emplaced in a drill hole prior to mining operations to determine the in situ stress distribution both before and after a mining operation. Consider point p (x, z) near a tunnel of radius a

Jan 1, 1969

By Paul A. Filteau

Asbestos ranks among the leading minerals produced in Canada. It is also mined in Russia, Rhodesia, South Africa, Cyprus, Italy, the U.S.A., Japan, China and several other countries. The most abundant variety, chrysotile, and also the most valuable form of asbestos produced, makes up 90% of the world's supply. In Canada, chrysotile is found in the provinces of British Columbia, Ontario, Newfoundland as well as in Quebec, the latter accounting for almost 90% of all the fibre produced in this country. A number of developments emerging this year could make 1968 a record production and export year for Canada's asbestos mining industry. Asbestos fibre consumption in increasing in the U.S., Canada, up 10% to date this year, Japan and in Latin America. Demand in Western Europe is again on the upswing, following a cut-back last year. As a result, shipments from Canadian mines for the first eight months of this year reached some 916,968 tons versus 873,402 in 1967, an increase of 43,566 tons or 5%. Indications are that Canadian asbestos production will for the first time ever top 1.5 million tons in 1968.

Jan 1, 1969

By P. S. Katval

It is interesting to note that an attempt has been made to rationalize the effect of prestrain on the strength of Hastelloy X-280 after various aging treatments. However, two points raised by the authors seem to be somewhat unclear. 1) Concerning their Fig. l(a), the authors state: "Extensive dislocation networks are still in evidence. The 24-hr aging at 1500°F and the 15-min soak at 1350°F did not eliminate the dislocations introduced by the 20 pct cold reduction." This is, of course, to be expected since complete "elimination" of dislocations would require recrystallization which does not occur at 1500°F in Hastelloy X. However, recovery

Jan 1, 1969

By Kiyoshi Azuma, Hiroshi Kametani

The variation of the dissolution behavior of a ferric oxide with calcining temperature has been investigated. Samples were prepared by thermal decomposition of ferric hydroxide, nitrate, oxalate, and sulfate at low temperature, followed by the calcination in the temperature range between 600" and 1200°C. The samples of eight series and a fine crystalline sample of hematite were dissolved in 1 N hydrochloric acid at 55.2°C and the results are represented on double-log graphs for convenience. It is confirmed that all dissolution courses follouj either the accelerated process or the parabolic process except in the special case of the crystalline hematite which dissolced in accordance with the uniform dissolution of a particle. Examinations of the physical properties of the oxide powders revealed that the surface area measured by the permeability method is strikingly relevant to the dissolution behavior of the oxide. In the previous paper,' detailed data were presented on the effect of the kind of acid, the solution temperature, and the concentration of acid on the dissolution of two ferric oxides. It was also shown that these sam ples dissolved in strikingly different ways. The present investigation was carried out on the dissolution of various calcined samples prepared from various ferri salts by various methods to ascertain the course of dissolution. Pryor and Evans2 pointed out a change of the dissolution rate at around 700°C for a series of calcined ferric oxides prepared from the hydroxide. Several papers374 reported also the dissolution of ferric oxide samples. It seems, however, that a systematic account of the relationship between the dissolution behavior and physical properties of the oxide has not yet been given. This paper presents the variation of the dissolution of the oxide in relation to the calcining temperature and the change of physical properties of the calcines. EXPERIMENTAL Raw materials were prepared by precalcination of ferric hydroxide, thermal decomposition of ferric nitrate, oxalate, and sulfate, and aerial oxidation of ferric chloride vapor, at as low a temperature as possible. The products were crushed, ground, if necessary, and sieved with a 100-mesh Tylor screen prior to calcination, after which the specimens were dissolved in acid solution. The following is a detailed description of the preparation of the samples. Sample H. About 500 g of ferric chloride (guaranteed reagent) were dissolved in 5 liters of deionized water and filtered. Ferric hydroxide was precipitated by addition of the minimum amount of ammonium hydroxide solution, and the precipitate was washed continuously till chloride ion was not detected by silver nitrate solution, and then filtered. The filter cake was dried at 120°C for a week and ground, and the -100 mesh portion was used. Sample S. Ferric sulfate (guaranteed reagent) was pyrolytically decomposed in a crucible at 700°C for 24 hr and the product was sieved. In this case the following calcination was carried out at temperatures over 700°C. Sample B. Commercial ferric oxide (guaranteed reagent). About 15 kg of ferric nitrate were decomposed in a furnace maintained at 800°C for 2 hr. The actual temperature of the decomposition was not measured. The product was crushed and sieved, and the -100 mesh portion was used. Sample N. About 50 g of ferric nitrate (guaranteed reagent) were decomposed in a beaker in a sand bath until a red-brown dense solid was produced. This product was crushed and sieved, and subjected to complete decomposition at 500°C. The precalcined product was again sieved and used. Sample N2.5. Since the decomposition temperature was not controlled for sample AT, a different sample was prepared in a temperature-controlled furnace. The subscript represents the decomposition at 250°C. The product was treated in the same manner as sample N. Sample Nc. Under atmospheric pressure it is prac-tically inevitable that ferric nitrate hydrate melts to form a brown liquid at about 50°C before pyrolysis. For this reason, the salt was first slowly heated under reduced pressure (about 10-3 mm Hg measured in a trap refrigerated by dry ice-alcohol) to achieve dehydration without melting. About 5 hr were required for the dehydration and the partial decomposition. Then the temperature was elevated to 500° C in air for complete decomposition. The relatively porous product was sieved and used. Sample Ov. About 200 g of ferric oxalate hydrate (extra pure) were dehydrated under reduced pressure (as described above) followed by thermal decomposition at 500°C for 6 hr in air. The decomposition of this salt was accompanied by liberation of carbon monoxide, by which the ferric salt was initially reduced to a black powder. The powder changed in turn into brown ferric oxide as the gas liberation decreased and reoxidation predominated. The product consisted of sparkling fine particles passing through a 100-mesh screen. However it was ground and sieved as for the other samples. Sample D. Commercial fine powder for magnetic tape purposes. The preparation was as follows.5 Ferric chloride vapor and preheated excess air were mixed and passed into a reaction tube where oxidation took place at 450°C. The fine powder formed was collected in a cottrell chamber. The product was vacuum-degassed at 450°C for 1 hr and sieved.

Jan 1, 1969

By K. E. Gray, M. S. Seth

In Part I of this work,1 equations of elasticity were formulated for transversely isotropic, axisymmetric, homogeneous, porous media exhibiting pore fluid pressure. Equations of elasticity and the thermal analogy method were used to determine transient horizontal, tangential, and vertical stresses and radial displacement in a semi-infinite cylindrical region when either a constant rate of pressure or a constant rate of flow is maintained at the wellbore. In this paper, the approach presented earlier is extended to finite reservoirs for the cases of (1) steady-state flow, (2) constant pressures at the well bore and outer boundary and (3) constant pressure at the wellbore and no flow at the outer boundary. Results of this work show that radial and tangential stress gradients are high near the wellbore but diminish rapidt; away from the well; the vertical stress gradient behaves in the same way but is less severe. Radial stresses are compressive or neutral, whereas tangential and vertical stresses may be tensile, neutral or com-pressive, depending upon the boundary conditions, the physical Properties of the system and the radial distance involved (vertical stresses are always compressive in an unbounded system1. For constant boundary pressures, both radial and tangential stresses increase with time whereas they both decrease for a closed outer boundary and constant pressure at the wellbore. The vertical stress decreases with time for both systems. For steady-state systems, radial displacement may be positive or negative, depending upon the dimensions of the system, the pressure differential and the porosity. Radial displacement may be positive or negative for a closed outer boundary but is positive for constant pressures at both boundaries. INTRODUCTION The importance, utility and complexity of a realistic appraisal of the stress state at and local to a wellbore were indicated in Part I. In this paper the analytical approach presented earlier is extended to finite, cylindrical reservoir geometry for the cases of (1) steady-state flow, (2) constant pressures at wellbore and outer boundary and (3) constant pressure at the wellbore and no flow at the outer boundary. Other than the outer boundary of the reservoir being finite, the physical system and assumptions pertinent thereto are the same as before. The reader may wish to review the mathematical development through Eq. 49 of Part I before proceeding here. SOLUTION FOR GENERAL BOUNDARY CONDITIONS THERMAL STRESSES AND DISPLACEMENTS Since normal stresses do not exist at the free boundaries of a system subjected to thermal stresses, the boundary conditions are

Jan 1, 1969

By R. E. Reed-Hill, W. H. Hartt, W. A. Slippy

An unusual form of double kinking has been observed at the ends of {1121} twins in deformed zirconium. These kinks lie partly outside of the twin and partly inside. While they are undoubtedly closely associated with accommodating the twinning shear into the matrix, they are apparently closely related to other important aspects of twin growth. A mechanism is proposed for {1121} twin growth involving interactions between 1/3 (1120) dislocations in the bend planes and twinning dislocations. It is also shown that boundaries without long range strain fields develop at the tapered ends of the twins. The {1121} twins can, therefore, grow without forming high-energy noncoherent twin boundaries containing large numbers of closely spaced twinning dislocations. NUMEROUS investigators have indicated that slip is often closely associated with deformation twinning. An example is twin accommodation kinking,1-3 where dislocations form bend planes and permit accommodation of a twinning shear within the parent crystal. Another is the incorporation of slip dislocations into twins, as proposed by Sleeswyk and verbraak4 and Ishii and Kiho5 for iron and ß-tin, respectively, and observed in hcp metals by Price.6 In addition, it has been shown that shear discontinuities exist at the points of twin intersections in zinc,7 magnesium,8 titanium,9 ß-tin,10 and bismuth," where the continuity conditions for twin intersections, originally proposed by cahn,12 are not satisfied. A similar situation occurs for zig-zag (1121) twins in zirconium13 and ?-phase silver-aluminum alloys,14 where the twinning shears of the two component twins are not parallel. In all these latter cases additional deformation by slip is believed to accommodate the twinning shear discontinuity. The present paper is concerned with a newly observed aspect of the slip and twinning interrelation, in which two kinks, one inside the twin and the other external to the twin, are formed. These kinks, observed in conjunction with (1121) twinning in zirconium, form to accommodate the twinning shear. A model has been constructed explaining the growth and accommodation of (1121) twins in terms of these kinks. This mechanism may be significant since it is concerned with an important twin mode, which occurs not only in zirconium but also in titanium and hafnium. The practical significance of (1121) twinning has been adequately demonstrated. At 77° K the high ductility of zirconium containing a large number of grains unfavorably oriented for slip is primarily due to (1121) twinning.'5 Also, (1121) twins nucleated at 77°K may grow during further deformation at room temperature. This growth can greatly increase the transverse ductility15 as well as produce large mechanical hysteresis effects.= EXPERIMENTAL PROCEDURE Arc-melted, sponge zirconium plate previously described17 was prestrained 0.65 pct at 77° K by cold-rolling to introduce {1121} twins into the structure. Tensile specimens were cut with axes normal to the plate rolling direction. These specimens were pulled in tension to near the point of failure in an Instron machine at room temperature at a cross-head speed of 2 x10-2 in. per min. This additional deformation caused growth of the twins nucleated by prestrain. Deformed specimens were then prepared for metallo-graphic examination. This included an anodizing treatment18 that made the surfaces sensitive to polarized light, permitting small lattice rotations to be revealed. EXPERIMENTAL RESULTS Nature of the Twin-Kink Band Structure. Fig. 1 is a photomicrograph of a typical specimen after prestrain at 77° K. The structure is characterized primarily by long, narrow, parallel sided (1121) twins which norma1ly traverse the entire grain. Fig. 2 shows several (1121) twins after additional straining at room temperature. These lie near the center of the polarized light photomicrograph and are inclined upward to the right. It is evident that this latter deformation has resulted in appreciable twin growth. The dark regions extending from the ends of these twins are accommodation kinks. The difference in reflected light intensity indicates the

Jan 1, 1969

By P. Bolsaitis, L. Skolnick

Vapor pressures of silver over ternary alloys of six different copper to gold ratios have been measured by means of the Knudsen effusion technique. The data obtained in the temperature range of 1330° to 1375° have been used to estimate the integral excess free energies of the ternary alloys and the activities of copper and gold. The results compare favorably to the predictions based on the electron cell model of alloys recently formulated by the authors. THE orifice effusion method for measuring vapor pressures of materials in condensed phases was first introduced by knudsen, and has since been used extensively for the determination of thermodynamic properties of condensed phases. The basis of the measurement is the effusion, through a small orifice, of vapor in equilibrium with a condensed phase. Assuming free molecular flow into high vacuum, the vapor pressure, P (in mm Hg), of the effusing species is calculated from the following equation:' where w (g) is the weight of effusing species lost during a run, t (sec) the time length of the run, A, (sq cm) the area of the effusion orifice, T ("K) the temperature at which the run is conducted, M the molecular weight of the effusing species, and k the Clausing factor, a constant that corrects for deviations from free molecular flow caused by the finite thickness of the orifice walls.17 The determination of partial and integral thermodynamic variables from vapor pressure data of ternary alloys is possible only if the vapor pressures of all but one component are negligible or can be esti-

Jan 1, 1969

By E. H. Erwin Gartner

The Rhenish lignite deposit in the Nordrhein-Westphalia province of the German Federal Republic covers an area on the left bank of the Rhine River of about 970 sq miles (Fig. 1). Here, in the Miocene era, some 20 million years ago a lignite seam was formed and later broken, through tectonic movements into several blocks, some thrown down into depths of over 1,500 ft. This deposit consists of a single seam, in places up to 300 ft thick, but averaging about 150 ft. In a few areas, it is split into as many as five seams, separated by barren strata. It contains about 60 billion tons (2000 lb/short ton) of lignite which, however, being relatively young geologically, has, because of approximately 60% moisture, 2 to 8% ash, and low sulfur, a net calorific value of 3,340 Btu. That calorific value increases, however, with rising thickness of the cap rock. About one-third of the yearly production of 90 to 100 million tons of raw lignites is converted into briquets. Raw lignite is pulverized and dried to about 18% water content and then pressed without binder into briquets under a pressure of about 14,000 psi. The briquets are being used primarily for residential heating; their sales, however, have been declining sharply since 1963. On the other hand, the volume of raw lignite used in steam power plants has been rising steadily and amounts at present (1968) to about two-thirds of the total production. Huge steam power plants, such as Frimmersdorf, shown in Fig. 2 (which, with an installed capacity of 2,600 MW [megawatt], represents the world's largest steam power plant) with a generating capacity of up to 300 MW per unit and a total installed capacity of over 6,000 MW, contribute about 26% of the total electric power production of the German Federal Republic.

Jan 1, 1969

By B. Chalmers, Stefan Wojciechowski

Rotary oscillation of the mold has been used to produce mechanical stirring of the melt during unidirectional solidification. Al-Cu alloys (1 to 4 wt pct Cu) were solidified to study the influence of alloy composition, temperature at which intensive cooling was initiated, and intensity of stirring on the temperature distribution in the sample, the resulting structure, and the copper microsegregation at the columnar to equiaxed transition. The Proposed explanation for the equiaxed solidification in stirred castings consists of the melting off of dendrite fragments, their partial remelting in hotter liquid, and the subsequent growth of the surviving part when the temperature of the melt is lowered. This may result in the formation of a crystal network, which can stop the growth of the columnar crystals and produce the equiaxed zone. It has long been known and many times affirmed that ultrasonic vibrations or relative motion of liquid and solid can significantly reduce the length of the columnar zone and refine the grains in the equiaxed zone in ingots and castings. Because of the technological importance of these phenomena many investigations have been conducted in which ultrasonic energy or mechanical vibration,1-6 electromagnetic stirring,7"10'17 magnetic stirring,"'12 or mechanical stirring13'14 were used to produce the relative liquid-solid motion. More recently, the question of the importance of natural (or thermal) convection has been raised.15-l7 Several possible mechanisms have been suggested.l,8,18-20 They can be divided into two main groups. The first group includes such nucleation hypotheses as nucleation frequency enhancement due to cavitation at the mold wall or other surfaces; cavita-tion in the body of the liquid resulting from the pressure wave, or an agglomeration mechanism, which involves the formation of nuclei by the accretion of subcritical nuclei. The second group considers the grain-refining action to be due to crystal multiplication phenomena such as the removal of the dendrite fragments by viscous forces or by a high-pressure cycle following cavitation or by a melting-off process. Sbme recent investigations give good experimental support to the melting-off proposa1.21-23 The purpose of the present study was to examine the effect of mechanical stirring during the unidirectional solidification on the structure of alloy samples and on the solidification variables. The motion of the liquid was produced by rotary oscillation of the mold around its vertical axis.

Jan 1, 1969

By S. R. Goodman, Hsun Hu

A detailed study of texture developmenf in poly crystalline copper atzd 70-30 brass has been completed. Textural changes as a function of deformation are shoum by pole jigmres and by intensity measurements oF- various rejlectiotzs from the rolling plane and the rolling direction. These examinations were accompanied by measurements of stacking fault frequency, hardness changes, and microstructure. Some of the results were briefly presented earlier. Additional results reported here are consistent with the idea that deformation faulting or slip by partial dislocations is of primary importance in the formation of deformation textures in fcc metals. lo examine the idea that deformation faulting is of primary importance in determining whether the texture is the copper type or the brass type an extensive study of the development of polycrystalline textures in copper and 70-30 brass was initiated. Besides the determination of complete pole figures, the intensities of the various reflections from both the rolling plane and the plane perpendicular to the rolling direction, the peak shifts due to deformation stacking faults, and the hardness of the rolled specimens were examined at various reductions from 10 to 99 or 99.5 pct. Mi-crostructures were examined by transmission electron microscopy. Some of the results were briefly presented in an earlier publication.' Since then, additional information has been obtained. This is given in the present paper. EXPERIMENTAL PROCEDURE Material and Specimen Preparation. The material used was a commercial electrolytic copper bar 1i in. wide and 2 in. thick and a 70-30 brass bar la in. wide and 1i in. thick. Chemical analysis indicated a purity of 99.97 pct for the copper, with 0.025 pct 0 as the major impurity. The 70-30 brass was of higher purity with 0.0016 pct 0 as the major impurity. Extreme care was taken in the preparation of the starting material to insure uniformly fine grains with a nearly random initial texture. The two bars were first cold-forged and then annealed to eliminate any original texture. The grains were then refined by several cold rolling (approx 30 pct reduction) and annealing treatments. The + -hr anneals were carried out in a salt bath at 390" to 440°C for copper and at 490°C for brass. The resulting penultimate grain size was 0.06 mm for copper and 0.03 mm for brass, and both showed very little preferred orientation. The number of prior cold rolling and annealing cycles was such that the final thickness after various final reductions of 10 to 95 (for brass) or 99 (for copper) pct was the same (0.020 in.). These annealed strips were rolled in two directions by reversing end for end between passes according to the following schedule: 0.006 in. per pass to 0.100 in., 0.003 in. per pass to 0.050 in., 0.002 in. per pass to 0.025 in., 0.001 in. per pass to 0.020 in. Texture Determination. The development of rolling textures was studied by examining complete pole figures determined from the (111) reflection. Specimens thinned from one face of the strip to half thickness (0.010 in.) were used to obtain the central portion of the pole figures, while specimens thinned from both faces to 0.003 in. were used to obtain the peripheral portion. The reflection and transmission techniques have been described previously. In addition to X-rav pole figures, texture development was also studied b; examining the intensity variation of the (Ill), (200), (2201, (311), (331), (420), and (442) reflections from the rolling plane and from the plane normal to the rolling direction, as a function of deformation. The same specimens used for the central portion of the pole figures were used for the intensity measurements of the various reflections from the rolling plane. For intensity measurements from the plane normal to the rolling direction, composite specimens were prepared by mounting sections cut parallel to the transverse direction of the strip. An epoxy resin was used to bond these sections together, and the entire composite was then mounted in a cold-setting resin to facilitate subsequent polishing and etching to remove distorted metal at the cut. The intensities were expressed in units of the integrated intensities measured from an annealed copper specimen having almost no preferred orientation. Stacking Fault Frequency Determination. Following the analysis of Warren: the stacking fault frequency, a, was determined from the change in the peak separation (A%) of two neighboring reflections of a deformed specimen, as compared with the normal peak separations of a fully annealed specimen. To obtain sufficient intensities for the second-order reflections, (222) and (400), composite specimens were prepared from parallel sections cut from the strip at 30 deg to the rolling direction for copper and 25 deg for the brass.* From texture data, these sections are known to contain a large population of both (111) and (200) planes. Since residual stresses can also cause X-ray line shifts (the direction of line shifts depends upon the sign of the stress), the use of composite specimens consisting of sectioned planes should help compensate for these effects as the residual stresses change sign from the surface to the central section of a rolled strip. Since the amount of peak shift is almost un-measurable in brass rolled 15 pct and in copper rolled

Jan 1, 1969

By L. V. Pirela, S. M. Farouq Ali

Some interest has been expressed recently in the application of solvents in conjunction with a thermal drive, such as a steamflood. At least one field project of this type has been reported. This paper makes the first attempt to provide some of the basic information necessary for choosing a solvent for such an application. Results of displacements conducted at elevated temperatures are also discussed. This paper shows that, in the case of alcohol-hydrocarbon-water or brine ternary systems, the system miscibility may increase, decrease, or both increase and decrease within the same system when the temperature increases. The distribution coefficient was consistently found to increase in favor of the oleic phase with an increase in temperature, which is advantageous from the standpoint of oil recovery. Results of solvent displacements in a sandstone core showed that even a relatively small temperature effect in the favorable direction (increase in miscibility and distribution coefficient) can lead to a 50 percent increase in oil recovery. On the other hand, if the system miscibility decreases with the temperature, even though the distribution coefficient increases, the oil recovery at the higher temperature may not increase. INTRODUCTION Miscible displacement has been the subject of many investigations. Miscible-phase solvent flooding, employing solvents such as alcohols that are miscible with both oil and water, has received considerable attention. Investigations conducted by Gatlin and Slobod,l Taber, Kamath and Reed,2 Holm and Csaszar,3 and Farouq Ali and Stah14 have helped in understanding the mechanism of solvent flooding. While the use of alcohols and similar solvents as oil recovery agents is economically unattractive, these solvents nevertheless provide a means of understanding the mechanistic aspects of important miscible-phase oil recovery processes such as the Maraflood process (discussed by Gogarty5). As shown by Taber et a1.,2 the phase behavior of a solvent-oil-water system is of .utmost importance in determining the efficiency of the oil displacement. This paper makes the first attempt to obtain the ternary phase behavior data for nine alcohol-hydrocarbon-water/brine systems at elevated temperatures. Results of core tests at elevated temperatures are also presented which corroborate the effect of temperature on oil recovery, as judged on the basis of phase-behavior data. The use of solvents at elevated temperatures has been suggested earlier by Farouq Ali.6 At least one field test of this type has been reportedO7 With the widespread use of thermal recovery techniques, it is possible in some situations (especially in steamflooding) that the use of a suitable solvent in conjunction with the heat carrier may be economically feasible. This paper attempts to provide some of the basic information needed for judging such feasibility. LOCATION OF THE PLAIT POINT The phase behavior of a typical ternary system consisting of a solvent, hydrocarbon and brine (or water) can be represented by a triangular diagram such as the one shown in Fig. 1 (for temperature TI). Point Pon the binodal curve represents the plait point, being the limit of tie lines such as Y1 Y2 The compositions of the coexisting oleic and aqueous phases are given by points Y2 and Y1, respectively, for any mixture composition along Y1Y2. The characteristics of ternary diagrams have been discussed by Findlay8 and others. Taber et aL3 have shown that the position of the plait point in a particular ternary system plays the decisive role in determining whether or not theoleic phase would be displaced in a continuous manner during an alcohol displacement. The area above the binodal curve also is important, since it represents

Jan 1, 1969

By D. Webster

It has been found that cold work and annealing treatments greatly retard subsequent grain growth and re-crystallization in thoria-dispersed nickel and NiCr. It is suggested that this is due to cavities which form at the particle-matrix interface durilzg cold work. Some of' the cavities formed are stable at elevated temperatures and prevent the mouement of large-angle grain boundaries. The movement of these boundaries at elevated temperatures is known to start recrystal-lization and when they are pinned by voids recrystal-lization is made more difficult. TD Nichro,me had a maximun resistance to recrystallization when the initial structure was coarse-grained and had a low dislocation density. A precipitation reaction occurred between 700° and 1200° F in cold-worked TD Nichrome. It has been shown by Grant and his coworkers1-3 that a large part of the strength of dispersion-hardened materials is a result of the cold-worked structure produced during fabrication. In a comparison of the strength of cold-worked copper with and without an oxide dispersion, Grant4 has demonstrated that there is little difference in strength at room temperature. The function of the dispersion is essentially to maintain the cold-worked structure at higher temperatures than is possible in the base material. The dispersion accomplishes this by making recrystallization more difficult. The mechanism by which this is achieved is discussed in this paper. The fabrication history of the material has been found to greatly influence recrystallization behavior and this aspect is discussed in some detail. I) MATERIAL Three different thoria-dispersed materials were examined. 1) DuPont 2 pet thoria-dispersed nickel (TDNi) in 0.050-in. seeet. Thoria particle size is in the range 100 to 2500A. 2) DuPont 2 pct thoria-dispersed nichrome (20 pet Cr, 80 pct Ni) (TDNiC) in 0.125-, 0.060-, and 0.040-in. sheet. In the as-received condition these sheets have

Jan 1, 1969

By M. J. Pool, P. J. Spencer, J. R. Guadagno

THE present work was carried out as part of a general program to study the magnitude and concentration dependence of exothermic heats of solution of various metals in liquid tin. Thermodynamic data for the Te-Sn system are very limited, particularly for dilute alloys. Indeed, apart from the prior heat of solution determinations of Pool,1 the only other published values are those of McAteer and seltz2 who carried out electromotive force measurements on solid alloys of compositions from 75 to 95 at. pct Te at temperatures between 543° and 668° K, of Colin and Dro-wart3 who made mass-spectrometric studies of the vapor in equilibrium with solid SnTe, and of Robinson and Bever4 who determined the heat of formation of SnTe by solution calorimetry. The present work thus provides further thermodynamic information for this system, specifically in a temperature range where the solubility of tellurium is very limited. The liquid metal solution calorimeter used in this investigation has been described previously.' No further discussion of its design or operation will therefore be given here. For each series of measurements a tin bath consisting of approximately 70 g of 99.99 pct pure Sn was carefully weighed out and inserted in the calorimeter which was maintained at the desired temperature to within ± 1/4°c. Tellurium, of 99.999 pct purity, was supplied by Atomergic Chemetals Co., a division of Gallard-Schlesinger Chemical Manufacturing Corp. Approximately 0.0006 to 0.001 g-atom specimens of tellurium were used for each experimental run and these were added to the calorimeter from a temperature of 273" K. Heat of solution values were calculated by analysis of a strip-chart recorder plot of the heat effect accompanying the solution of each sample in the tin bath. The heat capacity of the latter was determined at regular intervals during a series of tellurium drops by using pure tin or tungsten calibration samples, the heat contents of which were obtained from the standard compilation of Hultgren et al5 The composition of the bath was calculated after each drop from a knowledge of the weights of tin and tellurium added. Values of the heat of solution of tellurium at 725" and 775° K are listed in Table I together with the corresponding tellurium contents of the alloys. The data are also plotted as a function of tellurium concentration in Fig. 1, which includes the equivalent data obtained by pool' at 750° K. It can be seen that the heat of solution remains

Jan 1, 1969

By Charles E. Lundin

Pressure-temperature-composition data were obtainedfor the Er-H system. Measurements werecar-ried out in the temperature range of 473° to 1223°K, the composition range of erbium to ErH,, and the pressure range of 10-5 to 760 Torr. Solubility relationships were established from these data throughout the system. Three solid-solution phases were delineated: metal solid solution, dihydride phase, and trihydride phase. The trihydride Phase decomposes at about 656°K and 1 atm pressure. The dihydride phase is stable to about 1023°K, but becomes more deficient in hydrogen above this temperature. The equilibrium decomposition pressure-temperature relationships in the two-phase regions, erbium solid solution plus dihydride and dihydride plus trihydride, were deter- The differential heats of reaction in these two regions are AH = - 52.6 * 0.3 and - 19.8 i 0.2 kcal per mole of Hz, respectively. The differential entropies of reaction are AS = - 35.2 * 0.3 and - 30.1 * 0.4 cal per mole HZ.deg, respectively. Relative partial molal and integral thermodynamic quuntities were calculated in the system to the dihydride phase. RARE earth metal-hydrogen systems have been the subject of general survey,1"4 and all have been found to form hydride phases. The heavy rare earths, of which erbium is a member, form dihydride and trihydride phases with different crystal structures, whereas the light rare earths form only a single-phase dihydride which expands without structure change, as hydrogen is added, to the trihydride composition. These materials are of interest primarily because of their theoretical properties, such as bonding, defect structure, and thermodynamic and electronic characteristics. Erbium has been studied in several previous investigations.5, 6 It was deemed desirable to more thoroughly and accurately define the system, both for the phase equilibria and the thermodynamic properties. I) EXPERIMENTAL PROCEDURE A Sieverts&apos; apparatus was employed to conduct the experimental measurements. Briefly, it consisted of a source of pure hydrogen, a precision gas-measuring buret, a heated reaction chamber, a mercury manometer, and two McLeod gages (a CVC, GM 100A and CVC, GM 110). Pure hydrogen was obtained by passing hydrogen through a heated Pd-Ag thimble. The hydrogen was analyzed and found to have only a trace of oxygen and nitrogen. A 100-ml precision gas buret graduated to 0.1-ml divisions was used to measure and admit hydrogen to the reaction chamber. The reaction unit consisted of a quartz tube surrounded by a nichrome-wound furnace. The furnace temperature was controlled by a recorder-controller to ±1°K. An independent measurement of the sample temperature in the quartz tube was made by means of a chromel-alumel thermocouple situated outside, but adjacent to, the quartz tube near the specimen. Pressure in the manometer range was measured to ±0.5 Torr and in the McLeod range (10-4 to 10 Torr) to ±3 pct. The hydrogen compositions in erbium were calculated in terms of hydrogen-to-erbium atomic ratio. These compositions were estimated to be ±0.01 H/Er. The erbium metal was obtained from the Lunex Co. in the form of sponge. The metal was nuclear grade with a purity of 99.9 pct +. The oxygen content was reported to be 340 ppm and the nitrogen not detectable. Metallographically the structure was almost free of second phase (<1 vol pct). A quantity of sponge was arc-melted for use as charge material. The solid material was compared with the sponge in the pressure-temperature-composition relationships. They were found to be identical. Therefore, sponge material was used henceforth, so that equilibrium could be attained more rapidly. The specimen size was about 0.2 grain for each loading of the reaction chamber. The procedure employed to obtain the pressure-temperature-composition data was to develop experimentally a family of isothermal curves of composition vs pressure. First, a specimen of erbium was wrapped in a tungsten foil capsule to prevent contact with the quartz tube. After loading the specimen, the system was evacuated to less than l0-6 Torr, flushed several times with high-purity hydrogen, and evacuated again ready for the start of the experiment. The furnace was then brought to the desired temperature. A measured amount of hydrogen was admitted into the chamber. Equilibrium was allowed to be attained, the pressure read, and the process then repeated many times until 1 atm of gas pressure was finally reached. Other isotherms were then developed in the same manner. The partial pressure plateaus were determined by another manner. In the solid solution-dihydride region a composition of approximately 1.0 H/Er was selected on the plateau. The temperature was varied throughout the range of interest. At each temperature level, equilibrium was achieved, the pressure read, and the next temperature attained. The temperature was cycled both up and down. In the dihydride-trihy-dride region, the plateaus were determined in the 473" to 651°K range only by heating to the desired temperature and not by both heating and cooling. The data were much more reproducible in this manner. Equilibrium required long periods of time. Specimens were initially hydrided to 2.8 H/Er, so that at the higher

Jan 1, 1969

By G. L. Tufford, R. L. Bleifuss

Low-grade manganiferous iron ores of Minnesota&apos;s Cuyuna Range, in general, do not respond to conventional mineral dressing techniques because of their fine-grained texture. Reducing these ores to magnetite with subsequent magnetic separation and flotation have not given satisfactory results because, in many instances, concentrate grade and manganese recovery are low. Metallization of iron and concurrent reduction of higher manganese oxides to MnO, as in the R-N process, followed by recovery of iron by magnetic separation and manganese by leaching, seems to be a technically feasible process. High-temperature x-ray diffraction studies show that solid-state reactions between iron and manganese, with the formation of intermediate iron-manganese oxides, occur during reduction and affect recovery of both iron and manganese from the final product. Solid state reactions also occur between FeO, MnO, and SiO, at temperatures as low as 900°C. The kinetics of these reactions are such that they become an important factor in the treatment of ores by the R-N process. These investigations suggest a temperature and gas composition cycle that would maximize both iron and manganese recovery. During the past ten years, iron ore shipments from the Cuyuna Range of Minnesota have decreased sharp1y. Because of adverse grade, structure, and cost, many Cuyuna ores are no longer competitive with high-grade foreign ores and domestic pellets. The low-grade manganiferous iron ores from the Cuyuna Range, in general, do not respond to conventional mineral dressing techniques because of their fine-grained texture. Reducing these ores to magnetite for subsequent magnetic separation and flotation has not given satisfactory results because concentrate grade and manganese recovery are often low. However, a technically feasible process appears to be metallization of the iron and concurrent reduction of manganese oxides to MnO with recovery of metallic iron by magnetic separation and extraction of manganese from the tailings by leaching. In 1962 the R-N Corp., with a grant from the Area Redevelopment Administration, conducted an amenability study of the metallization of manganiferous iron ore from the Cuyuna Range. The results of this preliminary investigation were sufficient to interest the Economic Development Administration in sponsoring further studies of the process with emphasis on secondary recovery of manganese from the nonmagnetic tailings. Inasmuch as the metallization process has considerable influence on the final form of the manganese - its texture and distribution between the magnetic concentrate and nonmagnetic tailings-the investigation included a study of metallization of the ore as well. Therefore, the investigation conducted at the Mines Experiment Station covered three interrelated phases: (1) laboratory R-N roasting studies and magnetic separation tests, (2) laboratory chemical extraction experiments of the nonmagnetic tailings, and (3) a mineralogical study of the crude ores and their various roast products. High-temperature x-ray diffraction investigation of the Fe-Mn-Si0,-0, system is the main topic of this paper and an extension of the mineralogical work. GENERAL GEOLOGY The Cuyuna Range is known for its complicated geologic structure, complex orebodies, and generally indifferent response to attempts at conventional beneficiation. Several geologists have made intensive studies of the Cuyuna Range, including Leithl (1907), ~darns&apos; (1910), Zapffe3 (1925), Grout and Wolff4 (1955), and schmidt5 (1963), whose study was the most comprehensive of all. The Range is covered with glacial deposits - till, out-wash, and lake sediments -up to 250 ft thick. Bedrock stratigraphic units of the Cuyuna Range consist of three tightly folded Precambrian sedimentary formations. The lower unit is the Mahnomen formation, composed of 2000 or more feet of argillite, slate, siltstone, and quartzite. The middle unit is the Trommald formation, which varies from 45 to 500 ft in thickness and comprises the major iron-bearing formation. The upper unit is the Rabbit Lake formation, consisting of over 2000 it of argillite, slate, and interbedded lenses of lean iron formation. In the central part of the Cuyuna Range, the units have been folded into a series of

Jan 1, 1969

By C. Cronquist

Since April, 1962, Shell Oil Co. has operated a peripheral line-drive waterflood of the 10.750-ft lower Tuscaloosa (Cretaceous) Denkman sand in the Little Creek field. Located in southwestern Mississippi in the lower Tuscaloosa trend, the field was discovered by Shell in Jan., 1958. Among the largest in the trend, the accumulation is controlled stratigraphically and occurs in an extensive series of alluvial-point bar deposits across a nose that dips gently to the south. The crude oil is 39" API gravity and was highly undersaturated at initial conditions. Early production behavior indicated a depletion drive with slight water influx; primary recovery wm estimated to be 25 million bbl, or 24.5 percent of stock-tank oil originally in place. A.s a result of a favorable mobility ratio and remarkably uniform rock properties, the volumetric sweep eficiency in the waterflood has exceeded 90 percent. Despite the high connate water saturation (56 percent), the displacement efficiency by water injection has been quite efficient, contrary to traditional concepts. Based on observed field flood-out performance, ultimate recovery is calculated to be 46 million bbl. As anticipated, the production rate began declining during 1964 due to a continu ing reducrion in the number of producing wells as flood fronts advanced across the field. Cumulative recovery as of Jan., 1968, was 44.8 million bbl; waterflood operations ~hould be complete by 1970. Introduction Most waterfloods described in reservoir engineering literature involve pattern operations, the most common of which is the five-spot pattern. Only occasiona&apos;lly are linear drives described, even though there probably are increasing numbers being put into operation. Increasing use of linear floods may reflect the accelerating trend towards early application of fluid-injection programs when linear drives are more efficient, as was the case at Little Creek. However. the Little Creek operation is unusual in several respects. It is one of a few successful waterfloods conducted in sands with connate water saturations approaching 60 percent, and it is among the deepest successful water-floods being operated anywhere. Development The Little Creek field was discovered in Jan., 1958, in the lower Tuscaloosa trend in southwestern Mississippi (Fig. 1). The discovery well, Shell-Lemann No. 1, was drilled on a seismic closure about 2 miles southeast of lower Tuscaloosa production at Sweetwater. The well was completed in the Denkman sand at 10,752 ft, and on initial potential it flowed 588 BOPD of 39" API crude on a %+-in. choke; psi was 730 and GOR was 442:l. Development proceeded rapidly on 40-acre spacing, and by the end of 1958 the field was producing approximately 9,100 B/D from 56 wells. Almost all this production came from the northern half of the field. The southern part was discovered in Nov., 1958, at a location almost 2 miles from previously established production. Subsequent drilling established an apparent conneotion about half a mile wide between the twd areas. Development of the field was practically complete by 1961 with the drilling of 155 producers and 35 dry holes. Some early wells were completed open hole but moslt are completed with casing cemented through the productive interval and perforated for production. Geology The lower Tuscaloosa structure in this area is a north-south nose with maximum dips of about 2" on the flanks. There is no discernible faulting at the producing horizon. Productive limits of the field are shown in Fig. 2, which is contoured on a marker just above the main productive zone. A common water level at 10,415 ft subsea was logged at both the northwest and southeast ends of the field. There is a gross oil column of nearly 100 ft (Fig. 2). Since there is less than 40 ft of closure, it is apparent that bhe accumubtion is controlled stratigraphically, being limited by a sand pinch-out across the creslt of the nose. The total produc-

Jan 1, 1969

By R. M. Brown, W. J. Murphy, B. M. Kapadia

An investigatiott was conducted to study the influence of nitrogen, titanium, and zirconium on the boron llardenabilzty effect in a low-carbon constructiona2 alloy steel. The experimental steels investigated exhibited a significant variation in hardenability, the variation being dependent on the interactions of boron, titanium, and zirconium with the nitrogen. Only the boron not combined with nitrogen was effective in increasing hardenability. Titanium, and with lesser effectiveness zirconium, combined with available nitrogen, thereby protecting the boron. The hardenabil-ity effect mas related to an empirical expression for the "effective" boron content, P, deduced from experimental evidence of these interactions. The hardenabzlity effect reached a maximum at about 0.001 wt pct 0, and decreased somewhat as P increased further. The physical understanding of this relationship is discussed. FOR many years boron has been added to steels to obtain high hardenability. Although a great deal of research has been conducted on boron-treated steels, certain aspects of the boron hardenability effect have not been fully understood. For instance, the magnitude of the hardenability effect has been observed to vary markedly, depending on the steelmaking technique, even when the amount of boron in the steel was essentially constant. Furthermore, the optimum amount of this element to be added has not been definitely established. A better understanding of the boron hardenability effect is essential because too small an addition of boron is likely to be ineffective, while an excessive amount can cause brittleness&apos;&apos; and hot shortness. The findings of earlier investigations have shown that the hardenability effect cannot be consistently related to the amount of boron added or retained in the steel. Grossmann observed that in a 0.60 pct C steel the hardenability increased to a maximum with mold additions up to about 0.0025 pct B and then decreased with larger additions. Other investigators5 likewise reported a maximum in the hardenability at about 0.003 pct B. Crafts and Lamont, however, found that in commercial open-hearth heats of medium-carbon steel the hardenability increased linearly with boron up to 0.001 pct and remained essentially unchanged with larger percentages up to 0.006 pct. Other investigators7,&apos; also observed a rather constant hardenability effect in the range about 0.0005 to 0.0035 pct B. These observations and other evidence suggest that the effectiveness of boron in increasing hardenability probably depends, in addition to the amount, on the form of boron retained in the steel, this form being influenced by the presence of other elements. Both oxygen and nitrogen apparently exert the strongest influence on the hardenability behavior, since, at the temperature of liquid steel, boron readily combines with these elements, thereby losing its effectiveness as most experimental evidence seems to indicate. For consistent recovery of the boron effective in increasing hardenability, it is necessary that the oxygen and nitrogen in the steel be either reduced to extremely small amounts by the steelmaking practice or neutralized by combination with other elements before the addition of boron. The importance of achieving adequate deoxidation prior to the addition of boron in order to realize the full hardenability effect of boron has been sufficiently emphasized by earlier investigators. Digges and Reinhart&apos; and others have investigated the role of nitrogen and have shown that nitrogen also interacts with boron and reduces or nullifies altogether its effect on hardenability. Moreover, their work also demonstrated that the addition of strong nitride formers such as titanium and zirconium reduce the deleterious effect of nitrogen on boron hardenability by combining with nitrogen to form stable nitrides. Another element which has a pronounced influence on the boron hardenability effect is carbon. It has been shown7&apos;10 that the hardenability effect of boron diminishes with increasing carbon content, and becomes almost negligible at the eutectoid composition. This observation is useful in comparing the potential increase in hardenability from boron of steels with different carbon contents, but is not relevant to a study of the effects of normal steelmaking variables. The amounts of oxygen and nitrogen in steel vary with the steel composition and steelmaking practice employed. Most commercia1 low-alloy steels are fully deoxidized by the addition of silicon and aluminum, or other strong deoxidizers, which adequately protect the boron from oxidation. In addition, one or more of the elements such as titanium or zirconium are usually added, either separately or in combination with boron, in the form of complex ferroalloys, to protect boron from combination with nitrogen in the steel. However, the actual amount and type of addition employed for a given processing requirement are usually selected by trial and error, and have a rather limited range of applicability. As a result, substantial variations in the hardenability of boron-treated steels are often observed in practice, particularly when the nitrogen content of the steel is a significant processing variable. These variations might therefore be reasonably attributed to the interactions between boron, nitrogen, and titanium or zirconium present in the

Jan 1, 1969

By W. B. Morrison

The principal factors influencing the total percent elongation of a lead-tin eutectic and several low-alloy steels which exhibit superplasticity were investigated. These factors are: a) Strain-rate sensitivity of the stress (m). b) Specimen geometry; in particular, diameter-to-length ratio (d0/l0), and surface irregularity (e.g. notches). A feature of the tensile deformation of a superplastic alloy is the early appearance of a neck which continues to extend throughout the test. As a result the total elongation is directly related to the diameter-to-gage-length ratio. The strain-rate sensitivity of the stress varies during extension, mainly because of microstruc-tural changes. A satisfactory correlation exists between the minimum strain-rate sensitivity and total elongation, as indicated in the equation shown below. Notches cause a considerable reduction in total elongation and their effect is greatest at high values of strain-rate sensitivity. An initial notch depth exists below which there is no appreciable effect on elongation. An equation relating elongation to strain-rate sensitivity and specimen geometry is proposed, THE total percent elongation of a tensile specimen is usually regarded as a measure of superplasticity. However, little attention has been given to the fact that total elongation is also a function of specimen diameter and gage length, even though the importance of geometry has long been recognized in the tensile testing of materials in which elongations are relatively small.* In the present study, the effect on superplas- tic extension of the ratio of specimen diameter to length was investigated and an analysis was made of strain distribution along the gage length. Superplastic alloys are characterized by having a flow stress sensitive to strain rate but relatively insensitive to strain.2"&apos; In an earlier study,5 it was found that the strain-rate sensitivity of several low-alloy steels changed during the test and that the minimum value correlated best with total elongation. In the present study, the variation of strain-rate sensitivity during the straining of a lead-tin alloy was investigated. EXPERIMENTAL PROCEDURE Lead-tin eutectic alloy (32 pct Pb 68 pct Sn), made from high-purity lead and tin, was cast in the form of 1-in. diam rod. The rod was cold-rolled in stages to 0.25 in. diam and then swaged to 0.125 in. diam. Samples were cut from the rod at various stages of the mechanical working process. Tensile test specimens were then made by attaching threaded steel ends to the rods by an epoxy-base thermosetting adhesive which required a setting treatment of 2 days at room temperature. The rods were seated in the steel ends in holes approximately 0.01 in. oversize. The test pieces thus made were of various diameters and gage lengths. These were stored at a temperature of about -70°C (-94°F) until required for testing. The distribution of strain along the gage length of a specimen was determined at various stages of the tensile test. The lead-tin alloy was superplastic at room temperature and direct observations during testing were simple. The gage length was divided by reference marks into five initially equal units. These reference marks were made with ink and were reinforced during the test when the initial marks became faint. Photographs were taken, at intervals, of the deforming specimen and measurements of the elongation in each of the gage units were made on these photographs. Tests were also done on several superplastic low-alloy steels whose properties were described earlier.5 The chemical compositions of these steels are given in Table I. A diagram of the notched tensile specimen used in the steel tests is shown in Fig. 1. The specimens were tested at 900°C (1650°F) in a furnace through which a mixture of He + 2 pct H was continuously circulated.5 RESULTS Strain Distribution. Approximately 20 tests on lead-tin alloy specimens were conducted to determine the strain distribution during the test. An example is shown in Fig. 2 of the strain distribution in the gage

Jan 1, 1969

By S. C. Jones, J. A. Davis

This paper describes displacement mechanisms of micel-lur solution slugs, displuced by a thickened water "mobility buffer", in a glass micromodel and in consolidated Berea sandstone cores. Colored motion pictures, taken through a microscope, recorded interactions on a pore-to-pore bash in the micromodel. Production and differential pressure data from consolidated cores previously waterflooded to residua1 oil saturation revealed displacement mechani.sm.s macroscopically. Oil is displaced miscibly, while interstitia1 water is displaced immiscibly by the injected micellar. solution slug. Part of this water is dispersed and carried near the lead ing edge of the .slug, and some may remain as a residual saturation. Thickened water displaces any residual water. It also emulsifies with the. slug material, thereby displacing it. The displacement sequence forms banks of oil and water with relatively constant fractional flows, saturations, and mobilities. The mobility of oil and water flowing ahead of the .slug defines .slug viscosity required for stable displacement. Equations are presented that describe. several aspecis of the displacement flow behavior: oil breakthrough, oil cut during production of the stabilized bank, breakthrough of banked water and the resulting decreased fractional flow of oil, fluid mobilities, etc. Breakthroughs, calculated from the equations, are compared with experimental data. Slugs of micellar sollution, ranging from 1 to 5 percent PV, produced unusually high oil recoveries (up to 100 percent) in previously waterflooded consolidated cores. Investigation of the effect of mobility buffer size on oil recovery indicated that recovery is reduced in 3-in. X 4-ft cores for mobility buffer sizes .smaller than 50 percent of the pore volume. Introduction A new oil recovery process,* conceived in 1962, utilizes a slug of micellar solution&apos; that has sufficient viscosity to avoid an unfavorable mobility ratio with respect to the oil and water it displaces. These micellar solutions are composed of hydrocarbons, water, and surfactants, and may contain electrolytes and co-surfactants. The micellar solution is displaced by a "mobility buffer". The mobility buffer is a bank of reduced-mobility fluid, preferably an aqueous polymer solution. The entire system is displaced by unthickened water. This paper describes some of the microscopic and macroscopic displacement mechanisms observed during laboratory development of the fluids for a potential field test. Microscopic phenomena were observed photographically in a specially constructed glass flow model and macroscopic data were taken from constant rate, tertiary displacements conducted in Berea sandstone cores. Qualitative Description of Micellar Solution Flooding This section qualitatively describes displacement mechanisms that occur when a slug of micellar solution is injected into a previously waterflooded core. The slug completely removes oil from the portion of core it contacts, and banks oil in the process. The oil saturation in this bank and the flowing WOR reach definite, fixed values that are determined by water and oil mobilities and slug characteristics. This zone of constant WOR and oil saturation will be called "stabilized oil bank" in the following discussion. When this stabilized bank reaches the outlet end of the core, the oil cut jumps from zero to a constant value equal to the fractional flow of oil. Saline water has little or no solubility in the slug. Because of this. the slug displaces in-place brine immiscibly. During slug injection, most of the brine is displaced ahead of the slug, some is carried along in the leading portion of the slug, and part of the brine may become immobile. The immobile, residual brine is later miscibly displaced by thickened water. Displacement of all the oil and only part of the water during slug injection results in a higher fractional flow of oil ahead of the slug than occurs when all the water is displaced after injection of thickened water is begun. The slug spontaneously emulsifies fresh (low-salt content) water. By emulsification, the slug can become infinitely diluted, and hence totally displaced, by thickened water. Fluid saturations in the core are shown schematically in Fig. 1. Parts A and B show conditions before and after the start of the thickened-water injection, respectively. Since thickened water displaces any residual brine by-

Jan 1, 1969

By Colin M. Sargent

ALTHOUGH annealing twins are frequently observed in many fcc metals, their occurrence in aluminum is relatively rare. ~ahn&apos; in his review of twinning has listed only a few references to observations of twins in aluminum, e.g., Refs. 2 and 3. They have also been shown to occur in evaporated aluminum layers.4 During the present work, several annealing twins were studied in aluminum. The specimens of 1099-grade aluminum had the following thermomechanical treatment: deformed 90 pct by rolling, partially re-crystallized, further deformed 60 pct to a final thickness of 100 p, then annealed for 24 hr at 120°C. This treatment produced several annealing twins—-about ten per electron microscope specimen. The specimens were produced by the window technique and examined in a Phillips E.M. 200 operating at 100 kv. A typical twin boundary is shown in Fig. 1. For several of the twins studied the twin plane could be tilted so that it was parallel to the electron beam, e.g., Fig. 2. The associated diffraction pattern, Fig. 3, shows the twinned relationship between the grains. The twinning plane in each case was (111). Use of a reflection common to both the twin and the matrix,* i.e., using reflecting planes parallel in the twin and the matrix, the coherent twin boundary becomes invisible and only the noncoherent segments of the stepped boundary are seen, e.g., Fig. 4. Trace analysis of the boundaries showed that the long straight portions were invariably the twin plane; i.e., these portions are coherent. The planes of the shorter segments are shown by Fig. 5 to be (551 1, (7111, and {211).

Jan 1, 1969