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By T. S. Spice, H. L. Lovell, R. W. Utley

With the increased demand for lightweight aggregate, such materials have been manufactured from slags, clays, slates and, to a minor extent, the refuse of coal preparation processes. The latter source is attractive due to current interest in eliminating air pollution and improving the unsightly appearance of refuse piles as well as potential economic advantages, if a satisfactory product can be manufactured. A study has been made relating the composition of coal refuse, expressed as washability data, and the properties of a resulting aggregate. Three different refuse samples (bituminous and anthracite) were separated at gravities ranging from 1.4 to 2.96. Their chemical composition was determined. Aggregates were prepared in the laboratory from these fractions before and after ashing, at temperatures between 1250' and 1350°C. The specific gravity, expansion and compressive strength of the products were measured. The response of the refuse to bloat is related to the chemical composition of the ash to yield a glass of desirable viscosity and to the presence of a material which will form a gas in the appropriate temperature range. Carbonaceous material within the particle is a negative factor since after the glassy phase forms, oxygen cannot enter the mass thus inhibiting bloating. Precombustion of the refuse is also detrimental since it removes substances of gas-forming capability. The fraction sinking at 2.60 yielded an aggregate which had the lowest specific gravity, greatest expansion and greatest compressive strength. The purpose of this study was to seek and evaluate possible relationships between the composition of coal refuse, as expressed by washability data and factors affecting the production of a lightweight aggregate from refuse by bloating. The study was related to an intense program in the Department of Mineral Preparation at the Pennsyl- vania State University to study the possible elimination of air pollution from coal refuse fires by producing a low-carbon secondary refuse. Another phase of this program is considering possible uses of such a secondary refuse. Thus one study was to determine if a lightweight aggregate could be produced from this new refuse material and what effect the nature of refuse beneficiation would have upon the characteristics of a commercial aggregate product. It was hoped that these studies would assist in the design of a process and in establishing the optimum specific gravities at which refuse separation could be made in respect to the production of a low grade fuel from the float product and a raw material for lightweight aggregate from the sink product. The combination of producing a saleable low grade fuel and a lightweight aggregate, while at the same time minimizing disposal costs and air pollution contributions would be attractive to the coal mining industry. MECHANISM OF BLOATING Austin, Nunes and Sullivan,1 Ehlers,3 Everhart, 4 Riley7 and others, have stated that bloating is an expansion process in which two essential conditions exist simultaneously. These are: the development of a glassy phase over a relatively wide temperature range (the viscosity of this glassy phase plays a major role in the retention of the evolved gases) and the evolution of gases (SO2, SO3, CO2 and O2) from mineral decomposition in sufficient quantities at appropriate temperatures to form a cellular structure in the mass. Unless these two "type" reactions take place at the same time or in overlapping ranges of time and temperature, cellulation will not occur. In this event, the gas will escape or the melt will be too fluid to retain it; or if retained, the cells may be too large or the walls too thin for good strength in the product. The stages that occur when clays and shales are heated in an oxidizing atmosphere may be summarized as follows: 1) Drying and removal of free water to 200°C. 2) Absorbed water dehydration period (200 to 480°C). 3) Chemically-combined water dehydration period (480 to 700°C).

Jan 1, 1965

By F. M. Yans, A. D. Donaldson, A. R. Kaufmann

Beryllium was mixed by powder. metallurgical techniques with copper, nickel, iron, and chromium, respectively, to form beryllium -rich binary alloys which Mere then extyuded and rolled transtverse to the extrusion direction. The effect of each alloying element was determined by tensile testing. In solid solution, small amounts of iron and nickel had an embrittling effect, while copper in solution increased the strength but had no effect on ductility. The effect of chromium was complicated and not readily explainable. Observations concerning the planes and modes of fracture were made. BERYLLIUM possesses some very attractive properties for general design applications, especially its strength to weight ratio which is approximately twice that of aluminum and three times that of stainless steel. Equally significant, however, is its combination of high moduli , high strength (approximately 70,000 psi tension and 40,000 psi shear), and low density (0.0658 Ib per in.3), which has made it a potentially important structural material for use in high-speed aircraft and missiles. The main attractions of beryllium are most marked when compared to other constructional alloys now in use. For example, while its density is approximateiy that of magnesium, its modulus of elasticity is approximately seven times that of magnesium, three times that of titanium, four times that of aluminum, and 1 1/3 times that of steel. Furthermore, its relatively high strength and high melting temperature permit design for service temperatures to about 1100°F. It is felt by the aircraft industry in general,' that the high cost of beryllium can easily be amortized by the savings in fuel costs, and increases in aircraft payload and range. The only factor which has prevented the use of the metal in structural applications is its lack of sufficient ductility. It is this property that has retarded the development and utilization of beryllium. Beryllium's modes of deformation, Fig. 1 indicate that the main fracture planes at room temperature in a randomly oriented sample are the (0001) basal planes; the (1150) prism planes are the planes of secondary fracture.' Klein, Macres, Woodard, and Greenspan3 obtained elongations of up to 40 pct in beryllium sheet rolled above 700°C when the (0001) basal planes were oriented parallel to the plane of the sheet (see Fig. 2).

Jan 1, 1962

By J. E. Smith, P. B. Crawford, B. L. Laudrum

A method is presented by which the displacement efficiency of a steam-injection process may be determined. The method consists of a determination of the position of the steam front at a particular time and the application of the Buckley-Leverett theory to the hot and cold regions of the reservoir with the appropriate hot or cold fluid properties. A uniform, linear flow system is assumed for this study. The method is applied to a number of reservoir conditions. The primary properties which affect the results of a steam-injection process are the oil viscosities at steam and reservoir temperatures, injection rate, pay thickness and oil saturation. The efficiency of steam injection is compared with that of water injection for a 10-acre, linearly flooded reservoir. In reservoirs where the oil viscosity is about 35 times the water viscosity, the steam process yields recoveries about 20 per cent higher than the water flood. Where the oil viscosity is near 500 cp, the steam process may recover from three to four times as much oil as a water flood. INTRODUCTION In a previous paper,' a method was suggested for evaluating a steam-injection process. Emphasis was placed upon the determination of the steam-front position in the reservoir at various times. In the present paper, the displacement process is studied in more detail. The approach is essentially that employed by Jordan, Rayne and Marshall3 in their study of hot-water injection. The steam-injection process is quite complex, and an exact description of the process has not been found; however, a qualitative description can be made. When a quantity of steam is injected into a relatively cold reservoir, the leading edge of the steam front continaally flows into cool sand, and some steam condenses. As more and more steam condenses, a bank of condensed water will form which is augmented by displaced connate water. The reservoir may be divided in three regions—(1) a region containing displaced fluids at reservoir temperatures, (2) a region contain- ing water at reservoir temperature and (3) a region occupied by steam. The reasons for the lack of a region of hot water or oil of any appreciable size have been discussed.' A method has been presented by which the location of the steam front can be determined even when heat losses to the regions surrounding the reservoir are sizable compared with the amount of heat injected. It remains to show the effectiveness of steam injection in increasing the ultimate oil recovery. To illustrate the technique for determining the increase in displacement efficiency and, hence, the increase in ultimate production, two sets of hypothetical reservoir conditions will be studied in detail.

By A. D. Mutch

IT has long been known that there are wide variations in the thermo-electric potential of pyrite. In the last few years a study of this variation and other properties of pyrite was carried out at the University of Toronto by F. G. Smith on specimens of pyrite from many localities.1-3 As a result of these studies the pyrite geothermometer was developed by Professor Smith. The calibration of the pyrite geothermometer is based on the assumption that "crystals of any one electronically conducting mineral species deposited at a high temperature have a more positive thermo-electric potential than crystals deposited at a low temperature, and the thermo-electric potential varies continuously between any given limits of the temperature of deposition." The cause of the variation was postulated to be crystal discontinuities, such as lineage boundaries. As yet this postulated relationship has not been established as fact. On theoretical grounds it is indicated that the thermo-electric potential of pyrite or any other partial conductor is dependent upon a number of factors as well as the temperature of formation. For this and other reasons there is ground for doubt as to the validity of the relationship postulated above. To date a large number of readings have been made with the pyrite geothermometer which have been recorded in terms of the calibration of the instrument in degrees centigrade. So far most of the pyrite tested by this technique has been in association with gold ore. The values for the temperature of formation obtained in these tests appear to be reasonable and, in relation to geological problems, to vary in the right sense. Determinations on some specimens not in association with gold ore have given readings that appear to be much too high, taking into account the probable maximum temperature of the host rock. To sum up, although many determinations made with the. pyrite geothermometer appear to give reasonable values for the temperature of formation of the pyrite, there are at the same time other readings which seem anomalous. On the basis of an examination of available results of work with the pyrite geothermometer, two problems must be considered: 1-the validity of the calibration of the pyrite geothermometer; and 2-the nature of the distribution of the thermo-electric potentials of pyrite in relation to the specific problems that have been examined. In this paper the academic problem relating to the validity of the calibration of the pyrite geothermometer will not be discussed. Instead, the variations of thermo-electric potential of pyrite in association with gold veins will be discussed with regard to specific examinations. The first of these two examinations deals with the distribution of thermo-electric potentials of pyrite in association with a gold vein and was carried out in the McIntyre Porcupine Mine, Schumacher, Ont., in the summer of 1949 as part of a study with this technique. The second problem deals with variations of thermo-electric potential of pyrite in gold ore specimens from all over the world. The specimens used in this study were part of the private collection of Frank Ebbutt, geologist for Howe Sound Exploration Co. Results of Detailed and Reconnaissance Studies In discussion of the results of determinations made in these two studies the values of thermo-electric potential in millivolts will be used. It will be noted that in some of the diagrams the determinations are recorded in terms of pyrite geothermometer temperatures. Fig. 1 is a calibration chart relating, pyrite geothermometer temperatures and thermo-electric potentials. A full discussion of the technique is given in the original paper by F. G. Smith.' Briefly, the determinations are made by placing two stainless steel probes, one hot and the other cold, against the surface of the pyrite crystal being tested. The thermo-electric potential that is developed is read with a null-point potentiometer that is calibrated in what

Jan 1, 1952

By S. Dinda

A series of as -quenched 4340 bars were drawn through a carbide die to various reductions. The X-ray diffraction technique of Lopata and Kula was employed to detect preferred orientation in drawn martensitic steel bars with low amounts of deformation, as lord as 0.8 pct The specimen face of each bar examined was cut at a 45-deg angle to the bar axis. The reflecting planes in the 45-deg face were varied by appropriate rotation of the sample using a spectrogonionzeter. TIE X-ray bean of a diffractometer was reflected from the center of the bar and the diffracted intensity was delected with a proportional counter and recorded. Intensity peaks were developed by cold working for 110 planes oriented at 0 and 60 deg to the bar axis. The intensity peaks increased with increasing defortnalion us a preferred orientation with a 110 texture developed parallel to the drawing direction. The intensity peaks for deformed as-quenched specimens remain unchanged after tempering at temperatures as high as 1000°F. The same amount of preferred orienlalion was observed both inferritic (hot-rolled) and martensitic (as-quenched) structures after an equivalent amount of deformation. THE deformation of martensite with medium carbon content. less than 0.5 pct, has been studied by Breyer et a1.1,2 It was reported that changes in properties such as resistivity, carbide precipitation, and the introduction of a yield point phenomenon were produced after cold reduction of as-quenched AISI 4340 steel bars. Later, Breyer and Nachtman3 studied the effect of cold reduction upon X-ray line intensity. They showed that the integrated 110 line intensity increased with increasing deformation when the planes examined were perpendicular to the die drawing direction. The integrated 110 line intensity for planes oriented at 45 deg to the die drawing direction, in contrast, were found to slightly decrease. These changes were proposed to be consistent with the previously proposed model of a stress-induced ordering of carbon atoms in the vicinity of dislocations.1,2 Objections can be raised to the above interpretation of the X-ray results on two grounds: a) Rough structure factor calculations indicate that the intensity changes are too large (50 pct observed vs 2 pct calculated4,5) to be the result of changes in the location of iron atoms produced by the stress-induced ordering of the carbon atoms. b) The results might be explained in terms of preferred orientations, although X-ray evidence of the development of texture has not been reported in the literature for deformations as slight as 1 or 2 pct. The aim of the present work was to determine if preferred orientation was present in such cold-drawn martensitic steel bars. In drawn rod or wire there is generally a certain crystallographic direction which is aligned in the direction of the wire axis, and the crystallographic planes are distributed symmetrically around this "fiber axis".6-8 This type of cylindrical specimen, with the fiber axis located at the center, will show rotational symmetry. Lopata and Kula9 proposed an experimental method utilizing a specimen cut at 45 deg, see Fig. 1. The X-ray beam is diffracted from the center of this bar cross section. The specimen is rotated around an axis perpendicular to the bar axis and lying in the 45-deg cut face. This permits the angle between the normals to the reflecting planes and the bar axis to be varied from 0 to 90 deg.9 With this arrangement the errors due to absorption and irradiated volume compensate each other.' This greatly simplifies analysis of the data and is of considerable advantage for quantitative measurements. If there is preferred orientation in the specimen, more planes are oriented in a particular direction in the bar. When the bar is rotated to the favorable Bragg condition for that particular orientation, the intensity will be higher than that for some other angle. This technique was adopted for the present investigation.

Jan 1, 1969

By R. W. Borio, T. S. Spicer

Inflammability and crossing point apparatus were used to study the influence of increasing amounts oi such inerts as ash, fly-ash, pyrite, limestone and Portland cement with several pulverized bituminous coals. The results indicate that it requires large proportions of inerts to substantially suppress the ease of ignition. The ignition phase of the combustion of solid fuels has been under study periodically since 1900. With the advent of pulverized coal firing some 60 years ago, a technique now dominating the coal utilization field, the ignitibility characteristics have become increasingly important. Much of the early work was directed toward the prevention of coal dust explosions and improved mine safety rather than combustion. Many factors affecting ignitibility have been studied and numerous methods devised in an effort to measure the ignition temperature and these have been reviewed by other authors. A recent survey was made by Finney and Spicerl in 1959, so a discussion of previous work will be omitted. Despite these efforts, the initial stage of combustion, termed ignitibility, is still a little understood phenomenon. In fact, no ASTM method has been adopted for the calibration of this illusive property. However, a D-5 Subcommittee XVI on Ignitibility of Coal and Coke of ASTM (now inactive) defined ignitibility:' "The ignitibility of a fuel is that char-

Jan 1, 1963

By K. J. Brondyke, P. D. Hess

Lack of correlation between densities of aluminum alloy samples solidified under reduced pressure (vacuum gas test) and hydrogen content of the metal is explained on the basis of inclusions serving as nuclei for hydrogen bubble formation. As a result of these findings, the vacuum gas test is suggested as a practical tool to indicate metal cleanliness and the potential effects of hydrogen. Visual obseroation of the sample during solidification under vacuum provides more useful information than that obtained either from density meas -urements or sectioning of the solidified sample. A rapid, practical method of detecting and measuring gas in molten-aluminum alloys has been sought for many years. The development of the vacuum gas test appeared to solve this problem. However, the vacuum gas test is subject to certain limitations, and the results must be interpreted mindful of these limitations, as described herein. Since the only gas which is appreciably soluble in aluminum is hydrogen, the terms gas and hydrogen will be used interchangeably in this paper. In the early days of the aluminum industry, when techniques were not as refined as they are today, it was customary to pour small "pancakes" of alumi- num on a metal plate. These were allowed to solidify under atmospheric pressure. Excessive gas in the metal was evidenced by the appearance of small bubbles on the surface of the "pancake".' It is obvious that such a method would only show very high gas levels far above any which could be tolerated by today's standards of quality required for most applications. Various attempts were made to develop methods which would be more sensitive. Among these were measurements of density of aluminum alloys solidified under controlled conditions, radiography of cast slabs, and examination of fractures. The method which showed the greatest promise and appeared most practical was the solidification of a sample of the molten aluminum alloy under vacuum. The samples so solidified are evaluated either by observation for bubble emission during solidification, by sectioning the solidified sample and examining for porosity, or by determining the density of the solidified sample. This test is known internationally as the Straube-Pfeiffer test or the reduced-pressure solidification test, but in America it is commonly referred to as the vacuum gas test2-' and will be so designated in this paper. The determination of density appeared an attractive and convenient means of providing a numerical rating for the samples. Attempts were made in some instances to correlate densities to hydrogen contents. Unfortunately, the visible loss of gas during solidification of samples with high gas contents precluded a correlation of vacuum gas test densities with the observed gas evolution. This led to Alcoa's use of two different pressures; 50 mm of

Jan 1, 1964

By Kenneth M. Bravinder, Jonathan E. Koogle, Dean H. Sheldon

THE solution of subsurface geological problems requires an analysis of vertical and horizontal dimensional relationships. For many, the ability to visualize structures in three dimensions is not easily acquired, and for areas where the structural conditions are complicated by faulting the need arises for illustrative models. This has led to the many forms of peg models, in which the usual course of construction includes a peg for the well bore, and the suspension of strings from peg to peg to illustrate the formation correlation between wells, thus developing the usual folds and flexures. Such models proved unsatisfactory for the analysis of fault problems. Consideration was then given to the use of transparent materials. A model of the Dominguez oil field was constructed in 1935, which consisted of a series of glass panels from well to well on which the formations were shown in color. This model, though serving its purpose at the time, proved to be impractical from the standpoints of cost, breakage hazard, and extreme difficulty in maintenance. The cost of materials was estimated to be approximately $300, and the construction required the services of one man for a period of from 10 to 12 months. Maintenance after actual construction was an additional expense. Consideration was then given to the use of celluloid, and after some experimental work it was found that the advantages in its use were: (I) a short construction time, (2) ease of handling the material, (3) sections are easily reworked, (4) low cost. CONSTRUCTION It would be of little value to recount here the difficulties encountered in the building of the first celluloid model. The conclusions drawn, however, suggest the following procedure for those who contemplate the construction of such a model: I. Determination of the Scale.-Accurate geological interpretation requires the use of the same scale horizontally and vertically. It should be emphasized that the limited size of the celluloid sheets (20 by 48 in. maximum dimensions), the area to be studied, the maximum depths to be plotted, and area of possible future development are the controlling factors in adopting a scale to be used. 2. Construction of the Base.-A satisfactory base may be constructed by using two pieces of three-ply wood separated by strips of i by 2-in. material. This type of construction prevents warping of the base. The size of the base is determined by the dimensions of the area to be studied plus 5 in. on all sides. A map of the same scale as that adopted for the model, indicating the lines of section to be used, should be fastened to the base. 3. Construction of the Frame (Fig. I).-In the construction of the frame the use of 1/2-in. o.d. pipe welded in a box shape is suggested, with two horizontal rods on each of the four sides, top and bottom. The top rod should be at least I in. higher than the

Jan 1, 1941

By T. J. Bosworth

The effect of hydrogen pretreatment of alumina, magnesia, and zirconia crucibles on reduced oxygen levels in iron charges has been studied. Hydrogen treatment of commercial high-purity magnesia crucibles was observed to produce as high as 70 pct reduction in oxygen content in iron melts. Hydrogen treatment of the commercial high-purity grade zirconia crucibles produced a 25 pct reduction in oxygen levels in iron melts. An average reduction of Knoop hardness of 47 pct was recorded on the iron charges melted in hydrogen-treated crucibles. On the basis of the experiments and the free-energy diagram, it appears that the major source of reducible oxygen to the iron charge is the suboxides and impurity oxides rather than the major oxide of the crucible. Suitable pretreatment of the crucibles to reduce and remove these oxides yields low oxygen levels in iron melted in the crucibles. DURING the last decade, attempts to produce more pure and uniform alloyed metals have brought about the development of many new melting techniques. Notable among these are vacuum-induction melting, inert and consumable-electrode melting, the cold-mold technique, and numerous techniques for removal of impurities by chemical reaction. However great the achievements in this field, metals must still be melted in contact with media of varying reactivity; i.e., gas, ceramic, and slag. Studies have been made to attain an understanding of the reactions that take place during melting, including slag-metal reactions and equilibria, equilibrium of hydrogen and water vapor, and carbon dioxide and carbon monoxide with oxygen in molten iron. These reactions have been treated quite thoroughly. There is one condition, however, that has been widely overlooked, and, to the author's knowledge, only cursive investigation has been made of it. This is the reaction between the ceramic crucible material and the iron charge. In recent years, Hadley and Bianchi' made a series of studies on hydrogen deoxidation of iron in magnesia crucibles. Bianchi2 studied crucible-FeO equilibria in the temperature range 1525°to 1650°C in high vacuum with, however, inconsistent results. Richardson and Jeffes3 in their series of articles on thermodynamic reactions in the making of iron and steel refer to Wentrup and Hieber's4 work on iron and aluminum deoxidation. Their pork included melting iron in alumina crucibles and measuring the aluminum and oxygen content in the iron. Because of the low values obtained, question has arisen of their analytical accuracy.3 Dastur and chipman5 obtained values on hydrogen-oxygen equilibrium in molten iron contained in alumina crucibles similar to those obtained in experiments in the present program. Hochmann6 studied removal of impurities in chromium irons in high vacuum. His results with respect to oxygen level in chromium-iron melted in magnesia crucibles are consistent with results we have obtained.

Jan 1, 1959

By E. C. Skinner

Cardox, which consists essentially of a steel tube containing carbon dioxide compressed to the liquid state, is a trade name designating a device used principally in coal mines to break down coal. The use of Cardox to break down coal was developed in the Middle Western coal fields around 1927 or 1928. At first, a large, heavy tube was used, requiring many parts. Through experimentation and technologic improvement, the weight of the tube has been brought down from 88 lb. to 20 lb. and the new, light tube makes use of larger volumes of CO2 at lower pressures than formerly was thought possible. This blasting method is extensively used today in coal mines and probably one tenth of the bituminous coal produced in the United States is prepared with Cardox. Construction and Application As used in the coal mine, Cardox looks like a piece of steel pipe 2 to 3 in. in diameter and 3 to 5 ft. long. When it is necessary to fire a shot, the tube is wired with two leg wires that are long enough so that when the tube is pushed the desired distance into the hole the wires will protrude 5 to 6 in. It has been found that No. 18 insulated copper annunciator wire is the best material for leg wires. A two-conductor rubber-covered shot-firing cable of sufficient length is then attached to the leg wires. A 2 to 6-volt current is applied, either by means of shot-firing batteries or the standard type of shot-firing generator. Upon the application of the current, the charge in the cartridge is set off. Because the breaking action upon the coal is supplied by the relatively slow physical expansion of the carbon dioxide gas rather than by the rapid chemical formation of gases as in more familiar explosives, the result is a slow heaving action, somewhat similar to that produced by black powder, rather than a shap detonating effect. Permissible powder does its work at roughly ten times the pressures in use with Cardox. The escaped gas from a Cardox shot apparently works along the planes of weakness in the coal face, such as the coal cleats, the edges of the cut, and along the top of the seam, breaking off the coal toward the free faces and heaving the mass of coal outward. Cardox tubes are manufactured in various sizes to take care of variable conditions of seam size, undercut depth, cleatage, coal hardness, and so forth. The tubes range in diameter from 2 to 3 in. (Table I) and the normal CO2 charge is from 24 to 96 oz. For any one tube size, several sizes of shear disks are available, thus excellent control of the type of shooting desired is possible. In general, local experience and experimentation dictate the size of tube chosen for any particular job. For high coal, and deeper or wider cuts, a larger size is chosen to start with, and the opposite is true for low coal, softer coal, or small cuts. After the tube size has been experimentally selected, tests are run in the mine to determine how many shot holes are needed and where the holes should be placed. The size of the disk,

Jan 1, 1944

By Parke A. Dickey

Potential differences between strata of shale and sandstone have been recognized for about years, and they form the basis of the electrical logging of oil wells. Hitherto these potentials have been ascribed solely to electrochemical reactions caused by the disturbing effects of the water in the drill hole through which they are generally measured. Observations by the author in wells empty of water and in a mine shaft suggest that potential differences between sandstones and shales are natural and specific properties of the rocks, although they are modified in measurement by the disturbing effects of the water in the drill hole. The cause of these potentials probably is to be sought in the relative polar adsorptive capacities of quartz and clay particles. Introduction The existence of potential differences in the surface of the earth has been known for some time, and their measurement has facilitated the discovery of geological discontinuities such as ore bodies. The technique of measurement has been well established.'-a In measurements in oil wells, it has been found that the potential of shales with respect to some arbitrary reference is very nearly constant in any one well, at least below the zone to which meteoric water has gained access. Sandstones and some other types of sedimentary rocks have a difference of potential with respect to shale that is negative and may attain a value of 200 millivolts or more. The difference of potential, as usually measured commercially with water in the hole, is distributed over about one foot vertically at the top and bottom contacts of the sandstones. The sharpness of the curve at the formation contacts can be improved by using a short electrode that is close to the wall of the hole. These potentials generally have been ascribed to the disturbing effects of the water in the drill hole. Potentials have been found, however, in wells in which no water was present. In the course of experiments in electrical logging in Pennsylvania, carried out by the Pennsylvania Geological Survey, observations were made of several phenomena that hitherto have not been described, to the author's knowledge, in the published literature. The potential differences across the contacts of sandstone and shale are called in this paper "natural potentials," as distinguished from the potentials caused by electroendosmosis (electrofiltration) and concentration differences, which will be discussed subsequently. Potentials in Cored Well In the spring of 1942, the author measured the potentials in an exploratory well (Day 13, near Grand Valley, Pa.) which had been cored with diamond tools. The potentials were first measured with fresh water in the hole. A null balance potentiometer was used in this and all the other measurements described in this paper. One nonpolarizing porous pot electrode, containing copper sulphate solution and crystals surrounding a pure copper elec-

Jan 1, 1944

By J. R. Hauber, N. R. Borch

A study uras made on the creep behavior of cast and extruded SR grade beryllium. It is shown that, for stresses below about 1000 psi in the temperature range 760" to 85o° c, the creep behatior is nearly exactly described by the Nabarro-Herring mechanism. The activation energy is apparently that for self-diffusion, 42 2 kcal per mole, below 1000 psi, but it rises to 88.6' kcal per mole at higher stresses. The slress exponent is 4.5 at the higher stresses. Tertiary creep in this material is clearly related to void formation apparently caused by grain boundary sliding. BERYLLIUM is becoming an increasingly important technological material. A search of the literature has revealed a lack of fundamental studies on the creep of beryllium. This investigation was therefore undertaken to gain insight into the creep behavior of this material. EXPERIMENTAL PROCEDURE Tensile creep samples were prepared from cast and extruded SR grade beryllium. The vendor's chemical analysis of the beryllium tested is shown in Table I. The test specimens were machined as shown in Fig. 1 from i -in.-diam rods. The machined creep specimens were annealed to remove surface damage and to establish a variation in grain size. The heat treatments and their resulting grain diameters are shown in Table 11. The average grain diameters were determined by the intercept method. True average grain diameters were estimated by multiplying the measured average grain diameters by 1.5.' The creep tests were performed at temperatures from 700" to 850°C in a vacuum of 105 Torr or better in a tantalum-element resistance furnace. Loads were applied by an Instron testing machine such that the stress was held constant to within 20 psi. The test temperature was measured by thermocouples on the sample. With one exception the deviation from the desired test temperature was 2"C, and in that case the deviation was 4"C. Elongations were measured by an extensometer within the vacuum chamber which was fastened to the creep specimens at the grooves in the grip ends, as shown in Fig. 1. The precision of measurement of elongation was 1 X loe4 in. The creep tests were begun only after thermal equilibrium had been established in the sample and the extensometer to insure that there was no strain rate component due to transient thermal effects. Two kinds of creep experiments were performed. First, at constant grain size, the effects of varying stress and temperature were studied. In the second set of experiments, the temperature was held constant and the grain size was varied. The activation energy for creep was determined by varying the temperature at constant stress, as described by orn, during the first set of experiments. The variable grain size experiments revealed that creep at low stress apparently occurred by the abarro-errin' mechanism. In all of the creep tests, the stress was held constant only until sufficient strain had occurred to accurately determine the creep rate. The stress was then raised to a new value and the new creep rate determined. This process was reported until tertiary creep occurred. In this manner several data points were obtained from each specimen. The assumption was made that the structure was not changing appreciably between the incremental stress levels. This was verified by reducing stresses to previously tested levels and comparing the creep rates with the creep rates obtained at the lower strains. The re-producibility was within experimental error over strains on the order of 1 pct. EXPERIMENTAL RESULTS A typical series of creep tests is shown in Fig. 2. Primary creep was not observed in any test. Transient creep, which we define as creep rates that are nonlinear with time, was not observed for any change in stress except where tertiary creep occurred. The absence of both primary and transient creep has been previously reported for hot-pressed powder beryllium.= The data for the creep behavior at constant grain size are summarized in Fig. 3. The data show two distinctly different stress dependencies. At stresses below about 1000 psi, in the equation:

Jan 1, 1969

By W. R. Evans, H. H. Kaveler, Jack Tarner

The geological features, development history and engineering detail of the Shuler Field and the results of approximately two years of unitized operation of the Shuler Jones Sand Pool, were discussed in a prior publication.' The purpose of this paper is to present the results of pressure maintenance in the Shuler Jones Sand Pool after nine years of unit operation. GENERAL INFORMATION The Shuler Jones Sand Pool is located in and about Section 18, Township 18 South, Range 17 West, Union County, Ark. The pool was discovered .in September, 1937, unitized in February, 1941, and subjected to gas injection operations in July, 1941. Water was first returned to the reservoir in July, 1944. The reservoir is an anticlinal trap covering about 4,000 acres. The 154,000 acre-ft of sandstone initially consisted of approximately 150,000 acre-ft of productive oil zone and 4,000 acre-ft of gas-cap. The average depth of production is 7,400 ft. Maximum closure of the reservoir is 135 ft and the oil column lies between a gas-oil contact at -7,270 ft and a water-oil contact at -7,370 to -7,380 ft. The field is approximately four miles long. east and .west, and one and one-half miles wide. The sand grains are angular and vary from fine to medium size. The porosity of the sandstone averages 20.2 per cent. The specific permeability averages 400 md. Some zones have as high as 30 per cent porosity and specific permeability of 4,000 md. The reservoir rock is not uniform in character but consists of sandstone zones interspersed with shale. The variation in rock characteristics is evident in the electric log and core analyses presented in the original publication. Asphalt present in the pore space of the sandstone limited the reservoir to the southeast and apparently blocked any encroachment of water from that direction. The initial reservoir pressure at a subsea depth of 7,300 ft was 3,520 psi. The reservoir temperature was 198ºF. Initially, the solution gas volume was 765 cu ft per bbl and the reservoir volume factor was 1.45. The gas solubility and formation-volume-factors of the reservoir liquid are related with reservoir pressures above 300 psi as follows: Solution gas, cu ft per cu ft, S = 0.0334 P + 18.65 Formation volume factor of reservoir oil, FVF = 8.0 x 10 -5 P + 1.168 Gas volume factor, standard cu ft of gas equivalent to one cu ft of gas at reservoir conditions of temperature and pressure, F = .062 P - 4 Pressure (P) measured in psia. The equation for the gas volume factor presented above is based on a direct measurement of a sample of the gas and is a correction of that used in the original paper. The gravity of the oil produced is from 32 to 34" API. CALCULATION OF INITIAL OIL IN PLACE The Jones Sand production history is interesting because it lends itself to analysis by material balance. Production statistics from discovery of the Jones Sand through 1949 and material balance calculations of the initial stock tank oil in place are shown in Table I. The usual procedure in testing the application of material balance calculations is to compute the apparent initial volume of oil in place, using production and pressure information obtained at different time periods. If the apparent oil in place volumes computed increase with successive time periods, water encroachment is indicated and approximations must be mads to correct for its influence. The first requirement in utilizing such calculations is reliable reservoir pressure, accumulated gas, oil and water production, and PVT data. Calculations of apparent oil in place in the Jones Pool, based on field data

Jan 1, 1951

By P. Dayal, L. S. Darken

THE migration of carbon in austenite under the influence of an electric current has been observed qualitatively several times.14 Lebedev and Guterman5 recently have reported quantitative measurements; their method consisted of welding a low-carbon to a high-carbon wire, passing current, and later estimating the carbon distribution metal-lographically. We believe the method reported in this paper is superior in principle since electrolytic migration and ordinary diffusion are not necessarily coupled as in the weld method; also for the first time the extent of migration is determined by combustion analysis for carbon. A uniform tubular specimen (S.A.E. 1045 or 1095) was mounted as illustrated in the figures. the whole assembly being in an atmosphere of purified nitrogen. Direct current (129 to 226 amp at 0.65 to 1.0 v) served as source both of heat and of potential gradient for carbon migration. The duration of experiment was 7.5 to 12 hr, during which time the temperature was controlled (±10°C) manually. The experimental conditions are indicated in the first five columns of table I. With this experimental arrangement, the temperature initially has a maximum value at the central plane. Also, in this vicinity (by virtue of the symmetry), the carbon entering any volume element is equal in quantity to that leaving; the loss or accumulation of carbon occurs near the electrodes since the carbon moves uniformly near the center and is "frozen" at the cold ends. Hence, providing the time of experiment is not sufficiently long to seriously influence the conditions at the central plane, carbon crosses this plane only under the influence of the electrical potential gradient and not under the influence of temperature or concentration gradient. The amount of carbon which has crossed this plane was determined by combustion analysis of the two halves of the specimen. The results of these analyses are shown in the sixth and seventh columns of table I. It will be noted that substantial amounts of carbon migrated from the anode portion to the cathode portion (except at 920°C, which temperature was too low to exhibit the effect in the allotted time). In spite of precau-tions taken, considerable decarburization occurred as may be seen by comparing cols. 8 and 5. In three cases (indicated by asterisks in table I) the specimen was ground on one side, polished, and examined metallographically before analysis. One specimen was normalized and re-examined. Micrographs of selected areas in specimens 4 and 6 are shown in figs. 1 and 2, respectively. Evidence of carbon migration from the anode toward the cathode is quite apparent. Fig. 2 shows abundant graphite as well as cementite in a region near the cathode. The temperature of this zone is estimated at about 800°C. In fig. 1, particularly in the micrograph on the extreme right (the right side of which is of unaltered carbon content), there is evidence of slight depletion of carbon in the immediate vicinity of the cathode as contrasted to the general increase in carbon of the cathode half of the specimen. Although this may be attributed in part to decarbur-ization, it is believed that it is occasioned also by thermal diffusion—migration (of carbon) from a cool to a hot zone4—a phenomenon superimposed upon the electrical migration. Evidence of carbon migration was visible particu-larly during the course of the high-temperature,

Jan 1, 1951

By P. M. Blair

This paper presents numerical solutions of the equations describing the imbibition of water and the countercurrent flow of oil in porous rocks. The imbibition process is of practical importance in recovering oil from heterogeneous formations and has been studied principally by experimental means. Calculations were made for imbibition of water into both linear and radial systems. Imbibition in the linear systems was allowed to take place through one open, or permeable, face of the porous medium studied. ln the radial system, water was imbibed inward from the outer radius. The effects on rate of imbibition of varying the capillary pressure and relative permeability curves, oil viscosity and the initial water saturation were computed. For each case studied, the rate of water imbibition and the saturation and pressure profiles were calculated as functions of time. The results of these calculations indicate that, for the porous medium studied, the time required to imbibe a fixed volume of water of a certain viscosity is approximately proportional to the square root of the viscosity of the reservoir oil whenever the oil viscosity is greater than the water viscosity. Results are also presented illustrating the effects on rate of imbibition of the other variables studied. INTRODUCTION The process of imbibition, or spontaneous flow of fluids in porous media under the influence of capillary pressure gradients, occurs wherever there exist in permeable rock capillary pressure gradients which are not exactly balanced by opposing pressure gradients (such as those resulting from the influence of gravity). The importance of such capillary movement in the displacement of oil by water or gas was recognized in early investigations and described by Leverett, Lewis and True in 1942.1 Methods advanced by these authors for studying the process using dynamically scaled models were rendered more general and flexible by the research of later workers.2"4 The influence of capillary forces in laboratory water floods has also been discussed by several authors.6 While imbibition plays a very important role in the recovery of oil from normal reservoirs, Brownscombe and Dyes7 pointed out that imbibition might be the dominant displacement process in water flooding reservoirs characterized by drastic variations in permeability, such as in fractured-matrix reservoirs. In water-wet, fractured-matrix reservoirs, water will be imbibed from fractures into the matrix with a countercurrent expulsion of oil into the fractures. If the imbibition occurs at a sufficiently rapid rate, a very successful water flood can result; if the imbibition proceeds slowly the project might not be economically attractive. Scaled-model studies have demonstrated the vital importance of imbibition in secondary recovery in fractured reservoirs. It is therefore important in the evaluation of waterflooding prospects to develop a thorough understanding of the quantitative relationships of the factors which control the rapidity of capillary imbibition. The imbibition process serves reservoir engineers in still another important way by providing a technique for studying the wettability of reservoir core samples. Such experiments are usually conducted by observing the rate of expulsion of oil or water from core samples submerged in the appropriate fluid. Several papers have been 'published on the experimental techniques involved?? Although Handy has recently published a method for calculating capillary pressures from experiments with gas-saturated cores, it has not yet been possible to deduce quantitative information regarding water-oil relative permeability and capillary pressure characteristics of the rock from the experimental results. Thus a technique is needed for studying the quantitative dependence of imbibition rate on oil and water viscosity, initial water saturation, relative permeability-saturation, and capillary pressure-saturation relations. The development of such information, including saturation and pressure profiles by laboratory experiments, would be very difficult. However, recent advances in the applica-

Jan 1, 1965

By L. Guttman

THE equilibrium diagram of the indium-thallium system was of interest to us in connection with a study of the superconducting properties of metallic solid solutions in progress at this Institute. For this purpose, a series of alloys was prepared covering the range from pure indium to 75 atomic pet TI, and X-ray diffraction patterns were obtained. Roughly speaking, the results indicated a region of continuous decrease in the axial ratio of the face-centered tetragonal structure from the value ca. 1.08 in pure indium to unity at about 23 atomic pct TI. From this concentration to the solubility limit, the structure was face-centered cubic, a form not reported by Hansen.1 At this point we became aware of the work of Valentiner,2 who had found the same structures at room temperature but had not investigated further the relationship between them. To study the transformation f.c.c.??f.c.t., and to clarify the phase diagram, we undertook the work reported in this paper and that which follows." Preparation of Alloys Pure indium and thallium* (both about 99.9 pct, as estimated from spectroscopic analyses) were weighed out in quantities sufficient to prepare 10 to 25 g of alloy of the desired concentration. (Occasionally indium was mixed with a previously pre- pared solution.) The metals were melted over a flame, in an open graphite crucible, stirred with a graphite rod, and poured into a graphite trough. The rough slug was hammered and swaged into a rod of 2 to 3 mm diam, and annealed in a drying oven at about 125°C for 1 to 2 days. Samples were taken from the rod for analysis, as well as for diffraction and other measurements. The thallium was determined by electrometric titration, using a modification of the method of Beale and co-workers.' The precision of analysis was generally about 2 0.2 pct of the thallium content. The rods were sometimes found to vary in thallium content as much as 1.5 pct from end to end, but since analyses were also made close to the segments used in the various studies, the composition was usually known as accurately as the analyses could be made. Where one less significant figure is given, the error is estimated to be ±0.4 pct of the thallium content. X-Ray Diffraction Measurements Three different cameras were used: (1) A 7 cm Debye camera, with oscillating specimen (manufactured by the Picker X-ray Corp., Cleveland, Ohio); (2) a 9 cm diam Debye camera of the type designed by Bradley;" (3) a 10 cm diam symmetrical focusing back-reflection camera (manufactured by Geo. C. Wyland, Ramsay, N. J.). Samples were prepared from the homogenized rods, either by filing under liquid nitrogen, or more often, in the form of wires or foils made by working at room temperature or liquid nitrogen temperature. Sharp patterns were obtained from specimens annealed at room temperature, although higher annealing temperatures were also used (cf. below). Generally, copper radiation was used; a few patterns were obtained with

Jan 1, 1951

By J. M. Roberts, N. Brown

The stress-strain behavior of zinc single crystals was measured over a strain range of 10-6 to 10-2. The phenomenon of macroyielding was observed in detail and plastic strains were detected at almost zero-stress. Closed hysteresis loops were observed during loading and unloading in the strain region of about 10-5. From the hysteresis a frictional stress on the dislocation of about 6 psi was obtained. A preliminary analysis indicates that impurities are primarily responsible for the friction. Nonelastic Strains as much as 10 -4 were recovered depending on the amount of prior deformation. Part of the recovered strain occurs instantaneously upon unloading and the remainder occurs at zero stress. The time dependence of the recovered strain was measured. THIS investigation is concerned with the details of plastic deformation preceding the ordinary yield point as measured with the usual strain sensitivity of about 10-4. The approach leads to internal friction observations in the hitherto neglected frequency range below 10-1 cycles per sec. It is believed that if the phenomenon of macroscopic yielding is to be understood, then the stress-strain curve in the neighborhood of the macroyield point should be greatly magnified. It may then be possible to determine whether macroscopic yielding is a unique event or whether it is a process which begins gradually at a lower stress. In the case of low-carbon steel a unique event obviously occurs at the macroscopic yield point as indicated by a drop in the load, but copper appears to exhibit a gradual transition from the elastic to the plastic state. In zinc the yield point is rather abrupt although the data indicates that some plastic deformation precedes large scale yielding.' One of the purposes of this investigation is to determine whether there is an abrupt transition from the preyield microstrain region to the region of macroscopic deformation. Such a rapid transition would support the concept that there is a critical stress for yielding. The concept that yielding is a unique event associated with such phenomenon as activating a Frank-Read source, freeing the dislocation from solute atoms, dislocations cutting through dislocations, or dislocations moving freely by one another, has been expounded widely on theoretical grounds. It is hoped that highly sensitive measurements of strain in the neighborhood of the macroscopic yield point will shed some light on the event known as the "Yield Point". EXPERIMENTAL METHOD 1) Specimens—High-purity zinc was cast into spherical graphite moulds in air and grown into spherical single crystals by the Bridgman method under a positive pressure of Argon gas. Spectro-graphic analysis of cleaved sections from four crystals showed a purity of 99.994 pet Zn. The specimens were acid machined with an 1/8 in. gage section in a form similar to those used by Parker and co-workers.2 Bausch type grips were fastened to the specimen by Epon VI adhesive. The specimens were oriented so that only [1120] (0001) slip occurred. Fig. 1 shows two of the specimens in the grips. Prior to each test, the gage section of the specimen was given a concentrated HNO3 chemical polish followed by alcohol rinsing and air blast drying. 2) Test Method- The shear tests were performed on an Instron testing machine and the experimental set-up was made very "hard". Strain could be measured to a sensitivity of 10 -6 by means of a capacitance gage extensometer. The design and calibration of this type of extensometer to measure microstrain, as applied to pure shear and tensile tests of metals, will be the subject of a separate paper—therefore, only a brief account will be presented here. The method essentially consists of attaching a

Jan 1, 1961

By N. J. Grant, C. F. Flo, F. B. Cuff

An investigation of the Ti-Cr system has shown the presence of a complete series of solid solutions in the ß phase, with a minimum in the solid us near 50 pct Cr. An intermetallic compound, TiCr2, forms during cooling from the ß solid solution. There is a eutectoid reaction at the low chromium side of the system. IN view of the recognition of the potentialities of titanium and its alloys as important structural materials there has arisen a need for a systematic investigation of various titanium binary diagrams. Of these, the Ti-Cr system was of particular interest because of the improved properties imparted to titanium by small chromium additions. A literature survey disclosed a partial constitution diagram that had been suggested by Vogel and Wenderott,¹ This diagram, shown in Fig. 1, is the result of work done on the Fe-Cr-Ti ternary system. Alloys containing less than 43 pct Cr were not investigated. In addition to this, a study of alloys in the Ti-Cr system was reported by McPherson and Fontana.² Adenstedt3 furnished a number of dilato-meter curves obtained from specimens containing 5, 10, and 15 pct Cr. Very recently, McQuillan4 submitted a proposed diagram covering the complete range of compositions between titanium and chromium. This diagram was in general agreement with the one described here. Experimental Procedure Sponge titanium (99.7 pct) and electrolytic chromium (Bureau of Mines analysis: 99.03 pct Cr, 0.40 pct Fe, 0.53 pct O2) were used for the initial determination of the system. Subsequent refinement of points, particularly for the low chromium side of the diagram, was accomplished by using iodide titanium and high purity chromium (National Research Corp. analysis: 0.050 pct C, 0.045 pct O2). The Ti-Cr alloys were prepared by melting 25 g charges in an enclosed, water-cooled copper crucible using a movable tungsten electrode. The atmosphere was helium, prepurified by first passing it through a drying agent and then through sponge titanium heated to 850°C. Particular care was taken to avoid any large scale segregation resulting from insufficient mixing of the components. Each charge was melted and kept molten for approximately 1 min, allowed to cool, inverted, remelted, and kept molten for an additional minute. In order to ascertain the amount of impurity pickup (oxygen and nitrogen) during the melting procedure, three iodide titanium specimens were melted in sequence and then checked for increased hardness. The specimens in the as-cast condition showed a relatively large hardness increase over the hardness of the as-received iodide titanium. The scattering on these readings was large. However, after the specimens had been homogenized at 840 °C for 2 hr and slowly cooled, the measured increase in hardness over the as-received titanium was small with a corresponding decrease in scatter. The reason for this hardness change is that in heat treating these specimens below the transformation temperature (885°C) there was a conversion from the as-cast structure to the more nearly equilibrium structure of the annealed specimen. The alloys were analyzed for chromium content and although the actual percentage was invariably low the deviation from the nominal composition never exceeded 0.6 pct Cr.

Jan 1, 1953

By M. D. Hassialis

[Surface Areas of Concentrates and Collector Coatings (T.P. 2002, by A. M. GAUDIN and G. S. PRELLER, Min. Tech., May. Discussion by M. D. HASSIALIS and the authors) . I Activation of Minerals and Adsorption of Collectors (T.P. 2082 by J. ROGERS and K. 1'. SUTHERLAND, Min. Tech., Nov. Discussion by A. F. TAGGART and the authors). . . . 3 Correlation between Mineral Behavior in Cataphoresis and in Flotation (T.P. 2005 by A. If. GAUDIN and S. C. SUN, Min. Tech., May. Discussion by M. D. HASSIALIS). . . . . . 8] Surface Areas of Concentrates and Collector Coatings M. D. HASSIALIS.*-In the current flotation theories there exists a common gap spanned by a common assumption pertaining to the arrangement and orientation of the collector ions at the solid surface. Also common is the belief that contact angle and flotation performance are dependent upon the arrangement and orientation of collector ions. This stimulating and informative paper sheds some light upon this general problem. One of the indices of arrangement is the area available per collector ion; in this connection, Gaudin and Preller have applied the B.E.T. method for surface determinations. In a surprising number of cases, their results show a greater specific surface for tailing than for concentrate. This cannot be accounted for by the differences in specific gravity and is attributed to the presence of clay minerals of "primary" sluices in the tailing. This is not a satisfactory explanation, for experience shows that when free slimed clay minerals are present in a flotation cell they will be carried mechanically into the concentrate. A part of the answer to the decreased specific surface of the concentrate would appear to be its usual flocculated condition, yet this should not entirely account for the large spreads reported. The possibility occurs that the nitrogen adsorption isotherms for clean mineral and collector-coated mineral are different. If that were true, and if the coated mineral surface exhibited decreased adsorptive powers, the discrepancy might vanish. In discussing the disposition of collector ions at mineral surfaces, the authors adopt the more consistent viewpoint that there exists some agreement between the ions of the substrate and those of the superstrate. In the case of xanthate ions on galena, a possible arrangement is shown in Fig. 2. This arrangement shows every xanthate ion being shared by two lead ions, whereas the chemical composition calls for two xanthate ions for each lead ion (p. g). This whole discussion is misleading. In the first place, it is known that xanthate ions are not abstracted by unoxidized galena, hence Fig. 2 should show as the substrate not Pbs but PbS„ Om. It would be equally erroneous to use the lattice arrangement of PGSO4, since the surface properties of xanthate-conditioned anglesite differ from those of xanthated galena. It is highly probable that the state of the galena surface exploited in its flotation is ephemeral, since weathered galena is only poorly, if at all, collected by xanthate. Just how a substrate of oxidized galena is to be pictured depends upon one's conception of the transformation from galena to anglesite. This writer is inclined to the following sequence of events. Surface sulphide ions undergo progressive oxidation. As more oxygen is taken up by the sulphide ions they become displaced from their equilibrium positions in the galena lattice, thus accommodating for the larger volume of the S„ Om ions. Concomittant with this change the forces acting on the lead ions

Jan 1, 1946

By K. P. Gupta

The Cb-rich boundary of the (Cb,Al) a phase field at 1250OC is near 41 pct Al. The Al atoms tend to occupy the C. N. 12 sites in this structure. A homologous (Ta,Al)a phase was identified. No a phase was found in the Mo-Al system at 1200°C. The first binary o-phase with a non-transition element as a major component was found1,2 in the Cb-Al system. The composition of this phase was reported2 as approximately 34 at. pct Al, based on X-ray diffraction patterns taken of alloys in the as-cast condition. Further study of the composition of this o-phase, therefore, appeared desirable. Since Si was previously found3,4 to occupy preferentially the lowest C.N. sites (I and IV) in the a phase, and preliminary resultsa indicated that Al may show similar ordering, one of the aims of the present work was to obtain more complete information on ordering in (Cb, Al) o. Among the binary systems of Al with Ti-, V-, and Cr-group elements, the Ti-Al, Zr-Al, V-Al, and Cr-Al systems are known to comprise no o-phase. In the present work a Ta-Al and a Mo-Al alloy were studied in an effort to find additional o phases with Al as a major component. EXPERIMENTAL PROCEDURES AND RESULTS An alloy with the intended composition of Ta + 40 at. pct Al was prepared by arc melting in He atmosphere. In both the as-cast condition and after annealing for 10 days at 1250°C and quenching in cold water this alloy consisted of two phases, as seen in the X-ray pattern and the microstructure. One of these phases was identified as the o-phase; the observed and calculated d-spacings are shown in Table I. The lattice parameters of this o-phase are a = 9.972 A, c = 5.214 A and c/a =0.5228, as determined from a Debye-Scherrer pattern using Fe K a radiation. The d-spacings for the unknown second phase are given in Table 11. The alloy contained approximately 25 pct of the unknown phase after annealing, as estimated on the basis of microscopic examination. A Mo-Al alloy was prepared by arc melting, with an intended Al-content of 35 at. pct. The alloy button was annealed for 7 days at 1200°C and water quenched. The X-ray pattern of the alloy in both the as-cast and the annealed state showed the reflections of Mo3Al (Cr30 type structure) and an unknown phase different from a. Six Cb-Al alloys were prepared in the composition range 30 to 50 pct Al. All alloys were arc melted in He atmosphere. After annealing for three days at 1175oC in evacuated silica capsules and quenching in water, the alloys with 30 to 40 pct Al contained three phases, namely the o-phase, Cb3Al (Cr3O-type structure) and an unknown phase. The alloys with more than 40 pct Al contained two phases, namely, what appeared metallographically, the o-phase and the same unknown phase. In the alloys containing less that 38 pct Al, the unknown phase was not present after annealing for 4 days at 1250°c,

Jan 1, 1962