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By Otto H. Henry, J. J. Cordiano

Though powder metallurgy is one of the oldest of metallurgical processes, it is in its infancy as a branch of the modern field of metallurgy. As early as 3000 B.C., the ancients produced implements and weapons of iron by reducing iron ore in a charcoal fire and forging the resultant sponge while still hot into the desired shape. Melting and casting soon superseded the powder metallurgy practice, and it was not until the turn of the twentieth century that powder metallurgy was applied to the commercial manufacture of tungsten lamp filaments. From this beginning, the use of the powder metallurgy process spread" to the manufacture of porous oil-impregnated bearings, cemented carbide tools, contact points, diamond grinding wheels, clutch facings, starter brushes, resin-bonded radio cores, magnets, metallic filters, and other parts. More recently, and particularly during the present war, there has been a definite trend toward the manufacture of machine parts by this process in competition with the more conventional fabricating methods. Notwithstanding these many developments, scientific progress has been slow. While many articles on powder metallurgy have appeared in the press and various publications, there have been too few contributions to our technical societies, with the result that there is a dearth of the type of information necessary for the full development of this science. It is of primary importance that the results of research and development be freely disseminated if powder metallurgy is to realize its fullest potentialities. Purpose of Investigation Excluding the refractory metal field, all commercial powder metallurgical products made by a cold compressing and sintering operation contain voids. These voids can be substantially eliminated by subsequent severe working and heat-treatment, but ' such practice has not proved economical in most applications. By applying heat during the compressing operation, plastic deformation of the powder particles is substantially increased, and the resultant compact or briquette is practically free of voids. However, hot-pressing has many attendant problems, which at present preclude its use in the manufacture of precision parts. The more important of these are to devise: 1. A die steel capable of withstanding high pressures at elevated temperatures. 2. A high-temperature lubricant capable of preventing excessive die wear and welding of the compact to the die walls. 3. A method of retaining a neutral or reducing atmosphere in the compacting zone of the die assembly. 4. A means of ejecting the hot-pressed specimen into a neutral atmosphere until reasonably cold.

Jan 1, 1946

By Otto H. Henry, J. J. Cordiano

Though powder metallurgy is one of the oldest of metallurgical processes, it is in its infancy as a branch of the modern field of metallurgy. As early as 3000 B.C., the ancients produced implements and weapons of iron by reducing iron ore in a charcoal fire and forging the resultant sponge while still hot into the desired shape. Melting and casting soon superseded the powder metallurgy practice, and it was not until the turn of the twentieth century that powder metallurgy was applied to the commercial manufacture of tungsten lamp filaments. From this beginning, the use of the powder metallurgy process spread" to the manufacture of porous oil-impregnated bearings, cemented carbide tools, contact points, diamond grinding wheels, clutch facings, starter brushes, resin-bonded radio cores, magnets, metallic filters, and other parts. More recently, and particularly during the present war, there has been a definite trend toward the manufacture of machine parts by this process in competition with the more conventional fabricating methods. Notwithstanding these many developments, scientific progress has been slow. While many articles on powder metallurgy have appeared in the press and various publications, there have been too few contributions to our technical societies, with the result that there is a dearth of the type of information necessary for the full development of this science. It is of primary importance that the results of research and development be freely disseminated if powder metallurgy is to realize its fullest potentialities. Purpose of Investigation Excluding the refractory metal field, all commercial powder metallurgical products made by a cold compressing and sintering operation contain voids. These voids can be substantially eliminated by subsequent severe working and heat-treatment, but ' such practice has not proved economical in most applications. By applying heat during the compressing operation, plastic deformation of the powder particles is substantially increased, and the resultant compact or briquette is practically free of voids. However, hot-pressing has many attendant problems, which at present preclude its use in the manufacture of precision parts. The more important of these are to devise: 1. A die steel capable of withstanding high pressures at elevated temperatures. 2. A high-temperature lubricant capable of preventing excessive die wear and welding of the compact to the die walls. 3. A method of retaining a neutral or reducing atmosphere in the compacting zone of the die assembly. 4. A means of ejecting the hot-pressed specimen into a neutral atmosphere until reasonably cold.

Jan 1, 1946

By Y. C. Liu, G. A. Alers

The effect of rolling reduction on the textures of Cu-A1 alloys has been investigated both by pole figure and by modulus methods. In alloys which exhibit complete copper or brass types of rolling texture, the rolling reduction has little effect on the texture except to increase the degree of preferred orientation. In alloys which exhibit a transition texture, however, increased rolling reduction increases the amount of brass-type texture at the expense of the copper-type texture. The present experimental results show that there is no one-to-one correspondence between the SFE and the rolling texture of fcc metals. Additional data taken from the literature for fcc metals also support this conclusion. On the other hand, the present and previous experimental results are shown to be in good agreement with the suggestion that the texture transition occurs at a critical value for the separation distance between two partial dislocations—a consequence of the "dislocation interaction" hypothesis for texture. formation. This critical separation occurs when the parameter .r/ub is 3.75 x 10'3. From this, a value for the SFE of 39 ergs per sq cm may be deduced for a Cu-2.85 at. pct A1 alloy. ThE correlation between the rolling texture of fcc metals and the stacking fault energy, SFE, was one of the first attempts to relate atomistic properties with the type of rolling texture.' This correlation gives a qualitative explanation for the experimental observation that the addition of alloying elements, which generally lower the SFE, changes the copper-type texture to a brass-type texture. The simplicity of this correlation had led to its general acceptance and even its quantitative use.' However, it is only a correlation and is largely based on descriptive features of pole figures, and on the poorly known SFE values in dilute alloys. Quantitative verification of this phenomenologi-cal correlation is, in fact, completely lacking. One purpose of the present study is to test this correlation. Another atomistic description for the formation of rolling texture is the "dislocation interaction" hypothesis of texture formation.3 In this hypothesis, the factor controlling the type of rolling texture depends on whether or not the separation distance between two partial dislocations exceeds a critical value. Materials having a separation of less than the critical value are supposed to exhibit a copper-type texture while those with a separation above the critical value are supposed to have a brass-type texture. At the critical value, it is expected that the material should show equal amounts of copper- arid brass-type orientations in their textures, i.e., a 50 pct transition texture. The SFE appears in this hypothesis as only one of several factors which determine the separation distance between partial dislocations. It is possible to test the validity of these two concepts by studying the rolling texture as a function of rolling reduction. Since the SFE per se is an intrinsic property of the metal, it should not, by definition, be influenced by local irregularities, such as variable stress conditions. Thus, no change in texture-type is expected to occur with changes in rolling reduction. On the other hand, according to the "dislocation interaction" hypothesis, any factor that effectively influences the separation distance of partial dislocations would be expected to change the rolling texture. Since the separation distance between partial dislocations is known to depend upon local stresses,4-6 it is anticipated that there would be an effect of the degree of reduction on the texture-type. Also, since applied stresses are more likely to increase, rather than to decrease, the separation between partials,4'5 the overall effect would be to increase the amount of material in the brass-type orientations as rolling reduction is increased. Furthermore, this reduction dependence would be most prominent in alloys exhibiting the transition texture since the distance between partials in those alloys is thought to be close to the critical value. Experimental data in the literature is insufficient to distinguish between these two alternatives. Haessner studied the effect of rolling reduction on textures in a series of Ni-Co alloys by means of the X-ray intensity-ratio technique,' and found that while one texture parameter indicated no reduction dependence the other indicated a slight dependence of the rolling texture on reduction in the range of 96 to 99 pct. As has been noticed previously, the intensity-ratio technique is a convenient but controversial method7 because there is no a priori reason to suggest which intensity-ratio would describe the texture most meaningfully. A more quantitative method of describing textures is found in terms of the orientation dependence of Young's modulus. Here, the type of modulus aniso-tropy associated with the copper-type texture is sufficiently different from that observed for the brass-type texture to allow the two types to be easily distinguishable and a quantitative measure of the amount of each can be deduced from the numerical results. This ability to provide quantitative data is particularly valuable when the two textures occur simultaneously in one alloy as is the case for the transition textures. In this paper the modulus method, supplemented by pole figure data, is used to look for an effect of roll: ing reduction the texture. Also by combining the texture measurements with recent determinations of the SFE in Cu-A1 alloys'0'" it should be possible to test for a relationship between the SFE and textures.

Jan 1, 1970

By O. L. Culberson, J. J. McKetta

INTRODUCTION The equilibrium constants for methane and for water, and for ethane and water have been calculated from experimental data for the two binary systems.2,3,11,12 These constants are for the two-phase systems for the temperature range of 100" to 340°F and the pressure range of 200 to 10,000 psia. The constants for ethane are greater than those for methane. Equilibrium constants for a natural gas from a natural gas-water system6 are about the same as those for methane. Equilibrium constants for water in all three systems are very nearly the same over the greater part of the range of temperatures and pressures studied. In ideal solutions, the vapor-liquid equilibrium constants for a component should be the same in all such solutions at a given temperature and pressure.5 Few solutions are ideal, and consequently the use of generalized constants often leads to error in situations where they do not actually apply. In decidedly non-ideal systems, it is desirable to have equilibrium constant data for the specific system. Vaporization equilibrium constants may be calculated either by thermodynamic methods or from experimental vapor-liquid equilibrium data. In the thermodynamic calculation. the equilibrium constant K may be shown to be" K = fP,/fl'..........(1) where fPi is the fugacity of the pure component i at the given temperature and at the vapor pressure of the pure component, and fp is the fugacity of pure i in the gaseous state at the temperature and total pressure of the system. At best the thermodynamic calculation results in a K applicable to ideal solutions. Equilibrium constants calculated from Equation (1) have been found to have only limited agreement with experimental values, even though the solutions for which they were calculated approached ideality."'" If the more volatile component is at a temperature above its critical, the accuracy of the equilibrium constant for the component is made more doubtful by the use of the vapor pressure term under such conditions. In order to make the thermodynamic calculation on a component above its critical temperature, one must resort to one of the empirical methods of extrapolation of the vapor pressure to conditions above its critical point.13 Application of the thermodynamic equilibrium constant then to the methane-water or the ethane-water systems would be risky since the systems are non-ideal, and the methane and ethane are above their critical in most petroleum operations. ETHANE-WATER SYSTEM In the temperature range of from 100° to 340°F and for pressures up to 10,000 psia, the vapor-liquid equilibrium data 'References given at end of paper. Manuscript received in the office of the Petroleum Branch March 16, 1951.

Jan 1, 1951

By J. J. McKetta, O. L. Culberson

INTRODUCTION The equilibrium constants for methane and for water, and for ethane and water have been calculated from experimental data for the two binary systems.2,3,11,12 These constants are for the two-phase systems for the temperature range of 100" to 340°F and the pressure range of 200 to 10,000 psia. The constants for ethane are greater than those for methane. Equilibrium constants for a natural gas from a natural gas-water system6 are about the same as those for methane. Equilibrium constants for water in all three systems are very nearly the same over the greater part of the range of temperatures and pressures studied. In ideal solutions, the vapor-liquid equilibrium constants for a component should be the same in all such solutions at a given temperature and pressure.5 Few solutions are ideal, and consequently the use of generalized constants often leads to error in situations where they do not actually apply. In decidedly non-ideal systems, it is desirable to have equilibrium constant data for the specific system. Vaporization equilibrium constants may be calculated either by thermodynamic methods or from experimental vapor-liquid equilibrium data. In the thermodynamic calculation. the equilibrium constant K may be shown to be" K = fP,/fl'..........(1) where fPi is the fugacity of the pure component i at the given temperature and at the vapor pressure of the pure component, and fp is the fugacity of pure i in the gaseous state at the temperature and total pressure of the system. At best the thermodynamic calculation results in a K applicable to ideal solutions. Equilibrium constants calculated from Equation (1) have been found to have only limited agreement with experimental values, even though the solutions for which they were calculated approached ideality."'" If the more volatile component is at a temperature above its critical, the accuracy of the equilibrium constant for the component is made more doubtful by the use of the vapor pressure term under such conditions. In order to make the thermodynamic calculation on a component above its critical temperature, one must resort to one of the empirical methods of extrapolation of the vapor pressure to conditions above its critical point.13 Application of the thermodynamic equilibrium constant then to the methane-water or the ethane-water systems would be risky since the systems are non-ideal, and the methane and ethane are above their critical in most petroleum operations. ETHANE-WATER SYSTEM In the temperature range of from 100° to 340°F and for pressures up to 10,000 psia, the vapor-liquid equilibrium data 'References given at end of paper. Manuscript received in the office of the Petroleum Branch March 16, 1951.

Jan 1, 1951

By A. R. Elsea, E. E. Fletcher

This paper describes a metallographic investigation of the influence of tungsten or molybdenum additions upon the transformation and precipitation reactions occurring in Co-rich Co-Cr alloys. It is shown that tungsten has little effect upon the a-ß transformation temperature range, while molybdenum tends to raise it. Both elements tend to promote the formation of ? phase, molybdenum being more potent in this respect than tungsten. HIGH temperature alloys, that is, alloys which have load-carrying ability at elevated temperatures, have been developed at an increasing rate during the past few years. This has resulted from the requirements in the design of modern aircraft engines. Although many alloys of this type are available, they have been developed on an empirical basis. Metallurgists do not have a clear understanding of the phases or structures that are responsible for these high temperature properties. In order to determine why these alloys possess this particular ability, a project was started at Battelle Memorial Institute with the object of learning more about the fundamental factors which promote high temperature strength in alloys. This study was to include a correlation of microstructure and the high temperature properties of Vitallium, an alloy which is widely used for high temperature service. Vitallium is a complex material both from the standpoint of composition and microstructure. Consequently, it was necessary to obtain informa- tion regarding the phase relationships in this alloy. The Co-Cr binary diagram was determined as the first phase of this investigation.' A second paper described the effects of iron, nickel, or nitrogen on the reactions occurring in the Co-rich end of this system.' The present paper covers a continuation of this investigation in which the effects of tungsten or molybdenum on the reactions occurring in Co-rich, Co-Cr-base alloys were determined. Preparation of 'rest Materials Two series of ternary Co-Cr-base alloys, representing Co-Cr ratios of 80:20 and 68:32 ( Cr x 100 =20 and 32 ) , were prepared containing ( Co + Cr = up to 6 pct W and up to 12 pct Mo. Melting stock consisted of electrolytic Co, electrolytic Cr, 99.9 pct pure W, and 99.9 pct pure Mo. Table I lists the chemical analyses of these materials. The melting furnace was a vertical porcelain tube

Jan 1, 1952

By W. Jolley

Decarburized iron and Fe-3.28 pct Ni alloys were impact and tension tested in the temperature range of ambient to 4°K. It was found that alloying with nickel improves the fracture properties of the ferrite matrix. The improvement in toughness of iron alloyed with nickel is attributed to the effect of the nickel addition on the temperature and strain rate dependence of the yield stress as well as on slip behavior. The Fe-Ni alloy exhibits wavy slip when strained at temperatures down to at least 50°K. This behavior contrasts with that of the unalloyed iron where a change It is a generally accepted fact that of the common alloying elements of steel only nickel and manganese improve both the room-temperature yield strength and the notch impact properties. It has been argued for a number of years that manganese refines the ferrite grain size, the pearlite spacing, and the grain boundary carbides in medium- and low-carbon steels and thereby increases resistance to brittle fracture.''' This hypothesis recently was confirmed for a 0.04 pct C iron containing manganese, but at the same time from wavy to planar slip occurs at about 120°K. The observed lower temperature and strain rate dependence of the lower yield stress in the Fe-Ni alloy as compared to the unalloyed iron may be attributed to this difference in slip behavior. In contrast to suggestions published previously, transmission electron microscopy showed that the uniform dislocation distributions and the lack of dislocation tangles which are produced by low-temperature straining of bcc materials cannot be attributed to the absence of cross slip at these temperatures. no increase in notch toughness was observed in a decarburized Fe-Mn alloy.3 It thus appears that manganese only increases the toughness of Fe-Mn-C alloys by refining grain boundary carbides and has no toughening effect in carbon-free iron. On the other hand, the mechanism whereby nickel improves toughness has not been established. Hodge et a1.4 have clearly shown that a 3.28 pct Ni addition lowers the impact transition temperature of 0.02 pct C steel approximately 35°C when the grain size is maintained constant. Recently, Wullaert and Tetelman6 stated that nickel refined the grain boundary carbides of an Fe-C alloy and consequently increased the toughness. They also observed the previously reporteda-'

Jan 1, 1969

By D. E. Marks, Arnold, C. W, R. J. Robinson, A. E. Hoffmann

The efficiency of operation of a fixed-bed adsorption unit is infEuenced both by the absolute adsorption capacity of the bed and by the rate of adsorption. This paper describer studies of adsorption rate which were conducted in an experimental unit designed such that conditions existing in the treatment of high-pressure natural-gas mixtures could be duplicated. Variables investigated included pressure, temperature, gas composition, adsorbent particle size, depth of packed bed and gas velocity. The adequacy of a simplified mathematical model for predicting the observed phenomena was tested. A correlation is preserited which relates adsorption rate to the process variables stlldied. This correlation is useful in combination with the matheinatical model. INTRODUCTION Of the techniques available for contacting adsorbent particles with fluid streams to be treated, fixed-bed adsorption columns offer definite advantages in simplicity and ease of operation. As a result, they are often used in preference to others for such petroleum industry applications as dehydration and purification of natural gas and hydrocarbon recovery. Fixed-bed adsorption units usually consist of two or more towers filled with a desired adsorbent and operated in a cyclic manner. While one is being used to process the main flow stream, the others are undergoing regeneration to remove the adsorbed phase. When the tower on stream becomes saturated with the preferentially adsorbed material, the roles of the towers are switched, and the freshly regenerated tower is placed on stream. Cacle duration is determined by the bed capacity under the process conditions and by the flow rate through the bed. The sharpness of separation which can be effected is a function of both the absolute capacity of the bed and the rate of adsorption in the bed. The effect of rate for a particular set of conditions is evidenced by the sharpness or diffuse-ness of the adsorption front as it advances through the bed. Since data needed for design of adsorption units to treat high-pressure natural-gas systems were not available, an experimental program was designed to investigate the effects of different variables upon adsorption rate in fixed beds. In the present paper, effects of gas composition, column length, temperature, pressure, adsorbent particle size and flow rate (actual linear flow rate of the gas) are shown, and utility of a simplified mathematical model for describing the process is discussed. As gas enters the top of a cool, clean bed of adsorbent, preferentially adsorbed materials are stripped from the main flow stream by the uppermost particle layers. As these layers become saturated with a particular component, new supplies of this component are carried further down the column until fresh adsorbent is encountered. An adsorption wave thus moves through the column as material is supplied to saturate succeeding elements of the bed. Adsorption from a Multicomponent gas stream occurs as a succession of such moving waves corresponding to the different components in the gas. The leading edge of an adsorption wave for a component of a natural-gas stream moving through a bed of a common commercial adsorbent such as silica gel would be sharp but for the influence of certain broadening fac tors. These factors include a nonuniform velocity profile in the bed, longitudinal dispersion or mixing in the main gas stream, and the time required for a molecule to migrate from the main gas stream and be adsorbed at a site within the body of an adsorbent particle. If packing is uniform and the ratio of column to particle diameter is greater than approximately 15:1, the first factor is relatively unimportant' Longitudinal mixing is of importance only for the case of moderately high mass transfer with extremely slow flow rates.' The sharpness of an adsorption front, therefore, is, primarily a function of the rate of adsorption or the time required to saturate a particle of zdsorbent. Two methods for defining adsorption rate are used in this work. The first is a normalized or relative rate which describes the rate of saturation of a differential element of the packed bed. This can be measured by observing the time required for the concentration of the preferentially adsorbed material in the effluent gas from the bed to rise from zero to a value equal to that in the inlet gas stream. The second definition describes the absolute rate of mass transfer from the gaseous to the adsorbed phase. This definition is used in a mathematical description of the adsorption process. If the concentration of a component in the gas strcam leaving an adsorption column is measured and plotted as a function of time, a curve such as that shown in Fig. I results. It is seen that for a period of time the effluent gas is devoid of the component under consideration. As the bed approaches saturation, a small percentage of this material will appear in the effluent gas. The concentration will then rise with time, or increasing cumulative gas flow, until it is equal to that in the inlet gas stream. If adsorp-

By T. T. Read

A short time ago, one of the large steel companies courteously furnished the author with detailed records of the operations of a considerable number of iron blast furnaces over a period of two months. These will be made the basis of a subsequent study, but in beginning this study one of the first points requiring consideration was the probable error of the records, for what otherwise might be regarded as significant differences of performance under different conditions were perhaps really due to errors of observation, or failure to observe and record variations. If it is assumed, in blast-furnace records and calculations, that known quantities or factors are constant, .when as a matter of fact they are variable, the effects of these variations may erroneously be ascribed to some other cause. This is quite clearly expressed in the following quotation from E. Buckingham:l Theory always operates on an ideally simplified picture of reality because real phenomena are unmanageably complicated. The results obtained are not exactly true for any real phenomenon, though they may be for an ideal one; and the approxi-mation with which a theoretical equation, however obtained, represents the actual facts, always depends on the approximation in essentials between the ideal picture and its real prototype. The purpose of dimensional reasoning is to find out how some quantity which is involved in the phenomenon under consideration is related to certain others; or to find the relation connecting two or more quantities which vary, or may vary, simultaneously during the course of the phenomenon. Since we know that we must have a complete equation to start with, we begin by thinking the matter over, to see whether the quantities we have in mind are the only ones involved. Usually it is evident that they are not; so we next make a list of all the quantities we can think of which might under any circumstances be important. Upon considering this list, which is often a long one, it is usually evident that under the actual circumstances a number of these quantities may safely be ignored; so we cross them off the list and thus pass from our most general conception of the phenomenon to an ideal simpler one, in which these quantities are not involved at all.

Jan 1, 1926

By CHARLES F. DEISS

The total pipe-line runs of petroleum in Indiana during 1945 were 4,114,000 bbl., a decline of nearly 17 per cent below the estimated 4,950,000 bbl. produced in 1944. Drilling activity during the year was centered in Posey and Gibson Counties, where seven new pools were discovered in the state. Four of the pools are in Posey County-Crunk, Farmersville, Jeffries and St. Wendells East-and the other three are in Gibson County-Johnson West, Lysle and Mt. Carmel East.

Jan 1, 1946

By P. A. Beck, A. Merlini

Quantitative texture determinations were made for rolled and for rolled and annealed strips of 3, 6, and 10 pct Zn brasses. The main components of the rolling texture gradually shift over a wide composition range from the orientation characteristic of copper to that of 70-30 brass. At least the main features of the corresponding gradual changes in the annealing texture may be accounted for qualitatively on the basis of the oriented growth theory of annealing textures. All the oriented nucleation-type theories are notably less successful in accounting for the observed textures. EARLIER investigations by von Goeler and Sachs,' Dahl and Pawlek,' and Brick, Martin, and Angier" suggested that the annealing texture of copper is more sensitive to the addition of solute elements than the rolling texture. It was reported3 that the cube texture changes over into a brass-type recrys-tallization texture on addition of about 1 pct Zn, while the deformation texture changes only at about 5 pct Zn. Such behavior would be difficult to reconcile with any theory of annealing texture formation that relates the annealing texture to the deformation texture. In particular, the oriented growth theory of the cube texture" is based on a certain orientation relationship between the cube texture and the main components of the deformation texture which could not be reconciled with the reported behavior of low brasses. It was, therefore, of interest to re-examine these textures by means of the quantitative methods now available. The deformation and annealing textures of rolled a brasses with approximately 3, 6, and 10 pct Zn have been determined in terms of (111) and (200) pole figures. Experimental Methods The chemical analyses of the Cu-Zn alloys of commercial purity used in the present work are given in Table I. Chill-cast bars of the tabulated compositions were rolled and annealed according to the following schedule: I—rolling from 1.2 to 1.02 in. thickness, 15 pct reduction area, annealing 15 min at 450°C; 2— rolling from 1.02 to 0.867 in. thickness, 15 pct reduction area, annealing 15 min at 450°C; 3—rolling from 0.867 to 0.600 in. thickness, 31 pct reduction area, annealing 2 hr at 540°C; 4—rolling from 0.600 to 0.400 in. thickness, 33 pct reduction area, annealing 2 hr at 480°C. In the final straight rolling of 96.25 pct reduction area, the strips were reversed end to end after each pass. The final annealing temperature was determined for each alloy by annealing specimens of the cold-rolled strips in salt bath for 5 min at varying temperatures. The results of the hardness measurements are given in Fig. 1, where the final annealing temperature used for each alloy in determining the annealing texture is indicated by a cross.

Jan 1, 1956

By D. M. Collingwood

The year 1928 has been marked by scattered but considerable wildcat drilling considering the overproduction prevalent in the oil industry. This wildcatting has resulted in the discovery of oil in one interior salt dome, several small fields producing from serpentine, Taylor marl, and Austin chalk, and two new fields producing from the Edwards limestone, one of which in the Bruner or Salt Flat area of Caldwell County promises to be of major importance if not quite as large as the Luling field. Fig. 1 shows production by fields for 1928, compared in the case of the older fields, with that for 1927. New Production From Salt Domes Boggy Creek Dome This salt dome was discovered in 1927 by core drilling and deep tests recommended on the evidence of surface geology. A large block of acreage controlled by the Humble Oil & Refining Co. covers the dome. Since the discovery of the deep-lying salt plug and oil on the flank of this dome in 1927, development has proceeded slowly. Since most of the acreage is controlled in a large block by one company there has been no intensive competitive drilling. Approximately 8 producers and 16 dry holes have been drilled. Production is from the eastern equivalent of the Woodbine and Eagleford horizons of the Mexia district, and has been found extending in a northeast-southnlest direction across the River Neches on the southeast flank of the dome. One of the best wells, the T. H. Jones No. 2, had an initial production of 90 bbl. per hr., and others have made from 100 bbl. per day to 50 bbl. per hr., but production of the better wells has either been shut in or choked down to less than 2000 bbl. per day. At the end of the year the daily average, production was about 2500 bbl. from 8 wells. Considerable gas pressure is present and one well, the Elliot Clark No. 2, drilled in 1927, was shut in with an estimated wet gas production of over 5,000,000 cubic feet.

Jan 1, 1929

By D. P. Koistinen, K. E. Beu

THE application of the integrated intensity X-ray diffraction method to the measurement of retained austenite concentrations in hardened steels has been fully described.'-' In developing this particular method, the assumption was made that the samples used would have flat surfaces which were free from voids and in which austenite was homogeneously distributed. The original calculation procedure' was modified to include the constant factor G which relates the intensity of a given diffraction line to the concentration of the component giving rise to that line. In order to include A (0) in the constant factor G, it was further assumed that the geometrical conditions relating the X-ray beam, camera cylinder, and sample surface were precisely met.V has been demonstrated that these geometrical conditions can be met experimentally without difficulty in many cases;' however, for those samples which have irregular surfaces or where it is impossible to locate the sample in the proper position with respect to the X-ray beam and film cylinder, it is desirable to evaluate experimentally what effect these nonideal conditions have on the reliability of the austenite determination. This note decribes the results of such experiments. SAE 1095 bar stock was used throughout and all samples were heat-treated as follows: 1600°F for 1 hr in a neutral atmosphere, brine quench, and 300°F temper for 30 min. To control heat-treatment conditions as closely as possible, all samples were plated with 0.002 in. copper to protect the immediate surface from the heat-treating atmosphere. After heat treating, the samples were deplated electroly-tically so that only the copper was removed. The heat-treated surfaces thus obtained were nearly as bright and polished as the original surfaces before copper plating although no mechanical work was done on the samples after heat treating.

Jan 1, 1954

By D. R. Parrish, T. M. Geffen, R. A. Morse, G. W. Haynes

Flow tests on small core plugs have indicated that a large amount of gas is trapped and not recovered by water flooding a gas sand. Instead of I to 15 per cent pore space, as is usually assumed, the residual gas saturation is 15 to 50 per cent pore space, and is thus of the same magnitude as residual oil after water flooding oil sands. A thorough investigation was made to ascertain that large amounts of residual gas actually remain in reservoirs after a water flood and that this condition is not merely a laboratory phenomenon. In field experiments, the amount of gas left in a watered-out gas sand was measured by use of a pressure core barrel and the residual gas saturation of two watered-out gas sands was determined by electric log evaluation. In the laboratory, an investigation was made of factors that could possibly cause the value of residual gas saturation as measured on small core plugs to differ from that in the reservoir, and the effect of these factors on the amount of residual gas saturation was studied. The factors studied include flooding rate, static pressure, temperature, sample size and saturation conditions before flooding All evidence established that a relatively high gas saturation is trapped in water flooded gas sands and that this residual gas saturation can be measured in the laboratory by tests on small core plugs. INTRODUCTION There. has been general agreement among engineers that very high recovery of gas could be obtained from natural reservoirs By water displacement. Gas recoveries of 80 to 95 per cent of the original gas in place have become the normal expectation in water drive fields. The assumption of high recovery has been based on: 1. low density and viscosity of gas compared with water; 2. the erroneous assumption that the flow relationship in a gas-liquid system where gas is the displaced phase will be the same as when it is the displacing phase. It has long been recognized that gas can flow at very low gas saturations (in the range of 1 to 15 per cent pore space) in systems where liquid is being displaced by gas. By assuming the reversibility of this process, the conclusion was reached that the residual gas saturation following water flooding of a gas reservoir would be the qame (1 to 15 per cent) as that at which gas first flowed continuously as a displacing phase. Recent laboratory relative permeability Studies have demonstrated that the flow characteristics are very different in gas-liquid systems, depending on whether gas is displacing or being displaced by, a liquid. Also, it has been shown that there is no difference between the flow characteristics of oil and water or gas and water in water wet porous rocks. The residual gas saturation that can be expected following water flooding of a gas reservoir then would be in the same range as the residual oil saturation normally expected after water flooding an oil reservoir! i.e., in the range of 15 to 50 per cent pore space, depending on the rock characteristics. Obviously, such a difference in residual gas saturation means very important differences in recoverable gas reserves from water drive reservoirs. For example, if the original gas saturation in a field were 70 per cent, and the residual gas following flooding were 35 per cent, only half of the gas in place could be recovered by complete water drive, compared to the previously expected 80 to 95 per cent. This is a situation in which complete pressure maintenance could result in very greatly reduced recovery, since straight pressure depletion recoveries from gas reservoirs can approach 80 to 90 per cent. Such a change in thinking must be based on more complete information than a series of small core tests. Hence the work reported herein was undertaken with the objective of determining whether or not residual gas saturations indicated from small core relative permeability tests at atmospheric pressure and room temperature are representative of the residual gas saturations which could be expected after water flood of natural reservoirs. A study was made both through laboratory and fields tests to determine any differences in residual saturation which might be occasioned by differences in pressure, temperature, rate of flooding, and original saturation conditions. Four separate types of laboratory experiments and two field mesurements were made in this investigation. The apparatus and testing methods of each will he discussed individually. LABORATORY EXPERIMENTS, APPARATUS AND PROCEDURE Relative Permeability Tests Steady state flow experiments Here conducted using the Penn State type apparatus. The equipment used has beer (described in a previous publication? "Irreducible" water satu-ration was established in the core' by imposing ,a capillary pressure of 45 psi before simultaneous flow of air and water

Jan 1, 1952

By R. I. Jaffee, F. C. Holden, H. R. Ogden

The effects of ternary and quaternary additions of aluminum, oxygen, and carbon on the mechanical properties of high-purity titanium-molybdenum alloys were studied for several microstructural conditions. Heat treatments were designed to produce 1) ß-quenched, 2) equiaxed ß) transformed (acicular) and 4) stabilized -P microstructures. Tension, impact, and hardness tests were performed. Transformations from the ß phase were followed by hardness measurements and metallography. The ß-to-w transformation was slowed by aluminum additions; carbon and oxygen additions increased the transformation rate. In addition to solid-solution strengthening, these solutes may increase or decrease strength by altering the /3 transformation kinetics. Aluminum additions promote the formation of strain-induced martensite, and lower yield strengths at compositions near 12 pct molybdenum.. a-P alloys are more ductile with equiaxed than with transformed microstructures. High strength levels can be reached by aging in many cases. Strength levels of the aged specimens usually are lowered slightly by straining prior to aging. ALLOYS of molybdenum with titanium form an iso-morphous alloy system which has been the subject of several investigations. Additions of substitu-tional and interstitial -stabilizing elements provide means of improving mechanical strength and con- trolling the heat-treatment response of the binary alloys. The work reported here forms a part of a continued study of the effects of microstructure on the mechanical properties of high-purity titanium alloys. Previous papers have considered the various binary alloys (Ti-Mo, Ti-Al, Ti-C, and Ti-0) that form the bases for the ternary and quaternary alloys included here. The compositions were selected to correspond with the previous binary alloys. Further, the high purity of the alloying components was maintained, so that direct comparisons with earlier work can be made. The total research program included a large number of compositional, microstructural, and testing variables. The data reported here have been selected to provide a reasonably complete and representative summary of the results. The reader is referred to the original Air Force Report for a complete tabulation of the results. EXPERIMENTAL PROCEDURES All the alloys used in this work were prepared from high-purity electrolytic titanium produced by the U.S. Bureau of Mines. A typical furnished analysis showed the following impurities in wt pct, balance This analysis is equivalent to that of iodide-refined titanium. In addition, hardness, tensile, and impact tests made using unalloyed electrolytic titanium showed it to have properties equivalent to those obtained with iodide titanium and suitable for these studies of high-purity base alloys.

Jan 1, 1962

By H. E. Stauss, G. Sandoz

THE purpose of this note is to draw attention to the possibility that a melt may be contaminated by a material not in direct contact with it by means of gaseous intermediate agents. In recent years silicon has assumed a position of importance because of its use in rectifiers and transistors and close attention has been required to control of both purification and contamination during all stages of preparation.' This note reports the observation that a graphite heater may have contaminated silicon ingots without direct physical contact through reactions that developed gaseous products. Several ingots made with the equipment of Hino and Stauss,2 using a graphite heater in a dried helium atmosphere, were found to have a small amount of a very hard substance on the free surface. X-ray analysis by F. W. von Batchelder showed the sub- stance to be Sic. Similar contamination was not found when the heater was tantalum, indicating that the carbon had not come from an original impurity in the silicon powder. One source of the carbon could have been volatile matter released from the graphite heater. This heater had been used about ten times at the time of the observations. A second source of carbon could have been a direct reaction between the quartz crucible and the graphite heater to form CO, or an indirect reaction involving a crucible-melt interaction and volatile SiO as an intermediate product. Such reactions should have developed Sic on the heater; and in fact a yellow powder did form on the inside of the graphite heater although its composition could not be determined. References 'H. C. Torrey and C. A. Whitmer: Crystal Rectifiers (1948) Chapter 10. New York. McGraw-Hill Book Co. 2 J. Hino and H. E. Stauss: Trans. AIME (1952) 194, p. 656; Journal of Metals (June 1952).

Jan 1, 1954

By Rana P. Singh

Electrolytic metal reduction operatios in both aqueous and molten salt electrolytes are being studied by digital signal analysis. The purpose is to determine the relationship between the physical processes occurring in the cell and the frequency spectrum of the cell's fluctuating electrical parameters. The fast Fourier transform of cell voltage (in galvanostatic operations) or cell current (in potentiostatic operations) is computed on-line in real time for the electrorefining of zinc in aqueous acid chloride solutions.

Jan 1, 1984

By John W. Weeton, Donald W. Petrasek

Relatively few metal-metal systems exist that would permit the creation of fiber-metal composites consisting of mutually insoluble constituents. It is anticipated that most high strength-to-weight ratio and high -temperature fiber composites ultimately to be produced will utilize high-strength fibers embedded in a highly alloyed matrix. An investigation was conducted to determine the effect of alloying on the tensile Properties and micro-structure of tungsten-fibey-reinforced composites. Composites were made of tungsten fibers infiltrated with copper binary alloys that contain elements of varying solubility in tungsten. Room-temperature tensile tests were made on the composites, and a metallographic study of the microstructure of the fiber-metal-matrix interfaces was conducted. It was shown that, as the depth of penetration of some alloying elements into the fiber increased, a decrease in both tensile strength and ductility of the composite results. A notch effect, due to the formation of a brittle alloy zone with the tungsten fiber, was observed and gave rise to greater reductions in tensile properties and ductility behavior than would be Predicted by a law-of-mixture relation alone. In recent years, investigators have considered combining fibrous materials with relatively weak binder materials. The interest in fiber-reinforced composites results from the fact that fibers or wires may be exceedingly strong and exhibit mechanical properties superior to those of the bulk materials from which they are derived. For example, tungsten wires drawn to less than 1 mil in diameter may have strengths of over 600,000 psi,' while steel wires ranging from 10 to 3 mils in diameter may have strengths of the order of 300,000 to over 600,000 psi.2 Both metallic and ceramic whiskers are known to have very high strengths. For example, iron whiskers have been shown to have strengths of 1.9 million psi3 and sapphire whiskers have been reported to have strengths of the order of 1.7 million psi.4 If all or part of the strengths of such fibers could be retained, subsequent to the incorporation of the fibers in an engineering material, a superior material could result. In previous work done at the Lewis Research Center, McDanels, Jech, and weeton5 demonstrated the feasibility of fabricating metal-fiber—metal-matrix composites that utilized the full strengths of the fiber and matrix materials. Tungsten fibers were combined with a copper matrix by a liquid-infiltration method such that the tungsten fibers were uniaxially oriented parallel to the tensile axis of the composite. A linear relation was established that related the tensile strength of the composite with the volume percent of the fibers. Mutually insoluble constituents were selected for the study so that the strength of the composite could be quantitatively related to the strength of the individual constituents. The fact that there are only a few metals that are mutually insoluble with tungsten, e.g., copper, silver, gold, and zinc, and that these either have low melting points, high vapor pressures, or poor oxidation resistance, makes it necessary to utilize other metals that are soluble in tungsten, where high-temperature applications are ultimately contemplated. It was anticipated that, for most practical fiber-reinforced composite materials, it would be necessary to use a fiber and metallic matrix that would have varying degrees of solubility for each other. A logical extension of the earlier work was thus felt to be a study that would determine the effects of elements that had mutual solubility with the tungsten. Numerous investigators have found that tungsten fibers may be damaged by thermal treatments or contamination of the surface of the fiber by alloying elements.6-10 On the other hand, surface treatments may improve the strength of such fibers."-" Relatively little work with composites containing tungsten fibers have been reported. The work of parikh14 has shown that kinked, short-length tungsten, steel, and molybdenum fibers could str'engthen such matrices as silver, gold, and copper. Some of the combinations of fibers and matrices studied by

Jan 1, 1964

By T. W. Harris

This paper was written in conjunction with the work being undertaken by the Technical Committees on Classification of Coal, and an effort has been made to compile information relative to the use of coal for stationary steam generation in order to use this information to assist the Committee on Classification of Coal for the ultimate purpose of elimination of losses both by the reduction of individual effort and waste in the consumption of material. Under the auspices of the National Association of Purchasing Agents, a questionnaire was drawn up to develop this information from stationary steam plants throughout the United States in order to consolidate the information developed from the many hundreds of boiler tests on coals consumed by various coal-burning equipment. These questionnaires covered: 1. The company reporting, location and method of delivery to the plant. 2. Complete coal data, including description of coals used (with sufficient space to include first, second and third preference) on source of coal used, complete analysis and factors affecting choice of coal used. 3. Plant data, divided into: (a,) hand-fired, (b) overfeed stokers, (c) underfeed stokers, (d) traveling grate stokers, (e) pulverized coal; and included complete description of furnace data, draft data, coal-burning rate, type of stoker, type of pulverizer, efficiency data and remarks. The questionnaire was drawn up by consultation with various combllstion engineers, including B. J. Cross, Test Engineer of the Combustion Engineering Co., W. H. Fulweiler, of the United Gas Improvement Co. and the U. S. Bureau of Mines. In all, 11,538 copies of the questionnaire have been distributed, of which 4369 were sent in duplicate. Our estimate of the total volume of bituminous coal consumed in stationary steam boilers over the 12 months of 1930 is approximately

Jan 1, 1934

By G. H. Cady, L. C. McCabe, D. R. Mitchell

While running certain float-and-sink tests, unit coal calorific values were determined for gravity fractions of a series of Illinois coals from several districts in the southern part of the state. When these values were plotted against specific gravity what appear to be characteristic curves of somewhat different shape were obtained for each district represented. This in itself seems noteworthy. The shape of the curves seems to indicate that the lightest fraction of the coal, which inspection shows to be largely vitrain, suffers the least deterioration in storage. It was also observed that on dilution curves established with dry ash and B.t.u. values the fractions of 1.35, 1.40 and 1.50 sp. gr., which constitute the greater weight per cent of a given coal sample, fall more frequently on a straight dilution line than do the lighter or heavier fractions of the same sample. In most instances there is a marked steepening between the 1.35 and the fraction of lighter gravity. In general the curve increases in steepness between the fractions of 1.50 and 1.70 specific gravity. The variations in the unit coal-specific gravity curves as well as those observed in dilution curves which appear to be pertinent to this problem are: (I) variation in coal substance with change in specific gravity, (2) variation in kind and quantity of mineral matter with the specific gravity of the fraction, (3) factors of analytical procedure which tend to introduce error in analysis, particularly in high-ash and high-sulfur fractions. DISCUSSION (A. C. Callen presiding) E. Stansfield, ? Edmonton, A1ta.-—The necessity of avoiding oxidation in grinding and in drying should be emphasized. My assumptions as to pure coal coincide with t,he author's but most of my curves are nearly straight lines. The low sulfur content

Jan 1, 1934