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By C. E. Sims, C. A. Zapffe

AN investigation of the behavior of inclusions in steel several years ago1 led to the conclusion that some of the commonly occurring inclusions in steel have appreciable solubilities, particularly in liquid steel. In the belief that further study and clarification of this matter was warranted, a laboratory study of oxides in liquid steel was started. These oxides are generally the result of deoxidation treatment, and the basis of an understanding of their behavior must be, therefore, the behavior of the deoxidizer in liquid iron. The Fe-Si-O system was selected for the first study, and the apparatus used and experiments conducted are described herein. APPARATUS The apparatus is shown in Fig. I and the system is shown by diagram in Fig. 2. Furnace Atmosphere Commercial hydrogen (1) passes through an orifice (2) into a manometric system that measures the tankside pressure (3) and the back pressure (4) in the system. A water trap (5) guards against excess tankside pressure. A by-pass with stopcocks (6 and 7) is provided, so that the hydrogen can be routed directly from the tank to the furnace if desired. When stopcock 7 is closed and stopcock 6 is open, the gas proceeds through the conditioning train, of which the first unit is a furnace (8) that contains platinized asbestos at 350°C. The temperature is measured by a thermo-couple and potentiometer (9) and is controlled by a slidewire resistance (10). In [ ] this furnace free oxygen is converted to water vapor. The exiting gas passes over a water bath (11) kept slightly below boiling temperature by an auxiliary heating unit (12). This unit also heats a surrounding copper coil (13) containing water, and the heated water rises through a collar (14)

Jan 1, 1942

By Felix E. Wormser

REGISTRATION started bright and early Monday morning in the Silver Corridor at the Waldorf-Astoria with Mrs. W. H. Bassett as chairman. What a registration-over 200 ladies! Several joined us from as far away as California and Washington State. Apparently they enjoy our meetings so much that present travel inconveniences didn't discourage their coming. At noon the ladies joined the men at the All-Institute Luncheon and Monday evening we had our informal dance, which is separately reported. Tuesday morning was devoted to our annual meeting at which all Section annual reports were read. At noon we were all the guests of the W.A.A.I.M.E. at a luncheon at the Port Arthur Restaurant on Mott St. in Chinatown. Many of us rode down on the old 3d Ave. elevated railway-the last of four. It, too, is soon to be torn down. The luncheon was delightfully unusual, with huge dishes of delicious Chinese food on each table. Our chairman, Mrs. Read, who lived in China in her youth chose our menu, and she chose it well, for most of us indulged so heartily that as we arose from the table we felt we couldn't eat again for 24 hours. Someone donated sherry wine, and boxes of Chinese pencils as favors. We wonder who? All owe a big vote of thanks for this lovely party to Mrs. T. T. Read and Mrs. H. A. Prosser, chairmen, and Mrs. H. W. Hardinge, Mrs. R. Hursh, and Mrs. R. L. Lloyd, vice-chairmen.

Jan 1, 1944

By K. A. Johnson, F. H. Ellinger, C. C. Land

The Pu-La alloy systenz has been studied by thertnal, tnzcrographic, and X-ray diffraction methods. It is churacterized by a liquid miscibility gap, a maximum solubility of about 20 ut. pct PM in y lanthunum and 19 at. pct PI* in 0 lanthanum, very little soluibility of lanthanum in the plulonium allotropes, and the absence of intermediate phases. THE existence of immiscible liquids in the Pu-La system has been reported by Schonfeld.1 A tentative phase diagram based on the results of thermal-analysis experiments has been constructed by Poole et a1 2 This diagram shows a liquid immiscibility loop with a monotectic at 77 at. pct La and 846°C. 7 lanthanum is shown to dissolve 20 at. pct Pu and to decompose by an inverse peritectic reaction (y La = L , + p La) at about 82 at, pct La and 833°C. The ß lanthanum solvus was not determined, but the thermal work indicated a maximum solubility of 16 at. pct Pu in ß lanthanum. The present investigation has defined the solubility limits of plutonium in y lanthanum and 0 lanthanum, and, with the exception of minor discrepancies, has verified the results of Poole et al. 1) EXPERIMENTAL The electrolytic plutonium melting stocks were better than 99.9 wt pct pure, the main impurities being 90 ppm Fe and 50 ppm W. The lanthanum melting stocks, supplied by Research Chemicals and the Cerium Metals Corp., were about 99 wt pct pure, the main impurity detected by our spectrochemical analysis being 2000 ppm Fe. The components for each alloy button (-5 g) were weighed on an analytical balance and were melted together in a conventional arc furnace. If no significant weight loss occurred during melting, the as-weighed

Jan 1, 1968

By D. de Fontaine

A convolution procedure is described for obtaining an analytical expression for the composition profiles of solute concentration:; in binary solid solutions. The free energy of solutions containing such compositional inhomogeneities can then be evaluated and the stability of spherically symmetric clusters (G.P. zones, for short) us a function of their radii and central compositions can be studied accordingly. Two characteristic zone radii are defined: the minimum radius (RM) corresponding to the smallest zone for which growth is energetically favored over dissolution, and the critical radius RK) corresponding to zones associated with the minimum work of formation. The values of RM and RK coincide at the two classical limits of nucleation and growth and spinodal decomposition. As the spinodal is approached, however, RM and RK diverge increasingly and it is proposed that the initial] decomposition morphology is governed more closely by the minimum, rather than by the critical radius since the former possesses no singularity within the m eta stable phase boundary. Reversion is briefly discussed in the light of the foregoing and it is shown that a set of reversion temperatures located between the coherent miscibility gap and the coherent spinodal must correspond to a given distribution of low temperature zones. SINCE the early works of Guinier1 and preston,2 the kinetics and morphology of GP zones have been studied extensively, see Ref. 3, for example, for a recent review. Nevertheless, a completely satisfying theoretical treatment of the decomposition of meta-stable or unstable binary solid solutions is still lacking due to the almost unsurmountable mathematical difficulties that one encounters in attempting to solve the pertinent diffusion equation which, in principle, describes the whole process. This equation, first derived by Cahn for the initial stages of spinodal decomposition,4 is a nonlinear partial differential equation of the fourth order in anisotropic space, a general analytical solution of which is completely out of the question. From this equation, some prediction can be made, however, concerning the later stages of spinodal decomposition5 and a recent numerical solution6 of the equation in the case of one- and two-dimensional composition modulations of a solid solution inside the spinodal has led to the following considerations: the sinusoidal morphology7 is to be expected only for solutions of average composition c, located near the center of the coherent miscibility gap.8 For solutions with co closer to the spinodal decomposition, depleted shell zones9 should constitute the first recognizable decomposition product, later evolving to iso- lated, enriched preprecipitates in a uniformly depleted matrix as this must, in all cases, constitute the final metastable morphology, barring, of course, loss of coherency and change in crystal structure. In agreement with the qualitative description of Bonfiglioli and Guinier,l0 it thus appears that the various models discussed by previous authors are, in fact, idealized successive stages of the general decomposition process. Unfortunately, corresponding calculations for a solid solution outside the spinodal are not yet available because of two additional difficulties: it is essential that the diffusion equation be solved in three-dimensional space, and furthermore, one must include in the equation an appropriate "source term" describing the statistics of the creation of composition fluctuations required to trigger the nucleation events. At present, a general treatment of this problem does not appear to be tractable. Nevertheless, by using a modelistic approach, i.e., by selecting a priori certain composition variation profiles and by evaluating their associated free energies, one can draw certain conclusions relative to the stability of these isolated composition modulations or "zones", both outside and inside the spinodal. This is the object of the present investigation. THEORY We shall now describe a standard four-parameter spherically symmetric GP zone, evaluate its free energy according to the Cahn and Hilliard11 formula (Eq. [5], below), and plot the corresponding energy surfaces as a function of zone amplitude and radius as

Jan 1, 1970

By W. I. Garms, J. L. Stevens

Because of the many conflicting opinions regarding the functioning of the ball load and the characteristics of ball wear in ball-mill grinding, the following résumé of reports covering recent tests conducted at the Hayden plant of the Kennecott Copper Corporation is submitted with the view of pointing out certain salient features that should throw additional light on the subject. Mills Used Cylindrical drum mills with trunnion feed and discharge were used. The discharge trunnion was 13½ in. in diameter. Dimensions inside the lining were 6 ft. 6 in. in diameter and 9 ft. 6 in. long. The mills were Britannia-lined and nine lifter bars projected 2 in. from the lining. The mill speed was 162/3 r.p.m. Feed to the mill was 9 per cent on 10-mesh, 85 per cent on 100-mesh, 77 per cent solids. New balls measured 2 in. in diameter and the approximate weight of the ball load was 40,000 pounds. Initial Test During a test that was being conducted to determine the relative economic value of standard cast balls vs. forged steel balls in the local 'grinding operation, certain observations were made in regard to the functioning of the various ball sizes and the characteristics of ball wear, which warranted a supplementary test for the purpose of confirming such observations. For the initial test, the necessity for developing a graduated load of the new forged balls before the test could be started was realized, but the time required to obtain a graduated load and the functioning of the various ball sizes was not clear. No advantage could be seen for starting out with a full load of forged balls, as this initial load, at the least, would have to be completely ground out and replaced by daily additions of balls before the graduation could be complete and a normal static condition of ball sizes reached. For a considerable period prior to exhaustion of this initial charge there would be an unusual quantity of worn balls of a certain size, which would not be typical of a normal charge and could influence the characteristics and functioning of the entire load. Therefore, it was decided to start by daily addition of the forged balls to a mill that contained a normal operating load of cast balls. After 88 days of operation the mill was shut down for inspection. By that time the load consisted of a mass of forged balls functioning around a large core of the residual material of the former cast-ball load. This core of cast slugs, locally referred to as "the kidney," was well defined from the forged-ball load.

Jan 1, 1947

By W. I. Garms, J. L. Stevens

Because of the many conflicting opinions regarding the functioning of the ball load and the characteristics of ball wear in ball-mill grinding, the following résumé of reports covering recent tests conducted at the Hayden plant of the Kennecott Copper Corporation is submitted with the view of pointing out certain salient features that should throw additional light on the subject. Mills Used Cylindrical drum mills with trunnion feed and discharge were used. The discharge trunnion was 13½ in. in diameter. Dimensions inside the lining were 6 ft. 6 in. in diameter and 9 ft. 6 in. long. The mills were Britannia-lined and nine lifter bars projected 2 in. from the lining. The mill speed was 162/3 r.p.m. Feed to the mill was 9 per cent on 10-mesh, 85 per cent on 100-mesh, 77 per cent solids. New balls measured 2 in. in diameter and the approximate weight of the ball load was 40,000 pounds. Initial Test During a test that was being conducted to determine the relative economic value of standard cast balls vs. forged steel balls in the local 'grinding operation, certain observations were made in regard to the functioning of the various ball sizes and the characteristics of ball wear, which warranted a supplementary test for the purpose of confirming such observations. For the initial test, the necessity for developing a graduated load of the new forged balls before the test could be started was realized, but the time required to obtain a graduated load and the functioning of the various ball sizes was not clear. No advantage could be seen for starting out with a full load of forged balls, as this initial load, at the least, would have to be completely ground out and replaced by daily additions of balls before the graduation could be complete and a normal static condition of ball sizes reached. For a considerable period prior to exhaustion of this initial charge there would be an unusual quantity of worn balls of a certain size, which would not be typical of a normal charge and could influence the characteristics and functioning of the entire load. Therefore, it was decided to start by daily addition of the forged balls to a mill that contained a normal operating load of cast balls. After 88 days of operation the mill was shut down for inspection. By that time the load consisted of a mass of forged balls functioning around a large core of the residual material of the former cast-ball load. This core of cast slugs, locally referred to as "the kidney," was well defined from the forged-ball load.

Jan 1, 1947

ENROLLMENT of both undergraduate and graduate mineral engineering students rose approximately 11.8 pct over last year to a total of 12,830. Leading again in the enrollment climb was ceramic engineering which increased by about 21 pct. Approximated increases in enrollment of the other mineral engineering categories, in order, were: metallurgical 17.7 pct; petroleum 13.3 pct; geological and geophysical 3.3 pct: and mining proper, the lowest with 2.9 pct. Total ECPD school enrollment climbed to 242,405 -just below the 1947 peak, but 14.4 pct higher than 1955. Engineering enrollments have shown a general increase since 1951, and freshmen enrollments have climbed steadily since 1950.

Jan 5, 1957

By P. L. Raffo, T. E. Mitchell

Single crystals of Ta-Re alloys have been deformed in tension and compression as a function of solute concentration and temperature. The temperature dependence of the yield stress is decreased by alloying. At low temperatures there is a minimum in the yield stress (at about 2 at. pct) as a function of concentration. Three-stage hardening was not observed in the alloys. Linear hardening rates, where observed, were characteristic of stage II in pure tantalum. At low temperatures and high concentrations, work softening was often prominent at high strains. Electron microscopy revealed that dislocations are mostly of screw orientation, although heavily jogged and cusped, and often occurring in dipole pairs. The alloys become more prone to cleavage with increasing rhenium content, due mostly to an increasing yield stress rather than a change in cleavage strength. Alloying apparently decreases the Peierls stress of bcc metals at low temperatures by facilitating kink nucleation at solule atoms on screw dislocations. Higher solute concentrations further increase the yield stress. Quantitative calculations and comparisons with other bcc alloy systems are made to show that the predominant hardening mechanism is due to the interaction of dislocations with misfitting solute atoms close to their slip planes. The interaction is so localized that the core dilatation of dislocations could be important. CONSIDERABLE interest has arisen in recent years concerning the mechanical properties of unalloyed bcc metal single crystals.'-7 These and similar studies on polycrystalline materials have resulted in a considerable understanding of the macroscopic yielding characteristics8, 9 and the process of work hardening.'' This latter advance is due in a large part to the increased use of transmission electron microscopy in P I RAFFO junior Membar AlMF is Metallyureist Iewis such studies and the general observance of three stages of work hardening in the shear stress-shear strain curves. The properties of substitutional alloy single crystals of bcc metals have not been determined in as much detail as in the pure metals. Insufficient systematic studies have been made on the effect of alloying on the magnitude and temperature dependence of the yield stress or the stress-strain curves. The alloy systems which have been studied to some extent have been Ta-W,11, 12 Ta-Mo," Ta-Nb,12'14 Mo-Re,15 W-Re,16 and alloys of iron with nickel,17 platinum,17 vanadium,18 and aluminum.18 A large body of data exists on Fe-Si alloys, but these have mainly been a result of the experimental convenience of using this material in place of unalloyed iron, rather than a comprehensive study of the mechanical properties of the alloy system per se. The present authors have previously reported additional data on the properties of Ta-Re, Ta-W, and Ta-Mo alloy single crystals.1g Some of the data on Ta-Re alloys will be described later in this paper. Briefly, single crystals of Ta-Re (1.2 to 10.6 pct), Ta-W (6.2 and 10.2 pct), and Ta-Mo (2.9 and 9.0 pct) were grown by the floating zone method in vacuum. Compression tests were performed in the temperature range 77" to 623°K. Slip was found to occur in Ta-Re alloys at 77' and 298°K on the (~ll)[lil] system and slip lines were coarser and straighter than in unalloyed tantalum. No three-stage hardening was observed in any of the alloy systems and the curves were nearly parabolic. At temperatures above 175°K the yield stress* increased monotonically with in- creasing composition while at 77" and 175°K the yield stress initially passed through a minimum after which it began to increase again for concentrations greater than about 2 pct Re. Similar minima were observed in Ta-Mo alloys and to a lesser extent in Ta-W alloys. The minimum was interpreted as being a result of a

Jan 1, 1969

By Lawrence Addicks

THrough the courtesy of Dr. James Douglas I am permitted to give a summary of some of the results obtained in leaching slimes tailings in a series of experiments conducted under my direction at Douglas, Ariz., during the past year. While the test run for which the data are given deals with a particular case, much of the work is general in its application and may therefore be of interest. This work was done upon the ores of the Burro Mountain Copper CO. A description of the geology of the district will be found in the paper by R. E. Somers published in this volume, p. 604. The mineral is pyrite and chalcocite very finely disseminated throughout the gangue and a characteristic of all the ores is the large amount of alumina present. A representative analysis of the particular ore under consideration would be about as follows: Cu, per cent..................... 2.35 S, per cent...................... 3.0 Ag, ounces per ton.............. 0.05 CaO, per cent.................. 0.5 Au............................ None K2O, per cent.................... 4.0 Fe, per cent..................... 1.50 SiO², per cent.................... 70.0 Alz²O³, per cent....................13.OO The leaching of the ore direct was early dismissed from consideration for the following reasons: 1. The ore would have to be quite finely crushed to liberate the mineral for leaching; concentrating after crushing would cost but a few cents a ton; and a higher total reeovery would result from leaching tailings rather than ore. 2. Rough concentration would yield a suitable material for roasting to make sulphur dioxide or sulphuric acid in connection with the leaching scheme. 3. Such a program put the question of cost vs. recovery on a basis where flotation and discarding of tailings were directly comparable. Concentrating experiments already available indicated that the tail-

Jan 1, 1916

By W. F. Rogers, J. A. Stewart, P. J. Kalish, E. O. Bennett

Detailed descriptions are given of materials, apparatus and the experimental procedure used to study the effect of bacteria on sandstone permeability. The factors affecting permeability during injection of bacterial suspensions which have been investigated are: (I) concentration of bacteria; (2) core permeability and median pore size; (3) species of bacteria, mode of aggregation and relative size; (4) injection rate or pressure differential; (5) mean pressure; and (6) depth of penetration of bacteria. The investigation demonstrated that bacteria cannot reduce core pertneability to zero and that their effect on permeability is subject to definite limitations. Remedial or permeability restoration studies also were made. Acidization in combination with reverse flow war found to be an effective method for restoring permeability In cores partially plugged with bacteria. The relationship between the bacterial quantities in the laboratory tests and those found in field operations is discussed. The linear laboratory flow data have been translated into terms of field radial systems; these data indicate the most practical methods of maintaining injection rates in the presence of bacteria are to increase injection pressures or hydraulically fracture the formation. INTRODUCTION It has long been known that various bacteria flourish in the above-ground components of oil field water-injection systems. The presence of these bacteria has led to the suspicion that they might enter into the causes for reduction of injection well permeability, but only recently has an attempt been made to describe the effects quantitatively.1 Biocides are used in many cases without a firm knowledge as to whether the bacteria are killed, or if they are, whether the dead cells affect formation permeability. This project was undertaken as part of a study to determine the effect of bacteria, residual oil and precipitated solids such as iron sulfide or calcium carbonate on the permeability of sandstones and to learn whether any of these materials adversely affect brine injectivity in secondary recovery or disposal operations. This report deals with that portion relating to the effect of bacteria. MATERIALS CORES Three different permeability ranges of Berea sandstone cores were used in the study. The range of initial, absolute brine permeabilities kj were: high — 278 to 400 md: medium—130 to 162 md; and low—17.7 to 48.3 md. The permeability data for the cores used in the tests are included in Table 1. All cores were cut to a nominal 1 in. diameter. Following air permeability determinations, they were molded with an epoxy resin in 1.5 in. ID aluminum sleeves. The sleeves had drilled and tapped holes for intermediate pressure connections along the length of the cores. After molding, the high- and medium-permeability cores were trimmed to 4 in. in length and the low-permeability cores to 2 in. These lengths resulted in pore volumes of approximately 10.9, 10.4 and 4.4 ml, respectively, for the high-, medium- and low-permeability cores. Pressure-transmitting channels were drilled through the plastic into the core proper, using the sleeve holes as drill guides. Width and depth of channel penetration into the core proper were approximately 0.03 in. and 0.05 in., respectively. Three pressure taps were used with all cores; for the high- and medium-permeability cores the taps were spaced 1 in. apart; for the low-permeability cores the taps were spaced 0.4, 0.8 and 1.2 in. from the inlet end. Pore size distributions were calculated from restored-state capillary pressure curves for representative cores in each of the three permeability ranges. In each case the pore size range with the greatest percentage of the pore space included the very small pores up to 0.5 micron in radius. The median pore radii were in the 5.5 to 6 micron range for the high-permeability cores; in the 4.5 to 5 micron range for the medium-permeability cores; and in the 3.5 to 4 micron range for the low-permeability cores.

Jan 1, 1965

By P. S. Kotval, H. Hahell

PRECIPITATION of M23C6 carbides at grain boundaries in austenitic steels and nickel base superalloys has received considerable attention. Hatwell and Berghezan,1 in a study using carbon extraction replicas, observed that dendritic growth of the M23C6 carbide phase occurred at grain boundaries in austenitic steels. Merrick and Nicholson2 have observed that in thin foils of "Nimonic 75" alloy the precipitation of M23C6 carbide was discontinuous at grain boundaries. Lewis and Hattersley3 have suggested that the type of M23C6 precipitation observed in Ni-Cr austenites represented the early stages of discontinuous precipitation. In a more recent study, Singhal and Martin4 have concluded that grain boundary M23C6 precipitation involves the migration of an austenite grain boundary by a mechanism very similar to that proposed by Tu and Turnbull.5 Tu and Turnbull's suggestion essentially involves grain boundary migration under the driving force arising from the difference between the surface free energies of the opposite sides of the plate. Thus, Singhal and Martin's observation4 implies that the first stage of discontinuous precipitation has taken place and that the grain boundary has provided a diffusion short circuit for the sub-stitutional solute atoms (principally chromium) which assist the preferential growth of the M23C6 plate in contact with the grain boundary. However, no evidence of the characteristic cellular morphology typical of discontinuous precipitation was found in Singhal and Martin's studies. Presumably, this is due to the low volume fraction (i.e., low supersaturation of solute) of the precipitating carbide reported by Singhal and Martin.4 Recently, Raymond6 has studied precipitation of the M23C6 carbide in Incoloy alloy 825 and shown that the growth of this phase is perpendicular to grain boundaries at 1400°F and in the plane of the grain boundary at 1700°F. The former aging condition resulting in discontinuous or "cellular" precipitation. Raymond has suggested an explanation for this behavior based on the relative rates of chromium diffusion by volume and grain boundary diffusion at the two different aging temperatures. In the course of a recent investigation on precipitation behavior in several ' strengthened superalloys, precipitation of M23C6 carbide at grain boundaries was studied. Under conditions of a high degree of supersaturation, the M23C6 carbide precipitates in the discontinuous or cellular morphology in Waspalloy (Ni-18.51 Cr-2.0 Fe-3.53 Mo-1.16 Al-2.78 Ti-0.09 C). This note presents electron microscopy observations of this mode of precipitation and its effect on mechanical properties. Specimens of Waspalloy after "solution" heat treatment at 1950°F show essentially single phase matrix with a few residual particles of "primary" MC carbide. In normal commercial heat treatments, precipitation of Ni3(Al,Ti) ordered fcc r' phase occurs throughout the matrix and M23C6 precipitates as globular particles at the grain boundaries. In these commercial heat treatments the degree of supersaturation during precipitation is low. However, if specimens of Waspalloy are quenched from the solution heat treatment temperature of 1950°F and then aged at an aging temperature where the degree of supersaturation is high, discontinuous precipitation of M23C6 occurs. Figs. 1 and 2 show thin foil micrographs of Waspalloy, solution heat treated at 1950°F, water quenched, and aged at 1292° and 1598°F, respectively, for 500 Fig. 1—Thin foil of Waspalloy, solution heat treated at 1950°F for 1 hr, water quenched, and aged for 500 hr at 1292°F. Magnification 15,500 times. Fig. 2—Thin foil of Waspalloy, solution heat treated at 1950°F for 1 hr, water quenched, and aged for 114 hr at 1598° F. Magnification 13,000 times.

Jan 1, 1970

[¦Abad, Leopoldo F., College of Min., Univ. of California Berkeley, Cal. '23 ¦Abarquez, Ramon F., Met., Bureau of Science Manila, P. 1. '24 ¦Abbey, Robert Graham, Student, Case School of Applied Science Cleveland, Ohio. '21 Abbott, A. N., Mines Supt., Mazapil Copper Co., Ltd ...Concepcion del Oro, Zacatecas, Mexico. '23 Abbott, Clarence B., Gen'l Supt., Iron Mines Div., Tenn. Coal, Iron & R. R. Co., 1405 Minnesota Ave., Bessemer, Ala.' '04] [ ]

Jan 1, 1925

By T. C. M. Pillay, John Chipman

The Si-0 equilibrium in liquid iron was investigated in some detail by Gokcen and Chipman1 who reported equilibrium constants of the following reactions: In each case the thermodynamic equilibrium constant K was obtained by extrapolating K' to infinite dilution. Their results on reaction [I] were consistent with those of earlier observers, and there seems to be little doubt as to the approximate validity of the equilibrium product determined. On the other hand, the results on reactions [2] and [3] indicated unusual curvilinear relationships between the activity coefficients of silicon and of oxygen and the silicon concentration. Since a linear relation is observed in all other similar instances, it was concluded that some source of error had affected the gas-metal equilibrium relationships. Recently the authors undertook a restudy of these equilibria with the view especially to establishing the equilibrium constant of reaction [2]. Their experiments, however, were discontinued before a tbroughly satisfactory answer had been obtained and consequently have remained unpublished until the present time. Quite recently Matoba, Gunji, and Kuwana2 published the results of a very thorough study of these equilibria. It is the purpose of the present note to Compare these three sets of experimental data, a comparison which leads to Confirmation of the results of Matoba and coworkers. The experimental arrangements described by Dutilloy and Chipman were employed. A controlled mixture of Hz, H,0, and argon was led into the induction furnace over the surface of the Fe-Si melt contained in a silica crucible. On account of the slow approach to equilibrium, runs were continued for at least 8 hr and, in some cases, as much as 12 hr. Samples were taken by means of silica tubes at the start and during the final 4-hr period of each run. Out of twelve runs only seven appeared to have approached equilibrium with sufficient certainty to be reported here. The results of these experiments, all at 1600°c, are shown by the triangles in Fig. 1. Equilibrium was approached from both oxidizing and reducing conditions and the direction of approach is indicated by the shape of the triangle. Attempts to extend the study to higher silicon concentrations were unsuccessful on account of the transfer of silica from the metal bath to the upper portions of the crucible by means of a silicon-monoxide mechanism. Matoba, Gunji, and Kuwana used similar methods and approached equilibrium from both sides. Their results at three temperatures are shown by the solid lines of Fig. 1. A line corresponding to 1600 deg is interpolated from their equations and is shown by the dotted line. The results of Gokcen and Chipman at 1600 deg in the range 0.02 to 2.0 pct Si are also shown. At concentrations up to about 0.6 pct Si, these investigators approached equilibrium from both directions, and their results in this range appear to be trustworthy. Above 1 pct Si, however, all of their experiments involved oxidation only, as shown by a decrease in the silicon content of the bath. It now seems certain that they failed to reach equilibrium at these higher silicon concentrations and that the curvilinear relation shown by their results is incorrect. It is evident that their results in the lower silicon range are in good agreement with those of Matoba and coworkers. In fact, a straight line drawn through their results would parallel the dotted line and would differ from it by only 0.05 in log K. The new data also lie close to that line. It may thus be concluded that the three sets of data are in good agreement and that the equations proposed by Matoba and coworkers for reaction [2] are satisfactory . They take the limiting value of log K', at 0 pct Si as log K ,. The slope of each line gives the value

Jan 1, 1962

By Walter A. Backofen, Donald H. Avery

Intense primary and cross-slip traces were observed in easy glide on Cu: 6 pct-A1 single crystals deformed in tension. A mechanism of cooperative source operation is developed which recognizes that both the applied stress and that resolved from dislocation arrays contribute to the stress on a source. By considering the stress from arrays, the activation of secondary systems in easy glide and the difference in appearance of slip markings on pure and solid-solution crystals are explained. Furthermore the cross-slip system is predicted to be second favored during easy glide for a large range of orientations. FROM many studies of easy glide in fcc metal crystals, a pattern of observations has developed which still requires full explanation. In pure copper, aluminum, and silver, the easy-glide, slip traces are fine and uniform with steps 50 to 100A on the primary* system.1-4 Yet it has not been at all clear why slip in the pure materials should occur in this way. On the contrary, one might expect, with simple slip and a low hardening rate, that the weakest sources on the primary system would operate extensively to produce strong slip traces. In a brass, however, intense slip steps up to 0.5 are found on both primary and cross-slip system4,6-9 seeger10 has pointed out that in a material of low stacking-fault energy such as a brass, extensive easy-glide cross-slip could not be thermally activated, but rather must originate on the cross-slip plane. In further explanation, the wilsdorfs4 and seeger10 noted that only the cross-slip system would not harden differently than the primary, whatever the latent hardening tendencies of other systems; therefore, in brass, which exhibits high latent hardening, the cross-slip is the only secondary system which could be expected to operate extensively, once it became active. The explanation of how the cross-slip system, on which the applied stress is low, becomes activated has been related, in a nonspecific way, to pileups by Hirsch11 and Honeycombe.l2 In the work to be described, deformation traces on solid-solution Cu: 6 pct A1 single crvstals were studied with conventional light microscopy and a mechanism proposed to explain both the observed activation of secondary systems in easy glide and the difference in appearance of slip markings on pure and solid-solution crystals. EXPERIMENTAL In preparing the Cu-A1 single crystals, rectangular bars approximately 0.4 in. by 0.4 in. by 6 in. were first machined from ingots made by vacuum melting copper of 99.999 pct and aluminum of 99.99 pct purity. They were then packed in powdered graphite and the crystals grown in a modified Bridgman apparatus at a rate of 5 mm per hr under an atmosphere of purified nitrogen. Crystal perfection as indicated by Laue back-reflection spots was good except for the last inch to freeze, which was discarded. Orientations so determined are shown in Fig. 1. Tensile specimens with a reduced gage section were obtained by masking the ends with electrical tape and chemically polishing in a solution of 20 pct HNO3, 24 pct HAc, 52 pct H3PO4, 2 pct Hcl, and 2 pct H20 at room temperature.13 Finally, the specimens were electropolished in a 30 pct ortho-phosphoric acid bath at 12 v. Tensile deformation was performed in an Instron testing machine at a strain rate of approximately 1 pct per min. During easy glide, extensive cross-slip was observed with all crystals, in spite of the low Schmid factor on this system, and in no case was any other secondary trace encountered. A certain sequence of slip-line development was associated with the extension. At yielding, intense primary traces passing completely through the crystal developed at some point on the gage section, generally near the grips; weak cross-slip traces also appeared, extending from the primary traces into the adjacent undeformed crystal, Fig. 2. Further extension led to primary traces adjacent to the first-formed and connecting with those of the cross-

Jan 1, 1963

By Rees D. Rawlings, C. W. A. Newey

The aging characteristics of an Fe-11 at. pct Mo alloy have been studied by means of light metallography together with density, Young&apos;s modulus, and hardness measurements. The results were consistent with the precipitation of a single intermetallic compound during aging; overaging was slow relative to that in other iron-based binary alloys. The solution treatment temperature had a small effect on the rate of hardening whereas deformation prior to aging had a marked effect on both the rate of hardening and the peak hardness. The density data indicate that the compound precipitated is Fe3MO2 and not the Laves phase Fe2Mo. Analysis of the modulus and density results gave values for the time exponent for precipitate growth of approximately 1.0 and 1.5 for the alloy aged with and without prior deformation, respectively. DETAILED studies of precipitation hardening in bcc matrices have been confined largely to the effects of carbides and nitrides. In view of this and the growing technological interest in intermetallic compound strengthening, e.g., in maraging steels, a study of precipitation in iron-based alloys with a low interstitial content has been undertaken. This paper is concerned with the aging behavior of an Fe-11 at. pct Mo alloy; the mechanical behavior of the alloy will be reported later. The early work of sykes on Fe-Mo alloys showed that precipitation of the intermetallic compound was accompanied by an increase in hardness and a decrease in volume of the material. More recent surveys of the strengthening associated with precipitation have been made3-5 and, in particular, Elsen and wassermann4 showed that deformation prior to aging increased the rate of hardening. These latter workers also followed the precipitation process by means of dilatometry, electrical resistivity, and lattice parameter measurements. Their results confirmed that there is a decrease in volume on aging. Except for the work of Hornbogen on an Fe-20 at. pct Mo alloy, neither clustering nor the precipitation of a nonequilibrium phase has been observed in Fe-Mo alloys. Studies of alloys of lower molybdenum content475 indicate that the equilibrium intermetallic compound is precipitated during aging. However, there is some doubt concerning the nature of the equilibrium precipitate phase. According to the phase diagram constructed by Hansen,8 the phase should be precipitated. This phase has a rhombohedra1 crystal structure which is characterized by the formula Fe706,&apos; although the composition of the molybdenum-rich boundary corresponds approximately to Fe3Mo2. The version of the diagram proposed by Sinha, Buckley, and Hume-Rother indicates that the A phase, a Laves phase Fe2Mo, should be precipitated. Their observation of a Laves phase supports the earlier findings of Bechtoldt and Vacher,13 although, in a recent study of the system by means of diffusion couples, Rawlings and Newey did not detect the phase. The work presented here describes the effect of solution-treatment temperature, aging temperature, and prior deformation on the aging characteristics of the alloy as revealed by light metallography together with hardness, density, and Young&apos;s modulus measurements. In addition the density data are used in an attempt to determine the compound precipitated during aging. EXPERIMENTAL PROCEDURE A 29-kg ingot of the alloy was cast at R.A.R.D.E., Fort Halstead, from deoxidized, Japanese electrolytic iron and sintered molybdenum. The ingot was homogenized for 6 hr at 1473°K and then worked, with intermediate anneals, into 6- and 16-mm-diam rods and 6-mm plate. Chemical analysis of the alloy gave, wt pct: Mo, 17.5 (11 at. pct); C, 0.003; Si, 0.002; S, 0.005; P, <0.002; and02, 0.0098. Solution treatments were carried out under a dynamic argon atmosphere in a vertical, "crusilite" element, furnace which had a facility for rapid quenching into iced water. Except for the study of the effect of solution treatment temperature, all specimens were solution-treated at 1573" * 2°K for 1 hr. Salt baths were used for the aging treatments. Specimens for hardness, density, and Young&apos;s modulus measurements were produced, after heat treatment, from the stock rod or bar using a precision silicon carbide slitting wheel. As described later, the quenching treatment produced local plastic strain in the stock material; consequently, care was taken to ensure that the specimens were not prepared from these regions. Those specimens used in the studies of the effects of prior deformation on the aging behavior were strained in compression in a Denison universal testing machine. Specimens for light metallographic observations were mechanically polished on successively finer grades of diamond paste down to and then etched in either alcoholic ferric chloride or in a 2 pct nital solution. Vickers diamond pyramid hardness data were obtained using a 30-kg load. At least five impressions were averaged for each determination. Density measurements were made using a displacement technique in which each specimen was weighed in air and in dibromoethane at 296°K. The specimens were cylindrical and weighed 3 to 4 g; all weighings were made on a balance reading to 1 x 10"5 g. For each specimen the mean value of five weighings was used to calculate the density. The density of the dibromoethane was determined using the displacement procedure and a standard nickel specimen. The error in an absolute density value was estimated to be HI.01 pct. To obtain the density as a function of aging time a single specimen was used and the density meas-

Jan 1, 1969

By Merlon C. Flemings, Theodoulos Z. Kattamis

Examination was made of the distribution of tnanganese and nickel in colutrrnar dendrites of a cast low-alloy steel; more limited work was corzducted on chromium. Corresponding "segregrction ratios" were calculnted and shown to be relntivelv insensitive to cooling rate (&apos;&apos;segregation ratio" is defined (Is the ratio of maximum to minimum concentrations within a volume whose dimensions are the order of the dendrite-arm spacing). Isoconcentratiorl curves were determined by the electron micropvobe and by rt7etallografihic studies on specimens subjected to isothermal-transformation treatments. From construction of isoconcentration curves, morphology of columnar dendrites is descvibed as intermediate between Perfect rodlike and sheetlike morphologies. The study is extended to equiaxed dendrites and it is shown that the strcture of these dendrites is sittlilar in many respects to that of columnar dendrites. On the basis of tlze sheetlike morphology of dendrites, a simple model is pvoposed for calculation of honzogenization kinetics. Results of trzatllevlatical analysis brcsed on this utzodel are given. This analysis relates residual segregation to time at homogenization temperature; it is in agreement with experiment. Calculations are given which show that even for relatively rapidly cooled material (of 1-ine dendrite-artn spacing) treatmets at 1200°C or above are necessary to achieve slgxificant Izomogenization of elenlents other than carbon itz reasonable time (e.g., rnangclnese, nickel). Conlplete homogenization of carbon is obtnined at much lowev tenlperatures (below 870°C). IN dendritic solidification of castings and ingots, solute redistribution during freezing results in mi-crosegregation of most alloy elements. The micro-segregation is such that minimum solute concentrations occur at the center of dendrite arms and maximum concentrations occur between dendrite arms. Residual segregation after subsequent therma1 processing (homogenization) depends on maximum and minimum initial concentration, on the detailed geometry of the isoconcentration surfaces within interdendritic regions, on the diffusion coefficient of the solute, and on time of thermal processing. The objective of this work was to determine, for a low-alloy steel, maximum and minimum concentrations, and the geometry of isoconcentration surfaces, primarily in order to permit calculation of homogenization kinetics. Most of the work reported was conducted on Samples from a unidirectionally solidified, fully columnar ingot. This type of ingot is made by extracting heat during solidification from one face; techniques for accomplishing this have been discussed.&apos; Samples were taken at several locations, up to 5.75 in. from the mold chill face; the bulk of the work was performed on samples at 5.75 in. Alloy cast was, nominally, 0.4 pct C, 1.8 pct Ni, 0.8 pct Cr, 0.7 pct Mn, 0.25 pct Mo, 0.3 pct Si, and the balance iron. Brief study was also made on samples from an ingot which solidified with equiaxed grain structure. SAMPLE PREPARATION AND ANALYSIS Samples for electron-microprobe analysis were incorporated in mounts that included pieces of electrolytic nickel, chromium, and manganese, in order to normalize the intensities of these solutes in the specimens; also, a piece of electrolytic iron was included to measure the background. All specimens were polished in the usual metallographic manner. After the microprobe traces were made, the path was revealed by etching the specimens with picral. All microprobe analyses were made by point counting, integrating for 30 sec. The distance between points was fixed from 2 to 10 p, according to the precision desired in each case, the fineness of the structure, and the concentration gradient existing in a given area. (The distance was chosen 2 to 5 p near the maximum-concentration regions and 5 to 10 p near the minimum concentration.) The "take-off" angle for the A.R.L.-Model No. 21000 microprobe employed was 52.5 deg. Samples for metallographic analysis of isoconcentration curves were prepared by austenitizing at 1540°F for 20 min, quenching to the nose of the TTT curves (1200°F), heat treating isothermally at this temperature for a given time 0, and then quenching to room temperature. Due to concentration gradients existing in a dendritic structure, no transformation will take place for a given time 0 of isothermal heat treatment in the regions where the a.lloy concentration is higher than a given limit. Thus, the dendrite appears limited by an isoconcentration curve and can be made to appear to grow by varying the time of isothermal heat treatment.

Jan 1, 1965

By B. S. Tani, R. V. Schablaske, M. G. Chasanov

In the Ti-Cd system two intermediate phases, TiCd and Ti Cd, have been found and characterized by X-ray diffraction powder techniques. An earlier reference&apos; had reported the existence of the compound Tisd. No structural details, however, were given nor was there any indication of the possible existence of other binary compounds. Studies of the solubility of titanium in liquid cadmium2 led to the discovery of both TiCd and Tisd. The solid phase in equilibrium with saturated solutions of titanium in liquid cadmium at temperatures below 620°C is TiCd, whereas TizCd is the equilibrium solid phase above 620°C. Both thermal analysis and X-ray studies show that a peritectic reaction between the y phase (~isd) and cadmium to form the 6 phase (Ti Cd) occurs at 620°C. X-ray diffraction powder photographs of material isolated from the ingots used in the solubility measurements as well as material prepared by a direct heat of the appropriate stoichiometric amounts of titanium and cadmium can be indexed on the basis of a tetragonal unit cell with a = 2.904 ± 0.002A, co = 8.954 * 0.004A, c/a = 3.083. No variation of lattice parameters indicative of a range of composition is evident. With four atoms in the unit cell the calculated density of the intermetallic is 7.05 g per cm3; the observed value is 7.07 g per cm3. The TiCd lattice is primitive as indicated by the fact that there are no systematic absences among hkl reflections. The absence of all hko reflections for which h + k = 2n + 1 is also evident. This systematic absence indicates the following two space groups, C\h — P4/n and D&~4/nmm; both groups, however, have the same two- and four-fold positions. Stoichiometry, symmetry and space group indicate two likely structure types. They are the PbO-litharge3 (B10) type and the Ti CU (B11) type. Spatial considerations favor the B11 structure with atoms placed in the following positions: 2Ti (c) 0, 1/2, Z; l/2, 0, Z 2Cd(c) 0, 1/2, Z; 1/2, 0, Z The TiCd structure may be summarily described as a layered structure in which double cadmium layers alternate with double titanium layers along the c-axis. The best agreement between calculated and observed intensities is obtained for the values ZTi = 0.608 and ZCd = 0.130. Calculated and observed powder intensities as well as other pertinent powder data are recorded in Table I. Interatomic distances for the proposed structure are recorded in Table II and are to be compared with the distances of closest approach for titanium and cad-

Jan 1, 1962

By C.P. Clingerman

The recent iastallation of a combination dust catcher, gas washer and precipitator at Carrie blast furnaces of the Homestead Steel Works has given very satisfactory results. The following description of the gas-cleaning installation is based on actual operating experience. When Carrie blast furnace No. 3 was rebuilt the decision was made to fine-clean all the gas produced by the furnace, because the management wanted fine-cleaned gas for fuel in the stoves and boilers. In order to keep the installation cost as low as possible, the gas-cleaning system was streamlined. All by-pass lines and goggle valves for bypass lines were eliminated from the system. A radical departure from the use of 8-in. tubes in the Cottrell-type precipitators was made by using 12-in. diameter tubes in a single compartment, the single compartment being divided into two units by a single partition wall in the top header. The Furnace Proper A few of the characteristic points and dimensions of the furnace proper are: Hearth diameter.............. 26 ft. o in. Bosh diameter............... 29 ft. 1 3/4 in. Stock-line diameter........... 20 ft. o in. Large-bell diameter........... 14 ft. 8 in. Small-bell diameter........... 6 ft. 6 in. Height of furnace from center of iron notch to bottom of large bell, closed............ 94 ft. 4 in. Height of furnace from center of iron notch to main platform ...................... 105 ft. o in. The furnace top is equipped with a MC-Kee revolving distributor, the operation of which is electrically interlocked with the skips, bell hoists, and coke-weighing and charging apparatus through a Freyn automatic charging control. The gas leaves the furnace first through four offtakes, 5 ft. 9 in. in diameter, then through uptakes that, are approximately 85 ft. high, which feed into a single down-comer that is 9 ft. in diameter. Dust Catcher The primary dust catcher installed (Fig. I) may be described as a single-cone type. The inlet pipe at the top of the dust catchei is 9 ft. in diameter; it is flared to a conical shape as it extends down inside the dust-catcher shell, which is 35 ft. in diameter, 37 ft. high on the straight side, and has a conical top and bottom. The slope of the bottom is so0 with the horizontal. The cone-shaped pipe inside the dust-catcher shell is 42 ft. high and is 19 ft. 7 in. in diameter at its bottom lip where it releases the gas inside the dust catcher. The ratio of the area of the inside cone at its bottom lip to the

Jan 1, 1943

By C. P. Clingerman

The recent iastallation of a combination dust catcher, gas washer and precipitator at Carrie blast furnaces of the Homestead Steel Works has given very satisfactory results. The following description of the gas-cleaning installation is based on actual operating experience. When Carrie blast furnace No. 3 was rebuilt the decision was made to fine-clean all the gas produced by the furnace, because the management wanted fine-cleaned gas for fuel in the stoves and boilers. In order to keep the installation cost as low as possible, the gas-cleaning system was streamlined. All by-pass lines and goggle valves for bypass lines were eliminated from the system. A radical departure from the use of 8-in. tubes in the Cottrell-type precipitators was made by using 12-in. diameter tubes in a single compartment, the single compartment being divided into two units by a single partition wall in the top header. The Furnace Proper A few of the characteristic points and dimensions of the furnace proper are: Hearth diameter.............. 26 ft. o in. Bosh diameter............... 29 ft. 1 3/4 in. Stock-line diameter........... 20 ft. o in. Large-bell diameter........... 14 ft. 8 in. Small-bell diameter........... 6 ft. 6 in. Height of furnace from center of iron notch to bottom of large bell, closed............ 94 ft. 4 in. Height of furnace from center of iron notch to main platform ...................... 105 ft. o in. The furnace top is equipped with a MC-Kee revolving distributor, the operation of which is electrically interlocked with the skips, bell hoists, and coke-weighing and charging apparatus through a Freyn automatic charging control. The gas leaves the furnace first through four offtakes, 5 ft. 9 in. in diameter, then through uptakes that, are approximately 85 ft. high, which feed into a single down-comer that is 9 ft. in diameter. Dust Catcher The primary dust catcher installed (Fig. I) may be described as a single-cone type. The inlet pipe at the top of the dust catchei is 9 ft. in diameter; it is flared to a conical shape as it extends down inside the dust-catcher shell, which is 35 ft. in diameter, 37 ft. high on the straight side, and has a conical top and bottom. The slope of the bottom is so0 with the horizontal. The cone-shaped pipe inside the dust-catcher shell is 42 ft. high and is 19 ft. 7 in. in diameter at its bottom lip where it releases the gas inside the dust catcher. The ratio of the area of the inside cone at its bottom lip to the

Jan 1, 1943

By G. J. Wolga, W. W. Tyler, A. C. Wilson

THE physical properties of uranium have been reviewed by Katz and Rabinowitch.1 Their review includes thermal conductivity data for ternperatures above 375°K. Recently, Mendelssohn and Rosenberg&apos; have published data on the thermal conductivity of uranium from 2" to 20°K. Our measuremerits indicate the temperature dependence of the thermal conductivity in the temperature interval from 20" to 300°K. Electrical resistivity and thermoelectric power were measured on the same sample. The material studied was normal uranium which had been heated at 700°C in a lead bath for 10 min and then quenched in a water bath held at 50°C. From this material a rod M in. in diameter and 2 1/2 in. long was machined. Two 0.040 in. holes were drilled into the rod 1 3/4 in. apart. Copper-constantan thermocouples for temperature and potential measurements were soldered to copper pins which were pressed tightly into these holes. Details of the equipment and experimental techniques used in making the measurements have been described elsewhere." Fig. 1 shows micrographs of a section of the sample studied. Fig. la was taken with unpolarized light and shows impurity inclusions, probably uranium carbide. Fig. lb, showing the same field, was taken with polarized light and gives some indication of the grain size and twinning within the grains. Experimental Results Thermal conductivity and electrical resistivity data are shown in Fig. 2. Table I shows values of

Jan 1, 1954