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The Second Pan-American Scientific Congress will be held under the auspices of the United States Government in Washington, D. C., Dec. 27, 1915, to Jan. 8, 1916. The organization officers are John Barrett, LL. D., Director General of the Pan-American Union, Secretary General; Glen Levin Swiggett, Ph. D., Assistant Secretary General; the headquarters of the Congress are the Pan-American Union, Washington, D. C. The program of the Congress is divided into nine main Sections, which are given below with the name of the Chairman of each Section: 1. Anthropology, William H. Holmes, B. S., Smithsonian Institution, Washington. 2. Astronomy, Meteorology, and Seismology, Robert S. Woodward, Ph. D., Carnegie Institution, Washington, D. C. 3. Conservation of National Resources, Agriculture, Irrigation and Forestry, George M. Rommel, B. S., Bureau of Animal Industry, Department of Agriculture, Washington, D. C. 4. Education, P. P. Claxton, LL. D., Bureau of Education, Washington, D. C.

Jan 12, 1915

By R. C. Hall

DEVELOPED to grow single crystals of alloys of high hardness and high melting points is a simple but effective apparatus described in this note. Growth from the melt, that is, by the Bridgman technique, hay be applied to metals or alloys which are physically hard as long as no phase transformation occurs on cooling to room temperature. The present apparatus was employed to grow single crystals of the ferromagnetic AI-Fe alloys above 1 wt pct Al and the Si-Fe alloys above 3 wt pct Si. Single Crystal Growth In a simple form, the method for growth of single crystals from the melt requires a molten metal charge in a pointed crucible which is slowly low-ered through a heated zone into a colder zone. Solidification starts at the bottom point and continues up the charge as the crucible is lowered through the heated zone. If a single crystal nucleates at the bottom, one crystal may grow throughout the charge under ideal conditions of slow growth.4,5 The presently developed method of growth was designed so that the chances that more than one crystal would grow were small. The single crystals were growth by the apparatus illustrated in Fig. 1. The charge was in the form

Jan 1, 1958

By H. J. Gluiskoter

The chlorine content of the coals in the Illinois Basin ranges from 0.00% to more than 0.60%. The chlorine content of the Herrin (No. 6) Coal has been mapped on a regional scale and, in general, increases with the depth of the coal. The depth-chlorine correlation exists because the coal is in apparent equilibrium with the composition of the ground water associated with it, and the salinity of the ground water generally increases with depth. At least part of the chlorine can be easily removed from the coal in the laboratory. In a natural weathering experiment, chlorine values decreased markedly during an 8-week period. Results to date indicate that none of the coals studied has a sufficiently high chlorine content to make it unusable in high-temperature steam boilers, although special steps may be necessary in the preparation or utilization of some of the highest chlorine coals. Investigations into the occurrence and distribution of chlorine in Illinois coals have been in progress at the Illinois State Geological Survey for over 35 years. Since 1948, chlorine analyses of face channel samples and of drill core samples of coal have been made routinely. The increased interest in chlorine and alkalies in coal in the U.S. followed that in Europe, where power plants during World War II were called upon to produce at higher levels than previously and with less down time for maintenance. Higher steam temperatures were reached, resulting in increases in the amount of fouling of external heating surfaces and in corrosion of boiler tubes when high chlorine coals were used. Early studies of the problem showed that coals with high chlorine content were more likely than those low in chlorine to cause difficulties in installations fired with powdered fuel. Crossleyl reported that the first rule of thumb developed for British coals was that coals considered to be high in chlorine (more than 0.30%) caused the most trouble, those intermediate in chlorine content (0.15% to 0.30%) were less likely to cause difficulties and those low in chlorine (less than 0.15%) generally were not associated with alkali bonded deposits and corrosion. However, this relatively simple picture was not adequate to characterize the difficulties that could be expected during the utilization of a large number of coals and Crossley1 developed another scheme for assessing the chances of superheater corrosion. This scheme took into consideration the observation that coals high in sulfur as well as chlorine are more likely to cause corrosion and fouling than coals low in sulfur and high in chlorine. Crossley also considered the ash content. When two coals had the same chlorine and sulfur contents, the one with the greater amount of ash would be the less likely to cause difficulties. Knowing only the amount of chlorine in a coal obviously will not give all the answers. Indeed, the significance of the chlorine content has been much discussed and it has been suggested that perhaps the total alkalies are a better indicator of possible troubles. The observation that the deposits that form

Jan 1, 1968

By P. W. Barton, A. A. Johnson, E. J. Hughes

THE only systematic work on the effect of carbon on the recovery and recrystallization kinetics of iron so far reported in the literature is that of Venturello et al.1 These workers found that doping high-purity iron so that it contained up to 86 ppm C caused a marked retardation of recovery but had little or no effect on the recrystallization kinetics. Such evidence for an effect as was obtained was inconclusive. In the course of a study of electron-beam zone-refined iron the authors have recently examined the effect of added carbon on the recrystallization kinetics of this material. The amount of carbon added was about 50 pct more than was used by Venturello et 01. and definite evidence was obtained that carbon at this level retards recrystallization. The starting material was taken from a batch of 0.2-in.-diameter Johnson-Matthey spectroscopically pure iron rods which had been further purified by being given three passes at 4 in. hr-1 in a standard MRC electron-beam zone-refining unit. The purity of this material. which was used in two other investigations of the properties of high-purity iron,2,3 was established by an extensive series of analyses. Four laboratories, the National Research Corp., Newton, Mass., the Naval Research Laboratory, Washington, D.C.. the Battelle Memorial Institute, Columbus, Ohio, and the National Physical Laboratory. Teddington. Middlesex, England. carried out analyses for carbon. oxygen. and nitrogen. and in addition a complete mass-spectrograph analysis was carried out at Battelle. In all, twelve analyses were carried out for carbon, seventeen for oxygen and twelve for nitrogen. The amounts of these elements found to be present were 10 * 7, 8 i 5, and 0.9 i 0.1 ppm, respectively. The limits given are rms deviations. Two results, one of 46 ppm of oxygen and another of 31 ppm of nitrogen, were rejected as anomalous. The mass-spectrograph analysis revealed the major impurity to be 25 ppm of tungsten. All of the other elements detected were present in amounts less than 0.5 ppm. Some of the rods were doped with carbon by being immersed in a suspension of carbon in oil, heated in a vacuum at 400°C, and then zone-leveled to make the distribution of carbon uniform. Carbon analyses carried out on three of the doped rods gave a mean value of 130 ± 45 ppm. Some of the doped and undoped rods were deformed 58 pct by swaging and cut into specimens 1/2 in. in length. Isothermal recrystallization experiments were then carried out on them at 575", 600°, 615", 630°, and 650°C, the volume fraction of each specimen recrystallized being measured by a point-counting method described by Hilliard and Cahn.4 The results for the two types of specimens are shown separately in Figs. 1 and 2. In Fig. 3 the pairs of recrystallization curves for each temper-

Jan 1, 1965

By J. K. Stanley

Knowledge of the diffusivity of carbon in the low temperature form of iron (alpha iron existing below 910°C) is at the moment of considerable interest in the study of the decomposition of austenite and martensite, the elastic after-effect,123 the magnetic after-effect4 and the decarburization of steel below 910°C. Information on the solubility of carbon in iron, and to a lesser extent its diffusion, is also important in consideration of such phenomena as blue-brittleness, temper-brittleness, "magnetic" aging, quench-aging, strain-aging, and possibly the yield point. In order to obtain more information on these subjects more fundamental knowledge is necessary. It is the purpose of this work to present data on the diffusion and solubility of carbon in the alpha iron. The high temperature form of iron (gamma; face-centered cubic) existing above 910°C is capable of dissolving relatively large amounts of carbon, up to 1.7 pet at 1130°C, while the low temperature form (alpha, body-centered cubic) existing below 910° dissolves only a limited maximum amount of less than 0.02 pet carbon at 725°C, according to data obtained here. Since the solubility of carbon in the face-centered or gamma iron is large, relatively speaking, no great analytical difficulties have been encountered in the determination of the solubility lines5 or of the diffusion of carbon.0 The limited solubility of carbon in alpha iron offers difficulties because experimental procedures and analytical methods for low carbon contents below say 0.01 pet have to be more refined than techniques used for work with gamma iron. Because of the difficulties of applying conventional methods to the determination of the diffusion of carbon in alpha iron, virtually no work has been done on this subject. However, by proper refinement of the analytical method for small amounts of carbon, the determination of the diffusion coefficient can be made readily using modified procedures. The solubility of carbon in alpha iron has been determined over a temperature range by various investigators, but the agreement among them is poor. The present investigation establishes the limits quite accurately. Information of this kind is useful in establishing the correctness of equilibrium diagrams but, more significantly, such information on maximum solubilities, especially when extended to alloyed ferrites, should be extremely important in the study of aging and related phenomena. Literature The literature existing on the diffusion, in particular, and on the solubility of carbon in alpha iron is not extensive. The data which exist are not of a high order of accuracy, much of them being in the realm of conjecture. THE DIFFUSION OF CARBON IN ALPHA IRON Whiteley7 made the qualitative ob- servation, using metallographic techniques, that the rate of diffusion of carbon at the A1 (725°C) point was very rapid and that its diffusion was still rapid at 550°C. Snoek,4 studying the magnetic aftereffect in high purity iron, arrived at the conclusion that the after-effect could be explained by the presence of small amounts of carbon diffusing under the influence of magnetostrictive strain (lattice distortion due to magnetic interaction). In later work, Snoek8 made an estimate of the ratio of carbon diffusion in alpha to its diffusion in gamma iron, and concluded that for a temperature of 910°C the ratio of Da/D? was 2600. Polder,9 basing his calculations of D on relaxation phenomena in the elastic after-effect, estimated that Da is about 1/3 of D? at 910°C (1183°K) and is about 1/12 of Dy at 727°C (1000°K). Polder's equation for the diffusion of carbon in alpha iron was calculated to be 18000 D = 5.2 X 10-4 e-RT cm2 per sec Ham10 obtained data for the diffusion and solid solubility of carbon in alpha iron at two temperatures by using one technique similar to that employed in this study. He found a D of 8.0 X 10-7 cm2 per sec at 702°C and of 2.7 X 10-7 at 648°C. THE SOLUBILITY OF CARBON IN ALPHA IRON Although pearlite is absent in steels containing 0.06 pet,11 0.05 pet,12 or 0.045 pet C,13 it appears that the carbon in these steels cannot be in solution in ferrite. The solubility of carbon at the A1 (725°C) point was first determined by Scott14 on the basis of cooling curves, and was found to be between 0.03 and 0.04 pet C. Tamura15 by interpolating between the solubility of carbon in delta iron at 1400°C and in alpha at room temperature (assuming zero solubility) ar-

Jan 1, 1950

By E. T. Turkdogan, P. Grieveson, J. F. Beisler

Experimental results are given for the rate of reduction of silica from silicate melts by paphite-saturated iron in the presence of carbon monoxide. It is shown that, when gas bubbles are present at the slag-metal interface, the interfacial chemical reaction is the rate-controlling process in the transfer of silicon from slag to metal. From the silicon-concentration profiles in the metal sample, the diffusivity of silicon in paphite-saturated iron is found to be (5.4 * 0.4) x 10 sq cm per sec at 1600°C. Some consideration is given to the transport of oxygen from the slug-metal interface to the walls of the gvaphite metal container as becoming the rate-controlling process in the absence of gas bubbles at the slag-metal interface. ATTEMPTS were made by Fulton and chipman1 to investigate the kinetics of reduction of silica from calcium alumino-silicate melts by graphite-saturated iron in an atmosphere of carbon monoxide. In these experiments with 400 to 500 g of metal and slag, both phases were stirred in such a manner that the interface was essentially undisturbed. Initially, the graphite-saturated iron contained about 15 pct Si and, after about 8 or 10 hr of reaction time at 1600°C, the silicon content of the metal in- creased by about 0.2 pct. In a written discussion on this paper of Fulton and Chipman, schuhmann2 pointed out the possibility that this observed slowness of the reduction of silica could be due to the transport of oxygen across the liquid metal boundary layer at the slag-metal interface. Although this explanation of Schuhmann is quite feasible for the experimental data of Fulton and Chipman on silica reduction, such a reasoning should not be extended to other rate data on slag-metal reactions unless sufficient evidence is available satisfying the boundary conditions for such a transport process. The hydrodynamics of stirred liquids are very complex and even for a simple method of stirring there is no exact mathematical solution which will predict the mass transfer coefficient accurately. The best available solution of this problem is that given by Lewis' and later modified by mayers~ for a two-liquid system where liquids are stirred by counter-rotating stirrer blades without disturbing the interface. In such a system the mass transfer coefficient is estimated from an empirical relationship using the data on viscosity and density of the two liquids, rate of revolution, the length of stirrer blades, and the diffusivity of the element which is transferred from one phase to the other. It was found in these investigations' that the estimated and observed mass transfer coefficients, in systems containing two immiscible aqueous solutions, agreed within *40 pct. Although this is not considered to be an unreasonable error for the study of industrial processes, uncertainties of this magnitude cannot be tolerated in any theoretical study of reaction kinetics. In view of the complexity of the

Jan 1, 1963

By R. W. Snyder, W. H. Guilinger, B. S. Gottfried

Two numerical methods are presented JOT solving the equations Jor one-dimensional, multiphase /low in porous media. The case oF variable physical properties is included in the Formulation, although gravity and capillarity are ignored. Both methods are analyzed mathematically, resulting in upper and lower bounds for the ratio of time step to mesh spacing. The methods are applied to two- and three-phase waterflooding problems in laboratory-size cores, and resulting saturation and pressure distributions and production histories are presented graphically. Results oJ the tuo-phase flow problem are in agreement with the predictions of the Buckley-Leuerett theory. Several three-phase flow problems are presented which consider variations in the water injection rate and changes in the initial oil-and ujater-saturation distributions. The results are different physically from the two- phase case; however, it is shown that the Buckley-Lez~erett theory can accurately predict fluid interlace velocities and displacing-fluid frontal snturations for three-phase flow, providing the correct assumptions are made. The above solutions are used as a basis JOT et~aluuting the numerical methods with respect to machine time requirements and allowable time step for a fixed mesh spacing. INTRODUCTION Considerable progress has been made in recent years in obtaining numerical solutions of the equations for two-phase flow in porous media. Douglas, Blair and Wagner2and McEwenll present different methods for solving the one-dimensional case for incompressible fluids with capillarity (the former using finite differences, the latter with an approach based upon characteristics). Fayers and Sheldon4 and Hovanesian and Fayers8 have extended these studies to include the effects of gravity. West, Garvin and Sheldon, l4 in a pioneer paper, treat linear and radial systems with both capillarity and gravity and they also include the effects of compressibility. Douglas, Peaceman and Rachford3 consider two-dimensional, two-phase, in compressible flow with gravity and capillarity and Blair and Peaceman1 have extended this method to allow for compressible fluids. No one, however, has examined the case of three-phase flow, even for the relatively simple case of one-dimensional flow of incompressible fluids in the absence of gravity and capillarity. In obtaining a numerical technique for simulating forward in situ combustion laboratory experiments, Gottfried5 has developed a method for solving the one-dimensional, compressible flow equations with any number of flowing phases. Gravity and capillarity are not included in the formulation. The method has been used successfully, however, for two- and three-phase problems in a variable-temperature field with sources and sinks. This paper examines the algorithm of Gottfried more critically. Two numerical methods are presented for solving the one-dimensional, multi-phase flow equations with variable physical properties. Both methods are analyzed mathematically, and are used to simulate two- and three-phase waterflooding problems. The numerical solutions are then taken as a basis for comparing the utility of the methods.

Jan 1, 1967

By R. O. Williams

It is shown that Ni3Al precipitates homogeneously from nickel-rich alwminum alloys as plates on the (100) planes. Prior to actual precipitation a process occurs which is believed to be one of increasing short-range order. After precipitating the Ni3Al plates enlarge through competitive growth. Discontinuous precipitation can occur simultaneously with the above processes. Recent ideas of the origin of precipitation strengthening appear adequate to explain the hardness changes. REMARKABLY little appears to be known about the precipitation process in Ni-Al alloys in spite of their technical importance. This investigation originated to supply additional information about precipitation in general, this system in particular. Information on the structures and kinetics have been obtained through the use of hardness, X-rays, microscopy, calorimetry, and resistivity on high-purity alloys. PROCEDURES Six alloys, Table I, were prepared by melting carbonyl nickel and high-purity aluminum in alumina crucibles in vacuum and casting into 1-in. graphite molds. All rods were homogenized at least once at 1300°C for 24 hr prior to swaging and this was repeated on the first three alloys after 75 pct reduction. Alloy 4 could be reduced only 10 pct at 1000°C (probably in two-phase field) prior to fracture but 1/4-in. samples quenched from 1100°C were readily reduced cold. Alloy 5 was reduced 15 pct cold but failed on the next pass while alloy 6 of essentially the same aluminum content failed inter-granularly without apparent flow up to 1000°C. The alloys were heated in hydrogen at the elevated temperatures and formed thin, coherent aluminum oxide coatings which provided excellent oxidation resistance at lower temperatures. However, freshly prepared surfaces showed considerably less resistance at 500"to 700°C in air and apparently resulted in internal oxidation. As a consequence, low-temperature agings were carried out in evacuated tubes. RESULTS The isothermal hardening behavior of these alloys at 500"and 565C is given in Figs. 1 and 2. These results were obtained from samples cold worked 75 pct, recrystallized at 1000°C (1100°C for the 7.8 pct Al) and quenched in water. This recrystallization was used to give smaller grain sizes so as to obtain more uniform hardness values and the points represent an average of five readings. The electrical resistivity was measured on 1/16-in. wires quenched from 1000°C during aging at 495°C to give Fig. 3. The energy release and its rate are given in Fig. 4 for the 6.9 pct Al alloy during aging around 500°C. Inasmuch as this was a single run, its accuracy is not known but certainly the general shape and magnitudes are correct. The method used to obtain these results is described elsewhere.' Data for the aging at 600°, 700°, and 800°C of these alloys cold worked 50 pct are given in Fig. 5. Supplementary information from microscopy and X-ray diffraction have been included to indicate recrystallization, discontinuous precipitation and the appearance of superlattice lines from the Ni3Al. The hardness of these alloys as annealed, aged, cold worked, and cold worked and aged is given vs composition in Fig. 6. Those samples which were isothermally aged, Figs. 1 and 2, were reaged at 532°C and at successively higher temperatures for the indicated times to give the data of Fig. 7. These results as well as certain others, support the idea that the level of hardness reached for temperatures above 600°C are equilibrium values more or less independent of path. This being the case, the breaks in the curves would be the complete solution of the Ni,Al. The electrical resistivity versus temperatures for some of these alloys, both aged and unaged, is given in Fig. 8 along with those data from heating slowly (10 deg per day) to high temperatures. Interesting points include the lowering of the Curie temperature (the change in slope), the lack of any indications of a solubility limit and the large temperature coefficient for the Ni3Al. A slight break for Ni3Al around 100C shows up but this is not a Curie temperature as Ni3Al is not ferromagnetic down to -190°C. Metallographically both the nickel-rich solid solution and the Ni3Al appear very much like pure nickel. Profuse twin boundaries are present both

Jan 1, 1960

By C. Burton Clark, J. Spotts McDowell

Refractories are defined as "materials having the ability to retain their physical shapes and chemical identities when subjected to high temperatures," or as "nonmetallic materials suitable for the construction or lining of furnaces operated at high temperatures." While resistance to "high" temperatures is thus the primary requirement for refractory materials, it is by no means the sole requirement. They must be able to withstand thermal shock resulting from rapid heating or cooling; other stresses induced by temperature change; pressures from the weights of furnace parts or contents; mechanical wear (abrasion) resulting from movement of furnace contents; and chemical attack by heated solids, liquids, or gases. Refractories of many kinds are needed for the many and widely diversified industrial applications. Those in greatest demand are classified on the basis of composition or properties into a few main groups, known as alumina-silica, silica, basic and insulating refractories. In each of these groups there are several classes. In addition to those included in the main groups, there are various special refractories, including silicon carbide, carbon, zircon, zirconia, alumina, and several others. Alumina-silica refractories comprise two main divisions: fire clay and high-alumina. The alumina content of fire-clay refractories covers the range from about 45 pct to 18 pct, and the silica content from 50 pct to 80 pct. The alumina content of fired high-alumina refractories ranges from about 99 pct to 45 pct, and the silica content from about 0.5 pct to 50 pct. Silica refractories of the different classes contain 94 pct to 97 pct silica. Basic refractories include periclase (magnesite), chrome spinel, forsterite, and dolomite. Refractory materials, including insulating firebrick, are supplied mainly as preformed shapes. Other products include bonding mortars and high temperature cements, ramming mixtures, plastic firebrick, hydraulic setting castables, dead-burned grain magnesite, and dead-burned dolomite. Refractory brick are classified on the basis of their physical form as Standard Sizes and Special Shapes. The Standard Sizes are brick of certain definite sizes and relatively simple design which are used in sufficient amounts to permit quantity production. The brick most widely used are the standard 9 in. X 4 ½ in. X 2 ½in. and 9 in. X 4½in. X 3 in. straights and corresponding series of sizes. All brick of nonstandard dimensions are regarded as "special shapes." They include a wide variety of brick regularly used for specific services, such as baffle tile for boilers, checker brick for regenerators, and others; together with shapes of special design manufactured on particular orders from designs submitted by the user. Not included in the broad classifications of Standard Sizes and Special Shapes are several specific-service refractory products, usually made by companies which specialize in their manufacture, or in some cases by the consumers themselves. These products include

Jan 1, 1960

By Theodore Simons

The rapid and comparatively recent development of flotation has opened so fascinating a field for study and research that the older processes of gravity concentration no longer receive the attention they deserve. The early work of Munroel and Richards12 and the more recent contributions by Clevenger and Coe,3 Laist and Wiggin,4 Ammon,5 Bardwell,6 Crowfoot,' and Hayden8 (to mention only some which have appeared in our own Transactions) and by Schu1z,9 have furnished so much data that to offer something new seems a difficult task. It is still possible, however, to present known facts from a different point of view, and, with this in mind, the writer has undertaken to express basic principles of gravity concentration in terms of simple mathematics and mechanics; the conclusions thus reached will be found to correspond, in general, with those obtained by experimental methods. Rittinger, in his classic Aufbereitungskunde (1867)) reached analogous conclusions by way of intricate higher mathematics, for which reason his interesting investigations have remained a sealed book to most of us. The writer hopes that a more elementary treatment of the subject, based in part on Rittinger's metheds, may arouse new interest in the study of basic principles.

Jan 1, 1923

By Theodore Simons

The rapid and comparatively recent development of flotation has opened so fascinating a field for study and research that the older processes of gravity concentration no longer receive the attention they deserve. The early work of Munroel and Richards12 and the more recent contributions by Clevenger and Coe,3 Laist and Wiggin,4 Ammon,5 Bardwell,6 Crowfoot,' and Hayden8 (to mention only some which have appeared in our own Transactions) and by Schu1z,9 have furnished so much data that to offer something new seems a difficult task. It is still possible, however, to present known facts from a different point of view, and, with this in mind, the writer has undertaken to express basic principles of gravity concentration in terms of simple mathematics and mechanics; the conclusions thus reached will be found to correspond, in general, with those obtained by experimental methods. Rittinger, in his classic Aufbereitungskunde (1867)) reached analogous conclusions by way of intricate higher mathematics, for which reason his interesting investigations have remained a sealed book to most of us. The writer hopes that a more elementary treatment of the subject, based in part on Rittinger's metheds, may arouse new interest in the study of basic principles.

Jan 1, 1923

By John V. Beall

It is difficult to understand why they did it. It was a demonstration of total commitment which sent chills of mixed admiration and fear up and down your spine. The scene was the bodega in Section A, 2660 Level on the 12 to 8 shift. The jefe was patiently waiting for the tea leaves to settle in a large metal cup. His attention was distracted by the appearance of a miner who had a problem. The long and short of it was that the miner believed the branch raise he was driving was unsafe and he wanted the jefe to come and see it. After lunch the jefe went around. First cautiously shining his light to peer up the raise from outside the chute, he then scrambled inside and swiftly climbed the cribs to the face. No question, it was hairy; about 4 crib sets were needed to catch up to the face. The unsupported raise was slabbing. It didn't take the jefe more than a few seconds to ascertain this situation and to slide back down. As he came out of the chute, a small avalanche arrived on his heels and provided a sort of exclamation point to his order; "cerrado!" In other words, shut 'er down.

Jan 1, 1970

By G. T. Higgins

PREVIOUS workers1,2 have found evidence of exaggerated grain growth or secondary recrystallization on annealing sponge zirconium at temperatures high in the a, phase field, but no details of the orientation relationship between the secondary grains and "as-recrystallized" matrix were reported. In other hexagonal metals, namely dilute Mg-A13 and Cd-zn4 alloys, secondary recrystallization has been observed in which the secondary grains are related to the primary recrystallized structure by rotations about the c axis. These rotations are thus comparable with the rotations about the (111) axis observed in the secondary recrystallization of fcc metals. In the current work secondary recrystallization has been observed on annealing iodide zirconium at 800°C and the associated changes in crystallographic texture have been examined. The material employed was arc-melted iodide zirconium of the following composition: Impurity O H Fe Hf Pb I Ni C1 A1 ppm by wt 130 5 230 98 23 28 200 39 30 This was received as 0.25-in. plate, and, prior to the annealing studies, was cold-rolled to 0.040 in. Specimens 1 in. sq were chemically polished and annealed for various times at 800°C in a vacuum better than 5x 10-6 Torr. For metallographic examination specimens were first chemically polished and then anodized8 to enhance contrast between the grains when examined under polarized light. Changes in crystallographic orientation associated with the development of secondary grains were followed by (1011) and (0002) pole-figure determinations using a conventional Schulz goniometer in reflection. Filtered Cr Ka radiation was employed and great care was taken to avoid spurious re- sults due to the close proximity of the Bragg angles for the (1011) and (0002) reflections. Figs. 1 and 2 illustrate the change in grain structure on annealing at 800°C. After 24 hr the structure has ceased to be equiaxed due to the development of certain grains in preference to others. It is notable that the secondary grains do not grow to the extent observed in sponge zirconium.1,2 This appears to be due in part to the fact that normal grain growth is inhibited in the less pure sponge zirconium, with the result that the driving force for secondary recrystallization remains high, while at the same time the number of grains able to develop in the presence of the impurities is also smaller. As a consequence, in sponge zirconium those grains that do develop preferentially are able to grow into the fine -grained matrix without impingement, while in iodide zirconium the preferential growth of many grains leads to early impingement. The pole figures determined for specimens annealed for 5 min and 24 hr at 800°C are illustrated respectively in Figs. 3 and 4. These indicate that the dominant feature of the initial recrystallized texture consists of basal planes at an angle of 321/2 deg to the sheet surface, with a (1120) axis lying parallel to the

Jan 1, 1967

By S. P. Burke

THE presence of gas in coal mines necessitates the use of costly ventila-tion arrangements and the use of expensive mining methods. On the other hand, the gas itself in many instances is of considerable intrinsic value, and its separate recovery might conceivably be a profitable under-taking. This paper is concerned with a study of the movement of gas in coal strata with the object of determining the laws governing gas move-ment and thus making at least a preliminary step toward the solution of the more practical problem of its control or recovery. Naturally, so important a subject has received much attention from scientists and engineers. In most cases, however, the studies have been concerned with the origin1?, the amount2, the composition3 and the method of retention4 of the gas in coal; or, from the more practical side, have been concerned with the phenomena and conditions associated with outbursts5 or explosions and their control. Numerous studies also have been made of the permeability of coal to gas6, of gas pressures measured in coal seams, etc. The authors are unaware, however, of any attempt to present a consistent or complete picture of the laws governing the movement of gas through the coal.

Jan 1, 1935

By M. Metzger, J. Intrater

IN the large number of important studies on high-purity aluminum (e.g., recrystallization and grain growth, creep, internal friction), it does not seem to have been generally recognized that the iron content, despite its very low figure, has a strong influence on a number of properties. In part, its influence is due to the very low solubility of the Fe-A1 6 phase. For aluminum of about 99.99 pct purity, the iron content may be 0.001 to 0.004 pct. For values in this range, a second phase will be present below 410" to 480 °C. This was determined by extrapolation of a log solubility vs inverse temperature plot of the solid solubility data of Edgar.' One consequence is the inhibition of grain coarsening below the solubility limit. This is shown in Table I, which gives, for three iron contents, the annealing temperature required for the absence of grains smaller than 1/2 mm average diameter together with the minimum temperature for the presence of some grains larger than 2 mm diameter. The specimens were 1/4x 1 1/2-in. strips cut from hard-rolled 1/16-in. sheet supplied by the Aluminum Co. of America.

Jan 1, 1954

By Jack A. Kanz, Samuel R. Shortes, E. C. Wurst

Zinc diffusion into GaAs from the vapor phase through reactively sputtered SiO, films Izas been inrestigated for various zinc pressures at 1000"C. Diffusions were carried out in evacuated quartz ampules with elemental zinc and with various Zn-Ga alloys. Sputtered films have proved effective in lowering surface concentrations and preventing surface deterioration during diffusion. Approxin.ate complenzentary error-function impurity distributions were found when surface concentrations were reduced to approximately 3 -—4 x 10" atoms cm'3 or less with dilute zinc sources or by diffusion through SiO, films. Zinc difhsions in GaAs tlzrough SiO, films produced more planar diffusion fronts than were observed with uncoated zuafers under identical conditions. A) Surface Deterioration During Diffusion. Device technolorn-- in compound semiconductors has been hampered by several difficult problems not normally encountered with silicon and germanium. 111-V and 11-VI compound semiconductors generally have volatile constituents at temperatures used for diffusion. To achieve specific junction depths in reasonable lengths of time, or to obtain particular impurity distributions and doping levels, it is often necessary to use temperatures which cause surface deterioration and erosion of the wafer. The resultant surfaces are generally unsuitable for devices. The type and extent of surface damage depends to varying degrees on the particular environment of diffusion and on the particular impurity in question. The most common type of deterioration results from simple dissociation of the gallium and the arsenic during diffusin.' The deterioration process is significantly enhanced by thermal gradients in the diffusion zone, usually resulting in vapor transport and condensation at the cooler portion of the system. The resulting damage sometimes appears as a general haziness over the surface or an array of pyramidal etch pits characteristic of the particular orientation. Occasionally, erosion of the surface occurs uniformly over the wafer so that surface loss is not readily apparent. Workers in GaAs usually resort to the sealed-ampule type of diffusion system3"5 rather than the more conventional open system used for silicon and germanium. Another type of deterioration results from direct interaction of the impurity with the surface. The form of deterioration may vary from surface alloying, as in the case of zinc, to direct chemical attack and vapor transport of the reaction products, as in the case of sulfur. Surface alloying with zinc occurs at higher temperatures and source vapor pressures.4 The process is largely controlled by the amount of free gallium on the surface of the wafer in equilibrium with the arsenic lost to the system. The group-VI elements, sulfur, selenium, and tellurium, are commonly used donor impurities for gallium arsenide. These elements are characterized by high vapor pressures and high chemical

Jan 1, 1964

By M. L. Fuller

The fundamental mechanism of the deformation of zinc has been thoroughly described by several prominent investigators, particularly Mark, Polanyi, and Schmid,1 Mathewson and Phillips,2 and Schmid and Wassermann.3 The deformation of zinc occurs primarily through slip along basal planes (00.11, and secondarily through twinning on pyramidal planes of the form (10.2). In addition to these basic studies on single crystals, there have been a number of determinations4,5 of preferred orientations developed in rolled, polycrystalline zinc. In no case, to our knowledge, has there been described the development of oriented structures in zinc as a result of a systematic series of rolling treatments. The work included in the present paper shows the changes in orientation produced in a zinc alloy by successively increasing degrees of cold-rolling reduction. This alloy has the same crystal form, hexagonal close-packed, as zinc, but its susceptibility to hardening for a given degree of working is much greater because of its higher recrystal-lization temperature. Experimental Procedure Composition of the Alloy and Rolling Treatment The alloy used in this investigation consisted of zinc of 99.9 per cent purity to which 1 per cent of copper and 0.01 per cent of magnesium had been added.

Jan 1, 1934

By Horace Pops, Jorge E. Kittl

In a recent study' of the martensitic transformation of Cu-Zn ß-phase alloys, it was noted that the MS temperature at the surface was raised due to the loss of zinc by volatilization. It seems likely, therefore, that the MS temperature may serve as a guide for the measurement of composition. From a knowledge of the dependence of the transformation temperature on composition, 2 it should be possible to detect variations in zinc content which are less than 0.1 at. pct by measuring the MS temperature throughout the sample. It is unlikely that an electron microprobe analysis could detect accurately such small zinc losses because the presently accepted limits of accuracy of the micro-probe analysis in simple ternary systems are of the order of 2 to 5 pct of the amount present.3 In the present study, a composition gradient was produced by precipitating the a primary solid solution, and reheating for a very short time within the ß-phase field. The nominal composition, in atomic percent, of the ternary ß-phase alloy used, 64.2 Cu, 34 Zn, 1.8 Si, was selected because it had an MS temperature of +4°C, thereby simplifying the experi-

Jan 1, 1968

By W. S. Pellini, F. N. Rhines

IN many of the otherwise well established alloy phase diagrams the solidus curves (temperatures at which liquid first appears upon melting) have not been located accurately, chiefly because the experimental techniques that have been most popular for determining solidus temperatures have been both cumbersome and subject to large errors. C. E. Homer and H. Plummer1 have described a sensitive and at the same time a very simple technique for locating the solidus curves in a number of alloys of tin. Their method consists simply in noting the temperature at which a specimen of the alloy ruptures under the influence of a light bending force. Although this method is not new, it has been little used for this purpose in the past; nevertheless, it appears so attractive in its possibilities of speed, simplicity, and precision that the investigations presently to be described were undertaken to verify its merits. The redetermination of the solidus and eutectic temperatures of the lead-antimony system was employed as a medium 0f experimentation. New values obtained in this way are believed to be sufficiently precise to warrant a revision of the currently accepted lead-antimony phase diagram (Fig. I). Determinations of the solidus of the lead-rich lead-antimony alloy series have been published by R. S. Dean2 and by E. E. Schumacher and F. C. Nix.3 Their points are represented in Fig. I. In their work the solidus was not located at antimony concentrations greater than 2 per cent; the curve was presumed to meet the eutectic horizontal at an antimony concentration of about 2.5 per cent. In the present studies the solidus has been traced to 3.5 per cent, where the eutectic horizontal is intersected (Table I and Fig. I). Within the range investigated by Dean and by Schumacher and Nix the agreement with their values is good. H. Seltz and B. De Witt,4 on the basis of activity measurements, have calculated that the intersection of the solidus and the eutectic reaction horizontal should lie at 3.86 per cent of antimony. The following determinations of the eutectic temperature have been reported: Roland-Gosselin,5 228°C.; Ewen,6 228°C.; J. E. Stead,7 247°C.; Campbell,8 228°C.; W. Gontermann,9 245° to 252°C.; R. Loebe,10 245°C.; E. Heyn and 0. Bauer,11 245°C.; H. Endo,12 250°C.; R. S. Dean,2 249° to 258°C.; E. Abel, 0. Redlich, and J. Adler,13 245°C.; W. Broniewski and L. Sliwowski,14 250° to 252°C.; H. Seltz and B. De Witt,4 250°C. A temperature of 249°C- appears to have been generally accepted in recent years; it is the value most frequently obtained by the method of cooling curves. Values below 249°C. have usually been obtained by inferior cooling-curve techniques; those above 250°C., by the method of heating

Jan 1, 1942

By J. J. Bikerman

In a recent study' of the martensitic transformation of Cu-Zn ß-phase alloys, it was noted that the MS temperature at the surface was raised due to the loss of zinc by volatilization. It seems likely, therefore, that the MS temperature may serve as a guide for the measurement of composition. From a knowledge of the dependence of the transformation temperature on composition, 2 it should be possible to detect variations in zinc content which are less than 0.1 at. pct by measuring the MS temperature throughout the sample. It is unlikely that an electron microprobe analysis could detect accurately such small zinc losses because the presently accepted limits of accuracy of the micro-probe analysis in simple ternary systems are of the order of 2 to 5 pct of the amount present.3 In the present study, a composition gradient was produced by precipitating the a primary solid solution, and reheating for a very short time within the 0-phase field. The nominal composition, in atomic percent, of the ternary ß-phase alloy used, 64.2 Cu, 34 Zn, 1.8 Si, was selected because it had an MS temperature of +4°C, thereby simplifying the experi-

Jan 1, 1968