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By T. S. Lundy, C. J. McHargue

HE diffusion rate of v48 in single crystals of bee vanadium has been determined at temperatures from 1002° to 1888°C. Standard techniques of lathe sectioning were used for specimens annealed above 1500°C while sectioning by grinding was used for specimens annealed at lower temperatures. As will be seen, the lower-temperature data is enhanced on an Arrhenius-type plot relative to values expected by extrapolation of the high-temperature data. Single crystals were obtained from Linde Co. In Table I the analysis supplied by the vendor is compared with an analysis at Oak Ridge National Laboratory of a sample after a diffusion anneal. The isotope v4' was prepared by the Isotopes Division of Oak Ridge National Laboratory. Proton bombardment of a titanium target in the 86-Inch ORNL Cyclotron was followed by a carrier-free chemical separation. Nineteen specimens, 1/2 in. diam and 3/8 in. long, were cut from the as-received vanadium single crystals. Each specimen was machined with the flat face perpendicular to the longitudinal axis. Specimens were polished through 1/0 emery paper and were etched with 25 pct HF-10 pct H2SO4-10 pct HNO3-55 pct H2O. The polishing and etching steps were repeated until a satisfactory surface finish was achieved. The isotope was electroplated onto the specimens from a neutral solution. Counting rates of the deposited layers were approximately 100 counts per sec. At temperatures above 1200°C specimens were annealed in a tantalum resistance furnace under an argon atmosphere. Temperatures were measured with a Pyro micro-optical pyrometer and a Pt-Pt 10 pct Rh thermocouple. At lower temperatures the specimens were sealed in evacuated quartz ampoules and annealed in Kanthal wire-wound horizontal tube furnaces. A severe reaction occurred at 1200°C between the quartz and the vanadium. This

Jan 1, 1965

By C. O. Burgess, W. D. Forgeng

The results of an investigation of the ternary system iron-chromium-silicon were reported in 1936 by the present authors.l Partly for the sake of theoretical interest, and partly because of the possible commercial importance of these alloys, the present investigation was undertaken to determine the effect of some of the commoner elements likely to occur, deliberately or otherwise, in such alloys if made on a commercial scale. The elements thus added were carbon, nickel or manganese. The alloys studied were, therefore, parts of quaternary systems. This investigation was concerned primarily with the effect of these additional elements on the alpha-iron phase and the boundary between this phase region and the alpha plus sigma two-phase region. The sigma phase is a ternary solid solution based upon the compound FeCr. The work was performed mainly by X-ray methods, but a number of microscopic examinations were also made and are reported. While isolated alloys in the composition ranges studied may have been discussed in metallurgical publications, no systematic investigation of any assistance to us was found. Of the earlier work, the investigations on the iron-chromium-carbon system and on the chromium carbides by Westgren and his coworkers2'3 enabled us to identify the carbide phase. Several articles appeared after the present experimental work had been completed. Lucas and Wintrup4 determined the solubility of carbon in molten iron-chromium-silicon alloys. Tofaute and his coworkers5'6 have made detailed studies of the iron-chromium-carbon system, which will be referred to later. Materials and Methods Materials.—The iron, chromium and silicon used were essentially the same as those used in the investigation of the ternary system.l The

Jan 1, 1938

By C. O. Burgess, W. D. Forgeng

The results of an investigation of the ternary system iron-chromium-silicon were reported in 1936 by the present authors.l Partly for the sake of theoretical interest, and partly because of the possible commercial importance of these alloys, the present investigation was undertaken to determine the effect of some of the commoner elements likely to occur, deliberately or otherwise, in such alloys if made on a commercial scale. The elements thus added were carbon, nickel or manganese. The alloys studied were, therefore, parts of quaternary systems. This investigation was concerned primarily with the effect of these additional elements on the alpha-iron phase and the boundary between this phase region and the alpha plus sigma two-phase region. The sigma phase is a ternary solid solution based upon the compound FeCr. The work was performed mainly by X-ray methods, but a number of microscopic examinations were also made and are reported. While isolated alloys in the composition ranges studied may have been discussed in metallurgical publications, no systematic investigation of any assistance to us was found. Of the earlier work, the investigations on the iron-chromium-carbon system and on the chromium carbides by Westgren and his coworkers2'3 enabled us to identify the carbide phase. Several articles appeared after the present experimental work had been completed. Lucas and Wintrup4 determined the solubility of carbon in molten iron-chromium-silicon alloys. Tofaute and his coworkers5'6 have made detailed studies of the iron-chromium-carbon system, which will be referred to later. Materials and Methods Materials.—The iron, chromium and silicon used were essentially the same as those used in the investigation of the ternary system.l The

Jan 1, 1938

By Cyril Smith

SOMEWHAT over ten years ago the author described studies1,2 on the constitution of the copper-silicon system. The copper-rich portion of this diagram is shown in Fig. 1. The experimental points freely dotted about the diagram seemed to justify an otherwise unconvincing diagram and for several years the curious reverse bend in the alpha-phase bound-ary was accepted as substantially correct, even by later investigators3,4 of the system who introduced changes in the high-silicon phases. The binary diagram has been used as a base for several ternary systems" without any suggested changes. Voce10 suspected the existence of another phase from his study of the cast alloys in the copper-manganese¬silicon system, but evidently hesitated to extrapolate this to the binary diagram, particularly in view of the too ingenious explanation that was advanced" to account for the pools of constituent clearly visible in castings; namely, that they were secondary alpha of twinned orientation deposited from beta. Von Schwarz,12 in 1932, called attention to the fact that this micro-constituent in copper-silicon alloy castings was anisotropic under polar-ized light and asserted that a new phase, not cubic, should be placed in the diagram adjacent to alpha. Sautner,13 on the basis of investigations with the polarizing microscope and with X-rays, introduced this phase into the diagram at about 6 per cent Si. The relevant part of his dia-gram is shown in Fig. 2. Sautner called the new phase beta, renaming the old beta phase zeta. To avoid confusion, in redrawing Fig. 2 the phases have been renamed in accordance with the terminology adopted in the present paper, in which the new phase is called kappa and the other phases retain the designation given them by Arrhenius and Westgren.4

Jan 1, 1939

By A. H. Geisler

INTRODUCTION THE correlation of property changes during precipitation with structure has progressed, sometimes rapidly but other times more slowly, since the fundamental discovery of Merica, Waltenberg and Scott.1 The predominent factor that hampered the progress has been limitations imposed by the various detection methods. Refinements in X ray diffraction techniques and in metallographic methods, which have been extended by the electron microscope, have contributed new information within the last few years. These permit an extension of the theory as proposed by Mehl and fetter in 1940.2 Now that a suffcient number of alloys has been investigated to establish a general mechanism of the precipitation process, a correlation of the facts into a generally applicable theory of age-hardening is both warranted and desirable. 'I he purpose of the paper is to provide an orderly correlation of the phenomenological facts of precipitation hardening. Speculation on mechanism of hardening will be confined to that consistent with existing theories of hardening. Age-hardening accompanies the formation of a new structure, the precipitate, as provided by an alloy system in which solid solubility decreases with decreasing temperature. Upon this premise alone all such systems would be expected to include age-hardenable alloys. Alas, this is not always the case. Few attempts have been made to explain the variable degree of age-hardening among different alloys or to explain the influence of small alloying additions upon the hardening. Dispersion hardening as originally postulated3 is not adequate.* Coherency hardening-the term that will be used to distinguish the properties of a two-phase mixture in the unique and unstable transition state at which the phases are strained into precise atomic registry (continuity or coherency) in planes

Jan 1, 1948

By K. M. Rolls, R. M. Rose, H. B. Shukovsky

Studies of the phase structure, critical current density, and resistive critical magnetic field of a 45 pct Nb-55 pct Zr superconducting alloy after final-size heat treatments are reported in this paper. A combination of optical metallography, X-ray diffraction, and electrical-resistivity measurements were used to determine the phase structure. Superconductivity measurements, made with heat-treated wires, are correlated with microstructure. Although no quantitative relationship between microstructure and critical current density is found, it is shown that SINCE Kunzler1 as well as Berlincourt, Hake, and Leslie2 first described the high-field, high-current-density superconductivity of Nb-Zr alloys, it has be- the critical current density is highest when the microstructure is finely divided by fibering, coring, precipitation, or fine-scale phase dispersions. The resistive critical field is very sensitive to the compositions of the phases present. Since the alloy investigated here is near the maximum resistive critical field for the Nb-Zr system, any phase decomposition results in a lower H,. Elimination of the effects of cold work lowers H, also. A possible interpretation of the latter in terms of internal surface superconductivity is suggested. come apparent that the resistive critical field and the current-carrying capacity of such alloys are, in large measure, dependent on composition and processing. The resistive critical magnetic field (Hr) for low current densities has been found to increase progressively with zirconium content until a flat maximum is reached between 50 and 65 pet Zr.3 For any single composition, a characteristic maximum value of H, is attained by heavily cold-drawn wire.4 critical current density (J,) depends not only upon cold work but also, apparently, upon microstructure. Heat treatments of cold-worked wires generally

Jan 1, 1965

By C. Kolm, E. P. Warekois, S. A. Kulin

MUCH insight has been gained into the nature of the cold-worked state of metals in recent years through the use of modern X-ray techniques. These methods have revealed the existence of stacking faults together with regions of high internal strain and have provided means of measuring the atomic perturbations in plastically deformed metals. In view of the recent increased interest in the solid state, it is desirable to extend these techniques to the study of lattice imperfections introduced into semiconductors during plastic deformation. It is of particular interest to compare the state of imperfection sustained by metallic bonding with that sustained by the covalent bonding found in semiconductors. A knowledge of the imperfections which can exist in semiconductors is important from both a theoretical and a practical point of view since they can greatly influence many of the physical properties. In order to determine the possible existence of stacking faults in covalently bonded structures, precise measurements were made of the diffracted peak positions of plastically deformed germanium, gallium antimonide, and indium antimonide. These measurements were based on the theoretical treatment of Paterson1 and are similar to those employed by Warren and warekois2 in their studies of deformed a brass. In addition, diffraction peak profiles were measured on the annealed and plastically deformed materials in order to obtain information concerning the distribution of internal strains through the use of the Fourier methods developed by Warren and Averbach.3 EXPERIMENTAL PROCEDURES AND TECHNIQUES Because of the room-temperature brittleness of the semiconductors studied, it was necessary to plastically deform the materials at elevated temperatures. The brittle-ductile transition temperature ranges of GaSb and InSb are sufficiently low to permit hot-filing operations. Therefore, high-purity, polycrystalline GaSb and InSb were filed in an argon atmosphere at 400' and 300°C, respec-

Jan 1, 1959

By G. Derge, M. Bourgon, G. M. Pound

A STUDY of electrical conductance in molten Cu-Fe sulfide mattes' has shown that pure molten Cu,S behaves like a semi-conductor in that it is an electronic conductor and its specific conductance, of the order of 100 ohm-' cm-', increases with increase in temperature. On the other hand, pure molten FeS, another electronic conductor, behaves like a metallic conductor in that its specific conductance, about 1500 ohm-' cm-', decreases with increase in temperature. Molten solutions of Cu,S and FeS follow a roughly additive rule of mixtures with respect to both specific conductance and temperature coefficient. The behavior of molten Cu,S may be understood, by analogy to the situation in solids, in terms of semiconductor theory.' It is thought that, although the melt consists of cuprous and sulfide ions, the bond between these atoms has a certain degree of cova-lency. According to the simplest concept the electrons in the partially covalent bonds are thermally promoted to a conduction band. In another concept, small amounts of impurities (undetermined) provide donor or acceptor levels in the forbidden zone between the valence and conduction bands and thus facilitate semi-conduction in the usual way. However, the metallic behavior of molten FeS is difficult to explain, because one might expect from similar reasoning that it too should act like a semi-conductor. It was suggested that the apparent metallic behavior of molten FeS might be explained by a large negative temperature coefficient of density. Thus if molar conductance instead of specific conductance were plotted versus temperature, the slope might prove to be positive, indicating semi-conduction instead of apparent metallic conduction. Accordingly, density measurements were made in order to answer this question in regard to molten FeS and also to provide data for conversion of specific conductance to molar conductance for molten Cu,S and a molten 50-50 wt pct Cu-Fe sulfide matte. Experimental Diagrams of the apparatus are given in Figs. 1 and 2. A 3 x 8-cm dense alundum crucible containing the prefused specimen is positioned in the uniform temperature zone of an induction furnace tube and melted under a helium atmosphere. Then the cell assembly, consisting of two 3-mm spectro-graphite rods, one of which is in a 1-cm ID open

Jan 1, 1959

By William Fink

ALUMINUM forms not only binary compounds with most of the metallic elements but also forms many ternary or more complex constituents. Several of those occurring in the more important alloy systems have been identified under the microscope and the action of various etching reagents has, been carefully studied.' The determination of the structure and composition of these complex constituents is a matter of some difficulty and little information is available. X-ray crystal analysis offers a promising method for the study of such constituents. First, and of considerable importance, is the possibility of recognizing the presence of a given constituent by means more positive than microscopic observation. Evidence can also be obtained concerning the nature and composition of the constituent in question and ultimately it should be possible, at least in some cases, to describe the structure including the relative locations of the various atoms. In this paper some results of an uncompleted study of the constituents of the aluminum-iron-silicon system are given and the methods employed are described. Inasmuch as iron and silicon are the chief impurities in aluminum, the constitutional relations of this system are of fundamental importance in the metallurgy of pure aluminum and its alloys; the system has been studied by several investigators and the more important contributions have been reviewed recently.2 Fig. 1 shows the structure of the aluminum-rich alloys after prolonged annealing at 560° C., in accord with one of the most recent investigations.3 The ternary alloys examined in the course of the present investigation were all annealed at 550° or 560° C.; in fact, some of the specimens were the identical ones used by Dix and Heath, who kindly supplied them for this work. Since the results

Jan 1, 1930

By Royal B. Jackman, Carle R. Hayward

Two comprehensive papers have appeared regarding the forms of copper that occur in smelter slags, one by Frank E. Lathe1 and the other by C. G. Maier and G. D. Van Arsdale.2 These authors comment on other published results and draw conclusions from their own investigations. The development of X-ray examination of minerals and improvement in high-power microscopic methods make it possible today to get additional evidence by means that were not available to earlier investigators. The present work was confined to reverberatory slags obtained from five different plants. Some definite conclusions were reached regarding the forms of copper present in these slags. In most cases these agree with some of the findings of Maier and Van Arsdale but new methods of attack were used in the investigation. Conclusions of Previous Investigators Various important conclusions reached by previous investigators are summarized in the following paragraphs, arranged chronologically. William A. Heywood:3 Slag losses increase with grade of matte but with the same grade of matte losses decrease as the acidity of the slag increases. Lewis T. Wright:' Slag losses are only partly due to prills of matte. It is suggested that part of the copper is dissolved in the slag. J. Parke Channing9 A considerable part of the copper enters the slag as silicate or oxide and not as sulfide. C. A. Grabill:6 Slag losses are both physical and chemical. Physical losses, due to poor settling, gas flotation and slight differences in specific gravity, are small under normal conditions. Chemical losses may- be due to formation of oxides or to solution of metals and sulfides. The last is considered the most important. John W. James:' The copper in converter slag is largely the oxide and as such enters the reverberatory slag when converter slag is added to the charge.

Jan 1, 1934

By William A. Edmiston, R. E. Grace

A simplified model for the theory of reaction rates near equilibrium has been applied to the reduction of wustite. A linear relationship between the net rate of reaction and the Gibbs free-energy change, ?F, is predicted. The reduction of wustite in H2 -H2O gas mixtures was studied with a microbalance technique at temperatures from 850° to 950 °C. The predicted model was found to be valid to -?F/RT = 0.1 or approximately -200 cal per mole away from equilibrium. ThE theory of reaction rates near equilibrium has been developed by a number of authors. Prigogine, Outer, and Herbo1 have studied the catalytic hydrogena tion of benzene in an attempt to deduce some intrinsic connection between reaction rates near equilibrium and thermodynamics. Manes, Hofer, and weller2 have derived more general expressions for reaction rates near equilibrium from classical thermodynamics. Hollingsworth3,4 has commented briefly on the work of Manes et al. Benson5 has summarized in a general way the results of the earlier contributions. It is the purpose of this paper to apply the theory of reaction rates near equilibrium specifically to the reduction of wustite in H2-H2O gas mixtures. The basic premise is that the reduction of wustite proceeds by a surface reaction, rather than by solid-state diffusion ,or gaseous diffusion. Richardson and Dancy6 and Gellner and Richardson7 have suggested that the reduction of wustite may be governed by iron diffusion in wustite. Mckewan8-11 has proposed that reduced iron layers on various oxides are sufficiently porous to offer a negligible impedance to the reducing gas. The linear motion of interfaces reported by McKewan and discussed by Themelis and Gauvin12 indicates the lack of diffusive control during reduction. The reduction studies of magnetite reported by Quets, Wadsworth, and Lewis13 give additional evidence that reduction rates are linear when the reaction products are porous and nonprotective. The interpretation of measurements reported in this paper is predicated upon a surface-controlled reduction reaction, at least in the earliest stages of reduction when the reduced iron layer is thin.

Jan 1, 1967

By M. Friedman

Applications of rock mechanics to the design of engineering structures in rock involve the assumption that the stresses are due entirely to the present applied loads. For instance, it is assumed that the vertical normal stress in undisturbed rock free of topographic effects is equal to the weight per unit area of the overburden. In fact, vertical dilatational strains associated with stresses of more than 100 times the present overburden pressure have been measured by strain-relief methods on outcrops. 1,2 The notion of residual strain (stress) or latent stress3 seems unassailable; and indeed this has long been recognized by metallurgists. It is difficult, however, to assess the residual component of the in-situ state of elastic strain with conventional strain relief methods employed in mines or down boreholes. That is, in principle, the in-situ state results from the superposition of present applied loads (natural or man- induced) and potentially recoverable elastic strains (stresses) that exist in a given volume of material even though there are no external forces across the boundaries of the body (Voight,4 and Fig, 1). Accordingly, only in unloaded blocks can the true residual strains be measured by strain relief methods. Using X-rays, the elastic strains locked within the quartz grains or crystals of a rock can be measured. These strains are known to persist even when the rock is reduced to small chips but to vanish when the rock is disaggregated and the grains are powdered. Although we have just begun to investigate the mechanisms by which the strains are stored (see Preliminary Results), we believe that "pressure solution'' at grain boundaries, secondary cementation under load, permanent ("plastic") deformation, and temperature changes are possible processes. In any event, in our study of naturally deformed rocks, it is significant that we are work-

Jan 1, 1972

By R. M. Brick, M. A. Williamson

Certain features of the response of copper and brass to deformation and recrystallization remain obscure. The textures obtained on rolled sheet are listed by Schmid and Boas1 as: No adequate explanation has been advanced for the presence of the secondary deformation texture of copper and its absence in brass or for the origin of the cubic recrystallization texture of copper.2 A recent publication3 attempted to rationalize the above empirically described annealing texture of brass on the basis of retention of the (110) [112] rolling orientation plus twinning about the central octahedral poles of the usual secondary (110) [115] orientation. The difierence in the textures of annealed copper as compared to 70-30 brass is also shown by the difference in the position of ears for drawn copper, at o° and go", as compared with drawn brasses, at 45o, for all compositions between oo-10 and 70-30.4 Data on indi- vidual crystals are as yet too few to permit of an analysis of these textures comparable to that of mild steel as made by Barrett and Levenson.5 Experimental Methods The materials studied included copper specimens cut from the central, equiaxed crystal portion of a tough-pitch wirebar; brass made from this copper and high-purity (99.99 per cent) zinc including alloys of 7 per cent, 15 per cent, 24 per cent, 29 per cent and 36 per cent Zn and large single crystals of 70-30 bras. Sections 1/4 in. thick of the cast polycrystalline copper and brasses were reduced 40 per cent by rolling, recrystallized to a common grain size of 0.045 mm. and then rolled directly to foil 0.002 in. thick. Hardness readings employing both the Vickers and Rockwell machines were taken at intervals during the reduction. For comparison, similar specimens were cross-rolled—i.e., turned through 90° for each pass—and comparable hardness data were secured. Finally sections from the single crystals of brass were cut to obtain the following initial orientations; these sections were rolled, hardness data secured and a complete micrographic record of structural changes obtained.

Jan 1, 1941

By R. M. Brick, M. A. Williamson

Certain features of the response of copper and brass to deformation and recrystallization remain obscure. The textures obtained on rolled sheet are listed by Schmid and Boas1 as: No adequate explanation has been advanced for the presence of the secondary deformation texture of copper and its absence in brass or for the origin of the cubic recrystallization texture of copper.2 A recent publication3 attempted to rationalize the above empirically described annealing texture of brass on the basis of retention of the (110) [112] rolling orientation plus twinning about the central octahedral poles of the usual secondary (110) [115] orientation. The difierence in the textures of annealed copper as compared to 70-30 brass is also shown by the difference in the position of ears for drawn copper, at o° and go", as compared with drawn brasses, at 45o, for all compositions between oo-10 and 70-30.4 Data on indi- vidual crystals are as yet too few to permit of an analysis of these textures comparable to that of mild steel as made by Barrett and Levenson.5 Experimental Methods The materials studied included copper specimens cut from the central, equiaxed crystal portion of a tough-pitch wirebar; brass made from this copper and high-purity (99.99 per cent) zinc including alloys of 7 per cent, 15 per cent, 24 per cent, 29 per cent and 36 per cent Zn and large single crystals of 70-30 bras. Sections 1/4 in. thick of the cast polycrystalline copper and brasses were reduced 40 per cent by rolling, recrystallized to a common grain size of 0.045 mm. and then rolled directly to foil 0.002 in. thick. Hardness readings employing both the Vickers and Rockwell machines were taken at intervals during the reduction. For comparison, similar specimens were cross-rolled—i.e., turned through 90° for each pass—and comparable hardness data were secured. Finally sections from the single crystals of brass were cut to obtain the following initial orientations; these sections were rolled, hardness data secured and a complete micrographic record of structural changes obtained.

Jan 1, 1941

By E. A. Kaarsberg

The electron photomicrographs shown in this paper are of samples of the A.P.I. Reference Clay Minerals Montmorillonite No. 27 and Kaolinite No. 4 and of a shale from Spraberry Oilfield in Texas. These samples are part of a larger collection whose physical properties, composition and internal structure were previously studied by ultra-sonic and X-ray methods. ' Elastic anistropy was indicated in the montmorillonite and shale samples by sound velocity measurements parallel and perpendicular to the bedding. In the montmorillonite the velocities parallel and perpendicular to the bedding were 2.12 and 1.92 km/sec respectively, a difference of about 11%; in the shale the same velocity measurements were 4.18 and 3.75 km/sec, a difference again of about 11%. Within the bedding plane the sound velocity was also found to be independent of direction. The electron photomicrographs of the montmorillonite sample, which are shown in Fig. l(a) and (b), clearly indicate the preferred orientation of the mica-like clay particles parallel to the bedding. In Fig. 2(a) and (b) similar orientation in the shale sample can be seen although not quite as clearly. This is probably because, in addition to the clays illite and chlorite, the shale sample contains grains of quartz, calcite and dolomite which do not as readily show an alignment pattern as the clays do. This suggests that the elastic anisotropy of these two samples is derived from a preferred alignment of component mineral grains which are themselves elastically anisotropic. The bulk elastic properties of these two samples therefore appear to be much like those of mica. Velocity measurements were made on the kaolinite sample in three directions at right angles because no bedding could be discerned in it. The values ob-

Jan 1, 1967

By J. D. Pennock

About a year and a half ago, Mr. Morris, an engineer of the Solvay Process Company, was sent to Belgium and France to study the manufacture of coke in the Semet-Solvay ovens, which were in operation at Havre. With complete plans of construction and a good understanding of the methods of running the ovens, he returned to Syracuse. Work on twelve Semet-Solvay ovens was immediately begun. These ovens, with plant for crushing and washing coal, and the necessary condensers, scrubbers, and concentrator for the recovery of the byproducts are nearly finished, and will soon be in operation. As the work approached completion it became necessary to determine what coal should be used. Accordingly, a chemical investigation of the various bituminous coals was made. I. Investigation of Coals. The samples of coal taken for analysis were: I. A sample of Reynoldsville coal that had been exposed to the weather for a year; 11. Reynoldsville coal taken from a car direct from the mine; 111. Morris Run lump coal; IV. Morris Run fine coal; V. Coal from the Fairmount Coal and Coke Company; VI. A special enginecoal from Pardee colliery, Phillipsburg, Pa.; VII. South Fork, Pa., coal; VIII. Coal from Laceyville, Ill.; IX. Pittsburgh bituminous coal from Ocean mines (gas-coal); X. Steubenville, Ohio, coal; XI. Evansville, Indiana, coal; XII. Coal from the Ohio Coal Company. Proximate Analysis. I. 11, 111. IV. V. VI. Water at 90° C.,* ..................................... Volatile,. .. 31.14 33.00 17.73 18.12 37.20 23.86 Fixed Carbon,. . 64.49 58.07 71.92 71.89 56.68 73.00 Ash,. .. 4.37 8.93 10.35 9.99 6.12 3.14 Coke,. .. 68.86 67.00 82.27 81.88 61.88 76.80

Jan 1, 1893

By T. N. McVay, E. E. Creitz

Rather large amounts of titanium minerals and some zircon and monazite are being recovered from dune sands about I. miles west of Jacksonville Beach, Fla. The Mining Branch of the Bureau of Mines, Southern Experiment station, has been interested in developing additional large deposits of similar sands in other areas of Florida. The results of a field study have been published1 concerning the sands occurring on Trail Ridge which runs north and south about 30 miles southwest of Jacksonville. This investigation was undertaken in order to identify the opaque titanium minerals occurring in Trail Ridge and because of the economic importance of Florida titanium minerals. Nature of the Problem The minerals present in the heavy fractions (sp gr > 2.94) of the sands are principally opaque minerals; staurolite, zircon, sillimanite, tourmaline, kyanite, rutile, a small amount of corundum, traces of the zinc spinel gahnite and garnet. Epidote, monazite, hornblende and ti-tanite are present in other dune sands but these minerals were not noted in the samples collected on Trail Ridge. All of the minerals except those which are opaque can be readily identified by the usual petrographic methods. However, Opaque minerals cannot be examined satisfactorily by transmitted light. Polished sections of the opaque-mineral grains were examined but these sections did not furnish useful information. Consequently, it was necessary to use means other than the usual petrographic methods to identify them. Previous Investigations of Heavy Minerals in Florida Sands Martens2 has described the heavy minerals in the Florida beach sands and has classified the opaque minerals as ilmenite with minor amounts of leucoxene. Miller3 studied a number of sands collected by Ross and Mertie in Florida. He states that the material from the Florida beach and dune sands that commonly has been called ilmenite has essentially the chemical composition of the material that has been called arizonite.4 The x ray diffraction patterns of several samples indicated that the supposed ilmenite is essentially amorphous, with only weak lines corresponding to ilmenite, and hence the material is unlike the type of arizonite from Arizona. Opaque Titanium Minerals Rutile is essentially titanium dioxide. However, as pointed out by Dana,5 important amounts of Fe+2 and Fe+3 as well as Cb and Ta are reported in some analyses.

Jan 1, 1949

By Charles Barrett

PLASTIC flow in metal crystals and the changes in orientation resulting from it are generally understood to take place by the following funda-mental mechanisms: (1) slip on crystallographic planes, (2) homogeneous crystal rotation resulting from the slip, (3) bending of the lattice between the planes of slip, and, under certain circumstances, (4) twinning. This paper and a preceding one on iron subjected to uniaxial compression1 concern two additional processes that must now be added to this list: (5) the formation of deformation bands, and (6) the bending and rotation of these bands. The present investigation yields a new understanding and definiteness to the common terms so loosely used when speaking of cold-worked metals -"grain fragmentation," "elongated grains," and "deformation twins," "deformation bands," "etch bands," or "X-bands." Bands have been noted on the polished and etched surfaces of cold-worked metals by vari-ous investigators for more than 25 years, ? yet their nature and their significance have been so little understood that they are not treated in the most comprehensive modern texts on the deformation of crystals. The experiments in this series show that they are one of the fundamental processes in the deformation of metals, of importance in the development of preferred orientations, in work-hardening (since they have the effect of reducing the effective grain size and interfering with slip), and in the recrystallization process. The present experiments were performed on the same stock of mate-rial that was used in the earlier compression experiments1-hydrogen-purified mild steel in which the carbon content had been reduced to the limit detectable under the microscope and in which single crystals could be grown by a strain-anneal treatment.2

Jan 1, 1939

By Nicholas J. Grant, Irmgard Rump, Bill C. Giessen

The system W-Hf was determined by use of metal -lographic and X-ray methods. The only interrnetal-lie phase W2Hf melts peritectically at 2650° ± 50°C. A eutectic between W2Hf and ß-Hf solid solution exists at 78 at. pct Hf arul 1930º ± 10°C. The addition of tungsten loulers the hafnium transfornzation; there is a eutectoid at 93 at. pct Hf and 1560°C. The solubility limits of the terminal solid solutions were determined. At the beginning of this investigation, the system had not been elaborated; only crystallographic work had been done to determine the structure of the occurring intermetallic compound W2Hf, and a certain analogy to the system W-Zr was to be expected. Special emphasis was placed in this program on the Hf-rich part of the diagram. Following the completion of our experiments, a phase diagram was suggested by Braun and RUdY.1 EXPERIMENTAL METHODS The investigation utilized tungsten powder supplied by the General Electric Co. with a purity of about 99.9 pct and hafnium crystal bar of about 97.7 pct purity, 2.3 pct Zr, supplied by Foote Mineral Co. Typical analyses are given in Table I. The procedures followed were identical with the ones described for the Re-Nb diagram.' Tungsten powder was compacted at 16,000 psi and the necessary amount of hafnium was added in the form of small pieces cut from the crystal bar, with a reasonable excess of tungsten powder to make up for powder losses on melting. High hafnium or tungsten melts were prepared from premelted tungsten and hafnium or by employing master alloys. The melting was done in a Heraeus arc-furnace under argon. Melting and remelting up to 8 times resulted in fairly homogeneous alloys. No weight

Jan 1, 1962

By Ancel St. John

At the New York meeting of the Institute of Metals Division in February, 1927, Jeffries and Tarasov presented a paper on Tungsten and Thoria,' in which the experimental facts were interpreted in accordance with the prevailing point of view that the thorium is present as the oxide, thoria. In discussing that paper the writer of this article stated that his own investigations, which had been unavailable to Messrs. Jeffries and Tarasov, showed that the so-called "thoriated" tungsten filament failed to disclose any sign of the oxide when subjected to X-ray diffraction analysis, but did give plenty of evidence of the presence of metallic thorium and, in certain cases, of a material believed to be an alloy of tungsten in thorium. Since these results were completely at variance with the results reported in the paper under discussion and with other papcrs which had preceded it from time to time in the past, it was felt that further discussion should be withheld until the new evidence could be presented adequately. Arrangc-mcnts were therefore made to present that evidence at this meeting. Material Examined The material exalllined was high-ernission filament such as is used in radio tubes, supposed to contain about 0.75 per cent. thoria. The actual analysis was not stated. Scope of the Investigation The investigation was undertaken because of a feeling that the thorium present in filamentary material of this type exists as metallic thorium or as an alloy of thorium and tungsten and not as the oxide. Attention was therefore directed to determining: 1. The minimum amount of thoria detectible in a mechanical mixture of thoria powder and finely divided tungsten. 2. The amount of t.horia detectible in the filament. 3. The condition of any thorium present in other form than as thoria. 4. The amount of thorium dissolved in the tungsten.