Search Documents

By R. C. Hall

The magnetic anisotropy and magnetostriction of single crystals of alloys between 25 and 59 wt pct Co in Fe have been determined in the disordered and ordered states. The magrzetostriction is large and positive for all alloys in both states of order (up to 150 x 10-6 for A,, and 40 x 10-6 for 111). The magnetic anisotropy becomes zero rzear 41 pct Co for the disordered state. Ordering shifts the zero-anisotropy composition to about 50 pct Co. COBALT-iron alloys have for many years been of interest as magnetic materials because they have unusually high magnetic saturation values.' This interest was increased recently by the development of Supermendur.' Supermendur is an alloy of 49 pct Co-49 pct Fe-2 pct V* which was found by suitable purification and heat treatments, including a magnetic anneal, to possess excellent magnetic properties. These included a square hysteresis loop with a low coercive force and a high magnetization, and a low total loss. Two factors which are important in determining the magnetic hysteresis properties are the basic magnetic properties of magnetostriction and anisotropy. Alloys having zero anisotropy and zero magnetostriction show improved hysteresis properties.3 Since very meager data4-' are available in the literature on the single-crystal anisotropy and magnetostriction of the cobalt-iron alloys, the present program was undertaken to determine these two properties in the disordered and ordered states. EXPERIMENTAL TECHNIQUES Ingots of the cobalt-iron alloys containing from 25 pct to 59 pct Co in iron were vacuum melted from electrolytic iron and cobalt of 99.9 pct purity. The ingots were cooled at a rate of about 1°C per hr through the transformation temperature (950" to 980°C dependent on the alloy content) for the growth of large grains. From these grains, single-crystal disks were fabricated with either the (110) or (100) plane parallel to the faces of the disk. The crystals were given two heat treatments to produce either the ordered state (cooling rate of 20°C per hr from 850 "C) or the disordered state (water quench from 850 °C). Since the iron-cobalt alloys order very rapidly, the water quench may not have produced complete disorder in all cases. Due to the method of growth, the crystals were not perfect. Most of the samples had low-angle boundaries and a few had some small included grains. These imperfections could and probably did affect the accuracy of both the magnetic anisotropy and magnetostriction measurements. Much of the scatter in the data may be attributed to the crystal imperfections. The methods of determining the spontaneous saturation magnetostriction and the anisotropy have been previously described.419110 MAGNETOSTRICTION The magnetostriction in the [loo] and [Ill] directions (hO0 and ?111 respectively) is illustrated in Fig. 1 for the disordered state. Both ?100 and ?111i became large positive values as cobalt was added to iron. The state of order did not have a large effect on the magnetostriction. The effect of order did not appear too consistent in these data. Tentative curves are shown in Fig. 1 for the ordered magnetostriction near the FeCo composition; here ?100 appeared to be lowered and ?111 raised as the degree of order was increased. These results agree qualitatively with the

Jan 1, 1961

By H. P. Leighly, F. C. Perkins

THERE have been several statements in the literature about the difficulty of producing single crystals of high-purity (99.99pct) by the strain-anneal method. Consequently, investigators tend to employ low-purity aluminum for their single-crystal experiments, or else resort to the Bridgman or other techniques which depend on solidification for the production of single crystals. The following paragraphs describe a solid-state method for the manufacture of single crystals of high-purity aluminum which should provide crystals with greater perfection than those formed by solidification. The starting material for this method of producing single crystals was secured from the Aluminum Corp. of America and has a purity of 99.99 pct, the balance being trace amounts of impurities. Specimens approximately 1 by 4 in. are sheared from sheet having a nominal 0.050 in. thickness. The specimens are given a preliminary anneal at 640°C for approximately 3 hr in order to remove fabrication strains and to produce an average grain size of about 1/4-in. diam. The specimens are then etched in Tucker's etchant (45 pct HC1, 15 pct HNO3, 15 pct HF and 25 pct H2O) to remove the oxide film. Critical strain is applied by wrapping each specimen about a 1 3/4 in. round and subsequently straightening it against a flat surface. The high-purity aluminum sheet is sufficiently soft that this operation can be accomplished by ordinary finger pressure. The specimens are immediately annealed again at 640°C for 3 hr and reetched for examination. Ordinarily, considerable growth of certain of the grains will have occurred, and occasionally a single crystal will be produced on the first attempt. The procedure of alternately straining, annealing and etching is repeated until the majority of a batch of specimens contains usable crystal sizes. Typical examples are illustrated in Fig. 1. The greatest changes in crystal sizes are produced in the initial treatments. As the average crystal sizes get coarser in the later treatments, the sever- ity of the strain must be increased in order to produce grain boundary- migration. This increase in severity is effected by decreasing the diameter of the round used for straining (to 1 1/2 in., for example) and/or wrapping the specimens about the round twice, with opposite faces in contact with the round, before flattening. Usually the strain treatments described are not severe enough to produce nucleation in coarse grain high-purity aluminum. The growth of grains occurs by strain-induced grain-boundary migration. It has been observed that the grain boundaries move most readily during the first hour or so of each annealing treatment and that the rate of movement decreases with extended holding times at temperature. Prolonged annealing treatments are therefore not usually beneficial. Similarly, the rate of growth of each crystal appears to depend upon the orientation of the crystal with relation to those of its neighbors. Frequently island grains are formed after the initial heat treatment as the result of slow grain-boundary migration. These sometime become stationary during later heat treatments. Twin orientation interfaces are frequently developed during annealing. These imperfections can usually be removed by increasing the severity of strain to produce actual nucleation of new grains of more favorable orientation at the imperfection interfaces. The largest single crystals produced in our laboratory by the above method measured 4 by 1 by 0.050 in. Examination of Laue back-reflection patterns from a limited area of the specimens, gave no evidence of polygonization. Probably there is some indication of polygonization in the original grain area provided a more sensitive technique is used for detection. Experiments to produce wider specimens were less successful, possibly because wider sheets increase the complexity of the strains induced by deformation and promote widespread nucleation. Grain boundary migration occurs preferentially in a direction parallel to the longitudinal axis of the specimen. The choice of specimen geometry with respect to the rolling direction of the sheet appears to be immaterial in regard to the production of single crystals.

Jan 1, 1961

President Howe : It is not so clear to me that the facts which Dr. Waldo brings forward really argue that the nature of the combination between copper and aluminum differs from that of the combination between copper and zinc or copper and tin. As regards electric conductivity, I suppose that the fact, which he thinks points to a special intimate kind of union between aluminum and copper, is that the line in his Fig. 1 is neither straight nor uniformly curved, but that its curvature varies rapidly, not to say abruptly. But we find just such variation in like curves for the copper-zinc and copper-tin alloys. Thus, a slight addition of zinc or tin to copper causes a change in color wholly out of proportion to the quantity added; and, as we add zinc or tin to copper, the tenacity rises very greatly, only to fall off abruptly with further additions of either of these metals. Dr. Waldo : My curve related only to electrical conductivity. The President : If irregularity in one physical property argues

Jan 1, 1895

By J. Washburn, R. Drouard, E. R. Parker

Temperature dependence of the rate of recovery in zinc single crystals after a simple shear deformation at low temperature was investigated. Some tentative suggestions regarding the annealed and strain-hardened states of a crystal are discussed. RECOVERY may be defined as the gradual return of the mechanical and physical properties of strain-hardened metal to those characteristic of the annealed material; an increase in temperature increases the rate of recovery. The annealing process in strain-hardened polycrystalline metals is complicated by the inhomogeneity of strain which always exists in aggregates. Polygonization in bent regions of the crystals and growth of new almost strain-free grains starting at points of severe local distortion1-:' make it almost impossible to isolate and study the recovery process. Homogeneously strained single crystals, however, do not polygonize or re-crystallize and hence they can be used advantageously to study recovery. In such crystals strain hardening is completely removed by recovery alone. Since recovery is a process whereby certain lattice disturbances introduced by plastic flow are gradually reduced, a knowledge of the rate and temperature dependence of this process for various conditions of prestrain might be helpful in formulating a model of the strain-hardened state. For simplicity it seemed desirable to limit the type of prestrain to the simplest obtainable, i.e., simple shear strain. In the experiments to be described, recovery was studied by observing changes in the stress-strain curve of prestrained zinc single crystals held for various times at temperatures above that employed for straining. Single crystals were grown from the melt by a modified Bridgeman technique from Horse Head Special zinc 99.99 pct pure, and from spectrographically pure zinc 99.999 pct pure. They were grown as 1 in. diameter spheres and acid-machined' to the final specimen contour. The test section was a cylinder about 1/8 in. high and 3/4 in. in diameter. The conical sections adjacent to the test section were cemented into the grips so the load could be transmitted to the crystal as uniformly as possible. The specimens were oriented so that in testing the maximum shear stress was applied along one of the slip directions, [2110], in the (0001) plane. Details of the production and testing of such specimens have been presented.' Each test was carried out according to the following schedule: 1—The crystal was strained at — 50°C until it reached a maximum shear stress, ,,,. The strain rate was approximately 5 pct per min in all cases. 2—After straining, the crystal was unloaded before the temperature was changed. Unloading required about 3 min. 3—The temperature of the specimen was then increased from — 50°C to the temperature, T, of recovery. This change in temperature was completed in a time of less than 2 min. The specimen remained at temperature, T, for a time, t, which differed for the various specimens. 4—Thereafter the temperature was again reduced to — 50 °C in approximately 3 min. 5—While at —50°C, the stress-strain curve after recovery was obtained. 6—The specimen was then unloaded and annealed for 1 hr at 375 °C in a helium atmosphere to bring about complete recovery. Cooling to room temperature after anneal required 90 min. 7—The same crystal could be re-used for another test because the plastic properties after annealing closely duplicated those of the original crystal. The specimen was immersed during the test in a bath of methyl alcohol which, through a system of tubes, could be pumped through either of two heat exchangers to regulate the temperature; this was accomplished by circulating the liquid through coils immersed in a bath of acetone and dry ice for cooling or in a bath of warm water for heating. Test temperatures were thus maintained constant within ±1°C. The — 50°C temperature was low enough so that no measurable recovery occurred during unloading and reloading. The stress-strain curve continued after recovery along a path below, but approximately parallel to, the path of a curve obtained in an uninterrupted test. Fig. 1 shows some of the results from a specimen of 99.999 pct Zn. The amount of downward displacement of the curve due to recovery was a

Jan 1, 1954

By V. Koump, T. F. Perzak, R. H. Tien

A series of experiments were carried out in which the rates of propagation of the liquidus and the eutectic fronts Mere measured during essentially one-dimensional freezing of Al-Cu alloys. The dimensions of the ingots were 3 by 5 by 6 in. Three different alloys containing 0.1, 4.5, and 17 pct Cu were used in these experitments. For each alloy the rate of heat removal was varied to give a total jreezing time in the range 3 to 30 min. The results of these measurements cowlpared favorably with the theoretical model of freezing of binary alloys with time-dependent surface temperature. IN engineering analysis of solidification of commercia1 steels and nonferrous alloys it is a common practice to assume that an alloy freezes by propagation of an isothermal solidification front, i.e., essentially as a pure metal. In two recent theoretical investigations'j2 the present authors explored the possibility of a more realistic approach to the problem of solidification of alloys. In the proposed model the freezing of an alloy is assumed to take place by propagation of two isothermal fronts, i.e., the liquidus front and the solidus (or eutectic) front. The region between the two fronts contains both liquid and solid and is referred to as the solid-liquid region. The width and the solid content of the solid-liquid region vary with alloy type, solute concentration, and cooling rate. For a given alloy system, initial concentration of solute, and the mode of heat removal, the proposed model yields the temperature distribution within the solid skin, temperature, solid fraction, and concentration distributions with the solid-liquid region, and the rates of propagation of the liquidus and the solidus fronts. This model is obviously of considerable practical importance in engineering analysis of solidification processes, since it gives a more realistic estimate of skin strength during solidification and a better estimate of the total freezing time. Before the new model can be used with confidence, however, it is necessary to test this model experimentally. The experimental testing of the proposed model is a relatively simple matter since the effects to be measured are large and a relatively simple experiment will suffice. The theoretical model predicts, for example, that during freezing of an alloy containing substitutional type solute (negligible diffusion in the solid during freezing) the solid-liquid region occupies an appreciable portion of the ingot, even at low concentration of solute.' Another prediction of the theo- V. KOUMP, formerly with U. S. Steel Corp., is now with Research and Development Center, Systems and Process Division, Westinghouse Electric Corp., Pittsburgh, Pa. R. H. TlEN is Senior Scientist, Fundamental Research Laboratory, U. S. Steel Corp., Research Center, Monroe ville, Pa. T. F. PERZAK, formerly with U.S. Steel Corp., is now with Fiber Industries, Greenville, S. C. Manuscript submitted March 6, 1968. IMD retical model, easily verifiable by experiment, is that the rate of propagation of the solidus (or eutectic) front increases as the solidus front approaches the center of the slab. This prediction is contrary to well-known behavior of the solidification front during freezing of pure metals, where the rate of propagation of the solidification front decreases with time and freezing is completed at the lowest rate. A rather severe test of the proposed model is provided by comparison of theoretical predictions and experimental measurements of the effects of cooling rate and composition on the rates of propagation of the liquidus and the eutectic fronts. In order to test the soundness of the formulation and the method of solution of the problem of solidification of alloys a series of experiments were carried out in which the rates of propagation of the liquidus and the eutectic fronts were measured during essentially one-dimensional solidification of A1-Cu alloys. The A1-Cu system was chosen strictly as a matter of convenience. Three different alloys containing 0.1, 4.5, and 17 pct Cu were used in these experiments. For each alloy the rate of heat removal was varied to give the total freezing time in the range 3 to 30 min. The results of these measurements are compared with the predictions of the theoretical model of solidification of binary alloys, with time-dependent surface temperature.' Before the experiments described in this paper were undertaken, a serious attempt was made to utilize the measurements of previous investigators to test the theoretical model. In the course of this preliminary study a careful review was made of experiments of Pellini and coworkers3 and Doherty and Melf~rd.~ The measurements in Pellini's work were carried out using a steel containing at least four major components. Evaluation of the solid fraction-temperature relation for this steel (required in the theoretical model) is difficult and uncertain. Doherty and Melford, on the other hand, measured the solid fraction-temperature relation experimentally, but did not give sufficient data to explore the effects of composition and the cooling rates on solidification. Hence it was not possible to utilize these measurements to test our theoretical model. EXPERIMENTAL METHOD The experimental technique used in this investigation differs somewhat from the more conventional techniques employed in solidification studies. This technique was developed primarily to eliminate con-vective mixing in the molten metal caused by pouring of molten metal into the mold. In our experiments A1-Cu alloys were melted directly in the mold. The mold assembly used in solidification experiments is shown in Fig. 1. The mold was fabricated from *-in. stainless-steel sheet. The dimensions of

Jan 1, 1969

By J. S. Aronofsky, J. P. Heller

This paper presents a mathematical analysis of the fluid mixing which occurs during flow through porous media. The analysis is based on the well-known diffusion equation with mass transfer term. It is pointed out that the use of this equation is justified by a single general assumption which does not specify any particular mechanism for the mixing process. Formulas are given for tracer fluid concentrations for two different boundary and initial conditions. Calculated numerical values compare closely with some published results of experiments in which no viscosity or density difference existed between displaced and displacing fluids. INTRODUCTION A phenomenological theory of the mixing and diffusion process is presented for the flow in a porous medium of two miscible liquids of equal viscosity and density. This is based on the classical diffusion equation which has been used to explain such processes as Brownian motion and heat conduction. More recently, this same differential equation has been derived (in a manner analogous to the work in this paper) for the problem of heat transfer during fluid flow in porous media.' The purpose of this paper is to show that the available experimental evidence justifies the use of this simple diffusion equation. The recent data of Koch and Slobod' and of von Rosenberg' are used to test this diffusion model by comparing concentration curve shapes and calculating "effective diffusion coefficients". The same differential equation for miscible displacement, as well as some experimental confirmation, has been published in Japan by K. Yuhara,4 and recently in this country by Day.5 Yuhara arrives at his con-clusions through analogy with turbulent diffusion, de- scribing the microscopic velocities in terms of "eddy motion" — although unlike the ordinary eddies of hydraulics. Day proceeds directly from Scheidegger's6 concept of the dispersion of velocities. After a very clear description of Scheidegger's theory, he applies it to calculate the motion first of a drop and then of a thin layer of brine into a bed of sand. For the latter case, Day derives and solves the same differential equation as Eq. 1. In our presentation no detailed assumptions are made as to the mechanism of displacement. In fact, several microscopic processes may well be involved—the only general assumption made is that their cumulative microscopic effect may be described by the addition of a second-order term to the differentirl equation of continuity. DERIVATION OF EQUATIONS Let us consider the displacement in one spatial dimension of Liquid A from a sample of porous media by Liquid B. A and B are assumed completely miscible and of the same viscosity and density. Both fluids are also assumed to be incompressible and it is specified that the total flow is the same for any cross section. It is evident that the rate at which Liquid B would be carried across such a section would be given by the product of the fluid velocity, u, and the concentration, C, of B in the fluid mixture assuming the constancy of u and C over the cross section. Since the volume of Fluid B is conserved, this leads to the one-way wave equation - u ?C/?x = ? ?C/?l where x increases in the direction of u—the "Darcy velocity", Q/A (or velocity flux per unit area), and 9 is the fractional porosity. Consider the case where fluid B is displacing Fluid A and the concentration distribution is represented by a step funcLon (with a vertical discontinuity). The solution of Eq. 1 predicts no mixing

Jan 1, 1958

By S. G. Cupschalk, J. J. Wert, R. A. Buchanan

The uniaxial deformation of thermally ordered and disordered polycrystalline Cu3Pt was studied by means of the X-ray line - broadening analysis according to Warren and Averbach and the extension of this analysis to ordered fcc materials by Mikkola and Cohen. Because of the heat treatment history, extinction had a pronounced effect on the X-ray spectra of ordered and disordered C%Pt at small plastic strains. After an appropriate correction for extinction, the long-range order in thermally ordered ChPt was found to decrease at a slow constant rate with plastic strain. Furthermore, the antiphase domain probability increased at a constant rate to 17.5 pct strain. The effective particle size behavior indicated that the stacking fault energy is lower in ordered than in disordered Cu3Pt. Analysis of the stress-strain curves shouled that ordered Cuzt has a slightly lower yield Point but a much higher work-hardening rate than disordered Cu3Pt. THE presence of long-range order in a solid-solution alloy has a marked effect on its mechanical properties. While this effect has been known qualitatively for many years, it was not until recently that detailed investigations have been performed to determine the exact role long-range order plays in this strengthening mechanism. The development of an advanced, quantitative. X-ray diffraction analysis by Warren and Averbachl and the extension of this analysis to the L1, type super lattice by Mikkola and cohen2 have greatly accelerated research in this field. The research reported in this paper consisted of two primary phases. The first phase was to determine the effect of long-range order on the tensile properties of polycrystalline Cu3Pt. This objective was accomplished by comparing the stress-strain behavior of thermally ordered CusPt to that of thermally disordered CusPt. The second phase of the research was to determine the difference between the atomic arrangements in thermally ordered and thermally disordered Cu3Pt as a function of uniaxial deformation and thereby gain a deeper insight into the mechanism by which long-range order affects the tensile properties. This second objective was accomplished by applying the Warren-Averbach method of peak profile analysis to the X-ray diffraction patterns obtained from ordered and disordered Cu3Pt after given amounts of uniaxial deformation. EXPERIMENTAL PROCEDURE The Cu3Pt was prepared by vacuum melting and casting. After a homogenization anneal, the ingot was cold-rolled to sheet form. Two tensile specimens with gage sections of 2.50 by 0.500 by 0.115 in. were carefully machined from the sheet. The specimens were polished with a final step of 600-grit paper to insure smooth diffracting surfaces. Finally, one specimen was heat-treated to yield an average grain diameter of 0.016 mm and an initial degree of long-range order, S, of 0.825. The other specimen was water-quenched from above the critical temperature, 645"C, to yield an average grain diameter of 0.017 mm and zero long-range order. The heat treatment history of each specimen is shown in Table I. The tensile tests were performed utilizing a Research Incorporated Model 900.95 Materials Testing System. This unit employs a closed-loop feedback system which maintains a constant strain rate through an extensometer clipped to the gage section of the tensile specimen. A strain rate of 1.32 i0.02 x 10"4 sec-' was employed in testing both specimens. In the X-ray diffraction analysis, a General Electric XRD-5 diffractometer equipped with a pulse-height analyzer set for 90 pct efficiency was employed. The goniometer speed selected was 0.2 deg, 20, per min. Filtered Cu radiation was used for all peaks and all peaks were chart-recorded. Because of nonuni-form grain size. it was necessary to spin the specimens during X-ray analysis in order to obtain reproducible integrated intensities. The spinning rate was 2000 i100 rpm. The application of the Warren-Averbach method of peak broadening analysis to a diffraction pattern is very time consuming if done manually. In this research, the calculations involved were performed with the aid of a computer program by wagner.3 As reported by Wagner, the program is written in Fortran TV computer language. It was modified to Fortran I1 so as to be handled by the IBM 7072 computer at Van-derbilt University. In the X-ray diffraction analysis of uniaxially deformed Cu3Pt, the 100, 200. 400. 111, and 222 reflections were recorded from the initially ordered sample after 'plastic strains of 3.0, 6.0, 9.0, 12.0,

Jan 1, 1970

By A. Sainato, E. Baker, J. Cervik

In Europe, water infusion is used widely to reduce generation of respirable dust during mining. Its use in the US is limited to a few plow operations in the deeper parts of the Pocahontas No. 3 Coalbed. The technology for infusing water into retreating longwalls is described and results of a recent Bureau test in the Lower Sunnyside Coalbed demonstrated dust reductions ranging from 47% to 64%. Because water infusion increases moisture content of the coalbed, face air velocities in excess of 2.5 m/s (500 fpm) are possible, further diluting dust levels before dust entrainment occurs. An economic analysis shows a 23% reduction in operating costs when coal production is increased by changing from unidirectional to bidirectional mining with water infusion.

Jan 1, 1986

By H. Nakazawa, I. Iwasaki

Galvanic contact, occurring between electrically conducting minerals in flotation pulps, may affect the nature of mineral surfaces and influence their floatabilities. Rest potential and galvanic current measurements were made on an electrode combination of pyrite and pyrrhotite under nitrogen, air and oxygen aeration conditions. The results were correlated with their oxygen-consuming characteris- tics and flotation behaviors. The galvanic contact improved the floatability of pyrrhotite, but adversely affected that of pyrite. Auger electron spectroscopy, X-ray photoelectron spectroscopy, and scanning electron microscopy indicated that the formation of hydroxide or oxide and sulfate species of iron on pyrrhotite decreased, whereas that on pyrite increased when these minerals were held in contact. An electro- chemical mechanism was proposed for the observed behaviors.

Jan 1, 1986

By C. K. Gupta, P. K. Jena

Niobium (columbium) metal in the form of a button has been produced by calciothermic reduction of niobium pentoxide using sulfur as the heat booster. In these experiments with 50 g of niobium pentoxide per batch, the influence of percentage of calcium in excess of the stoichiometric, the percentage of sulfur by weight of the niobium oxide, and the outer-wall temperature of the bomb on the quality and yield of the metal has been studied. The maximum yield on this scale was 78 pct using 50 pct excess Ca and 20 pct of S and at a bomb-wall temperature of 600°C. In experiments conducted on 500 g of niobium pentoxide, reduction with 40 pct excess Ca and 20 pct of S, and at a bomb-wall temperature of 500°C, the.yield of the metal improved to 82 to 84 pct. Some of the reduced-metal samples have been electron-beam melted and the button melts thus obtained have been observed to be extremely ductile and capable of cold reduction to 98 pct without intermediate annealing. NIOBIUM, because of its high melting point (2468oC), its ductility, its resistance to corrosion especially in liquid metals, its high-temperature mechanical properties, and its relatively low capture cross section (1.1 barns) for thermal neutrons, has potentialities as a structural material in the field of nuclear engineering. Niobium and its alloys are also gaining importance in high-temperature technology as components in aircrafts, jet engines, and missiles, electronics, chemical engineering, and surgery. In 1904 Weiss and Aichel 1 produced niobium by reduction of its pentoxide by misch-metal. Since then a large number of investigations have been carried out for the extraction of niobium from its compounds. The various routes through which the metal niobium has been extracted from its compounds can broadely be classified into the following groups: a) reduction of its halides, oxides, and fluo-salts with metals like calcium, magnesium, sodium, and aluminum;2-10 b) reduction of its halides with hydrogen and oxides with carbon or carbides;11-18 c) electrolytic winning from its halides and fluo salts;19-25 and d) thermal decomposition and disproportion ion of its halides26-30 Among the processes in commercial use at present are sodium reduction or fused-salt electrolysis of potassium niobium fluoride, carbide or carbon reduction of the oxide, and hydrogen or metallothermic reduction of the chlorides. In 1907 Von Bolton2 prepared niobium by reducing niobium pentoxide with aluminum. Dennis and Adam-sona attempted reducing the oxide with magnesium powder in argon atmosphere and the resulting metal contained as much as 5 pct O. Mondolfo8 claimed a method for the reduction of the oxides with aluminum. In the case of both magnesium and aluminum reduction, it has been stated31 that by-product oxides such as MgO or A12O3 would involve a major separation problem. Further, in the case of alumino-thermic reduction, the solubility of aluminum in niobium and intermetallic formation have to be reckoned with. In 1922 Bridge3 produced niobium by calcium reduction of niobium pentoxide. Dennis and pdamson' obtained the metal by a similar method with an oxygen content of 0.2 pct. In most of the cases of metallothermic reduction of niobium oxides mentioned above, the metal niobium is obtained in the form of powder. In an attempt to produce massive niobium metal, lock' used iodine as the thermal booster in the bomb reduction of niobium pentoxide by calcium. Massive niobium metal was obtained with a maximum yield of 75 pct containing 0.1 pct 0. Joly32 carried out experiments on calcium reduction of niobium pentoxide on a 2-kg scale using sulfur as the heat booster in a sealed bomb filled with argon. In his experiments, the reaction was initiated by passing a current through niobium spiral wire embedded in the charge. In a typical run consisting of 2000 g of niobium pentoxide, 3100 g of calcium, and 800 g of sulfur (S/Nb2O5 = 3.3), he obtained massive metal in the form of a very uneven mass with a yield of -57 pct. With lower amounts of sulfur and calcium, powder niobium mixed with small metal globules was obtained and the yield was also poor. From these experiments he concluded that this method is not a suitable one for industrial development considering the quality and yield of metal obtainable and the possible hazards with higher ratios of sulfur to niobium pentoxide in the -~charere. In the present work, a detailed investigation on the calciothermic reduction of niobium pentoxide in a stainless-steel bomb in presence of sulfur as the heat booster was undertaken on a laboratory scale.

Jan 1, 1964

By F. S. Norcross

DEVELOPMENT of the manganese deposits of Cuba is a matter of importance not only to those involved in this industry on the Island but to the United States steel industry and to our Nation as a whole. For years our domestic resources of manganese have been wholly inadequate, but the recent Cuban development points the way toward solution of this strategic mineral problem.

Jan 1, 1939

By F. D. Richardson

STAFF: Editor, Gerhard Derge Carnegie lnstitute of Technology Schenley Park Pittsburgh, Pa. 15213 Editorial Assistant, M. A. Redmerski Production Editor, Otto T. Johnson THE METALLURGICAL SOCIETY: Jack H. Scoff, President; Richard C. Cole, Past-President; Harold 0. Emerick, President-Elect; Ralph L. Hennebach, Treasurer; Robert W. Shearman, Secretary; Donald A. Parks, Assistant Secretary; Leslie S. Wilcoxson, Assistant Secretary. PUBLICATIONS COMMITTEE OF THE METALLURGICAL SOCIETY: R. E. Lund, Chairman; T. E. Dancy, H. O. Emerick, P. R. Gouwens, R. E. Grace, J. H. Jackson, H. H. Johnson, A. E. Lee, Jr., R. R. Nosh, R. D. Pehlke, and Paul Queneau. Review and selection of manuscripts is under the supervision of the following Publications Committees: Extroctive Metallurgy Division: R. E. Grace, Choirmon; G. M. Bell, D. W. Bridges, J. M. Cigon, G. W. Heoly, T. A. Henrie, R. D. (Holli-doy, C. E. O'Neill, C. S. Somis, A. W. Schlech-ten, and Charles Shull. Iron and Steel Division: R. D. Pehlke, Choirmon; T. P. Floridis, Arnulf Muon, G. R. St. Pierre, E. T. Turkdogan, L. H.Von Vlock, and J. M. Uys. lnstitute of Metals Division: H. H. Johnson, Jr., Chairman; J. B. Clark, Vice Choirmon; M. R. Achter, G. F. Bolling. J. O. Brittoin, G. P. Conard, II, R. S. Davis, L. A. Girifolco, G. T. Hohn, J. P. Hirth, L. Himmel, G.T.horn, George Krauss, J. D. Livingston, R. D. Manning, H. M. Otte, S. V. Rodcliffe, R. E. Reed-Hill, H. C. Rogers, E. ScaIa, O. Sherby, M. T. Simnad, G. R. Speich, E. A. Steigerwald, R. A. Swolin, W. A. Tiller, W. R. Upthegrove, J. B. Wagner, Jr., Derek Wolton, H. W. Weart, W. W. Webb, and D. Published seven times yearly in February, March, April, June, August, October, and December by the American lnstitute of Mining, Metallurgical, and Petroleum Engineers, Inc., 345 East 47th Street New York, N. Y. 10017. Telephone PLAZA 2 -6800. Subscription $30 per year for non-AtME members m United States and North, South, and Central America; $32, foreign; $7.50 for AlME members Single copies, $6.00, single copier foreign, $6.50. The AiME is not responsible for any statement made or opinion expressed in its publications . . . Copyright 1964 by the American Institute of Mining, Metallurgical, and Petroleum Engineers, Inc. . . . Registered cable address, AiME New York Indexed in Engineering Index, Industrial Arts Index, and Chemical Abstracts. Second dost postaas poid ot New York, N. Y.,ond Ann Arbor, Mich. Volume 230, Number 6.

Jan 1, 1964

By P. T. Chiang

Chemical etching methods for the simultaneous revealing of the tellurium or selenium Phase and the chalcogenide grain boundaries of the alloy systems are given. A tellurium eutectic was found Present in zone-melted ingots. Similarly, a selenium monotectic was present in ingots. In general, the second phase (tellurium or seleniumn) occubies three different sites; viz., along the chalcogenide grain boundaries, as inclusions within the chalcogenide grain, and on the undersurface of the ingot. The detection limit for the tellurium phase is about 1 u in width. THERMOELECTRIC materials based on Group V (bismuth, antimony) and Group VI (selenium, tellurium) elements have aroused considerable interest in recent years in the practical application of thermoelectric cooling. In many cases, a small amount of excess tellurium (or selenium) was added to the material to optimize its thermoelectric properties. Then the question immediately arises as to the number of phases present in the resultant alloy. In the binary systems of Bi-Te, Sb-Te, and Bi-Se, the congruent melting compositions have been reported to be non-stoichiometric and are represented by Bi~Te respectively. It is to beexpected and known that Bi2Te3 and SbzTe3 crystallize from the melt with an excess of bismuth and antimony in the lattice and that tellurium forms a eutectic.~' The same could be assumed to take place in the pseudo binary systems of (Bi,Sb)zTe3 and Bi2(Se,Te)3 as well as in the system studiedby puotinen5 and other workers. Likewise, BiaSe3 crystallizes from the melt with an excess of bismuth in the lattice and selenium forms a monotectic.~ Therefore, in practice, alloys solidified from the melt often contain a second phase (tellurium or selenium) in one region or another of the solid mass even without the addition of excess tellurium (or selenium). ~u~~recht' studied the thermoelectric properties of (Bi,Sb)2Te3 alloys with excess tellurium and simultaneous additions of selenium. He mentioned that the materials show two phases because of the considerable excess of tellurium or selenium. However, he did not report as to how the tellurium or selenium phase was identified. It is generally believed that the presence of an excessive amount of tellurium or selenium phase in the alloy would adversely affect its thermoelectric properties and its uniformity. Consequently, there is a need for a simple method for the identification of the tellurium and selenium phase. The quantity of the second phase present is usually too small to be detected either by chemical analysis or by normal X-ray techniques. This investigation was therefore carried out, first, to devise a simple metallographic method for the identification of the tellurium or selenium phase coexisting with the chalcogenides and, second, to determine the distribution and specific location of the tellurium or selenium phase in the ingots. EXPERIMENTAL PROCEDURE The starting materials used for the alloy preparations were 99.999 pct pure bismuth, antimony, and tellurium and 99.997 pct pure selenium. The bismuth and antimony were obtained from Consolidated Mining and Smelting Co. of Canada Ltd., while the selenium and tellurium were obtained from Canadian Copper Refiners Ltd. The tellurium was purified further in the laboratory by zone refining. The elements were pulverized in a stainless-steel pestle and mortar. The amounts for the desired composition were weighed out each time on an analytical balance to make up a 100-g sample. Then the sample was introduced into a Vycor ampule (19 by 150 mm), pumped down to a vacuum of 10"5 Torr for 15 min, and sealed off. The ampule was then heated in a horizontal resistance furnace at 800" to 900°C for about 20 hr. During this period the assembly was rocked back and forth several times to ensure good mixing. At the end of the heating period, the ampule was quenched in cold water and then transferred to the zone-melting apparatus described in a previous publications to grow large-size aligned polycrystals. The background and ring-heater temperatures were adjusted to make the freezing solid-liquid interface slightly convex to the liquid. The recorded temperature gradient in the vicinity of the freezing solid-liquid interface was around 15°C per cm. The ampule was moved horizontally at a speed varying from 0.4 to 2 cm per hr so that the ring heater would cover the whole ingot length from end to end. A single zone-melting pass was used for the Bi-Te, Sb-Te, and Bi-Sb-Te ingots. Two passes in the forward and reverse directions were carried out for the Bi-Se and Bi-Se-Te ingots. Six passes in the forward and reverse directions were performed for the Bi-Sb-Se-Te ingot. The zone-melted ingots were found to contain several large crystals, with their basal planes (0001) approximately parallel to the growth axis. Samples of bismuth and antimony tellurides coated with a layer of tellurium, and bismuth selenide coated with a layer of selenium, were prepared for comparison in phase identification. These coatings were made by dropping a piece of the zone-melted ingot into some molten tellurium or selenium under argon atmosphere and allowing them to cool slowly to room temperature. The metallographic specimens were prepared by

Jan 1, 1969

Jan 1, 1966

CHARLES F. WILLIS,* Bisbee, Ariz.-(written discussion?).-The consensus of the discussion of the paper of Dr. Lanza indicates that the physical examination, while it is probably a good thing, is fought by the workingman, and that, because of this fact, it has been proved unsuccessful. The physical examination standing alone is worth but little, and could easily be made a subject both of ridicule and dissension unless the company having such examination shows its own good faith in promoting a thoroughly better health program. It is easily seen why a workman would resent his employer expecting him to be physically fit, if at the same time the employer provides un-healthful, unsanitary, working conditions, or if the town in which the employees are expected to live is dirty and unkempt. One mocks the other. The employer cannot say, "You must remain healthy so that I can get by with unhealthy conditions." But if working- conditions are as good as can be obtained to keep men well, the employer can ask his men to be in a healthy condition. A State examination and standard would have many difficulties, owing to the fact that a man would pass or would not pass the standard set, thus eliminating the discretion on the part of the employer in placing men whose physical condition might well permit working in one place and not another. Any physical examination that is run for the purpose of eliminating the physically unfit is unjust, both to the worker and to the nation as a whole; a State examination would make a distinct dividing line, whereas examination by the employer is conducted with a vision of the positions available. The workman's opposition to the physical examination comes from the fact that he has been taught to believe that it is an interference in his personal affairs, that he can be clean or dirty as he chooses, that he can he healthy or unhealthy, and that it is nobody's business but his own. The war has taught us, however, that the individual is no longer the unit and that all such propositions must be based on the greatest good for the greatest number.

Jan 6, 1919

By J. Gordon Parr, D. H. Polonis

High purity alloys of titanium and iron, made by a technique of levitation melting, have been investigated with particular reference to martensite formation and decomposition in the hypoeutectoid range. A preliminary study has been made of the occurrence of the phase corresponding to the structure Ti2Fe. MANY of the previous investigations of Fe-Ti alloys have been made using Kroll sponge as a source of titanium; and the subsequent heat treatments to which alloys have been subjected has, on occasion, led to further contamination. Worrier,',' who suggested a part of the equilibrium diagram for the binary system, and Wallbaum and coworkers,3-5 who worked largely with iron-rich alloys, all used Kroll sponge. Van Thyne, Kessler, and Hansen,6 in their determination of the equilibrium diagram, used iodide titanium for alloys up to 30 pct Fe. Duwez,7 who measured the M. temperature of titanium binary alloys with many solute elements, used iodide titanium in all cases except in his work on Ti-Fe alloys for which he used Kroll sponge. The investigation of the supposed phase Ti2Fe by Rostoker8 nvolved the use of iodide titanium. A section of the constitutional diagram, after Van Thyne et al., is reproduced in Fig. 1. Frequently too much stress is placed on the effect of contaminants in equilibrium and nonequilibrium systems, but there is no doubt that titanium alloys are extremely susceptible to interstitial atoms. Consequently, the main purpose of the work to be described was to determine those features of phase transformations in pure Ti-Fe alloys that were considered of importance in commercial heat treatments. For, although commercial alloys may not be of high purity, the investigation of a system uncomplicated by traces of impurity is a desirable starting point. Another incidental feature, the occurrence of Ti2Fe, was also investigated. The entire study was carried out using powders obtained from alloy ingots, for diffusion reactions are often more rapid in small particles than in bulk specimens. The frequently adopted practice of ascertaining phase constitutions by X-ray analysis of powders, and relating these to the microstructures and mechanical properties of bulk specimens, is considered by the authors to be open to criticism. In the martensite reactions in the Fe-Mn system, for example, it has been shown- hat similar phase distributions in solid and powder may result in different hardness values and appearance under the microscope; and it is possible that similar anomalies might occur in the Ti-Fe system. Consequently, in order to

Jan 1, 1955

By William H. Spice

Exploratory drilling in South Central Texas for the year 1944 showed a marked increase over that of 1943 and resulted in a similar increase in new fields discovered. In this area, which comprises the 30 counties included in district No. I, Oil and Gas Division, Railroad Commission of Texas,? 61 exploratory wells were drilled during 1944 as compared with 29 exploratory wells drilled during 1943, or an increase of over 100 per cent. Three new oil fields, two new gas fields and one gas-distillate field were discovered during the year, as compared with one new oil field and one new gas field discovered during 1943. These new fields were the result of exploratory drilling throughout the district along the Wilcox trend and the deeper Edwards lime trend, which was started during the previous year. The Wilcox trend yielded the new Loma iilta-Wilcox oil field and the San Caja gas-* tlistillate field, both in McMullen County. The Charlotte field, in Atascosa County, was discovered along the deeper Edwards lime trend. These three discoveries were of considerable importance and subsequent development should indicate the desirability of continued exploration along these trends. The other three discoveries, United oil field in Guadalupe County, Pederson gas field in Milam County and Van Cleve gas field in Zavalla County, were of minor importance. Charlotte Field, Atascosa County, was discovered by the Humble Oil and Refining Company's No. 3 Pruitt, completcd on Aug. 9, 1944, flowing 176 bbl. per day, 3/16-in. choke, 710 lb. tubing, 475 lb. casing pressures, 37.7º A.P.I. gravity, from the top of the Edwards lime from 6917 to 6923 ft. Two oil wells were completed during the year in this field. This discovery is 14 miles southwest of the same company's Imogene field, also producing from the Edwards lime but with considerable difference in reservoir characteristics. The discovery of this field is the result of surface geology and subsequent seismograph survey of the area. Loma Alta-Wilcox Field, McMullen County, was discovered by the Atlantic Refining Company's No. I Atkinson, completed on June I, 1944, flowing 102 bbl. per day, 9/64-in. choke, 1900 lb. tubing pressure, 37º A.P.I. gravity, from Wilcox sand from 6866 to 6869 ft. after being drilled to a total depth of 7185 ft. This discovery is the result of subsurface geology and an extensive seismograph survey of the entire area. Sun Caja Field, McMullen County, was discovered by Edwin M. Jones No. 2-C Ezzell, completed on June 2, 1944 as a dual completion in the Wilcox sands, flowing 1,740,000 cu. ft. gas with 53 bbl. distillate, 1/4-in. choke, 2035 lb. tubing pressure, 53.2º A.P.I. gravity, from sand 6416 to 6453 ft. and flowing 2,000,000 cu. ft. of gas with 127 bbl. distillate, 1/4-in. choke, 2500 lb. tubing pressure, 50º A.P.I. gravity, from sand 6889 to 6916 ft., after being drilled to a total depth of 7264 ft. Three gas-distillate wells were completed during

Jan 1, 1945

By K. E. Gray, A. Podio

ABSTRACT Berea and Bandera sandstone samples were impacted with both 3/4-in. and 1/2-in. long wedges, each having a 60° included angle and a 0.05-in. flat, at various confining pressures, with borehole and pore pressures held fixed at atmospheric pressure. Samples were saturated with air, water, glycerine-water, solirol, mineral oil and soltrol-mineral oil mixtures to obtain a wide range of pore fluid viscosity. Penetration depth was held constant at 0.1 in. Dry and soltrol-mineral oil-saturated Berea samples were impacted at depths of penetration from 0.01 to 0.04 in. under 1,000 psi confining pressure to study crater initiation. Results indicate that viscosity of the pore fluid is influential primarily during the early stages of crater formation. Differences in bit force, crater volume and blow energy for tests parallel and perpendicular to bedding were significant, but decreased as the stress state was elevated. Crater volume, blow energy and bit force were nonlinearly related with depth of penetration. Crater volume was nonlinear with energy of blow. Fixed-penetration tests on saturated Berea yielded greater crater volume than did similar tests on dry samples. Differences in the nature of deformation for low values of bit penetration were noted between saturated and unsaturated samples. INTRODUCTION Rock failure during bit-tooth impact and scouring action constitutes a vital part of the drilling process and a difficult problem for researchers. Much study has been devoted to various aspects of the problem, and much has been learned about mechanics of rock failure. However, analytical treatment of drilling at depth remains difficult, partly because there are so many factors involved and because valid simulation of downhole conditions is extremely difficult. Forming individual craters by a bit tooth or chisel impacting, or indenting, a rock mass has been studied by many investigators.1-18 Similarity between single-tooth chisel impact and the corresponding action of a rotary bit has been discussed by Appl and Gatley, Garner, Podio, and Gatlin l8 compared the similarity in single-blow impact tests with microbit drilling data reported by Cunningham and Eenink.l9 Maurerll has used single-tooth impact data to develop a "perfect cleaning" theory of rotary drilling. Individual roller cutter-tooth impact data have been reported by Young. 20 Single-tooth tests in all of the cited literature were carried out on dry rocks. Inasmuch as any subsurface rock of oilfield interest is saturated with some fluid, it seemed desirable to study crater formation in permeable rocks saturated with a viscous pore fluid as a step, however short, toward more realistic simulation of subsurface conditions. This paper presents results of single-blow chisel impact studies on Berea and Bandera sandstones, both dry and saturated with pore fluids of various viscosities at confining pressures to 10,000 psi. EXPERIMENTAL APPARATUS AND PROCEDURE EXPERIMENTAL APPARATUS The same basic apparatus for single-blow chisel impact at elevated stress states, described in earlier papers was used in this study. l6. l8 Fig. 1 shows the complete experimental system; Fig. 2 shows a cross section of the pressure cell, with a sample ready to be impacted. EXPERIMENTAL PROCEDURE Two different rocks, Berea and Bandera sandstones, were used in this study. Both rocks have been used extensively in research, and rock descriptions can be found in a paper by Gnirk and Cheatham.15 Permeability to air of Berea is about 300 md normal to bedding and 540 md parallel to bedding. Bandera had vertical and horizontal air permeabilities of 18 and 57 md, respectively.

Jan 1, 1966

By Leendert de Witte, Fred J. Radd

In many areas caring failures can be directly related to electrical currents observed in the casings. It is the thesis of this paper that the observed casing currents are mainly due to electrochemical potentials of the type in evidence on spontaneous potential curves of electrical logs. The general nature of these potentials are discussed and an equivalent circuit is given for current and potential distributions around open holes. The casing forms a short circuit to these potentials and tends to average the effects of local cells. The case of casing corrosion opposite the Dakota water sands in the salt-mud area of Kansas is discussed anil used us a qualitative, illustration of the relation between SP's and casing currents. A method of quantitative derivation of casing current distribution frorn electric log SP curves, using linear transform theory, is described and results are compared with a measured current profile. The effects of hydrogen over-potentials at the cathodic portions of the pipe are considered and some laboratory data are given in support of conclusions regarding the over-1.01tuge.s. INTRODUCTION To date an appreciable amount of work has been done on the measurement of oil well casing currents and on the correlation of the anodic portions of the current profiles with corrosive casing failures. Speculations on the origin of the casing currents have, however, remained rather vague; and although almost every plausible cause has been mentioned, there is to the writers' knowledge no clear-cut expose' on the details of the causes of the corrosive currents in the literature. A study of current surveys and casing failures in the N.W. Burnett field, Ellis County. Kan.. indicated the probability that concentration cell emf's between the Wellington salt section and the relatively fresh waters in the Dakota sands were a major cause of the corrosion currents. A more general concept evolved upon analysis of the severe corrosive conditions in the Pleistocene sands in the Ventura Avenue and San Miguelito fields in California. In this area no major variations in the salt content of the formation waters occur and yet large casing currents are observed. An explanation is found in the fact that the local spontaneous potentials which are set up due to concentration contrast between the drilling fluid and the connate water are short circuited when casing is set. The very conductive path through the casing increases the magnitude of the currents and has the tendency to average local sources over fairly large intervals. Current will flow between the sections that are predominently shaly and the sections that are mostly sandy. At the places where the current leaves the pipe, corrosive attack will occur. This same phenomenon will be present wherever unprotected pipe is set through sections that show large SP kicks on the electric logs over reasonably thick interval~. GENERAL- NATURE OF THE SPONTANEOUS POTENTIALS When a sequence of sedimentary rocks is penetrated by a drill hole filled with a mud which has a different salt concentration from that in the formation waters, various types of electrochemical potentials are established between the formations and different parts of the mud column. Opposite clean sand sections. a simple liquid-liquid junction potential will be observed; while opposite argillaccous formations, a membrane potential, often referred to as shale potential, will be established. The first quantitative analysis of these emf's in terms of liquid junction and membrane potentials is due to Wyllie.1

Jan 1, 1956

By F. Weinberg

Measurements have been made of solute segregation during dendrilic growth by using radioactive solute elements and ,measuring the activity of den(12-ites cut from decanted specimens. This has been done for both lead awl tin based binary alloys contaitzing the following solute additions: Ag, T1204, was dependet on ko, the equilibrium distribution coefficient in the following way Fay k &apos;c 0.1, C/C 0.6; for k0 >0.1. 0.6 <c,/c,< I. Qualitative obse?-vations were madc of dendritic segregation, by using autoradiographic techniques, for the Sn + Ag110 and Sn + Tlo4 systems. The observation were found to he in general agreement with the measurements ofCA/Co. Autoradiographic were also obtained of scctiolccl delzr11-iie stalks. These indicated that the stalks had a substructure, dclileated by solute corzetlt?atio?zs nlolg the substructure walls. A new dendrite growth direction <JI2> is reported for tila. SOLUTE segregation in dilute binary alloys has been investigated by Pfann,&apos; Smith, Tiller, and Rut-ter,&apos; and others. They considered the case of a slowly advancing plane solid interface, and derived expressions for the distribution of solute in both solid and liquid during solidification. To determine these expressions, they assumed no diffusion in the solid and either complete mixing in the liquid:&apos; or diffusion controlled solute movements in the liquid without any convective mixing.&apos; The present investigation considers solute segregation during dendritic growth, in which case the solid-liquid interface is not plane, and the growth rates are rapid. Segregation under these growth conditions has not been treated mathematically, because of the relative complexity of the system. It has been suggested by Chalmer, on the basis of preliminary results, that an alternative to the diffusion and heat flow controlled conditions during growth is &apos;diffusionless" dendritic growth in which solid is formed with the same composition as the liquid. He suggests this type of growth may depend upon a solvent-solute relationship that permits some solid solubility without excessive increase in internal energy, as is the case for solutions of tin in lead. On the other hand, Montariol,4 and others, have shown experimentally that some segregation does occur during dendritic growth in metals using etching and radioactive tracer techniques to indicate the concentrations of the solute. The present investigation was undertaken to determine, both qualitatively and quantitatively, the extent of solute segregation associated with dendritic growth in a series of binary alloys, as a function of solute concentration. PROCEDURE The solvent materials used were Vulcan Electrolytic tin (99.997 pct purity) and Tadanac lead (99.998 pct purity). The solute materials were Zn, Sn, and Sb (better than 99.998 pct purity), Ag and Co (99.5 pct purity), and T1 (Fisher "purified" metal sticks). Activation of the solute metals was carried out in the reactor at Chalk River, Canada. Master alloys were prepared by induction heating from the radioactive solute metal and the pure solvent, under argon, in graphite crucibles. Pieces of these alloys were then added to the solvent to give the required solute concentration. Dendrites were grown in essentially the same manner as that described by Weinberg and Chalmer, , in which controlled orientation single crystals were grown dendritically in horizontal graphite boats, and the liquid decanted. The crystals were grown and decanted in an atmosphere of tank argon. Before decanting, a sample of the liquid was drawn up in a glass tube and allowed to solidify rapidly. The orientations of the single crystals were such that <loo> was parallel to the growth direction, and (100) in the horizontal plane for lead, and [1101 and (110) respectively for tin. With these orientations long dendrite stalks formed along the bottom of the boat in the dendrite direction (<100> for lead and [I101 for tin) from which secondary branches grew. Only these secondary branches, which grew freely in the liquid from the dendrite stalk to the liquid surface, were used in the measurements. Accordingly, effects due to substrates and oxides on the surface of the liquid need not be considered. In order to measure the solute concentration C, of the dendrites, individual dendrite stalks were cut from the decanted specimens, remelted, and formed

Jan 1, 1962