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By C. Hays, R. E. Swift, E. G. Kendall

Investigations of the Zr-Pt system, by metallography, incipient melting, and X-ray diffraction, determined the phase relationshifis from 0 to 50 at. pct Pt. Phase fields in the Pt-~ich region were outlined, and three intermetallics (ZrPt, Zr2Pt, and ZrPtd were located. A eutectic between Zr and Zr2Pt, and a eutectoid veaction between Zr and a Zr + Zr2Pt, were established. The maximum solubility of Pt in P Zr was approximately 13.5 wt pct, as opposed to less than 1 wt pct solubility in a Zr. EARLIER work on the Zr-Pt system was limited to an X-ray study on the intermetallic compound, ZrPt3, by H. J. Wallbaum,1 It was reported that ZrPt3 existed at 86.52 wt pct Pt, and had a hexagonal structure, isomorphous with TiNi3. Wallbaum's data revealed the following structural particulars: a = 5.633A, c = 9.21A, and c/a = 1.635A. Other studies allied to Zr-Pt alloys concerned only 1) Pt-rich alloys (0.05 to 5.0 pct Zr) for corrosion resistance,2 2) a Zr-base alloy with 5 pct Pt and 0.124 pct C for oxidation resistance,3 and 3) electroclad-ding of Zr with Pt for in-pile corrosion resistance of Zr to uranyl sulphate. 4 Metallographic, incipient melting, and X-ray diffraction techniques were applied to accurately resolve the phase relationships in the 0 to 50 at. pct (68.2 wt pct) Pt region, and to outline the phase fields in the Pt-rich area. Three intermediate phases: Zr2Pt, ZrPt, and ZrPt3, were also established by the same methods. PROCEDURE Melting stock for this program was of the highest purity obtainable. The Zr was iodide crystal bar with a low hafnium content of about 0.05 wt pct (Westinghouse "Grade 3"). The as-received Zr was treated to remove the surface film of corrosion product that resulted from a standard autoclave grade designation test. Next, the bars were processed to yield material suitable for arc melting and free of contaminants. Sheet platinum metal (Baker and Co. "Grade 2") was used for alloying additions. This material con-

Jan 1, 1962

By E. H. Crabtree

This paper traces the experimental and pilot plant work completed by the authors since 1939 including the various methods which have been developed in applying coarse activated carbon to cyanidation. The methods and results developed by the authors in desorbing gold and silver from carbons are given and the possibilities for the re-use of the desorbed carbons are discussed

Jan 1, 1950

By P. W. Gilles, B. D. Pollock

THE pioneering work of Steinitz1 and Steinitz, Binder, and Moskowitz2 has shown conclusively the existence at high temperature of two additional phases in the molybdenum-boron system and thus brings to a total of six the number of structures appearing in this system. To the structures Mo2B, MOB, and Mo2B5 they have added MO3B2, a new -MOB form, and have shown that MOB,, which has the same range of composition as Mo2B5, is only a high temperature structure of the latter. This solid solution, interestingly enough, includes neither of the compositions corresponding to the stoichiomet-ric compounds, MOB, or Mo2B5, but rather at all temperatures has intermediate values of composition. These workers have also, in the course of their work, measured melting points, transition temperatures, eutectic and peritectic points in the system and have shown that Mo3B2, because of its dispro-portionation at low temperature to Mo2B and MOB, is stable only in a limited high temperature range. During the course of the present work on the vaporization properties of the molybdenum-boron compounds, a few transition temperatures were observed. When the report of the other workers appeared, it was decided to repeat, in part, their study of the system. As a result, considerable evidence has been obtained that substantiates the specific kinds of melting processes they report as well as the general features of their diagram. However, a marked difference was found between the temperatures they report and the ones observed in this study, with the latter being higher. The purposes of this paper are to present the evidence obtained in this laboratory that verifies their diagram of the system, to give some important temperatures in the system, to compare them with those previously published, and to seek an explanation of the difference. Samples The metal starting material was 400 mesh molybdenum powder with a purity stated by the manufacturer to be 99.9 pct. The initial treatment, designed to remove volatile contamination, consisted of heating in a vacuum for 10 min to a temperature of from 800" to 1000°C during which a loss of 0.3 to 0.4 pct occurred. An assay following this treatment showed it to be 99.4 pct pure, with the principal impurity probably being oxygen. The boron starting material was obtained from the Cooper Metallurgical Laboratories and the Fair-mount Chemical Co. as 325 mesh powder with manufacturers' analyses of 99 pct or better. Initial treatment consisted of heating in molybdenum in a vacuum at about 1700°C for 10 min. During this time a loss of 3.5 pct occurred. An assay following this treatment showed the different samples to have purities ranging from 95.5 to 99.0 pct with iron and carbon as the principal impurities. Following the initial treatment, the elements were combined to form stocks of Mo2B and MOB by heating pressed mixtures in a vacuum to 1100" to 1200°C to accomplish reaction and to 1500" to 1900°C for a few minutes to evaporate the more volatile impurities. Analysis of the two compounds for boron by a modification of the method of Blumenthal3 and for molybdenum by the lead-molybdate method indicated them to have purities greater than 99 pct. The individual samples to be studied had compositions in the Mo2B-MOB range and consisted of mixtures of the stock compounds. Procedure As is usually the case in high temperature work the selection of containers for the samples posed some problems. For vapor pressure studies tantalum crucibles, allowing little contact with the pressed samples, were used and some of the observations made during these experiments are pertinent to the study of the phase diagram. Most of the experiments, however, were performed in graphite containers, as were those of the previous authors. Two kinds of spectroscopic grade graphite crucibles were used. One was a % in. cylinder, 3/4 in. high, containing seven 3/16 in. holes drilled 1/2 in. deep into which were packed samples of the different mixtures weighing 250 to 500 milligrams. The other, consisting of separate crucibles, was prepared by drilling 3/16 in. holes, 1/2 in. deep into 1/4 in. graphite rods % in. long. The 7/8 in. cylinder was heated directly by induction while the small crucibles were packed in a tantalum heating element for induction heating. All heating was done in a high vacuum system in which the pressure was generally less than 1x10-5mm and never rose above 2x10-5mm when the samples were hot. The general pattern of the heating in graphite was to heat rapidly to a temperature somewhat below the desired one, then to raise the temperature slowly. The samples were held for 2 to 5 min at the maximum temperature, which in all cases was far higher than that needed to produce reaction. The short time was employed to reduce possible contamination by the crucible material and to reduce composition changes that would occur because of vaporization. After examination following the heating, the samples were reheated to a higher temperature. Temperatures were measured with a Leeds and Northrup disappearing filament optical pyrometer, certified by the National Bureau of Standards, by sighting through a window at the top of the vacuum

Jan 1, 1954

By Robert Pike

THE first authentic description of an iron bath for the deposition of iron is probably that of Bottger in 1846, who used a bath containing ferrous sulfate and ammonium chloride. In 1861, Kramer deposited iron from ferrous chloride solution. Electrolytic iron was produced in 1.869 by Bietz, who used it for making some magnetic tests. In the same year, Klein is said to have worked out his process. Jacobi1 in 1869 described the results obtained in electroplating with iron on copper for making dies and plates for bank notes, by Klein's process. A letter from Klein to Jacobi describes the bath more fully. It consisted of FeSO4 + (NH4)2S04. Lenz2 described ?some properties of electrolytically precipitated iron. He used Klein's bath, FeSO4 + MgSO4 + MgCO3, to neutralize and obtained fine-grained and hard iron. His conclusions were as follows: 1. Electrolytic iron and copper contain gases, notably hydrogen. 2. The volume of gas absorbed by iron varies within wide limits, but it is easy for iron to take up very considerable quantities of gas. 3. The absorption of gas is principally in the first formed layers of iron. 4. When iron is heated, gas begins to come off below 100°, principally hydrogen. 5. Heated to redness, reduced iron oxidizes in water, in part at least at the expense of the oxygen of the water, decomposing it and setting free hydrogen, which is partly or wholly absorbed. Siemens,3 in 1889, was the first to propose a general process embodying a step for leaching a sulfide mineral with ferric chloride or sulfate and a step for regenerating the leach and depositing iron on a cathode in a diaphragm cell. So far as is known, Siemens did not carry out his patent

Jan 1, 1930

PERSONAL (Members are urged to send in for this column any notes of interest concerning themselves or their fellow-members.) Members and guests who registered at Institute headquarters during the period Oct. 10 to Nov. 10, 1914: Jintaro Kojima, Ashio, Japan. E. R. Hinckley, Seoul, Korea. J. Homer Stover, Trenton, N. J. S. A. Taylor, Pittsburgh, Pa. Kirby Thomas, New York, N. Y. Lawrence Addicks, Douglas, Ariz. Keijiro Nishio, Tokyo, Japan. Noel Cunningham, Bethlehem, Pa. Alexander K. Hamilton, Chicago, Ill. E. C. Vigeon, London, England. Harold N. Lawrie, Portland, Ore. S. E. Fairchild, Jr., Philadelphia, Pa. C. Spence Thomas, Cardiff, Wales. W. C. Schmidt, Jr., New York, N. Y. Henry Tackmann, New York, N. Y. Kenneth C. Browne, New York, N. Y. Dr. David T. Day has resigned his position with the U. S. Geological Survey and opened an office at 1331 F Street, N. W., Washington, D. C., for practice as a consulting engineer.

Jan 12, 1914

By Sir Robert Hadfield

Introduction.-I esteem it a great honor to be asked by this Institute to give them an address chiefly devoted to metallurgy. While it is with great regret that I find myself unable to be present to deliver this in person, I take this opportunity of wishing your society every success in its continued career of usefulness to the metallurgists of the great Republic. To be elected, eight years ago, along with Dr. J. E. Stead, F. R. S., as one of your Honorary Members, was a privilege which I greatly esteemed, for I consider that no society in America has done so much as ours for the advancement of metallurgy. Those who have Served our Society.-Where many have served so well, it is difficult, without appearing to make unavoidable distinctions, to select names from those of your members who have done so much for the cause we have at heart-the advance and progress of metallurgy. As typical, however, and not in any way meant as a complete list, there are among others the following names which in the past and to-day stand out prominently in this science of ferrous metallurgy. With most of those now mentioned I have personally come in contact, or by correspondence in some few cases, and have exchanged views, since I first came over to America 30 years ago. Holley; Jones; Weeks; Andrew Carnegie; Thomas Carnegie; Fritz; Sterry Hunt;. Egleston; Maunsel White and Taylor, who did so much for high-speed tool steel, and helped to revolutionize machine-shop practice; W. J. Taylor; Robert Hunt; Alfred Hunt of Pittsburg, who did so much in the early history of aluminum, and, alas! did. not live to see the wonderful progress which has been made in that particular branch of metallurgical industry; James Douglas; C. B. Dudley; Birkinbine; Howe; Metcalf; Barus; Langley; Raymond; P. H. Dudley; H. H. Campbell; W. R. Webster; E. D. Campbell; Talbot; Spilsbury; Gayley; Dinkey, under whose supervision and responsibility modern armor has been so successfully produced in this country, which the writer can testify from personal knowledge of , test results possesses very high Figure of Merit; Schwab; Kennedy; Wellman; Garrison; Wood; Moldenke; Webster; Swank; Unger; Richards; Sauveur; Strat-

Jan 5, 1914

By Robert Mehl

IN examining the progress of metallurgical science, the critic must remember that most of our present knowledge of metals and alloys has been accumulated through the needs of industry and commerce rather than through the desire and efforts of a large body of scientists interested primarily in developing a science of metals. The progress of metallurgy, scientifically speaking, has been irregular, and little given to the exhaus-tive exploitation of important scientific fields. The experienced engineer now recognizes the need for the development of the basic science upon which his engineering rests. In addition to the increase in knowledge which results from the normal requirements of industry, a development of the basic science of the behavior of metals and alloys is as desirable in metallurgy as in any other branch of science and engineering. The continued growth of the science of metals-as of every other science-requires studious attention to the principles that underlie the behavior of matter, with the result that knowledge in the several fields of interest should continue to increase. Among the various subjects recognized as important in physical metallurgy few have a wider significance than that of diffusion in solid metals. The phenomena of diffusion are intimately related to many basic problems of the metallic state, but in addition to this, the process of diffu-sion is of first importance practically. The formation of alloys by the annealing of mixed powders, first practiced by Faraday and Stodart81 in 1820 and in more recent years investigated by Masing187,189 and others, has led to the development of special alloys like Carboloy, Vascoloy-Ramet, Genelite, Elcon68, and has recently been applied to the production of noble-metal alloys for electrical contacts"'.

Jan 1, 1936

By C. J. McHargue, J. C. Ogle

Lightly deformed columbiun single crystals which contained only parallel hoins or purullel and intersecting trains were annealed at 1000' and 1600"C. No re-crystallizntion occurred in specimens hawing only parallel twins. Only noncoherent twin boundaries nzipated at 1000°C but both coherent and noncoherent ones moved al 1600°C. Recrystallization occurred within a few minutes at twin intersections at 1000°C. The orientation 01 the recrystallized grains differed front that of both the matrix and deformation twins, but could he derired by (110) and/or(112) rotations. ALTHOUGH twinning in metals has been extensively studied, there have been no definitive studies of the annealing behavior of crystals containing deformation twins. Some effects observed after annealing deformation twins have been summarized by Cahn1 and Hall2. Any or all of these phenomena are observed: 1) The twins may contract so that the sharp edges of the lens become blunted, and eventually the twin may disappear entirely. 2) The twins may balloon out at an edge, giving rise to a large grain having the same orientation as the twin. 3) The specimen may recrystallize; i.e., new grains are nucleated and grow at the expense of the twins and the crystal immediately adjoining the twin. Such grains have orientations which are not present before. Contraction has been observed in iron,3 titanium,3, 4 beryllium,5 zinc,8, 7 Fe-A1 alloy,' and uranium.9 Long anneals at high temperatures are required to have any appreciable effect in these metals and only thin twins are absorbed. Lens-shaped twins are absorbed from the edges: the thin, almost parallel-sided twins are usually punctured in several places and each piece contracts independently. Absorption is very gradual and no sudden cooperative jumps have been observed. The expansion of a twin into a larger grain of identical orientation is unusual, but such growth has been observed in iron,"'" zinc,6 and uranium." Crystals which have been deformed simultaneously by slip and twinning recrystallize first in the area adjacent to the twin. New grains appear faster where the twins intersect: but isolated twins, especially if thick, can also give rise to new grains. This type of recrystallization occurs in zinc.6, 7, 12, 13 and beryllium.14 Reed-Hill noted, in a single crystal of magnesium, the nucleation of a recrystallized grain at a twin intersection which had the same orientation as the second-order twin and which grew into the highly strained matrix.15 Short-time annealing has been reported to cause no change in the deformation twins in vanadium,16 columbium, 17, 18 tantalum,19 tungsten,'' and zinc.7 The purpose of this investigation was to note the effects of annealing on the coherent and noncoherent boundaries of deformation twins in columbium and to locate the nucleating sites for recrystallization. The orientation relationships, which the new recrystallized grains have with the parent crystal and the deformation twins, were also determined. EXPERIMENTAL PROCEDURE Single crystals of columbium were obtained by cutting large grains from electron-beam-melted buttons which contained 10 to 50 ppm C, 10 to 100 ppm O,, 1 to 10 ppm H2, and 10 to 15 ppm N2. The crystals were hand-ground and chemically polished until all grain boundaries were removed. The specimens were mounted in an epoxy resin and a face of each crystal was mechanically polished on a Syntron polisher using Linde A and then Linde B polishing compounds. After all faces were mechanically polished, the crystal was electrolytically polished to remove all distortion due to cutting and grinding. Laue photographs were taken of all faces of the crystals to determine the quality and orientation of each crystal. The crystals were compressed about 10 pct at -196 C in a specially constructed compression cage with an Instron tensile machine. Each crystal was separated from the top and bottom anvils by teflon films which acted as a lubricant. With the specimen crystal in position, the entire cage was cooled to -196°C by being submerged in a Dewar containing liquid nitrogen. The crystals were compressed at a rate of 0.02 in. per min and the load was recorded on a strip-chart recorder. After deformation the crystals were mechanically polished on 600-grit paper and Pellon cloth with Linde A and Linde B polishing compounds. The crystal faces were chemically polished and then etched. The twin planes were identified metallographically from an analysis of the twin traces on two surfaces. Annealing was carried out by placing each crystal in a columbium bucket made from the same electron-beam-melted material as the crystal itself and suspending the bucket by a tantalum wire in a quartz tube. After a vacuum of 10-7 Torr was attained, a furnace at 1000" or 1600 C was raised into position and the crystals held for various lengths of time. The crystals were repolished and etched after annealing to remove any surface contamination. Approximately 0.010 in. was removed during this process. The resulting surface was examined metallographically for microstructural changes due to annealing. A microbeam Laue camera mounted on a Hilger Micro-focus X-ray unit was used to determine the Orientstions of the recrystallized grains. This X-ray micro-beam camera had a 0.002-in.-diam collimator and incorporated the ideas of both and and chisWik21 and Cahn.22

Jan 1, 1967

By P. Douglas, G. M. Leak, B. Mills

The sinusoidal surface relaxation technique has been used to measure the surface self-diffusion coefficient of spectroscopically pure nickel over a wide temperature range under a hydrogen atmosphere. A kink in the Arrhenius plot has been observed. In the temperature range T/T 0.98 to 0.80 (T in O K and T, is the melting temperature) the average self diffusion coefficient is given by Below the temperature T/T,- 0.80a decrease in the slope of the log Ds us 1/T plot is observed. This is associated with a diffusion process characterized by a lower activation energy (-20,000 cal mole'') and smaller preexponential term (-10- sq cm sec"). A series of experiments were carried out at T/Tm = 0.61 under a hydrogen atmosphere of higher oxygen partial pressure than for the rest of the experiments. It was found that Ds was significantly depressed due to oxygen adsorption. This evidence supports the opinion that the low temperature process (activation energy -20,000 cal mole-') is unlikely to be due to oxygen adsorption. An interesting feature of the present data is that the transition temperature (T/Tm - 0.80) is a function of orientation. For a small number of crystals of measured orientation the transition temperature was observed to be higher towards the low index (100) pole. Theories of surface diffusion are briefly reviewed and it is concluded that the present reszuts are best explained by invoking a surface roughening process. GJOSTEIN has recently analyzed available surface diffusion data for a wide range of metals. He suggested that two mechanisms were operative for fcc metals, an adatom process at high temperatures and a vacancy process at low temperatures. Results for nickel can be summarized as follows. At low temperatures (T/T, - 0.3 to 0.44) under ultra high vacuum conditions, Melmed2 measured an activation energy Q of 21 kcal mole-' using field electron emission microscopy. At higher temperatures (T/T - 0.7 to 0.9) under a vacuum of 10- ' torr, Maiya and lakel measured y as 39 kcal mole-' using the multiple scratch smoothing technique. The present work was undertaken to try to find out if two distinct processes could be observed. High temperature results give Q about 47 kcal mole-': there is evidence also for a low temperature value of about 20 kcal mole-'. These measurements were all made under a hydrogen atmosphere, in the temperature range 860" to 1412°C. Concurrent with the present study Bonze1 and jostein> have also observed a break in the Arrhenius plot for the (110) surface of nickel. These measure- ments under ultrahigh vacuum conditions using the laser diffraction technique are in excellent agreement with the work reported here under hydrogen annealing conditions. THEORY The available surface relaxation techniques include single and multiple scratch smoothing and grain boundary grooving. The processes have been compared in detail by Gjostein for conditions where surface diffusion dominates6 and Mills et al? where volume diffusion dominates. In summary the relevant points are as follows. Grain boundary grooving gives an average Ds for the two surfaces adjacent to the boundary and this can, to some extent, be simplified by using symmetrical bicrystals. This technique has been used to study the effect of environment on Ds for silver and copper.'-'' Scratch techniques yield Ds values for the small orientation range exposed by the scratches (-2 deg). The multiple scratch process is preferable because the profile rapidly becomes sinusoidal and can then be interpreted theoretically in a relatively simple way. Also corrections for mass transport processes other than surface diffusion can be introduced easily. Mullins" considered a sinusoidal profile described the wavelength of the profile. After time t the profile can be described by the equation The terms A, A', C, and B which account, respectively, for contributions due to evaporation-condensation, diffusion through the gas phase, volume diffusion through the lattice, and surface diffusion are defined as: where Ds = the surface self diffusion coefficient ys = the surface energy per unit area p = the equilibrium vapor pressure over a flat surface pa = the equilibrium vapor density over a flat surface DG= the diffusion coefficient of vapor molecules in the inert gas DM = the mass transfer diffusion coefficient which for a pure cubic metal is Dv/f where Dv is the radiotracer diffusion coefficient and f is the correlation factor H = the molecular volume V = the surface density of atoms, il2'3 M = mass of an evaporating molecule

Jan 1, 1970

By E. M. Murphy

(Presented by invitation at a meeting of the Spokane Local Section of the Institute, Feb. 17, 1912.) EIGHT years ago the Hecla mine, a lead-silver producer, situated at Burke, Idaho, was producing ore from but two levels, the 300- and the 600-ft. All hoisting was done with a 12- by 16-in. slide-valve, double-reel, hoist. The hoist was being worked to its capacity and was unsuitable for hoisting from greater depths. As the work of opening a new level was about to be started, it became necessary to remodel the then-existing equipment or install a new hoist. The recent advent of electricity from Spokane had made available a cheaper power than steam. By a series of tests conducted throughout the Coeur d'Alène district, it was found that it cost $109 per year to generate a horse-power with steam. Electric power was to be had for $50 a horse-power per year. It was decided to substitute for the engines a motor-drive, of sufficient capacity to operate from the 900-ft. level, and ultimately install an entirely new hoist. After disconnecting the engines, installing a new shaft, and making a few minor changes, a 300-h-p., 2,300-volt, 514-rev. per min., variable-speed motor of the induction type was geared to the reel-shaft. The reels were supplied with 3/8 by 4-in. flat rope, and the duty of the hoist was about as follows: Cage, 1,700; ore, 2,600; car, 1,400; rope, 2,250; total, 7,950 pounds. The Bristol ammeter chart, Fig. 1, shows the combined current-consumption of the hoist- and mine-motors. The large intermittent load is clearly shown ; this produced harmful fluctuations in the voltage of the long, lightly-loaded, 60,000-volt transmission-line from Spokane to the Coeur d'Alènes. The power company received no compensation for the increased cost of producing power for this intermittent or fluctuating load. In order to protect its system from similar excessive

Sep 1, 1912

By J. C. Yannopoulos, N. J. Themelis

Ah electronic thermogravirnetric balance was used to measure the veductioiz rule o single cirpric oxide particles suspended in a stream of hydrogen. Very jzne thermocouples embedded in lie center and at the surface of the sphere recorded the variation of terw perature during reduction. In contrast to iron oxide reduction, where in most instances the rate of interface reactiokl is controlling, the heat- and mass-transfer phenotnena play a predolrinant role in the reduction of cupric oxide. The correlation of experitnental data or tnass lransfev lhrough the boundary layer at Reynolds nunlber 0-4 50 was as jollocs: ThE reduction of cupric oxide by hydrogen is represented by the equation: It is a highly exothermic reaction and the amount of heat released varies only slightly with temperature (-21,430 cal per g-mole at 400°C). Most of the published studies on this system have been conducted at temperatures in the range of 34 to 280c.l-&apos; The concensus of opinion has been that at temperatures below 200°C the reaction is preceded by an induction period during which there is very little or no reduction. The length of this period diminishes as the temperature of the reaction is increased1l5 and aseawa found that at 280°C reduction starts practically immediately when the oxide is exposed to hydrogen gas. The existence of an induction, or incubation, period has led experimenters to believe that the reduction of CuO by hydrogen is catalyzed by metallic copper.&apos; Boldurev and rmolaev found that mechanical additions of powdered copper to oxide did not affect its reduction, although metallic copper produced during the reduction seemed to have a catalytic effect. At least three other authors2&apos;5&apos;7 have reported that addition of copper had no effect on the rate of reduction. Pease and alor&apos; observed that water vapor had a strong inhibiting effect on the reduction at 1503C, but its effect was greatly diminished at 200 C. Pavlychenko and Rubinchik5 studied this reaction at 159 to 235 C and found that, once the reaction had been initiated, there was no inhibiting effect due to the introduction of water in the hydrogen stream; at temperatures above 183°C there was no inhibiting effect due to water vapor, either before or during reaction. The same authors noted that the rate of reduction was independent of pressure in the range of 200 to 700 mm Hg. aseawa investigated the kinetics of the CuO-Hz system at 160 to 280°C and estimated the apparent activation energy at 14,000 cal per g-mole. A similar value (13,500 1200 cal per g-mole) was reported by ond&apos; in the temperature range 148 to 216°C. Bond also reported that there was no incubation period and that water vapor had no inhibiting effect on reduction at temperatures above 190 C. The above studies have been conducted at temperatures below 280°C and the physical configuration of the system under investigation has not been defined adequately. However, it is well-known that the mechanism of gas-solid reactions depends on a number of in series physical and chemical rate prcesses.&apos;&apos; It is, therefore, essential to include among the experimental factors the geometry of the solid system and the mass-transport characteristics of the reducing gas. Scott studied the reduction of packed beds of cupric oxide cylinders by Hz-He streams of very low hydrogen concentrations at temperatures 400 to 600 C, pressure of 10 to 30 atm, and gas velocity from 0.18 to 5.8 ft per sec (3 < Rep < 30). The reduction rate was found to be mainly controlled by diffusion through the boundary layer and through the pores of the reduced copper phase. The following correlation was proposed: Scott in an earlier work studied the reduction of fixed beds of cupric oxide wire and found that the rate of flow of the gas stream through the bed had a controlling effect on the rate of reduction. The same mass-transfer phenomenon was observed by Bond and clark13 on a similar reduction system. The analogy between mass and heat transfer through the boundary layer which exists between a solid surface and the bulk stream stems from the similarity of the differential equations representing these phenomena

Jan 1, 1967

By N. Brown

IT has been observed that a hexagonal-close-packed crystal will undergo the same macroscopic displacements as an isotropic material if the basal plane is perpendicular to the axis of twist.&apos; Other orientations may produce both bending and twisting, but this analysis will be confined to pure torsion of a right circular cylinder. The z axis, the axis of twist, and the specimen axis are coincident. The displacements are given by Uq = rz, Ur = Uz = 0 [1] where 4 is the angle of twist per unit length. This requires rotational slip, as discussed by Frank&apos; and Wilman, which may be observed readily. The relative rotation of adjoining slip planes is simply produced by a movement of a planar grid of screw dislocations."." The screw dislocations are of the same sign and they move radially inward. For hexagonal-close-packed metals, the grid is hexagonal and the screw dislocations lie in the < 2110 > directions. The displacement of a point is the resultant of two displacements produced by intersecting screws sweeping over the point. The dislocations must pass over the point (r, o) in such a manner that its resultant displacement corresponds to the observed macroscopic displacement. If 6&apos; is measured from the [1010] direction, then for 0 < ? < ~/3, only the [1210] and 121101 type screw dislocations are needed to produce the required displacement. If n1 screws of type [1210] and n2 of type [2110] pass over a point, then, in order that Ur = 0 n, sin ? - n2 sin (/3 — 6&apos;) = 0. [2] If the tangential displacement is to be independent of 0, then n1 cos ? + n2cos (/3 —?) = N [3] where N is independent of ? and thus depends only on r. Nb is the tangential displacement where b is the Burgers vector. Since U? is a linear function of r, then N must be a linear function of r. If a2 is the outer radius and a, is the inner radius to which the plastic deformation has extended, then N = Nm2 r-a1 [4] This function meets the conditions that at

Jan 1, 1956

By W. H. Bassett

IN the commercial annealing of cartridge brass there are four points regarding which definite data are essential. They have to do with the correct interpretation of grain count in its relation to annealing temperature and, incidentally, to Brinell hardness. These points are: 1. The comparison of the grain sizes of two cartridge-brass mixtures: 69 copper, 31 zinc, 0.376-in. (9.5-min.) gage; and 68 copper, 32 zinc, 0.130-in. (3.3-mm.) gage. 2. The comparison of the grain sizes of annealed metal that had previously been reduced by rolling varying amounts; for instance, 20.0, 36.6, 50.9, and 59.1 per cent. 3. The determination of standards for grain sizes on annealed brass of the composition 68 per cent. copper, 32 per cent. zinc and 69 copper, 31 zinc. 4. The comparison of grain size with Brinell hardness on identical samples of annealed metal. In their comprehensive and thorough investigation of the recrystallization of cold-worked alpha brass on annealing,1 Mathewson and Phillips have discussed the relations between temperature of anneal, degree of deformation, and structural alteration in alpha brass. They have also shown certain comparisons between the ordinary physical properties and the grain size of annealed brass. The purpose of the present investigation is mainly concerned with the grain size of cartridge brass, its relation to Brinell hardness, and the publication of sufficient data to enable those engaged in the inspection of such material to have a correct foundation upon which to work.

Jan 1, 1919

By S. D. Dahlgren

The plasticity of unalloyed P plutonium was studied by evaluating the strain-rate-hardening exponent, m, in the equation Values of m up to 0.33 and tensile elongations up to 680 pct were obtained for ß plutonium formed directly from the a phase. Casl bars that were cycled and tested had lower flow stresses and higher values for than uncycled bars , hut their total plastic elongations were not as great as expected because of premature failure at voids formed during cycling. Flow stresses were higher and m was lower (m = 0.15) for 9 plutonzutn formed from the y phase. ThE strain-rate-hardening exponent for plastic flow of p plutonium was determined as a function of strain rate, test temperature, and heat-treating history, and it was related to the rather large plastic elongation found previously for some plutonium tensile samples. Gardner and ~ann&apos; obtained tensile elongations of up to 620 pct for P plutonium samples which had been completely transformed from the low-temperature a phase to the P phase before testing. Such a large percentage elongation is unusual for unalloyed metals or single-phase alloys.&apos; The a phase is stable below approximately 112°C and (3 is stable between approximately 112" and 190"c.~ Both phases have mono-clinic structures. A temperature of 160°C is 0.58 of the effective absolute melting point, 475°C) of the p phase. The effective melting point is obtained by considering the enthalpy and entropy changes associated with the higher-temperature phase transformations and it is not the same as the experimental melting point of the highest-temperature allotrope of unalloyed plutonium. Nelson, Bowman, and Bierlein observed a striking difference between the ductility, as well as other mechanical properties, of p plutonium formed from the next higher-temperature phase (y) and the ductility of /3 plutonium formed from the a phase. The total elongation of /3 plutonium formed from the y phase was less than 5 pct. Earlier, the creep rate of 13 plutonium formed from the a phase was shown to be 200 to 500 times faster than the rate for 0 formed from y for the same test temperature and stress.

Jan 1, 1969

By O. J. C. Runnalls, L. M. Pidgeon

Some observations on the kinetics of the iodide process are reported. The deposition rate is geometry-sensitive in a system containing a finely divided titanium charge. Further, results indicate that the iodine diffusion rate influences the velocity of the process. The nonvolatile iodide, Til,, forms in the hot filament zone, thus removing iodine from the cycle. TITANIUM metal of 99.9 pct purity may be prepared using a refining technique originated by Van Arkel and de Boer.&apos; The purity of this metal, commonly called iodide titanium, exceeds that produced by any known process. In a recent application, the method was employed by Gonser et al.² to prepare titanium rods up to 2 to 3 cm in diam. In the Van Arkel-de Boer system, the relative influence of the fundamental mechanisms: l—production of titanium iodides, 2—gaseous countercurrent diffusion, and 3—decomposition, on the deposition rate have not been clearly established. Blocher and Campbell" have indicated that the controlling step in the process under practical conditions of operation may be the reaction rate of iodine with the crude metal. Fast&apos; reported that crude titanium metal reacted with iodine rapidly, even at room temperature, in his apparatus. Little has been reported on the effect of gaseous diffusion or decomposition on the deposition rate. It is these aspects of the process about which this investigation is centered. An attempt has been made to separate these latter effects from those due to the formation of the iodides at the crude metal surface by a division of the experimental program. Reaction of Iodine with Titanium Apparatus: In the investigation of gas-metal reactions of this type, the chemical reactivity of the halogen and halide vapors dictates the use of all-glass apparatus. In such a system standard techniques for measuring reaction rates are difficult to employ. Here, a simple apparatus was devised (Fig. 1) so that some indication of the reactivity of titanium powder with iodine vapor could be obtained. A stream of iodine gas was evolved from a bulb of controlled temperature and passed over a sample of titanium powder heated in a horizontal tube furnace. The product of the reaction, TiI4, volatilized and was condensed outside the furnace in a series of four glass bulbs, each cooled to room temperature in turn. Preliminary experiments indicated that distillation was retarded in a sealed evacuated system due to a pressure build-up in the condensing end of the apparatus. Hence, the system was pumped continuously using a mechanical pump and two oil diffusion pumps in series, through a liquid air trap. The iodine bulb was made large and a capillary restriction was inserted between the titanium bulb and the condensers so that the iodine pressure over the metal would approach the equilibrium pressure over solid iodine crystals. The effect of this restriction on the evaporation rate of TiI4, was determined separately. The iodine bulb was heated in an oil bath controlled to ±2°C. The titanium bulb temperature was automatically controlled to ±5°C. Procedure: About 200 mg of —30 mesh titanium powder, weighed to 0.1 mg, was placed in the reaction bulb after part B had been joined to part A. The powder was tapped into a long (5 cm) shallow mass along the bottom of the tube. Two chromel-alumel thermocouples were inserted into the magnesium radiator which was clamped to the reaction

Jan 1, 1953

By M. Semchyshen, A. P. Coldren, W. G. Scholz

A survey of the Fe-Mo-B system was made to determine the extent to which boron might affect the microstructure and strength properties of iron-rich Fe-Mo alloys. Seventeen vacuum-induc tion melted ingots were prepared with approximate mo-lybednum contents 01 2, 4, 9, and 19 wt pct and approximate boron contents of 5, 14,50, and 630 ppm by weight. Phases extracted from annealed specimens and identified by X-ray diffraction analysis included E Fe3MO2, Mo2FeB2, and an oxide hazling a diffraction pattern practically identical to that of MnFez04. Three types of alloy strengthening were observed: a) Fe-2 pct Mo-B alloys were hardenable by a bainitic-type transformtion of austenite to ferrile; b) Fe-4 pct Mo-B alloys were hardened by the solid-solution mechanism; and C) Fe-9 pct Mo-B and Fe-19 pct Mo-B alloys were hardened by precipitation of the E Fe3Moz phase. Boron was observed to have a very strong hardening effect in the Fe-2 pct Mo alloys and a mild strengthening effect on the 1200°F properties of the Fe-4 pct Mo alloys. In the Fe-9 pct Mo alloys there was no consistent effect of boron on strength at either room temperature or 1200° F. The Fe-19 pct Mo alloys were so brittle that meaningful tensile or creep-rupture data could not he obtained. No dispersion hardening from borides was recognized in any of the alloys. THE high-temperature properties of iron-rich Fe-Mo alloys were studied by Reiter and Hibbard.&apos; They found that the strength of the alloys increased markedly as the molybdenum content was raised from 0 to 15.9 pct by weight. The authors explained the various degrees of strengthening in terms of a) solid-solution strengthening, b) strengthening from a martensitic-type transformation, and C) precipitation strengthening. The objective of the present investigation was to conduct a survey of the iron-rich portion of the Fe-Mo-B system to determine whether the beneficial effects of molybdenum on the strength of iron can be enhanced by the presence of boron. It was thought that perhaps fine dispersions of molybdenum- rich borides would be found which could improve the high-temperature strength of ferritic alloys beyond the strengths attainable by molybdenum additions alone. Also, it was considered worthwhile to study the effects of boron in alloys which are essentially free of carbon. Most, if not all, of our present knowledge about boron in high-temperature alloys pertains to alloys containing carbon and carbides. EXPERIMENTAL PROCEDURES Alloy Preparation. Seventeen 8-lb ingots were prepared from electrolytic Plastiron, unalloyed molybdenum chips, and boron powder by a vacuum-induction melting procedure employing hydrogen as the main deoxidizer. The alloys were melted in alumina crucibles using 35-lb melts, with each melt being split four ways to achieve varying boron contents within four Fe-Mo base compositions. The results of chemical analyses conducted on chips machined from the chilled ends of the ingots are presented in Table I. The boron analyses were performed by a spectrographic method utilizing primary standards prepared from boric acid. They indicated that in ingots to which no boron was

Jan 1, 1964

By J. VAN DEN BERC

Tin production and export from the Far East are still a long way off from the prewar figures. The Malayan Peninsula, which had a rather good start directly after the war largely because of stock piles found in Singapore and elsewhere, has since been hampered in the rehabilitation of its tin mines and dredging operations by material shortages and, more recently and more severely, by revolts and attacks of communist elements and gangster bands. These hindrances make working in the mines dangerous and form a daily threat against the valuable and highly vulnerable dredges. Contrary to the conditions in Malaya are those on the tin islands of Billiton, Banka, and Singkep-all in the Netherlands East Indies-where the Dutch have re-established peaceful relations with the population. Dutch efforts since the fall of 1945 have been rewarded by continuously increasing production, extension of production facilities, and return of moderate prosperity, complete safety, and all-out co-operation among the population ? native and Chinese ? to the benefit of all concerned.

Jan 1, 1949

By George D. Roberts

INTRODUCTION CIVIL engineers are primarily interested in maximum core recovery. This is even more important in foundation work than in mining investigations where sludge samples are of some value. The soft materials, such as clay, gouge, or partially decomposed seams that are most readily ground up or washed away, are the materials that usually have the greatest influence on foundation and leakage conditions. Undisturbed samples of such materials should be obtained for detailed geological examination and laboratory tests. Therefore the attainable goal of sampling in connection with foundation investigations is the recovery of 99.9 pct of undisturbed core. FACTORS CAUSING CORE LOSSES The principal factors contributing to core losses are: (I) coring badly fractured or very soft material; (2) use of improperly designed coring equipment, including the use of bits of too small a diameter; (3) lack of the proper training and attitude on the part of the drillers and pertinent technical information on the part of the supervising personnel. Little can be done about the character of the material being cored but the other two factors contributing to unsatisfactory performance can be corrected. Although the title of this paper is the improvement and standardization of core barrels, it is believed that the drillers&apos; shortcomings and the lack of pertinent technical literature are more detrimental to good core recovery than either of the other factors. USES FOR LARGE DIAMETER CORE BARRELS It is well known that the use of larger diameter bits and core barrels generally produce better cores, particularly when sampling soft or broken material. The use of larger and larger bit diameters and the insistence on better core recovery is well demonstrated by the change in practices of the various districts of the Corps of Engineers. Today NX core is the smallest diameter commonly permitted for investigational work and the more active districts are using coring bits up to 6 in. in diameter, as well as 36 and 40-in. calyx rigs. The latter size has proved to be just as economical because it provides more room for core removal and cleanup operations. The use of large diameter cores to replace the driving and jacking methods of obtaining soil samples is also increasing. The 5 7/8-in. Denison sampler, developed by H. L. Johnson to obtain samples from soft formations, is one example. The principal uses for bits larger than NX are: sampling soils and semi-consolidated rock; sampling decomposed rock or rock with soft seams; sampling concrete; obtaining samples for laboratory tests; drilling drainage holes, and other miscellaneous work. CORE DRILLING PRACTICES OF SEVERAL ENGINEER DISTRICTS Little Rock District The writer was employed in the Little Rock District from 1938 until 1942. Prior

Jan 1, 1947

By R. C. Edwards, Will Mitchell, T. G. Kirkland

THREE years ago, when the Process Research Laboratory at Allis-Chalmers Manufacturing Co. sought a remedy for the increasing cost of disposing of great quantities of spent sands from foundries, R. C. Edwards developed a continuous inclined paddle scrubber which removed a substantial amount of the charred coatings from the grains with a surprisingly small amount of degradation of the sand itself.1 The satisfactory results obtained on foundry sand, using this piece of equipment in conjunction with classification, suggested that a similar procedure could probably be applied to the cleaning of other sands, such as those required by the glass and chemical industries. This paper describes the flowsheet and the results of tests performed on impure natural sands. The four materials tested were silica sands obtained from widely separated geographical areas. Three of the sands tested contained various amounts of iron oxide and the fourth an excessive amount of calcareous bonding material. The iron oxide was present predominantly in the form of grain coatings, which were scuffed by the paddle scrubber, and in all cases a product was manufactured which would meet one of the sets of specifications imposed by the glass industry&apos; The Edwards paddle scrubber used in these tests consists of a rubber-lined steel cylinder 18 in. in diam and 48 in. long, mounted on a frame so that its slope can be varied 5 ° to 35º from horizontal. This variable slope permits controlled flow of material through the machine. Rubber paddles rotate inside the cylinder and are secured to a center shaft 2 in. square, which extends through the entire length and is turned at both ends so that it can be supported by sleeve bearings centrally fixed in the end plates of the shell. At the upper or feed end it extends through the bearing on the end plate into a sheave, to which the motor drive is connected by means of Texrope transmission. The four sets of paddles mounted on the shaft, two in each set, are made of rubber belting, 1/4 in. thick, 9 in. wide, and 16 in. long. The two paddles in each set are secured on opposite sides of the square shaft, but in the same longitudinal position along the shaft axis. In other words, the two paddles in the set operate 180° apart. Each successive set is mounted 90º from the preceding one. One end of each paddle is bolted to the square shaft and the other weighted by a steel bar, 1x1 ½ x9 in. long, which is attached about 1/ 2 in. from the outer tip of the paddle. By centrifugal force at proper shaft speed, these weights force the paddle surface to rub smoothly against the rubber lining of the cylinder. During operation, the sand forces its way between the paddle face and the surface of the cylinder, providing the necessary abrading action as the pulp flows by gravity down the length of the cylinder. The capacity of the machine is limited by the amount and the hardness of the coating material and by the quality of product desired. The degree of scrubbing is governed by the retention time in the scrubber, which in turn may be changed by varying the feed rate, water content of the feed, and

Jan 1, 1952

By Oliver Bowles

A NORTH CAROLINA miner dreamed that he found high-grade mica by excavating a certain corner of his mine. The next day he sank a hole on the exact spot and found mica of excellent quality. The dream came true. May not this be as good a method as any yet known for forecasting the valuable mineral content of pegmatites? The Federal Geological Survey has found in its recent detailed studies in New England that good sheet mica occurs most abundantly in zoned pegmatites, particularly in zones lying along the wall or contact of the pegmatite mass. Although this conclusion may be a valuable guide, pegmatite mining operations must still be classed as most uncertain and hazardous enterprises. Finding of the second largest diamond ever discovered in the United States-a stone of good gem quality weighing more than 34 carats-during the course of a horseshoe pitching contest at Peterstown, W. Va., is another example of unorthodox mining methods. These should not be considered, however, as characteristic mining methods developed in 1944.

Jan 1, 1945