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By A. W. D. Hills, M. R. Moore

An apparatus has been developed in which metals can bc solidified under closely controlled unidirectional heat flow conditions. The metals are cooled by a multiple-air jet system, designed so that the heat transfer coefficient is uniformly distributed over the cooled surface. They are contained in a special furnace system of low thermal mass which enables unidirectional heat flow conditions to be rigorously maintained for certain specific cooling rates. This apparatus has been used to study the solidijication of pure lead and pure tin at zero superheat, solid metal thicknesses being determined by thermal analysis, and by dipstick readings. Detailed thermal balances have been drawn up on the experiments in order to determzne the cooling conditions that most rigorously correspond to unidirectional heat flow. Solid metal thicknesses, measured experimentally for these conditions, have beetz shown to agree closely with the theoretical wedictzons of different integml-profile methods. lt is concluded that any errors inherent in the integval-profile method are no greater than the errors inherent in experimental investigations of solidification. A knowledge of the influence of heat transfer rates on the solidification of metals is essential to the understanding and control of industrial casting processes. Since very few formal methods are available for solving the heat conduction equation under solidification conditions several authors have developed approximate techniques for doing so. One of the most promising is the integral-profile technique that has been used by Goodman,1 Hills,2,3 Tien4 and Hills and ~oore' to predict solidification rates under certain specific heat transfer coniditions. In the first of this present series of papers6 Hills has further generalized the method and developed a universal integral-profile technique that can be used to predict solidification rates under a wide variety of unidirectional heat flow conditions. Since the method is approximate it is necessary to investigate the accuracy with which it predicts actual solidification rates. A review of the literature7 shows that solidification rates have seldom been measured under accurately known heat transfer conditions and it was therefore decided to develop experimental techniques that would enable this to be done. Results obtained would then be available as a check on the approximate solutions already developed, and in the development of further solutions that would be applicable under more complicated conditions. The initial work in this experimental program which is described here, is concerned with the solidification of pure metals at zero superheat under unidirectional heat flow conditions. Subsequent experiments have been concerned with the solidification of pure metals at appreciable superheats, under varying unidirectional heat flow conditions and under two dimensional heat flow conditions. In a series of experiments recently initiated, the solidification of binary alloys is also being investigated. The results of these subsequent experiments, together with relevant theory, will be described in later papers. The solidifying metal has been cooled in all the experiments, by a multiple air jet system designed so that the heat transfer coefficient to the cooled surface is constant and is uniformly distributed over the surface. This type of system has been chosen since only one parameter is needed to specify the heat transfer conditions and since these conditions are analogous to those met in certain continuous casting processes.' Air cooling was chosen in preference to water cooling, however, since it offers a wider range of heat transfer conditions, and since it can be investigated by analogous mass transfer techniques. The first part of this paper discusses the existing integral-profile solutions that correspond to the heat transfer conditions used in the experiments, and describes the development and use of the experimental apparatus. In subsequent sections the heat transfer and solidification results are presented, and the various theoretical predictions are compared with them, and with one another.

Jan 1, 1970

By C. J. Bechtoldt, H. C. Vacher

Quenched alloys, prepared by powder metallurgical techniques, were examined by microscopic and X-ray diffraction methods. The compositions and heat treatments were chosen so that the chromium and nickel solvuses could be determined and a range of composition and temperature, in which a eutectoid had been reported, could be explored in small intervals. The results showed no evidence of eutectoid reactions having taken place. ALLOYS containing iron, chromium, molybdenum, and nickel are extensively used in high-temperature applications. In order to provide basic information on the solid-state reactions that occur in such alloys, the National Bureau of Standards is engaged in an extensive study of the equilibrium phases in the binary, ternary, and quaternary systems involving these four metals. Attention was directed to the chromium-nickel system because a review of the literature showed conflicting data. A recent compendium1 of the constitution of binary alloys gives two diagrams for the chromium-nickel system, one a simple eutectic and the second a diagram showing a eutectoid and a eutectic. The eutectoid was the result of an allotropic transformation in a high-temperature solid-solution form of a chromium-rich phase called 0. The approximate temperature and composition of the eutectoid was 1200°C and 30 at. pct Ni. In the preliminary study, at the Bureau, no transformation was indicated in the chromium-rich phase of ternary and quaternary alloys in which chromium and nickel were major components. Similar results have been reported from time to time in the literature,2-8 In consequence of this situation, a systematic study was made of the constitution of heat-treated chromium-nickel alloys using metallographic and X-ray diffraction methods. The compositions of the alloys were selected so as to determine the boundaries of the chromium-rich and the nickel-rich phases and to explore in small intervals the ranges in composition and temperature in which the eutectoid had been reported. The results of this study are reported and discussed in the present paper. EXPERIMENTAL PROCEDURES Materials, Alloys, and Heat Treatments—The alloys were prepared by a powder metallurgy technique similar to that used in earlier work.9 Analyses of the materials used are given in Table I. Powders were mixed using a vibrator in 30-g batches of predetermined composition; 2-g pellets were made from the mixture by compacting at room temperature in a 1/2-in. diam mold under 60,000 lb per sq in. pressure. The pellets were sintered in dry hydrogen for 10 days at 1300°C. At the end of the sintering treatment the specimens were quenched in water, which caused a pale green film to form on the chromium-rich alloys and thin black scale to form on the nickel-rich alloys. The pellets after sintering were approximately 1/2 in. diam by 3/32 in. thick. The purification train9 was modified by inserting a tube of titanium turnings, heated at 700°C to increase the efficiency of the removal of oxgen and nitrogen. It was found in the earlier work that the sintering treatment lowered the carbon, oxygen, and nitrogen contents of chromium-rich alloys to 0.01, 0.01, and 0.004 wt pct, respectively, and that there was a loss of chromium. In order to ascertain the extent of this loss, the chromium contents of certain alloys were determined chemically. They included those alloys used to determine the parameter-composition curves and those of critical composition, used to determine the chromium-solvus microscopically; these analyses were made on samples after the final heat treatments. The mixed powder values for the chromium content of those alloys that were not analyzed were adjusted to conform to a smooth curve based on the chemically analyzed values for

Jan 1, 1962

By J. Kostuik, M. J. de Bastiani

The method of mining the uranium orebody at Denison mine in the Elliot Lake district of Ontario is discussed. Details of the development of haulage-ways and rooms are giuen, as well as methods of ore haulage. The milling and beneficiation stages are noted briefly. Located in the Elliot Lake mining district of Canada, the Denison mine lies between Sudbury to the east and Sault Ste. Marie to the west, Fig. 1. This area is overlain by Huronian sediments filling a basin in the Keewatin basement complex. Subsequent folding of these sediments developed a synclinal structure, known locally as the Quirke Lake Trough, which forms the northern portion of the now famous big Z structure, the geological trademark of this region. Plunging to the west and extending nine miles from the granite outcropping in the north to the Keewatin lava contact to the south, the syncline has dips of 10" to 45" on the north limb and 10" to 20" on the south limb, Fig. 2. The Denison orebody, located on the north limb of the syncline, lies between 800 and 3000 ft below the surface. The main ore zone is within 50 ft of the Missisagi-Keewatin contact (see Fig. 3), and it varies in thickness from 6 to 32 ft. This ore zone has a composite dip of 19" to the south and is composed primarily of two pyritized conglomerate beds separated by a band of pebbly quartzite stratum. The upper conglomerate bed of the main zone varies from 2 to 15 ft in thickness, while the lower conglomerate varies from 2 to 12 ft. Over extended areas, mining is carried out over the entire section comprising the two conglomerate layers and intercalated quartzite; in other areas, the conglomerates are selectively mined, depending on the thickness of the quartz-ite. The ore zone contains approximately 6 pct sulfides and 80 pct silica. The predominant uranium-bear ing minerals are brannerite, uraninite, and an unidentified mineral (probably thucolite). Some of the uneconomic metallic minerals identified to date are pyrite, pyrrhotite, and chalcopyrite. MINE LAYOUT Shafts: Underground exploration and development (Fig. 4) were performed through two shafts 1/2 mile apart. The No. 1 shaft, sunk to a depth of 1856 ft with the main station established at the 1600-ft ore level, is a 250-sq ft, 5-compartment shaft capable of handling 4500 tpd. Two 5x5-1/2-ft compartments serviced by a 12-ft diam double-drum hoist, are used for hoisting 190-cu-ft bottom-dump skips in balance. A 30-man cage, offset by a counterbalance, operates within a 5-1/2x11-1/2-ft compartment. The fifth compartment is used as a manway, pipe, and cable-way. This shaft is also provided with an intermediate pumping station used during the initial mining phase as well as loading-pocket and spill-pocket installations and pumping facilities. The 480-sq ft No. 2 shaft, located down-dip from No. 1 shaft, has a 2776-ft depth. Serving as the main hoisting shaft with a maximum capacity of 9000 tpd, it has eight compartments, four of which are used for hoisting ore in 10-ton capacity bottom-dump skips. These four compartments, measuring 5x6-ft in section, are serviced by two 12-ft diam double-drum semi-automatic hoists. A 50-man cage is operated in a 15x8-ft compartment, and it is counterbalanced by a 12-ton weight. Two compartments are used for ventilation, manway, electric cables, and pipes. A station was constructed at the 1325-ft horizon of the No. 2 shaft for relay pumping. The main sta-

Jan 1, 1961

By R. I. Jaffee, C. M. Craighead, G. A. Lenning

Hydrogen forms a beta-stabilized system with titanium, with a beta eutectoid at about 300°C and 44 atomic pct H2. 'The solid solubility of hydrogen in alpha decreases from about 8 to about 0.1 atomic pct from 300°C to room temperature. Hydrogen has little effect on tensile properties, but decreases notch-bar toughness to a large degree. This latter effect appears to be the result of increased notch sensitivity. PRIOR to this investigation, only a small amount of information was available on the effect of hydrogen on the mechanical properties of titanium. The effects of the other interstitially soluble elements, carbon, oxygen, and nitrogen, had received detailed study. Jaffee and Campbell1 indicated that hydrogen up to 1 atomic pct did not affect tensile properties deleteriously. Pitler' indicated that 1 atomic pct H, in titanium reduced the impact strength appreciably, but his alloys contained appreciable amounts of oxygen, and it was difficult to attribute the embrittlement entirely to hydrogen. The high temperature portion of the equilibrium diagram for the Ti-H system was established by McQuillan," and his data generally corresponded with the results of Kirschfeld and Sieverts," Gibb and Kruschwitz," Bevington, Martin, and Mathews," and other investigators. The lower concentration limit of the hydride phase varied considerably among investigators, and Gibb and Kruschwitz9 ad shown that small amounts of contaminants in either titanium or hydrogen caused considerable variation in this lower limit. In view of this pronounced effect of contaminants, the extrapolated value of McQuillan's, about 48 atomic pct at the 325°C eutectoid, appeared the most reasonable. McQuillan's lowest experimental value was 54 atomic pct at a temperature of 450 °C. The density of titanium had been shown to decrease with increasing hydrogen content, but discrepancies were noted among the various investigations. The best values indicated that the density was decreased from 4.56 grams per cc at 0.27 atomic pctl to 3.84 grams per cc at 61.3 atomic pct? This investigation was conducted to determine the effects of hydrogen on a titanium, both in high purity and commercially pure metals, and on high purity a titanium alloys. Material and Fabrication The literature indicated that impurities in either the hydrogen or the titanium must be kept to a minimum. For this reason, the initial studies were made with high purity iodide-refined titanium. The vendor's analysis of the iodide titanium and the hydrogen content of the as-fabricated Y4 in. diameter rods are shown in Table I. Two 1 lb ingots were prepared by arc melting under argon in a water-cooled crucible, using a water,cooled tungsten electrode. This equipment has been described.' As-cast Brine11 hardness numbers of 88 and 58 for these ingots were low enough to insure that the high purity of the metal was maintained during arc melting. The ingots were hot forged to % in. diameter rods at 800°C, cleaned by grit blasting, and then cold swaged to Yz in. diameter rods. The rod was then air annealed at 725 "C, ground to remove scale, and cold swaged to Y4 in. diameter (75 pct reduction in area). The material was then annealed for 1 hr in argon at 800°C to develop an equiaxed a grain size of about 0.05 mm. Micro tensile specimens and microimpact specimens were machined from this rod prior to treatment in the Sieverts-type absorption apparatus. Two lots of commercially pure RC-55 titanium were also used in this investigation to determine the effects of hydrogen and the normal impurities on mechanical properties. The commercially pure RC-55 alloy was obtained in the form of % in. diameter rod. The analysis of this material is also given in Table I. The % in. diameter rods were hot swaged

Jan 1, 1955

By Bernard G. Carbajal

The dielectric properties and thermal stability of glow-discharge polytnerized films of styrene, chloro-benzene, and other organics and photoresist filrns are presented. Variations in the glow-discharge polymerization procedure are related to thermal stability. Thermal treatwzents to improve the dielectric properties of both positive (A2 340) and negative (KMER) photoresists are given. THIS study of the dielectric properties of thin organic polymer films is part of a program to investigate the electronic applications of organic materials. Thin organic polymer films have been produced in an ac glow discharge,13 with a low-energy electron-beam process,4 and in an rf dicharge. A process has been developed during the course of this program for forming thin organic polymer films in a dc glow discharge. These glow-discharge polymerized (GDP) films exhibit some useful dielectric and insulative properties. Variations in the properties of the GDP films can be induced by changes in the source material (monomer) andor in the conditions of the glow discharge. Thin organic polymer films can also be produced from typical positive and negative photoresists. Some variations in the properties of the photoresist films can be induced by suitable post-application treatments such as thermal crosslinking. The properties of interest in this study are dielectric constant, dielectric strength, resistivity, and thermal stability. POLYMER FILM PREPARATION I) GDP Films. The GDP films were prepared in a dc glow discharge in an atmosphere of organic monomer vapor. The details of the glow-discharge procedure have been presented previously.6 Briefly, under the influence of a dc glow discharge organic vapors can be polymerized in the vapor phase and the resultant polymer (GDP film) deposits on and in the vicinity of the cathode. Substrates placed behind a screen cathode can be uniformly coated over all exposed areas. Pattern definition can be achieved using normal mask stencil techniques. Table I presents the pertinent parameters in the preparation of GDP styrene. Conditions of Forrrzation of GDP Styrene. The rate of deposition for GDP films was monitored using a current-time integrator. The thickness of the deposited film for a given set of experimental conditions was a function of the current-time integral. The fifth row in Table I is a compilation of the deposition rate of GDP styrene films. Other organic monomers behave in a similar fashion. With the exception of the highly halogenated saturated hydrocarbons, all organics subjected to the conditions of the glow discharge form GDP films. 11) Photoresist Films. Photoresists are normally recognized to exist in two forms, a low molecular weight, soluble polymer form (A) and a high molecular weight, crosslinked insoluble form (B). Typical negative photoresists are applied in the low molecular weight form A and converted to the high molecular weight form B by the action of light. (Positive photoresists are applied in form B and converted to form A by the action of light.) Eastman Kodak Metal Etch Resist (KMER) has been chosen as a typical negative photoresist. Polymer film samples were prepared in the same configuration used for GDP films. The KMER was applied in the usual fashion using a 120°C drying step (infrared-lamp heating) and a 180°C post-bake. Care must be taken to completely remove the solvent in the drying step and to properly develop and postbake to exposed photoresist. If the photoresist film is not properly dried and postbaked, severe blistering and peeling will occur during subsequent elevated-temperature exposure. Thickness can be controlled by varying the viscosity of the form A photoresist and the spin rate at application. AZ 340 was chosen as a typical positive photore-

Jan 1, 1967

By L. Luini, E. Lee

An exploratory survey of the heat treatment response of commercial titanium alloys (Ti-150A, RC-130B, and MST 3AI-5Cr al-loys) shows a wide range of possible hardness and microstructural characteristics. The hardening is primarily dependent on the solid state transformation of the phase. An age hardening reaction which apparently is associated with ß decomposition and precipitation has been shown. Brittleness and notch sensitivity appear to be characteristic of age hardening to high hardness. Ductility, tensile strengths, and elongations are given. A NUMBER of commercially produced titanium-base alloys have been made available by the titanium metals industry. These alloys were developed to combine the light weight of titanium with increased strength through alloy additions. Usually the properties of these alloys are reported for material in the hot rolled and annealed condition. Since the production of commercial titanium has preceded the investigation of titanium-base alloy systems, the potential of these alloys is not well known. Although heat treatability has been indicated for these alloys, data on the response to heat treatment are quite limited. The heat treatability of titanium is based on the allotropic transformation of the high temperature, body-centered cubic ß structure to the low temperature, hexagonal close-packed a structure at approximately 1625 °F. This transformation in the pure metal is of little practical significance in heat treatment since the high temperature phase is not amenable to controlled transformation. Alloy additions serve to alter the transformation kinetics and permit control of the transformation by heat treatment variables. The effects of different alloys on the allotropic transformation in titanium classify them in two general categories,1 a stabilizing and ß stabilizing elements. The a stabilizers, represented by aluminum and oxygen, raise the temperature limits of the low temperature phase and introduce a two-phase a + ß temperature range. The ß stabilizers, represented by molybdenum and columbium, lower the equilibrium temperature of ß and give rise to an extended temperature range where both a and ß phases are stable. Another type of ß stabilizer, represented by iron, chromium, and manganese, introduces a eutectoid reaction. Some commercial titanium alloys belong to complex multiple element systems. Based upon the phase diagrams of the binary systems, the general effect of commercial compositions is to vary the stability of the high temperature phase and significantly alter its transformation characteristics. Therefore it is expected that the characteristics of alloyed titanium can be altered by heat treatment. The present investigation was undertaken to survey the variations in hardness, microstructure, and mechanical properties as affected by heat treatment variables. Commercial Alloys lnvestigated The commercially available titanium-base alloys selected for this investigation and obtained as 3/4 in. diameter hot rolled and annealed bars are listed in Table I. The producer did not determine the chemical composition of the Ti-150A heats X1052 and L685. The early heats of Ti-150A, prefixed with the letter X, were melted with tungsten-tipped electrodes and cast in approximately 500 lb ingots 12 in. in diameter. The heats prefixed with the letter L were melted under a revised melting practice yielding approximately 1300 lb ingots 16 in. in diameter. The final annealing treatment was at 1200" to 1250°F for 1 hr. The MST-3A1-5Cr alloy was melted in an induction furnace and cast in 7 in. diameter ingots. This practice produces high carbon material and some variation in the amount of carbides was found in different sections of the same bar. The RC-130B alloy was melted with a carbon arc. This alloy showed approximately 2 pct carbides. No large segregation effects were observed.

Jan 1, 1955

By R. R. Boucher, O. J. C. Runnalls

A pronounced thermal effect has been observed on heating or cooling a1wninum-rich Al-U and Al-Pu alloys. From microscopic and X-ray diffractionstudies, the effectl has been attributed to trnsfor)nations in the inlemetallic phases UAl, and PuAl , involuing rearrangement or cluslering of vacancies The transformation obsrved in Al-20 wi oct U alloys occurred near the a Al-UAl4 eutectic tem-perature of 646°C making it difjicult to detect from heating curves. When cooling, howeoer, thermal mad X-ray analyses indicnted that the high-temperati~re phase labeled p UAL, precipitated initially during euitectic solidification. As solidification continued and after an induction period o-f 5 lo 20 tnin the nu-cleatiorz and growth of the low- twmperature phase, a UAl4 produced an euolution of energy which raised the observed alloy temperature by 1° to 2°C. in Al-Pu alloys the transformation occurred at 645°C, 5 deg below the eutectic solidification temperccture. The eslimated latent heat of transformation was 25 +5 cnl per g PuAl,. The high-tetnpevcl-ture forms of UAl, and PuAl, were easily 9-etccined by chill casting Al-U and Al-Pu alloys and on reheating the alloys the trcltzsforrnation to the a phase was sluggish even above 600°C. Separated single cryslals o-f UAl4, joy example, showed no evidence Of transformalion after heating for 16 hr at 620°C. The transformation rates increased yapidly enough with increasing temperature, however, that a a spontaneous liberation of energy lens observed on occasion when bealing cast Al-20 wt pet U to neal- the RECENT phase studies on A1-Pu alloys have indicated that earlier reported equilibrium diagrams should be modified to take account of several poly- morphic transformations in the intermetallic compound PuAl,.' During the course of the latter work an unexpected heat evolution was observed while cooling a solid alloy consisting of a mixture of a aluminum and PuA1,. The evolution occurred at 645°C, y below the a A1-Pu A1, eutectic solidification temperature. Subsequent thermal-analysis experiments with A1-U alloys showed that heat was evolved there also at a temperature nearly coincident with the a A1-UA1, eutectic solidification temperature of 646°. A search of the literature revealed that similar thermal effects had been observed before for both A1-U and A1-Pu but had never been fully explained.2,3 The purpose of the present paper is to describe thermal-analysis and X-ray diffraction experiments which have led to the conclusion that the thermal effects are due to transformations which involve the rearrangement of vacancies in the intermetallic compounds UA1, and PuA1,. EXPERIMENTAL PROCEDURE The A1-U alloys were prepared by heating super-pure aluminum (99.99 pct +) obtained from the Aluminum Co. of Canada in a graphite crucible surrounded by an induction coil. At 1000°C high-purity uranium metal produced by the Eldorado Mining and Refining Co., Ltd. was dropped into the liquid aluminum and was dissolved completely within 15 min. The impurities in the uranium were A1—4 ppm, Ca-4, C-70, Cr-3, Cu-6, Fe-30, Mg-2, Mn-10, Ni-25, Si-25, and Zn-2. The A1-Pu alloys were prepared by reacting plutonium dioxide with liquid aluminum under cryolite (3 NaF . AlF,) for 10 min at 1100°C in graphite crucibles exposed to the air. The plutonium was 99.8 pct pure, containing trace impurities of Ca, Cu, Fe, Pb, Si, and Zn. The liquid alloys were usually poured into water-cooled molds to provide castings of uniform composition from which samples could be cut for heat treatment and thermal-analysis experiments.

Jan 1, 1965

By A. R. Elsea, E. E. Fletcher

Cast X-40 alloy with the lowest nitrogen content studied had a 100-hr rupture stress at 1500°F about equal to the reported value for the commercial alloy. Increases in nitrogen content progressively decreased the rupture strength, and with about 0.1 to 0.2 pct N a minimum strength was reached, but there was no accompanying change in microstructure. Further increases in nitrogen resulted in the fomzation of progressively increasing amounts of a lamellar, pearlitic-type structure at the grain boundaries, with accompanying increases in rupture strength, and above about 0.25 to 0.33 pct N, the rupture strength exceeded the normally reported values. Two series of melts representing different melting stocks exhibited minimum rupture strengths at different nitrogen contents. This suggests that some unidentwed trace element not removed by vacuum melting has a strong influence on the response of this alloy to variations in nitrogen content. In a series of melts with manganese contents ranging from 0.6 to 3.2 pct, the material with the lowest manganese content had the highest 100-hr rupture strength at 1500°F. The manganese variations had no appreciable effect on the microstructure. CAST cobalt-base alloys such as X-40* exhibit high strengths at elevated temperatures (1500°F and above), but they also show considerable scatter in high-temperature properties. Since the design of parts for critical applications must be based on the minimum expected properties, this broad scatter appreciably lowers the design strength of the alloy. If the relatively poor properties exhibited by a few test parts from any given group could be improved, the spread in properties would be narrowed, and the design stress could more closely approach the average expected properties. The purpose of this research investigation was to learn what were the causes of these erratic properties and, if possible, to find methods for eliminating them. Earlier unpublished work showed that vacuum melting markedly influenced the high-temperature strength of cast X-40 alloy. There were indications that this behavior may have been the result of changes in the nitrogen or manganese content of the castings. Consequently, in the current investigation, the influence of variations in nitrogen and manganese content on the structure and high-temperature properties of cast X-40 alloy was studied. In this program, X-40 melting stock was vacuum melted to produce a base material that was very low in nitrogen content and in volatile trace elements. Additions were then made to this base material to produce alloys of the desired composition. The metal was cast into investment molds producing coupons which were machined into stress-rupture bars. These bars were subjected to stress-rupture tests and me-tallographic study to determine the influence of changes in analyses (nitrogen and manganese content) on the structure and properties. Material—The melting stock used for these experi-ments was in the form of shot from two master heats of commercial X-40 alloy. Only one master heat was used in a given series of melts. Thus, any differences in structure or properties that showed up in the specimens from a given series would be the result only of the intended variations in composition. The certified analyses of the master heats were as follows: C Mn Si Cr Ni Lot No. 2 0.50 0.71 0.66 25.44 10.53 Lot No. 3 0.54 0.73 0.70 25.95 10.00 W Fe Co P S Lot No. 2 7.45 1.34 Bal. 0.011 0.013 Lot No. 3 7.58 1.53 Bal. 0.005 0.016

Jan 1, 1960

By J. G. Early, F. V. Lenel, G. S. Ansell

The isothermal shrinkage rates of copper-powder compacts were determined in the temperature range from 760o to 1060oC. The rates for compacts fabricated from a pure spherical copper powder were compared, on the one hand, with those fabricated from a spherical powder containing a dispersion of aluminum oxide in the copper matrix and, on the other hand, with those fabricated from a pure copper powder having irregularly shaped particles. The irregular copper-powder compacts shrank much faster than the spherical copper-powder compacts and these, in turn, shrank faster than dispersion -strengthened copper -powder compacts. The experiments were run under a small external load. By varying this load, the stress dependence of the isothermal shrinkage rate could be measured for compacts from spherical-copper powders. This stress dependence was found to be approximately proportional to the 4th (dispersion-strengthened alloys) or 4.5th (pure metals) power of the stress. It is concluded that the material-trans port mechanism is due to dislocation climb rather than to Herring-Naharro creep. In this investigation the isothermal shrinkage rates of compacts made of copper powder with an average particle size of 70 g in the temperature range from 780o to 1060°C were studied. The aim of the investigation was to determine the mechanism of material transport responsible for the shrinkage of these compacts. Since the phenomenon observed in this investigation was shrinkage of compacts at high temperatures, it will be necessary to consider all the material-transport mechanisms possible in sintering. It is unlikely that evaporation and condensation, surface diffusion, or even volume diffusion of vacancies, in which surfaces of small radius of curvature are vacancy sources and those of larger radius of curvature vacancy sinks, will materially contribute to a sintering process involving shrinkage, i.e., one in which the centers of adjacent particles move towards each other. The two principal mechanisms which were considered were the so-called Nabarro-Herring mechanism and a plastic deformation mechanism by dislocation movement. Both of these mechanisms were originally conceived to explain creep, i.e., the plastic deformation of metals at elevated temperatures under a constant applied stress. The shrinking of metal-powder compacts which was studied in this investigation can be readily treated as a creep process. This means that the shrinkage rates observed are considered as creep rates under the influence of an applied stress. It is true that the stresses in sintering experiments are generally not constant but decrease continually with time, but, by considering creep rates or shrinkage rates over a relatively short time interval, the small changes in stress during this time interval can generally be neglected. Nabarro-Herring microcreep is a high-temperature deformation mechanism which is caused by a diffusional flow of vacancies from boundaries under a tensile stress towards those under a compres-sive stress. Herring1 has shown that in this type of microcreep the strain rate e is proportional to the applied stress and follows an equation of the form ma, aexp(-Q/RT) [l| where <j is applied stress, Q is the activation energy for self-diffusion, R is the gas constant, and T is the absolute temperature This type of creep can explain the shrinkage of a porous compact. The surface of the pores are subjected to the tensile stress of surface tension, while the grain boundaries are under a compressive stress also due to surface tension. Vacancies diffuse from the pore surface through the lattice to the grain boundaries, where they are eliminated. In order to maintain vacancy equilibrium at the pore surface the vacancies leaving the region of the pore surface are replenished from the volume of the pore, which means that the pores shrink.

Jan 1, 1964

By George R. St. Pierre, John Chipman

METALLURGISTS have been studying the chem-ical behavior of sulfur in steelmaking for many years in order to have a better control of the sulfur content of finished steel. During the refining period in the open hearth, molten steel is separated from a gas phase by molten slag. Chemical reactions occur principally at the slag-metal interface and at the slag-gas interface. A need for physical-chemical investigations of reactions between sulfur-bearing gases and steelmaking slags was recognized some time ago.&apos;.&apos; From the early work, it can be qualitatively concluded that increased sulfur content and low partial pressure of oxygen in the gas phase favor the passage of sulfur from gas to slag. Using radioactive sulfur S Koch and Fink&apos; have demonstrated the rapid rate of exchange of sulfur between gas and slag in an open hearth furnace. Gurry and Darken and Darken and Shields (as reported by Derge and Marshall&apos;) have equilibrated lime-iron oxide slags with SO—O2 gas mixtures. The major conclusion from the reported results is that sulfur content increases with increasing lime content in lime-iron oxide slags equilibrated with a gas of high oxygen pressure (10-2). The data were interpreted as indicating the presence of SO, and S,O, ions. Richardson and Fincham&apos; have conducted the most extensive experimental study of sulfur equilibria between gas and slag. Their results confirmed many of the conclusions drawn from calculations of Richardson" and Withers. Richardson and Fincham&apos;s data fitted very well into the sulfur scheme represented by the reactions 1/2 s2 (g) + (0) melt - 1/202(g)+ (S) melt [II 1/2 S, (g) + 3/2 O (g) + (0) melt - (SO,) melt. [2] At oxygen pressures greater than 10 to 10 they found that reaction Eq. 2 was predominant while reaction Eq. 1 was controlling at oxygen pressures less than 10." to 10.". The slag compositions and gas mixtures used in their investigations were different from those used in the present study. Wherever possible, comparison has been made between their results and these, and agreement is excellent. It is evident that the distribution of sulfur between slag and gas depends upon the oxygen pressure of the gas. In FeO slags, a change in oxygen pressure produces a change in ferric oxide content, and a knowledge of this equilibrium is a prerequisite to studies of sulfur distribution. The data are found in the work of Darken and Gurry" on the FeO system and the more recent experiments of Gurry and Darken" and of Larson and Chipman" on FeO slags containing lime and silica. The effect of oxygen pressure on the ratio Fe /(Fe" + Fe ), the so-called j-ratio, reported by these investigators will be used in interpreting the results which follow. Experimental Method The purpose of the experimental program was to determine the equilibrium sulfur content in slags exposed to gases of known oxygen and sulfur pres- sures. The slag compositions selected for study were from the lime-silica-iron oxide system. Additions of magnesia were made to some of the slags. Apparatus—The apparatus used by Larson and Chipman was modified slightly to accommodate the addition of SO2 to the gas mixtures. As in their work, slag samples of 0.5 to 2.0 g were held at temperature (lcc) in platinum crucibles under a steady stream of gas, 100 to 200 ml per min, for several hours and then rapidly lowered to the bottom of the furnace where they were quenched in mercury. Preparation and Analysis of Gas Mixtures—Mixtures of SO,-CO were prepared from Virginia Smelting Co. Extra Dry liquid SO, and Pure Co. CO,. After removing traces of water vapor with an-hydrone, the CO, was passed over graphite at 1200°C, at which temperature the conversion to

Jan 1, 1957

By H. L. Lovell, L. H. E. Weyher

Cyclones have been used successfully in the mineral industries to solve solid-liquid as well as solid-solid separation problems in the processing of fine particles. Substantial information is available about the operation of cyclones as thickeners, classifiers, and concentrators using a dense medium. However, very little is known about the operation of the cyclone as a fine coal concentrator not using dense medium. This application of the cyclone, namely to wash fine coal in water, requires that classification phenomena be minimized in order to arrive at an effective separation of the high density ash and sulfur-bearing mineral particles from the low density coal particles over a wide particle size range. The authors have investigated the role of feed pressure, orifice diameters, and vortex-finder length in the cyclone washing of fine coal (--1/4 in.) in water. The results of this investigation show that cyclone washing of fine coal in water is an effective unit operation particularly capable of reducing the inorganic pyritic sulfur content. The combination of hydrocyclones with complimentary equipment such as Sieve bends, shaking tables, and flotation units appears to be especially promising and may ultimately yield fine coal processing systems that could approximate the high recovery efficiencies of today&apos;s coarse coal cleaning circuits. In the future, fine coal beneficiation can be expected to receive even greater research emphasis as a result of increasing sulfur restrictions on all major coal markets. In a previous paper, work, conducted at the Pennsylvania State University, on the hydrocyclone washing of fine coal was discussed.&apos; The initial evaluation based on that wo-rk demonstrated the feasibility of hydrocyclones as fine-coal cleaning devices, and in that previous paper selected test data were presented that showed in principle how product yield and assay respond to variations of the major cyclone operating variables. The present paper reports in greater detail on the findings and presents a comprehensive evaluation of the data as follows: (1) Hydrocyclone throughput rates were related to feed pressure and other variables by regression equations. These equations are compared with other capacity-vs.-pressure drop expressions taken from the literature on classification cyclones. (2) The flow ratio was found to be the most important variable for the separation of the solids. Control of this ratio through various cyclone operating parameters is discussed. (3) The data on the product yield as well as the ash and sulfur assays from the tests were evaluated by means of correlation and multiple regression analyses. Because size-classification phenomena cannot be suppressed completely in hydrocyclone washers, product yield and assay data are regressed against cyclone operating variables separately for different size classes. These equations then reveal how the interactions of the cyclone operating variables vary in terms of the separation for different size classes. (4) Density partitions from additional tests were analyzed by supplementing product-size analyses with sink-float analyses of the separated product size classes. The evaluation of these data show how classification phenomena affect separation by density. The results demonstrate in particular the feasibility of the hydrocyclone washer for removing pyritic sulfur from fine coal. In addition to these specific findings, the investigation points up the value, in general, of using hydrocyclone washers in combination with unit operations such as screening, table concentration, and flotation. In order to make optimum use of the hydrocyclone washers and work out the most effective combination of unit operations, it is important to have careful flowsheet analyses corresponding to the given feed and product requirements. Analyses of this kind are now possible by means of computer simulation of flowsheets and other operation research tools. INTRODUCTION Before proceeding with the detailed treatment and evaluation of our results, it will be useful to review the fundamental aspects of cyclone separators and also restate the experimental procedures and data handling employed in these studies. Review of Cyclone Fundamentals: AS shown in Fig. 1, the basic components of cyclones commonly used

Jan 1, 1970

Said Plutarch a long time ago, ?To appreciate a man&apos;s work at the full, it is well to know the man himself, his circumstances and the incidents of his career." He might as truly have said "gift" instead of "work." Ambrose Swasey, engineer, collaborater with scientists, promoter of engineering research, patron of Engineering Foundation, advancer of the good of mankind, modest gentleman and generous giver, is, happily, well known to a great many engineers, who will therefore more fully appreciate his recent additional gift, for the use of the Engineering Foundation, which; purpose is "the furtherance of research in science and engineering, and the advancement of the profession of engineering and the good of mankind." But full appreciation of a gift of money necessitates more than acquaintance with -the giver and knowledge of the amount. Its timeliness; its inspiration; the character and continuity of its benefits, all must be comprehended. But whose imagination, though far-visioned as the great telescopes Mr. Swasey has built, can see the limits of benefit of such gifts as he has made to the Engineering Foundation, attracting-as they will-other gifts and evidences of, devotion to a great cause-? Every such gift lays responsibilities upon the recipients. Will American engineers grasp not merely, their pecuniary value but also emulate the spirit of fraternity and desire for harmony which have accompanied them? Shall we not work together and with Ambrose Swasey to advance still further the good of mankind, thus to demonstrate an acceptance of our obligations to humanity which is a counterpart in a democracy of the noblesse oblige of aristocratic tradition?

Jan 12, 1918

By J. W. Ristori

During the year 1940, production of crude oil in RiIexico totaled 43,914,000 bbl., or 2,776,000 less than in 1937, the year before expropriation. The 1940 output was I,2000,000 higher than in the previous year. In 1937, Poza Rica production accounted Declines in exports of Panuco crude, fuel oil and gasoline were recorded but these were more than offset by increased exports of 4,000,000 bbl. of Poza Rica crude, which was the approximate amount shipped to Sinclair during 1940 under the terms of the settlement. Over-all exports increased by 1,500,000 bbl. over the preceding year. The outstanding development regarding the destination of Mexican exports in 1940 was the increase of I0,000,000 bbl. in the exports to the United States. Exports to Germany ceased toward the end of &apos;939 and to Italy in the second half of 1940. During the year 1940 the Sinclair interests and the Mexican Government settled their expropriation question. By the terms of the settlement Sinclair is to be compensated by cash payments and oil-purchase contracts. On Dec. I, 1940, Ada Camacho was inaugurated President of Mexico for a term of six years. Among his first acts following his election were: I. A proposal to change the Constitution to restore Supreme Court Judges&apos; terms to life tenure. This has been ratified by both chambers of the Mexican congress and is now before the legislatures of the States of Mexico for ratification. The, taking away of the administration of the railroads from labor and restoration to the State.

Jan 1, 1941

By J. W. Ristori

During the year 1940, production of crude oil in RiIexico totaled 43,914,000 bbl., or 2,776,000 less than in 1937, the year before expropriation. The 1940 output was I,2000,000 higher than in the previous year. In 1937, Poza Rica production accounted Declines in exports of Panuco crude, fuel oil and gasoline were recorded but these were more than offset by increased exports of 4,000,000 bbl. of Poza Rica crude, which was the approximate amount shipped to Sinclair during 1940 under the terms of the settlement. Over-all exports increased by 1,500,000 bbl. over the preceding year. The outstanding development regarding the destination of Mexican exports in 1940 was the increase of I0,000,000 bbl. in the exports to the United States. Exports to Germany ceased toward the end of &apos;939 and to Italy in the second half of 1940. During the year 1940 the Sinclair interests and the Mexican Government settled their expropriation question. By the terms of the settlement Sinclair is to be compensated by cash payments and oil-purchase contracts. On Dec. I, 1940, Ada Camacho was inaugurated President of Mexico for a term of six years. Among his first acts following his election were: I. A proposal to change the Constitution to restore Supreme Court Judges&apos; terms to life tenure. This has been ratified by both chambers of the Mexican congress and is now before the legislatures of the States of Mexico for ratification. The, taking away of the administration of the railroads from labor and restoration to the State.

Jan 1, 1941

By Stanley W. Ivosevic

The commercial success of this low-grade property by Houston Oil and Minerals Corp. (succeeded in interest by Houston International Minerals, Inc.) resulted from credibility of analytical data furnished by the property vendor upon initial examination and from other favorable geologic criteria in evidence; from negotiation of lease terms not detrimental to project economics; from entrepreneurial exploration management; from an encouraging attitude by the US Forest Service; and from the favorable mining and metallurgical characteristics of the ore body. The potential of the property, but not its location, was brought to the attention of the project manager (the author) by the vendor some time before accepting employment with HO&M. In December, 1977, the vendor granted an examination to the project manager, by then an employee; and a lease to the 15 mining claims embracing the property was executed in April, 1978. (See Fig. 1.) Field work and extensive claim staking in this virgin district commenced in May, with drilling beginning in August. At the point that an apparent discovery was recognized in October, only $98,000-including property payments-had been expended on the project. By April, 1979, the deposit was drilled out on 60-m (200-ft) centers and a preliminary re- serve estimate, discounted cash-flow analysis, and recommendations for mine development and additional exploration submitted to management-all at a cost well below budget. The property was recommended for acquisition after matching favorable geologic criteria developed by the project manager. Favorable lithology, structure, and geochemical zonation converged on a subdued low-temperature hydrothermal alteration zone subtly expressed on a pediment surrounding the heart of the property, from which approx [ ]

Jan 1, 1985

The Library of the above-named Societies is open from 9 A.M. to 10 P.M. on all week-days, except holidays, from Sept. 1 to June 30, and from 9 A.M. to 6 P.M. during July and August. The Library contains about 55,000 volumes, including sets of technical periodicals and the publications of scientific and technical societies. Members of the Institute, with few exceptions, are forced to spend a portion of their time in localities isolated from sources of information. To these the Library can render valuable service through correspondence; letters requesting information will receive special attention. The Library is prepared to furnish references and copies of articles on mining and metallurgical subjects; to determine the existence of mining maps, and to furnish general information as to the geology and mineral resources of all countries. All communications should be made as definite as possible so, that the information received may be what is desired and not include collateral matter which may not be of interest. The time spent in searching for such collateral matter will be saved, and the information will be sent more promptly and in more usable shape. The members of the Institute can be of service to the Library by forwarding copies of mining, reports, maps privately issued, and similar material, which will be classified, indexed, and made available to other members. Suggestions for additions to the Library, either by purchase or personal solicitation as gifts, will be welcomed. It is hoped that members while in the city will, use the Library freely, and assurance is given that most careful service will be rendered to them.

Jan 6, 1916

By G. Austin Schroter, Ian Campbell

ALTHOUGH there is now an extensive literature on the bleaching clays, not a great deal of material is to be found concerning the geological features of these deposits and their bearing on problems of exploration and development. At the same time, chemical and crystallographic research on the clay minerals during the past few years has laid a suitable foundation upon which to base conclusions of economic value drawn from field observations. All of the criteria and deductions herein presented are based upon extensive field work by the senior author, both in the United States and Canada, and when subjected to the ultimate tests of development and exploitation they have held up remarkably well, despite the fact that many of these conclusions apparently have not been reviewed in the literature heretofore. The nomenclature of the bleaching clays is rather confusing in the light of present-day commercial standards and has even led to litigation." The old term "fuller&apos;s earth" is largely based upon trade usage and the definition of the term therefore is dependent upon the changing standards of commerce. For statistical purposes the Bureau of Mines81 classes as "fuller&apos;s earth" all natural bleaching or filtering claylike materials that possess high adsorptive capacity without previous chemical treatmerit or activation. Conversely, the so-called activated or acid activated clays are now generally recognized as any clay mineral or mixture of the clay minerals whose adsorptive capacity has been developed to commercial standards by chemical or physical treatment. Therefore, without attempting to propose any additions to the nomenclature of bleaching clays, this paper will refer to naturally adsorptive clays and activable clays, respectively, for the two types indicated.

Jan 1, 1940

The Library of the above-named Societies is open from 9 A.M. to 10 P.M. on all week-days, except holidays, from Sept. 1 to June 30, and from 9 A.M. to 6 P.M. during July and August. The Library contains about 55,000 volumes, including sets of technical periodicals and the publications of scientific and technical societies. Members of the Institute, with few exceptions, are forced to spend a portion of their time in localities isolated from sources of information. To these the Library can render valuable service through correspondence; letters requesting information will receive special attention. The Library is prepared to furnish references and copies of articles on mining and metallurgical subjects; to determine the existence of mining maps, and to .furnish general information as to the geology and mineral resources of all countries. All communications should be made as definite as possible so that the information received may be what is desired and not include collateral matter which may not be of interest. The time spent in searching for such collateral matter will be saved, and the information will be sent more promptly and in more usable shape. The members of the Institute can be of service to the Library by forwarding copies. of mining reports, maps privately issued, and. similar material, which will be classified, indexed, and made available to other members. Suggestions for additions to the Library, either by purchase or personal solicitation as gifts, will be welcomed. It is hoped that members while in the city will use the Library freely, and assurance is given that most careful service will be rendered to them.

Jan 2, 1916

By A. B. Parsons

Perhaps this Index is the most useful volume the Institute has ever published. At least, it is likely to be referred to more frequently and by more people than any other single volume. It covers the contents of 27,058 pages of TRANSACTIONS in addition to special volumes, MINING AND METALLURGY and sundry pamphlets (T.P.&apos;s) that were not subsequently included in the TRANSACTIONS. In the 54 years from 1871 to 1925 the Institute published 72 volumes; in the following ten-year period covered by this index it published 57 volumes, including TRANSACTIONS and special publications sponsored by the Rocky Mountain and Seeley Mudd Memorial Funds. These include the complete series for the Institute of Metals, Iron and Steel, and Coal Divisions, and all of the volumes on Petroleum Development and Technology. Indexing is an exacting task at best; it is something of an art. And a composite index like this, covering a wide range of subjects contained in volumes appearing over a period of ten years, presents added problems. Miss Katharine Lovell developed the system of indexing as the years went along, and did most of the original work. Mrs. Harriet K. Broughton, under Miss Lovell&apos;s direction, sorted and organized the accumulation of 33,000 cards on which the entries were made. For five years the Institute has needed a cumulative index badly; but until this year the Directors have not felt justified in authorizing publication. The delay has caused much inconvenience in the past; but to some extent this will be compensated by the great advantage of being able to find items covering the entire ten-year period in a single volume.

Jan 1, 1936

By T. S. Liu, E. A. Peretti

A LITERATURE survey of the In-Sb system, which was made before a study of the binary diagram was undertaken, revealed that the intermediate phase InSb existed and that its crystal structure is face-centered cubic of the zinc blend type. In 1929 Goldschmidt&apos; determined the lattice constant for InSb and obtained a value of 6.452A. A more recent value, 6.461A was reported by Iandelli2 in 1941. The purity of the indium used was not very high, however. The indium used by Iandelli contained 2 pct Ge. In view of this fact it was decided to remeasure the lattice parameter using high-purity indium (99.97+ pct In) and spectrographically standardized antimony of the highest purity available (99.91 pct Sb). Specimens corresponding to the InSb composition were made by carefully weighing the ingredients on an analytical balance and heating them in vacuo in a quartz tube at 700°C. As melting losses were negligible, the alloys were not analyzed chemically, but the intended analysis was taken as being accu- rate. Powder samples were prepared by either filing or crushing of the brittle alloy, followed by screening at 325 mesh. The powders were then annealed at 400°C in evacuated capsules for about an hour. X-ray photograms were taken with a Debye and a back-reflection focusing camera, using characteristic cobalt K. radiation. Lattice parameters were calculated by Cohen&apos;s³ method. The results of a Debye pattern and of a back-reflection pattern at 25°C are given in Tables I and 11. The lattice parameter at 25 °C is 6.47602A.

Jan 1, 1952