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By A. Aly Selim

A computer model was developed to calculate the fragmentation cost for in situ leaching operations as a function of the blast design and deposit parameters. The model is based on blasting an ore zone only or an ore zone plus overburden by either a coyote blast or a vertical blasthole system. The model calculates the blast design parameters and the fragmentation cost based either on a user input powder factor value or on a powder factor calculated by the model as a function of the overburden height and the ore zone thickness. Examples of blast design parameters calculated by the model are the number and spacing of blastholes for a vertical blasthole system and the number and spacing of crosscuts for a coyote system. The model also calculates the total amount of explosives, the detonating cord length, and the number of primers. The cost of blasthole drilling can be calculated by the model based either on purchasing and operating a drill or on a user input value of the contracted cost of drilling. Application of the model to an example ore deposit showed that the vertical blasthole systems were more economical than the coyote system when there was no overburden and the deposit had an average ore thickness less than 45 meters. With no overburden and ore thickness greater than 45 meters, the vertical blasthole system was either more or less expensive than the coyote system depending on the number of levels used in the coyote system. With overburden, the coyote system was less expensive than the vertical blasthole system for blasting either the ore only or the ore plus the overburden. A coyote blast will usually produce larger particle sizes than a vertical blasthole system. Larger particle sizes can result in lower copper recoveries so that a less expensive coyote blast may not improve the overall economics of an in situ leaching operation. Blasting the ore zone only was generally less expensive than blasting the ore plus the overburden by either blasting system. Also, for the example considered, the coyote system costs were less sensitive to changes in overburden thickness and powder factor while the vertical blasthole system costs were less sensitive to changes in ore thickness.

Jan 1, 1977

By David R. Poirier

Activity data of carbon as a function of both temperature and composition throughout the stable austenite range is correlated by mearts of an equation derived from a quasi-chemical model. The carbon activity data of austmite for temperatures between 800° and 1200°C are utilized in conjunction with the activity of carbon calculated for the y solidus using the activity of carbon in liquid iron and published austenite-liquid equilibria. The results agree very well with Chip-man's correlation; however, a small difference in the activity of carbon in the high-temperature range of the austenite field is evident. Excellent agreement is found for the heat of solution of graphite in infinitely dilute austenite; from this study the value is 10,550 cal as compared with Chipman's value of 10,680 cal. AS part of a program to study microsegregation in dendritic solidification of ternary Fe-C-Cr alloys, it was desirable to be able to describe the equilibria between austenite and liquid iron in Fe-C-Cr alloys. In this regard, it was necessary to correlate existing data on the activity of carbon in Fe-C austenite as a function of both temperature and composition. At that time, Chipman's analysis1 of the thermodynamics of binary Fe-C austenite was not available. It will be shown that this study and Chipman's study agree rather well throughout the stable austenite range of temperature and composition; however, some small differences appear at temperatures greater than the eutectic temperature. Benz and Elliott 2 presented isoactivity lines for austenite superimposed on their revised Fe-C phase diagram. Using an expression from Darken and Gury 3 representing Smith's4 activity data between 800" and 1000°C, they found that the activities extrapolated above 1000°C to the solidus did not agree with the activities determined from the corresponding liquidus compositions. It is the purpose of the following argument to reconcile carbon activity data of austenite with the activity in liquid Fe-C alloys as determined by Rist and Chipman. 5 In addition, a simple analytical expression is sought for computational convenience. ACTIVITY DATA OF CARBON IN ZRON Fig. 1 shows the activity of carbon in Fe-C austenite as determined by Smith, 4 Schenck and Kaiser, 6 Scheil et a1.,7 and Bungardt et al.' The lines are merely drawn to separate the data into the respective isotherms. These data are inadequate to determine the activity of carbon at temperatures greater than 1200°C. The activity coefficient in Fe-C liquid alloys was assumed by Rist and chipmans to obey the following

Jan 1, 1969

By GEORGE L. CHRISTIAN

T HE Tonopah Extension assay office is a two- story, concrete structure on a solid foundation of andesite, situated about 100 yd. from the company's mill, so that it will not be affected by the stamps or the tube-mills; also it will not be affected by under- ground blasting. On the second floor are the mine superintendent's office and drafting and blueprint rooms. On the ground floor are the assayer's office,' mixing room, furnace room, crusher room, chemical laboratory, parting room, store room, and change and shower room for the mine superintendent, assayers, and engineers. The crusher room is outside of the main building, and has four concrete walls, thus eliminating the jar of the crusher; it is so situated that the least possible amount of dust spreads through the main building. An 8 by 10-in. jaw crusher, which crushes to ¼ in., was made by a local foundry. Attached to the top is a small galvanized-iron hopper covered with a ¼ in. screen, on to which the sample is dumped. The fines-pass through the screen into the hopper, while the oversize is dumped into the crusher. The crushed sample and fines from the screen drop down to a set .of splits suspended from an iron rod below the crusher jaws. The small sample is caught below in a small pulp pan. The rejects drop from the splits through a 2-in. pipe on to a bucket conveyor, which dumps into a galvanized-iron hopper in an upper corner of the room. The rejects drop through a 2-in. pipe to a reject bin outside the build- ing. This bin is constructed high enough for a truck to be loaded from it by means of a chute door on the side.

Jan 1, 1921

By T. A. Wright

The sampling of waste materials containing copper, lead and tin has taken on a new significance within recent years, and is of increasing importance, on account of the entry of some of the copper refineries into this field and the tendency towards consolidations among the smelters. In the past, such material was sold on the basis either of a rough or grab sample or of casual inspection of the lot. The two principal sources of this waste are the processes of fabrication and the scrapping of automobile, electrical, plumbing, railroad and other equipment. In both cases much material can be sorted, salvaged and sold by classification and grade to be melted "as is" or with the addition of new or virgin metal. The increasing care in classifying exercised in the large manufacturing plants tends to increase the proportion of this usable scrap; on the contrary, the increasing use of more complex and special non-ferrous alloys tends to make sorting and grading more difficult in turnings, borings, clippings, etc., and consequently is making sampling of more moment. In tin, lead, aluminum, and zinc furnace by-products such as ashes, drosses, skimmings, etc., the trade practice of evaluation has not varied much. For instance, tin drosses, battery lead, and aluminum skimmings are ordinarily sold on what is called "metallic button" or "metallic recovery" or ('metallic yield." Copper and lead waste, however, is being sold more and more on actual copper and lead contents based on sample and chemical analyses. This paper will be devoted chiefly to the sampling of materials suitable only for refining and recovery of one or more of the metals present. The methods described are often based on the fact that but one metal, such as copper, is to be paid for. The loss of volatile constituents in melting does not appreciably affect the final copper result, as the "after-melting" assay can be readily calculated to the "before-melting" basis, but if smelter efficiency continues to increase, so that in time zinc, for instance, may be recovered on a paying basis, the method of sampling dirty brass, for example, will have to be changed also. As a matter of fact, we may expect that improved refining processes will make possible the partial recovery of lead and tin which are now lost.

Jan 1, 1928

By D. H. Forbes, I. B. Cadoff, H. M. Manasevit

Single-crystal silicon films have been obtained on several natural crystal faces of BeO using the thermal decomposition of silane and the hydrogen reduction of silicon tetrachloride. From an analysis of X-ray diffraction data it was determined that the following film-substrate orientation relationships exist: (111) Si 11(0001) BeO, (111) Si 11(1011) BeO, (100) Si 11f1010) BeO. and (110) Si 11(1010) BeO. An analysis of the crystallographic relationships between the film and substrate indicates that a match occurs between the silicon atoms in the film and the berylliuni ion sites in the substrate. This correspondence is in agreement with previous work on the deposition of silicon on sapphire.1-3 silicon on spinel: and tungsten on sapphire. The high resistivity, thermal conductivity, and radiation resistance of beryllium oxide make it an important substrate material for the deposition of thin films of silicon or other semiconductors. The importance of semiconductor-insulator composites to the field of integrated microelectronics has been well-documented in the case of silicon on sapphire.'-' The successful growth of large-area single-crystal silicon on an insulator, sapphire, was first reported in 1963.1,2 Since that time studies have been made of the crystallographic relationships between the deposited film and the sapphire substrate. On the basis of the observed relationships, a model has been proposed relative to the crystallographic requirements for epitaxy between the semiconductor film and the metal oxide substrate.3 It is proposed in this model that epitaxy is the result of a match between atoms of the deposited film and the metal ion sites of the substrate plane. This match is not limited to a 1 to 1 correspondence between sites in the two lattices. Sub- sequent studies of the deposition of silicon on spinel4 and tungsten on sapphire5 have yielded data which support this model. On the basis of this previous work it was felt that silicon on BeO should also fit this model. In the present study, the choice of substrate orientation was limited to the natural faces of synthetic BeO crystals. Of the faces available, the (0001) plane seemed the most favorable for epitaxial growth. EXPERIMENTAL PROCEDURE Silicon films were deposited from silane and silicon tetrachloride in the apparatus shown in Fig. 1. The hydrogen ambient gas was purified by passage either through a DEOXO unit, molecular sieves, and a liquid nitrogen cold trap, or through a heated Pd-Ag thimble. The gas was then mixed with the silicon source materiai and passed over the substrate which lies on a spacer above an inductively heated silicon pedestal. The following deposition conditions were used: a hydrogen flow rate of 3 liters per min with silane and silicon tetrachloride concentrations of 0.2 mole pct and a pedestal temperature of 1175" * 5°C as observed with an optical pyrometer assuming an emissivity of 1.0. Deposition was preceded by a 15- to 30-min hydrogen-etch period conducted at a temperature of 1275°C (obs). Adherent silicon films from 2 to 10 u were grown on the various BeO faces. The substrates were synthetically grown beryllium oxide single crystals ranging from 5 to 10 mm in

Jan 1, 1967

air-lift and equipped with tapered tubing of proper design, we would have a gas input consumption of about 2500 cu. ft. per bbl., which at 3 to 4c. per 1000 cu. ft. would be 7 1/2 to l0c, per bbl., and there would be very infrequent loss of production due to stoppages. It has been demonstrated that with efficient design of air-gas lift, the production of wells can be increased much beyond that obtained with the former type of air-lift employed; also that small wells can be operated by air-lift with tapered tubing at a cost that places this method in competition with beam pumps in many fields. The next step in conservation that the writer expects to have an opportunity to demonstrate is that of restoring the pressure in a pool and producing by air-gas lift all of the oil possible to lift economically. This combined operation is probably the method toward which we shall eventually be working in recovering the maximum quantity of oil from pools where the oil is recovered through bore holes. General Discussion on the Air-gas Lift H. P. Porter, Tulsa, 0kla.—The papers presented at this meeting contain a great amount of valuable information. Wonderful progress has been shown in the development of air and gas-lifts. There has been nearly everything brought out that touches upon the subject. The real point that is lacking is exact knowledge of the velocity with in the flow column which will produce the best effect—that is the thing we must know more about. Velocity in Gas-lift Flow In other lines of industry the matter of velocity of fluids in pipe lines has been well analyzed and there are known laws by which to calculate velocity of flow; for instance, in irrigation work large pumps are designed with intake pipos to employ an intake velocity of 4 ft. per scc. By reduced cross-sect'ion the velocity is increased rapidly as it enters the pump and the discharge rate is at 12 ft. per src., which in turn is reduced in the discharge column to 4 ft. per sec. Crushed coal, grain and granular material is found to be best conveyed by air when a pneumatic conveyor is employed at 100 ft. per sec. As in the design of a pumping plant or a pneumatic conveyor, the velocity at the lower end of the column in the flowing well must be controlled within certain limits for best results. Mr. Griswold, I believe, stated that they had velocity as low as 15 it. per scc. and from that up to 78 ft. per sec. Mr. Pierce and Mr. Lewis showed an ideal flow column showing how the velocity increased as the fluid was carried up the column, hut did not give any figures as to the velocity. It would be well to take that sort of a diagram to establish an ideal velocity at the lower or intake end, and then calculate the velocity from expansion of the gas as it goes up. It may be that the, ideal intake velocity would vary, depending on the depth of the well, the quantity of liquid to be handled or the pressure which it may be desired to hold. The subject is one that might be worth much research.

Jan 1, 1928

By Charles R. Cavanaugh, John F. Elliott

The activity of nickel in liquid Pb-iVi alloys which are rich in lead was measured in the temperature region of 700° to 1100°C by means of the galvanic cell: The electrolyte used was stabilized zirconia. Tlze data were correlated using the a function, and a plot of the temperature coefficient aE/aT All subsequent calculations of the thermodynamic properties are based on these two functions. The activity, activity coefficient, and molar properties of mixing of nickel are reported. Nicke1 shows extreme positive deviations frorn ideality while lead shows a very slight positive deviation in the composition range studied The study of the activity of nickel in liquid Pb-Ni alloys reported herein was undertaken to explore the use of stabilized zirconia, an oxygen-ion electrolyte, with liquid-metal electrodes, and to obtain further information on the thermodynamic properties of the liquid binary Pb-Ni system. The cell The reversible electromotive force of the cell results from the difference in the chemical potential of the oxygen at the two electrodes: po, (left) - p~ (right) = -4E5 [I] The chemical potential of oxygen on the right is fixed by the activity of nickel in the solution and pure solid nickel oxide. That on the left is set by pure solid nickel in equilibrium with pure solid NiO. By definition: Since the chemical potential of nickel is related to the chemical potential of oxygen through the equilibrium constant for the formation of NiO from nickel and oxygen gas, the electromotive force of the cell is also expressed In this case, n is 2, E is the reversible potential of the cell, and 5 is Faraday's constant. The work of Kuikkola and wagnerl and Schmalz-reid2 has shown that the stabilized zirconia electrolyte is essentially an ionic conductor at the oxygen levels encountered in the experimental arrangement of the work, i .e., PG > 10-l7 atm. THE EXPERIMENTS The advantage of this type of reversible cell over those using a liquid electrolyte is the simplicity arising because the electrolyte also functions as one of the containing crucibles. A further simplification was the choice of the Ni (sat.)-NiO electrode as the standard. This permitted a ready check on the behavior of the electrolyte, as the potential of the cell must become zero when the right electrode becomes saturated with nickel, either because of a change of temperature or because of the addition of nickel to the electrode. It also permitted the potentials being measured to lie in the most satisfactory experimental range of 0 to 100 mv. Although it was not theoretically necessary, lead was included in the standard electrode as it assured good contact between the electrode and electrolyte. Cell Design. The general arrangement of the experimental cell assembly is shown in Fig. l(a) and the details of the cell itself are contained in Fig. l(b). The anode lead wire on the interior of the cell was connected to a coil of perforated sheet nickel. Within this coil were nickel oxide pellets which were held beneath the surface of the liquid Pb-Ni alloy. A disc of nickel oxide was held at the bottom of the external crucible (alumina) by means of the thermocouple protection tube. The nickel oxide disc and pellets were compressed dry at 10,000 psi and sintered at approximately 1000°C for an hour in air. A major experimental difficulty of reversible electromotive force cells with liquid electrodes is the selection of suitable materials for connecting

Jan 1, 1964

By Carlos G. Valenzuela

The value generally accepted for stacking-fault energy, of copper has been approximately 40 ergs per sq cm based on Fullman's2 value for the coherent twin-boundary energy and the assumption that is twice the twin boundary energy However, Thornton and coworkers8 determined that the lower limit of for copper is approximately 60 ergs per sq cm, based on measurements of dislocation-node radii. They suggested that the assumption of = 2t is invalid. It is the purpose of this note to present results which indicate that the values of obtained by measurement of twin-grain boundary intersections and the values obtained by measurement of dislocation-node radii are actually compatible. The most reliable values for of the a brasses, based on electron-microscope observation of dislocation nodes, are probably those values reported by Smallman and Green6 who applied the Siems correction (1961) to data obtained by Howie and Swann.3 These values shown in Fig. 1 give an extrapolated value of approximately 70 ergs per sq cm for pure copper. In the present work, Fullman's method for determining the stacking-fault energy of copper was extended to the a brasses. High-purity copper (99.999 pet) and high-purity zinc (99.999 pet) were mixed in proportioned amounts and melted in sealed and evacuated quartz tubes. The alloys were homogenized for a week at 750°C and chemically analyzed by means of X-ray fluorescence. These alloys, along with a specimen of pure copper, were rolled to 98 pet reduction and a thickness of 0.009 in., resealed, and annealed for 40 hr at 715°C. Values for the ratio of twin-boundary energy to the grain-boundary energy, it gb, were obtained from measurements of dihedral angles formed at the intersections of twin boundaries and grain boundaries by using Fullman's2 mechanical analogy of surface tensions acting at the intersection of an annealing twin and a grain boundary. The angles between the twin traces and the grain boundaries were measured for a large number of twin-grain boundary intersections at a magnification of X500 using a rotating mechanical stage on a Reichert metallograph. The rotary stage has a calibrated angle scale with vernier so that measurements can be made to 0.1 deg. The mean twin-grain boundary energy and standard deviation were calculated for copper and each of the brasses by the use of an IBM 7072 computer. It was found that the mean value of gb stabilized after approximately 100 twin-angle measurements. This was determined by plotting the mean against the number of angles measured. Since the measured angles deviate from true dihedral angles, a correction factor for grain orientation, discussed below, was applied. The stacking-fault energy was then calculated from these values and the values of grain-boundary energy derived by Taylor.7 The data obtained are tabulated in Table I. Values for stacking-fault energy are plotted in Fig. 1. The value of gb for the specimen of 1.03 pet Zn is close to the value obtained by Fullman2 for OFHC (99.98 pet) copper, 0.045. It is believed that the purity of the copper affects gb significantly. The 99.999 pet purity Cu used in this investigation yielded a value of yt/ygb, 0.76, which is much higher than that obtained by Fullman. Additional evidence suggesting that the purity of

Jan 1, 1965

By Meguru Nagamori

DURING the smelting of the sulfide ores of copper, nickel, and certain other metals, a matte phase is formed. For a better understanding of the physico-chemical properties of mattes, binary systems such as Cu-S, Ni-S, Fe-S, and so forth, should be studied, especially in the vicinity of liquid compounds such as Cu2S, Ni3S2, FeS, and so forth. These compounds are relatively stable in the solid state although they can exhibit appreciable deviations from stoichiometry. With small deviations from stoichiometry there are large changes in the activity of both sulfur and metal this is a characteristic of both solid and liquid sul-fides near the stoichiometric compositions. In the vicinityof molten Cu2S,1 for instance, the activity of sulfur increases about 100 times for a 0.012 increase in the mole fraction of sulfur and, correspondingly, the activity of copper decreases greatly. In this sens the minor deviations from stoichiometry should be carefully taken into account in studies of such metal-sulfur melts. Metal-sulfur melts may be considered to have properties intermediate between metallic solutions and molten salts, i.e., neither entirely metallic nor entirely ionic. The radius of the ion sZ- is 1.84 as compared with 1.04? for a single bond covalent s.2 It is therefore inferred that when the sulfur is more ionic its partial molar volume is larger, although metal-metal, metal-sulfur, and sulfur-sulfur interactions may bring about further complexities. Thus, it is to be expected that the molar volumes, which are derived from density-composition relations, will help in resolving the structure of the melts. In this study the maximum bubble pressure method with bubbling gases of H2, H2S, and Ar, .was employed to measure the density. EXPERIMENTAL Materials. Silver of 99.95 pct purity was melted in an alumina crucible and hydrogen gas was then bubbled through the liquid for the deoxidation. In preparation of Cu2S, electrolytic copper powder (>99.9 pct Cu) was mixed with precipitated sulfur and heated to 1200°C in an alumina crucible under a hydrogen atmosphere. Mixtures having the approximate compositions FeS and Ni3S2 were prepared by heating reagent grade electrolytic iron or reduced nickel powder with precipitated sulfur under a hydrogen atmosphere. The H2S gas was of 98.5 pct purity, the impurities being mostly CO2 and CS2 which hardly contaminate the melts. Apparatus. The crucible system is shown schematically in Fig. 1. To minimize the variation of melt composition during a density measurement, the apparatus was designed in such a way that either Ar, H2, H2S, or mixtures of these gases could be used as the bubbling gas. When the melt had a high partial pressure of sulfur, H2S gas was used. When the partial pressure of sulfur was so low that oxygen might dissolve in the melt, the use of H2 was preferred. In intermediate cases, argon or mixtures of H2-H2S were used. Density of Dibutylphtalate. Dibutylphtalate was used as the manometer fluid. Relative to distilled water, the density of the dibutylphtalate, pdib g per cc, was measured and found to be: pdib (25°C) = 1.046 i 0.002. With the use of the temperature coefficient reported by Kemppinen and Gokcen,3 the following value was

Jan 1, 1970

By J. R. Hornaday, A. E. Morris, N. A. Parlee, D. C. Carmichael

Rates of absorption and effusion of hydrogen in solid iron were measurede by a Sieverts type of apparatus. With clean a iron these rates are diffusion controlled down to 420°C and are represented by the equation D = 6.70 x e-'100' crn2 sec-I Certain surface impurities can affect these rates at all temper-atuves. Thin oxide films lower, the apparent diffusivity of annealed iron markedly. Cold-worked iron (75 pct) annealed at 430°C has practically the same solubility and diffusivity as anealed iron. THE mechanism of absorption and evolution of hydrogen in solid iron alloys is not fully understood despite the large number of investigations on the subject. While there appear to be many instances of simple solid-state diffusion control of rate, there are many cases where investigators have either concluded that surface reactions are rate controlling or that some "nondiffusible" hydrogen resides in discontinuities. The purposes of this research were 1) to develop a sound method for studying this absorption and evolution behavior, 2) to examine it in pure annealed iron, and 3) to determine the effects of important variables, such as cold work, surface condition, and composition. This paper relates the progress toward these objectives. Much of the present knowledge of the movement of hydrogen through iron alloys comes from permeability studies which involve the measurement of the rate of passage (under steady state conditions) through membranes of the order of 1 mm in thickness. This method is open to question on various grounds. If surface reactions are involved, two different surfaces operating under two different conditions must be considered. The presence of defects in the membrane even of microscopic dimensions may lead to erroneous results. A few people have studied evolution of hydrogen into vacuum, under carefully controlled (unsteady state) conditions, and some of the best diffusivity data come from these sources. Most of these methods measure rates of evolution only and thus do not make a rigorous test for reversibility of behavior. It appeared that an "unsteady state" method that would permit the measurement of both rates of evolution and absorption under controlled temperature, pressure, and other conditions would offer several advantages. Accordingly the modified Sieverts apparatus described below was designed and built. APPARATUS This apparatus is shown in Fig. 1. The sample bulb is detailed in Fig. 2. Hydrogen of 99.5 pct purity and argon of 99.99 pct purity were used. The hydrogen was deoxidized and dried by means of a Deoxo unit followed by a "Dri-erite" tower. The argon was only dried. The gas burette was graduated in tenths of a cubic centimeter, and, with the aid of a travelling magnifier, readings could be estimated to the nearest 0.01 cc. The level of mercury in the burette was adjusted by means of a leveling bulb operated by a fine screw adjustment. An electrical system, consisting of two slightly separated platinum electrodes inserted in one leg of the manometer and a small light bulb was used to obtain rapid accurate adjustment of the pressure. The capillary tubing of the Vycor sample bulb was 3 mm bore as was all tubing back to the gas burette. The samples were discs made from vacuum-melted Ferrovac-E iron of greater than

Jan 1, 1961

By C. H. Lee, R. Maddin

The diffusion rates of Ag110 in cylindrical single crystals of 99.99 pct pure silver, which were twisted to a total surface strain of 0.91 during the diffusion anneal at temperatures of 700°, 750°, and 800°C, were measured by sectioning and counting as a function of the strain rates. The ratio of the diffusivities while strain ing occurred (Ds) to those of the unstrained specimens varies linearly with the rate of twisting and attains values of near 100 for some of the rates used. The enhancement of diffusion by straining is inversely proportional to the temperature at which diffusion occurs. The activation energy for diffusion determined from the data plotted as a function of the rate of twisting decreases from 44,090 cal per mole for zero strain, to an asymptotic value of 21,000 cal per mole for the strain rates of 22 x it)"5 see-l. Qualitative explanation for the observations based on the generation of nonequilibrium number of defects by plastic deformation will be discussed. The initial research of Buffington and cohen1 on self-diffusion in a iron under compressive stresses contributed the first quantitative information concerning the effect of applied stresses on diffusion. These results were obtained from radioactive Fe55 plated on one of the horizontal surfaces and compressing the large-grained specimens while the diffusion-anneal was occurring. Enhancement of diffusion of a maximum of seventeen times was observed provided the strain was in the tertiary stage of creep and the rates of straining were at least as fast as rates used in the normal creep test. On the other hand, Darby, Tomizuka, and Balluffi,2 extending silver single crystals up to 30 pct elongation at rates of straining about equal to those used by Buffington and Cohen observed no effect. For the past two and a half years at the University of Pennsylvania, we have been investigating the effect or torsional strains on self-diffusion in silver single crystals. If enhancement is observed as has been reported1 a possible explanation may be based upon the generation of fairly large numbers of point defects and their role in the diffusion process. Hence, since torsion should produce an abundance3 of point defects, an increase in the diffusivity while the crystal is being twisted should easily be measured. EXPERIMENTAL PROCEDURE Our research uses single crystals of silver prepared from 99.99 Ag by the Bridgman method in a dynamic vacuum of less than 25 µ. As grown, they are about 25 cm long by 1.3 cm in diam. The crystals are cut into 7.5 cm lengths with a jeweler's saw and machined to the shape shown in Fig. 1. The test length of the crystal is machined to a 0.6 cm diam after which the ends are masked and the test section etched heavily in HNO3, and KCN:(NH4),S2Os , solution to remove the effects of machining. The specimen is then annealed in vacuum for 8 to 12 hr at 800°C to remove any residual stresses and also to recrystallize the end sections. The recrystallized ends are necessary since experiments showed that single-crystalline end sections are too soft to transmit the desired torque. Occasionally, recrystalliza-

Jan 1, 1960

By Paul F. Sikora, John W. Weeton, Philip A. Clarkin

Effects of variations in carbon content and micro-structure on the stress-rupture properties of a liquid-phase-sirztered, Izeut-resistunt alloy were studied. Using the powder rnetallurgy technique, specimens could be produced having stress-rupture profierties equivalent to or better than those of the alloy in wrought form. In addition, sintered specimens were easily hot worked even when carbon contents were as high as I pct. Correlations between stress-rupture properties and micro structure were obtained in some cases. IT is well known that many alloys used in high-temperature service are quite complex both from the standpoint of chemical composition and microstruc-ture. During the development of these alloys their complexity has in some cases led to treatment schedules which, while practical, often do not fully utilize available alloying elements. For example, in some alloys, massive carbides that form during ingot practice may never be dissolved by reasonable solution treatments and therefore are unavailable for subsequent precipitation hardening, Ref. 1. This investigation was undertaken to determine whether the powder metallurgy method of consolidation might provide distinct advantages over the conventional melting method. First, segregation of alloying elements might be eliminated or reduced and thus a more efficient use of these elements obtained. Second, the structures produced in powder specimens might differ considerably from those normally seen in castings, which would perhaps result in better response to subsequent mechanical or thermal treatments. If these results could be achieved, it was felt that both forgeability and stress-rupture properties might be improved. The alloy used in this investigation was S-816 produced by powder metallurgy methods. The influence of carbon content over the range of 0.1 to 1.0 wt pct was studied for the alloy in the as-sintered condition and after three additional treatments involving heat treatment, hot swaging, and combinations thereof. EXPERIMENTAL Standard S-816 has the composition shown in Table I. It is a cobalt-base alloy having a nominal carbon content of 0.4 pct and is classified as a precipitation-hardening alloy. This alloy was chosen because it is representative of a class of heat-resistant alloys and because adequate information was available concerning its response to various treatments and its subsequent properties. For this study, -100 mesh alloy powder having essentially the same composition as shown in Table I but without the 0.4 pct C was used. Desired carbon variations, achieved by wet mixing the alloy powder with graphite, ranged from 0.1 to 1.0 wt pct. Specimens were hydrostatically pressed and then sintered in vacuum by slowly heating until incipient melting was observed. Sintering this way gave a liquid phase in the interstices of the powder particles and achieved reasonably high densities. The average density of as-sintered specimens was about 95 pct of wrought alloy density. In order to obtain various microstructures, some specimens were heat treated (solution treated for 24 hr at 2150°F, water quenched; aged 16 hr at 1400°F, air cooled); others were hot swaged at 2150 o F (50 pct reduction in area), while still others were hot swaged (50 pct reduction in area) and then given the above heat treatment. During hot swaging it was observed that forgeability was quite good even when specimens contained as much as 1.0 pct C. Specimens were evaluated by stress-rupture test-

Jan 1, 1962

By P. R. Sperry, P. A. Beck, Hsun Hu

As described by means of quantitative pole figures, the inside texture of highly rolled aluminum and copper strips may be approximately described by four equivalent ideal orientations near (123) [121]. If rolled in reversed passes, the surface texture of copper is also near (123) [121], that of aluminum is (100) [011]. The inside texture of highly rolled brass is (110) [112]. The surface texture is the same, if rolled in reversed passes. The surface texture of all three metals is related to the inside texture, but asymmetrical, if rolled without reversal between passes. MANY previous investigations dealing with the subject of the present work were reviewed by Wassermann.1 Barrett,2 Brick,3 and Richards.' The recent introduction of quantitative methods for pole figure determination by Decker, Asp, and Harker,5 Schulz5 and others made it possible to reinvestigate some of the finer points which the earlier more qualitative photographic methods left undecided. The rolling textures of silver and of 70-30 cartridge brass have been quite consistently characterized by the ideal orientation of (110) parallel to the plane of rolling and [112] parallel to the rolling direction. On the other hand, it has been recognized by several investigators that certain other face-centered cubic metals, such as copper and aluminum, developed rolling textures rather different from that of brass. These textures have been variously described by the following ideal orientations, singly or in combinations with each other: (110 [112]: (112) [111]; (135) [335]; (135) [211], etc. The discrepancies usually have been attributed to the lack of sharpness in the textures and to the attendant difficulty of associating "ideal orientations" with pole figures showing great scatter of orientations. It seemed desirable to investigate by the new quantitative methods to what extent the apparent lack of sharpness may have been brought about by the qualitative methods used previously, rather than by the textures themselves, and to decide, if possible. between the various ideal orientations which have been proposed. Another problem, not satisfactorily settled by earlier investigations. concerns surface textures in rolled metals. For instance, in rolled aluminum the surface texture in some cases appeared to be similar to the texture inside the sheet, whereas in other cases it was reported to be entirely different.' The conditions under which such differences may have arisen, and the possibility of the occurrence of different surface textures in other face-centered cubic metals do not appear to have been examined in detail. The present work was undertaken to investigate the above questions. Some of the results obtained have been described- riefly. Experimental Procedure Specimen Preparation: In the present investigation 2s aluminum, electrolytic tough-pitch copper, and commercial 70-30 brass were used. These materials were available in the form of cold-drawn rods. 1 in. diam for tough-pitch copper and commercial 70-30 brass and 11/2 in. diam for 2s aluminum. The cold-drawn bars were alternately annealed and rolled 30 pct lengthwise in several cycles until a penultimate thickness of 0.500 in. was reached. The intermediate and the penultimate anneals were carried out for 30 min at 380°C with 2s aluminum, and for 30 min at 550°C with 70-30 brass. For tough-pitch copper, the intermediate anneals were 30 min

Jan 1, 1953

By R. F. Domagala, M. Hansen, D. J. McPherson

On the basis of metallographic analysis, incipient melting data, thermal analysis work, and X-ray diffraction, phase relationships in the 0 to 50 atomic pct Cr region were carefully resolved. Phase relationships in the 50 to 100 atomic pct region were outlined. A single intermediate phase, ZrCr,, was established in the system. A eutectic and a eutectoid were found in the zirconium-rich region of the system, while a eutectic was located in the chromium-rich region. Limited solubility of chromium in both a and a zirconium was observed. THIS is another in a series of papers on zirconium-base binary phase diagrams based on a program sponsored by the Atomic Energy Commission. The Zr-Sn,' Zr-Si,' and Zr-Mo and Zr-W" systems have already been published. Previous work on the Zr-Cr system includes a partial diagram by Hayes, Roberson, and Davies' and a complete diagram by McQuillan." The phase relationships reported by these authors were determined with magnesium-reduced zirconium, whereas those reported herein are based on iodide metal. Some X-ray work on the intermediate phase in this system was also reported by Hayes et al., as well as by Wallbaum.' Comparisons with these data are made in the appropriate sections. Thermal analysis, metallographic and incipient melting techniques were employed to accurately resolve phase relationships in the 0 to 50 atomic pct Cr region, while the remainder of the diagram is outlined on a basis of cast structures and thermal analysis. A description and analyses of the metals used in the preparation of alloys for this study are included in Table I. A "low-hafnium" zirconium crystal bar (Westinghouse "Grade 3") was used. This material was produced by the decomposition of a volatile iodide onto a hot zirconium filament. The as-received crystal bar was coated with corrosion product from a standard autoclave test by which its grade designation is determined. A sand-blasting and subsequent HF-HNO, pickling treatment was employed to remove this contamination. The bars were cold-rolled to approximately 1/32-in. sheet, pickled again, sheared to 1/4-in. squares, washed with acetone, and stored for use. Ingot chromium metal from National Research Corp. and electrolytic chromium flakes from Johnson, Matthey and Co., Ltd., were available as alloy additions. The ingot chromium was received in granular form. The large granules were sized by crushing, treated for iron removal, rinsed with acetone, and stored. The flakes were broken to approximately 1/8 in. with mortar and pestle, cleaned with acetone, and stored for charging. Experimental Procedure A nonconsumable electrode arc furnace identical to that described by Hansen, Kessler, and McPher-son,' was used in this work. A 400 amp dc welding generator was the source of power. To insure homogeneity, ingots were melted in a water-cooled spun copper crucible, a total of four times without opening the furnace. No difficulties were encountered in the preparation of these binary alloys. Analyzed chromium contents were found to agree very well with the intended content. Melts of pure zirconium were interspersed in the course of preparing the alloys and their hardness was measured to keep a constant check on the melting technique. Vycor and quartz bulbs were used to contain the samples for isothermal annealing treatments. Vycor bulbs were employed for temperatures up to 110O°C, while quartz was used above this temperature. For treatments up to 950°C the bulbs were evacuated before sealing, but for higher temperatures a partial pressure of argon was admitted to the

Jan 1, 1954

By WALTER B. JONES

PIG iron was first produced in Alabama in 1818 from limonite or brown ore and since then much of this ore has come from the so-called mineral district of northern Alabama, especially along the Cretaceous-Paleozoic contact. For many years the Russellville district in Franklin County, where the first blast furnace was erected, produced more than 100,000 tons of brown ore annually. Limonite has been reported at many places in the Coastal Plain region, where the formations are of Mesozoic and Cenozoic age, but these scattered deposits were never considered to be of much commercial importance. However, in the last three years a considerable quantity of this ore has been scraped up and shipped, particularly from the city of Greenville in Butler County.

Jan 1, 1938

By Zay Jeffries

A SURVEY of rare metals and minerals for the past year places uranium as one of two partners, the other being the neutron, in what historians will probably say is the greatest discovery in physics at least during the year and probably for a consider- ably longer period. The uranium atom has been made to divide into parts somewhat after the style of reproduction of the amoeba. When an amoeba divides into two parts, however, it produces two amoebae substantially alike and each substantially like the parent: furthermore, there is no considerable change of energy when this happens. When the uranium atom divides it yields other atoms such as barium and krypton with the complete destruction of the original uranium atom but with the liberation of a tremendous amount of energy. This will be discussed more at length later.

Jan 1, 1940

By E. S. Bumps

A series of macrographs are presented for the purpose of graphically recording the strain phenomenon that accompanies the energy transition in the Charpy impact testing of a mild steel that is susceptible to strain aging. STRAIN patterns in mild steel Charpy impact specimens were obtained in order to determine whether, on the first appearance of plastic strain during deformation, the initial fracture cracks appear in the region of plastic strain or in the elasti-cally deformed regions between. Although this attempt to locate the initiation of cleavage was not successful, the observed strain patterns illustrating various stress conditions in partially deformed Charpy specimens are presented along with a discussion of the possible dependence of transition energy on the yield phenomenon. Earlier work on the development of strain patterns in mild steel have been reported by Fry1 and later by Jevon.2 Harris, Rinebolt, and Raring3 observed characteristic strain markings on the surface of Charpy V-notch impact specimens fractured above and below the transition temperature which they presented schematically. It is intended that the strain figures presented here will add to the literature a graphic correlation of strain with transition energy in impact specimens. Samples of % in. round hot rolled, 0.20 pct C steel were machined to standard 0.394 in. sq, V-notch Charpy impact specimens. Preliminary testing involved determination of transition temperature, Fig. 1, using a Sontagg impact tester. These data were subsequently used to select temperatures above, within, and below the transition range at which specimens were partially deformed. Partial deformation was obtained by either varying the energy or the testing temperature, see Table I. Macroscopic strain figures shown in Figs. 2 to 19 were produced by several metallographic repolish-ing and etching steps. The macroetchant used was as follows:4 120 g HCl, concentrated; 100 ml water; and 90 g cupric chloride. Strain figures were obtained on the outer surface and on sections through the central portion of the impact specimens in order to determine an approximation of the volumetric strain pattern. In the tensile strain figures reported by Jevon, it was found that strain etching would not work immediately following strain unless the material was heated to 200°C. The impact strain patterns presented here were obtained without this heating, but the specimens were not etched until ten months after straining. This confirms a discussion of Jevon's paper, in which it was pointed out that strain figures can also be developed after aging for long periods of time at room temperature. Hardness of the strained and unstrained portions, revealed by the etched pattern, was explored using R, impressions converted to R, hardness values. Discussion of Results In the impact test, as in the tensile test, some parts of the specimen yield and deform plastically, while other regions are deformed only elastically. The plastic deformation bears a relation to the imposed stress pattern. In the strain figures presented here, the plastically deformed regions are the dark etching ones. The strain figures are always symmetrical because the stress state in the Charpy-type specimen under impact loading is symmetrical. The difficulties encountered to produce initial cracks are intimated in Figs. 2 and 4. At a temperature of —75ºF, the stress was not sufficient to pro-

Jan 1, 1953

By Sven Fornander

An account is given of the way in which a new process for desulphurization of hot metal is carried out at a Swedish blastfurnace plant. In the process powdered burnt lime is used as a desulphurizing agent in a rotary furnace. Results are given. IN a paper by Kalling et al.* the fundamentals of a new process for desulphurization of hot metal using powdered burnt lime as a desulphurizing agent were outlined. The purpose of the present paper is to give a brief account of the way in which this process is being carried out in practice by Surahammars Bruks AB, Sweden, and of the results obtained. + The hot metal from the blast furnace is tapped into a ladle of 15 tons capacity and transferred to a rotary furnace, a simplified drawing of which is given in Fig. 1. The rotary furnace has a total length of about 160 in. and an outside diameter of the rings of about 130 in. The furnace is in a horizontal position, with its rings placed on four rollers, and can be rotated by a driving mechanism at various speeds of up to 34 rpm. The rotary furnace and its driving mechanism were designed and constructed at Surahammar. The hot metal is charged into the rotary furnace through the opening to the left in Fig. 1. See Fig. 2. An addition is then made to the furnace consisting of finely ground burnt lime amounting to 2 pct of the weight of the hot metal as well as 0.5 pct of coke breeze. After the additions are made, the furnace is sealed to the atmosphere by means of two lids and set in rotary motion at a rate of 34 rpm. The sulphur in the hot metal is rapidly absorbed by the lime added, the time of treatment needed is normally 30 min. The process is then stopped, the lid is removed, and the furnace is lifted up by a crane and used as a tilting ladle for pouring the metal into the pig-iron molds, Fig. 3. Process Metallurgy The hot metal charged into the rotary furnace has a composition which usually lies within the following limits: C, 3.70 to 4.10 pct; Si, 0.80 to 1.80; Mn, 0.40 to 0.80; P, 0.025 to 0.030; and S, 0.060 to 0.200. Figs. 4 and 5 give examples of the changes in hot metal composition taking place during the treatment in the rotary furnace. As will be seen from the diagrams, the sulphur content of the metal decreases very rapidly during the first 10 min of treatment from about 0.100 to about 0.020 pct S. During the following 20 min, the sulphur content goes down slowly to about 0.005 pct S. The carbon and silicon contents of the metal decrease by about 0.10 pct each during the treatment. The manganese and phosphorus contents remain unchanged. Thus, if the process is started with an iron of the composition given above, the finishing composition of the metal usually lies within the following limits: C, 3.60 to 4.00 pct; Si, 0.70 to 1.70; Mn, 0.40 to 0.80; P, 0.025 to 0.030; and S, 0.002 to 0.020. The chemical reaction taking place during the process can be written:

Jan 1, 1952

By William L. Batt

FROM the time the Japs overran the Far East, the United Nations faced a serious military problem in the critical shortage of many raw materials desperately needed to prose¬cute the war on two fronts. For many months this critical shortage threatened substantially to limit the gigantic effort to get shooting equipment into the hands of the fighting men on the far-flung battle lines. Now this crisis has been met. Solvency in raw materials has been achieved. Simply stated, this job of producing solvency has been done by "cutting cloth to fit the garment." This does not mean that we have all the raw materials we need. Unfortunately, a few raw materials are still short, thereby limiting the total production of certain war goods, or making these goods less effective. Where the supply of raw materials is known to be limited, however, substitutions have been made or production schedules have been geared to the amounts available, and an over-all balance has been achieved between various parts of the war-production program.

Jan 1, 1943

By Charles Law McCabe, Lyndon H. Everett, Edna A. Dancy

It has been found that the carbide phase present at equilibrium in the system M-H2-CH4, at about 600°C, is MC for the rare-earth metals Ce and Pr. X-ray diffraction analysis showed that the monocarbides have fcc structures with lattice constants of 5.036 + 0.009Å and 5.131 + 0.001Å for CeC and PrC respectively. Gaseous equilibrium measurements were used to calculate the standard free energy of formation of the monocarbides from the elements. for the formation of (+ 1300) for the formation of PrC. THE rare-earthdicarbides, and their crystal structures, have been known for some years,l but only more recently were the carbides CeC,2,3 Ce2C3 2 and CeCS3 reported. In 1958 to 1959, Spedding et al. published work on the lanthanum-carbon system4 and other rare-earth metal-carbon systems,5 proving the existence of M2C3 and MC2, and measuring the lattice constants. They also demonstrated that tri-rare earth carbides, M3C, exist for the rare-earth metals samarium through ytterbium. However, they concluded that the cerium monocarbide reported by Brewer and Krikorian2 and by Warf,3 and given a fcc structure with a lattice constant of 5.130Å bythe former workers, was, in fact, cerium metal with carbon dissolved in it. They were also unable to find any evidence for the existence of Warf's CeC3, for which no structural details had been given. Even more recently, Palenik22 reported the existence of only M2C3 and MC2, having been unable to find any evidence for the existence of any other rare-earth carbides. There are no published experimentally derived thermodynamic data for the formation of any of these carbides, although Brewer and Krikorian6 have estimated values of for CeC, Ce2C3 and CeC2. The objective of the present investigation was; to determine experimentally the free energy of formation of any of the reported carbides of cerium and praseodymium, through a study of the rare-earth metal-hydrogen equilibrium. EXPERIMENTAL A methane-hydrogen mixture was circulated, in a closed system over previously prepared cerium or praseodymium hydride, and when equilibrium had been attained, the gas mixture was analyzed by selectively oxidizing the hydrogen and condensing out the water formed. The metal hydrides were used as starting material for convenience because, otherwise, the hydrogen in the gas mixture would immediately dissolve in the metals; in addition, the metals would not react with methane alone at the experimental temperature (around 600°C). The circulating system was based on that used by Browning, DeWitt, and Emmett7 for similar studies on iron carbides. It consisted of a quartz reaction vessel, all-glass circulating pump, analysis tube containing copper oxide that could be heated to 300" C by means of a small furnace, a solid CO2-methanol trap, and a double limb absolute manometer, Fig. 1. A cathetometer, capable of reading to 0.005 cm, was used to measure the difference in height between the two columns of mercury. In its final form, the reaction vessel was enclosed in an outer jacket, containing approximately the same pressure of hydrogen as that within, to reduce errors due to diffusion of hydrogen out through the fused silica of the reaction vessel., The circulating system was supplied with

Jan 1, 1962