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By S. Skowronski

The melting of cathode copper, ususally containing 95.98+ per cent. • Cu, would appear to be a simple matter. Owing to the well known affinity of copper for sulfur, however, so much sulfur is absorbed by the copper during the operation that a long and expensive refining process is required to remove it, and the final product is inferior in purity and lower in electrical conductivity than the original cathode copper. The furnace operation, as now conducted, includes the following stages: 1. Charging the cathodes into the furnace. 2. Melting the cathodes. 3. Oxidizing period—saturating the copper with cuprous sub-oxide and bringing the metal to the condition known as "set copper;'' this is now done by blowing air into the molten bath of metal. 4. Reduction period, otherwise known as "poling," whereby the oxygen previously added is removed by covering the molten bath completely with coke or charcoal and introducing large poles of green wood; this reduces the cuprous sub-oxide, bringing the copper to the "tough pitch" stage ready for casting. 5. Casting Period. Many experiments have been made to obviate the long periods of oxidation and subsequent reduction, with no success. While the copper first cast will be good, as indicated by the set surface of the bars, it is impossible to hold it to the "tough pitch" condition, and long before the whole charge has been poured the copper will become "overpoled," entailing numerous difficulties. Sulfur has always been blamed by the furnace men as the reason why this refining process is necessary, yet the literature on the subject does not sufficiently emphasize how small a proportion of sulfur will ruin copper for practical purposes. The sulfur absorbed by copper during the melting period comes from two sources: (1) the sulfate left on the cathode sheets in the tank houses; (2) the fuel. The percentage of sulfates on the cathodes is variable, and depends on the care taken in washing the cathodes after removing

Jan 1, 1919

By M. A. Hunter

This paper gives the results of an investigation of the specific resistance and temperature coefficient of the electrical resistance of nickel and its important alloy, monel metal. For most of the pure metals, the temperature coefficient of resistance is approximately 0.004 per degree centigrade at 20" C. Nickel and iron, however, are exceptions. This property is important as it gives us good material for the construction of thermometers and other instruments involving electrical control. A summary of information on this subject has been publishcd by the Bureau of Standards.l The present experiments antedate this publication by several years and as the information obtained is not contained in it, the results of the experiments arc published as additional information. Electrical Properties of Pure Nickel It is generally conceded that the lowest values for electrical resistance are obtained in the purest metal. In the case of nickel, the best material obtainable is electrolytic nickel, which contains approximately 99.80 per cent. nickel, 0.15 per cent. iron, and 0.05 per cent. copper. Any cobalt that may be present is included in the nickel figure. If the elcctrolStic sheet has been deposited without intermission, it is possible to cut a section from the sheet and roll it into wire without melting. By this means a nickel wire may be obtained that is uncontaminated by any of the impurities always taken up by nickel during melting. Two samples of nickel wire obtained from different electrolytic nickels had the follolving electrical resistance and temperature coefficient of electrical resistance: Specific Temp. CofEE. Sample MateRial ReSISTance peR Deg. C. NO. 1 Electrolytic nickel.................... 7.55 0.00550 NO. 2 Electrolytic nickcl ................... 7.60 0.00553 * Rensselacr Polytechnic Institute. Director of Research, Driver-Harris Co. Russell Sage Laboratory, Rensselaer Polyt,ecllnic Institute. 1 U. S. Bureau of Standards, Circular 100 (March, 1921).

Jan 1, 1923

Through the generosity of Sir Robert Hadfield, Honorary Member, the Directors of the American Institute of Mining Engineers are enabled to announce the Hadfield Research Prize of $1,000 for the best contribution to the publications of the Institute upon the general subject of The Different Forms and Combinations of Carbon with Iron, including those in Iron Alloys. The prize will be awarded at the Annual Meeting of the Institute in February, 1916, to the best paper upon this subject which is presented to the Institute before Nov. 1, 1915, provided such paper is deemed worthy by the Institute's Iron and Steel Committee. The following suggestions are also added for the guidance of those who may take part in this research. While' it is not desired to define closely the exact lines or scope of the proposed research, as it is advisable to make these as broad as possible, the object in mind maybe said to be generally as follows: To elaborate and find out the best methods of determining the forms of carbon in steel or iron, including those in iron alloys. A portion of the work would probably be a continuation of the researches which have in the past been carried out by Jullien, Abel, Muller, Ledebur, T. Sterry Hunt, Akerman, Arnold, Stead, E. D. Campbell, Hogg, Parry, Upton, and others. In a generic way, metallurgists now speak of carbides, sub-carbides, double carbides, special carbides, and other combinations. It is very desirable that these should be accurately defined and understood. It is also desirable to know whether there are other or new forms; if so, can these be separated and their characteristics obtained. It may be interesting to point out that the carbon compounds now definitely known are stated to number over 80,000. It is very probable, therefore, that there is room for much valuable and useful research to be carried out with the object of increasing our knowledge of the various combinations of carbon with iron, as probably some of these are still unknown

Jan 5, 1914

By A. B. Stevens, C. J. Coberly

The absolute porosity of a rock or sand may be defined as the volume of the interparticle space expressed as a percentage of the total rock volume. The effective porosity as contrasted with the absolute porosity is the volume of the interparticle spaces which intercommunicate with passages of sufficient size to permit the entrance or recovery of gas or oil, also expressed as a percentage of the total rock volume. A knowledge of effective porosity is of prime importance in estimating the ultimate recovery to be expected from oil and gas-bearing formations. The determination of the effective porosity of a rock includes the measurement of two values: (I) the volume of the rock as a whole, and (2) the volume of the grains and sealed pore space. This paper deals with a new apparatus which has been called a "hydrogen porosimeter" for determining the volume of the grains and the sealed pore space. This volume is determined by means of the pressure relations established in the instrument by the introduction of a known quantity of hydrogen. The Hydrogen Porosimeter The apparatus used in this work consists of an upper chamber for measuring the gas, a lower chamber for holding the sample to be tested, a gage for measuring the pressures, a tank of hydrogen, and the necessary connections. (Figs. 1 and 2.) Of the several gases that might be used for this work, hydrogen has been chosen for three reasons: (1) it deviates less from the gas laws than most gases; (2) it readily penetrates the sample; (3) it is absorbed less than most gases by the solids and liquids with which it may come in contact. Method of Operation After placing the sample to be tested in the lower chamber, the apparatus is thoroughly flushed with hydrogen to remove all air from the system, which is then brought to atmospheric pressure Po. The valve connecting the two chambers is next closed and the pressure in the upper chamber is brought up to a pressure PI by admitting gas from the tank.

Jan 1, 1933

By F. G. Miller

Earlier studies of the mechanism of flotation showed that coal flotation products are contaminated by composite coal and mineral particles. The mineral matter of these particles has the dual effect of increasing the specific gravity and decreasing the coal surface of the particle available for bubble attachment. The present study showed that these particles are more loosely held in the froth column than the high grade coal particles, especially in the coarser sizes. Consequently, it is possible in the laboratory to produce a secondary concentration of the product by sprinkling the froth product with water to wash these loosely held particles from the froth during formation and recovery. To improve coal flotation, Bethlehem Steel Corp.'s research department has been working on a number of related problems based on both physical and chemical factors. The ideal is of course full understanding of the interrelated effects of both sets of factors. However, detailed studies1 of each physical factor have produced immediately usable results in commercial coal flotation and are providing the basis for our current work on the effect of chemical factors. Since these detailed studies provided the basis for the present investigation of froth sprinkling, their key results are highlighted here. For example, for a highly floatable bituminous coal, particle floatability was shown to be directly related to the percentage of coal surface available for bubble attachment and inversely related to particle mass. The data also underscored that in a given size range the addition of mineral matter to a particle makes flotation more difficult both by adding to the mass of the particle and by decreasing the amount of coal surface available for bubble attachment. Size also affects particle floatability in that as the size of particles of a given specific gravity increases, mass increases and the ratio between coal surface area and mass of the particle decreases. Flotation tests showed that any recovery of the coarsest particles in a coal feed is accompanied by progressively higher recovery of finer and finer particles. Consequently, fine high-specific-gravity particles are recovered with the coarse good coal. As a result, when the entire 14 mesh x 0 size range is processed by froth flotation, the good coarse coal is contaminated with high-specific-gravity fines. It is the small quantities of these fines that must be rejected from the froth product if flotation efficiency is to be increased above its present level. These principles and findings, together with work by Professor V. I. Klassen,' led to the froth sprinkling investigation reported in this paper. Working with Russian coals, Klassen had shown that froth sprinkling washes loosely held refuse particles from the froth and compensates for the water lost in the upper froth layers and increases its stability. As a result, the coal particles are retained in the froth and the loss of coarse coal from the froth is prevented. Decreases in ash of 0.1% to 1.5% were reported by Klassen. Working with a 28 mesh x 0 American coal, the author of the present paper found that single-stage flotation coupled with froth sprinkling produced a product comparable to that obtained by the more expensive method of roughing and cleaning.3 The investigation reported in the present paper expanded study of the effect of froth sprinkling to include each of the standard size fractions of a bituminous coal. The main findings are as follows: (1) For those size fractions between 48 mesh and 150 mesh, froth sprinkling produces a marked reduction in both sulfur and ash. In the case of those sizes coarser than 48 mesh, while this reduction is not as significant, the additional benefit of shorter retention time is still a plus for froth sprinkling. Furthermore, when froth sprinkling is coupled with normal fast flotation, the product purity approaches that obtained by starvation reagent feeding, i.e., gradual feeding of flotation reagent to float the recoverable coal from the pulp slowly in several increments. The specific results for these two size groups are: (a) 14 x 48 Mesh. By using froth sprinkling with fast flotation, product sulfur can be reduced to a level

Jan 1, 1970

By F. W. Archibald

The American Smelting and Refining Co. has standardized its copper converting practice to attain a maximum unit blister production with a minimum of refractory consumption by careful location of the tuyeres and by applying magnetite coatings on the hard-burned magnesite brick linings. THE American Smelting and Refining Co. operates four primary copper smelters in the United States with a total of 17 Peirce-Smith type converters; 15 of them are 13 ft in diameter by 30 ft long, and two are smaller. Some details of operations vary with locale; however, fundamentals of design, operation, and maintenance are common to all plants. All converter shells are l-in. thick except for one new converter with riding rings on the ends which has a shell thickness of 1 1/2 in. More tuyeres can be installed with rings on the ends and hence more air can be used. Welded construction is replacing riveted. Minor shell repairs are made after each campaign. Principal causes of complete shell replacement are warpage and cracking resulting from localized over-heating. A 13x30 ft shell is being replaced after 34 years of operation and a total production of approximately 750,000 tons of blister. Converters are driven by 80 hp DC motors through company-designed worm gear reducers. Rotation is 0.38 rpm which permits the skimmer to spot the converter quite accurately for skimming slag. At three of the plants, protection against unscheduled air or power failures is afforded by the installation of emergency drives, consisting of auxiliary air motors or storage batteries. In order to avoid excessive splash out of the converters, the converter mouths are located as far back on the shells as existing flue facilities will permit. At one plant, the back of the mouth is only 13" to the rear of the vertical center line of the converter,. whereas it is 28" at another plant. Newly-lined mouth areas vary from 36 to 44 sq ft with effective operating areas about 25 pct less. It is important to keep the converter mouths as clean as possible. Dirty mouths create back pressures in the converters and as a consequence the tuyere air volumes are reduced. Mouths are generally cleaned by bumping with an empty ladle. Small mouth-cleaning rams have been used but unless extreme care is exercised the brickwork may be damaged. After considerable experimentation, the plants standardized tuyere elevations at 4 to 4% in. below horizontal center line at the shell with a downward pitch of about 13/16 in. per ft of length. Tuyeres are spaced at 6 in. centers except at the riding rings where there are no tuyeres. With this tuyere location, several of the plants now freeze magnetite slag in the bottoms, fronts, and backs up to the bottom of the tuyeres to control the internal shape of the converter. This has the effect of improving the agitation and mixing so that there is a marked increase in converting speed besides affording protection to the brick lining. Currently, the trend is to increase tuyere diameters from 1% to 2 in. to increase the air flow. At present, all converters are hand-punched but one converter is being equipped with a set of mechanical tuyere punchers. Rods for punching are % in. hexagonal smelter bar upset to ll/s in. and rods for cleaning tuyeres are upset to about 1% in., or larger, depending upon the tuyere diameter. Two of the plants use pneumatic reamers for cleaning the tuyeres between charges to minimize disturbing the coating on the inside of the refractory lining. Most of the puncher's platforms are pneumatically or hydraulically mounted so that a convenient punching position can be maintained regardless of tuyere position. For normal operations, tuyere air pressures vary from 15 to 13.5 psi, although some cycles such as magnetiting require pressures down to 8 psi. Air requirements vary from an average of 25,000 cfm on the newer installations down to 12,000 cfm on the older ones. Converter hoods are designed to protect the punchers from sparks, splash or hood accretions as well as to prevent the escape of objectionable

Jan 1, 1955

By C. Gatlin, N. E. Garner, A. Podio

Experimental data from single chisel blows on Leuders limestone are presented. A pressure chamber, similar in design to well known microbit drilling chambers, was utilized to impose variorcs stress states on the sample. Confining pressure of zero to 10,000 psi and borehole pressures from zero to 5,000 psi have been used in the studies. Pore pressure was zero and the rock samples dry in all instances. Force-displacement records and visual examination of the craters indicate that the mode of failure depends on both confining and borehole pressure in certain ranges, ranging from brittle, through a transition, to near plastic. The mode of failure is reflected in the observed blow force and energy data, as well as the shape of force-penetration curves. INTRODUCTION A previous paper' presented initial data from the project on which this paper is the second report. While the first paper dealt with impact studies on synthetic rocks, the literature cited there is also pertinent to this paper, but will not be listed again in order to avoid needless repetition. This paper presents experimental data from single chisel impacts on limestone at certain simulated wellbore stress states. Specific variables investigated were combinations of borehole and confining pressure, crater geometry, a narrow range of impact velocity and the forces required to drive the chisel into the specimens under the varying conditions. EXPERIMENTAL PROCEDURE The same basic apparatus described in our earlier paper, except for the pressure vessel, was used in this study. Fig. 1 shows the complete experimental system. Fig. 2 shows details of the pressure cell, which is quite similar to the well known microbit drilling chamber. The confining (overburden) pressure system provides independent pressure control over the sample except for two, 21/4 in. diameter areas located on the sample ends. These two areas provide a pore pressure entrance on the bottom and a striking surface on the top where borehole pressure can be controlled. The ends are isolated from the confining pressure by O-ring seals. The borehole and pore pressures are related through the striking surface; they will be the same unless a seal is deposited on the borehole surface, either a mud cake or some other impermeable membrane. In these studies pore pressure control was not used, as the rocks were dry and unsaturated in all cases. Rock samples were prepared from 4-in. cubes as illustrated by Fig. 3. The circular disks of adhesive vinyl plastic protected the impact surface from the resin coating (Scotchcast No. 2) and were removed just prior to each test. This procedure insured a fresh uncontaminated surface for the impact. Fig. 4 shows the dimensions and loading of the sample, including the concentrations around the "borehole" periphery (O-ring seal). The rock used in this study was Leuders limestone, of Permian age (Leonard), quarried near Leuders, Tex. Geologically, Leuders limestone is a light gray, fossili-ferous limestone (oolitic foraminifera1 biosporite). Its fossil content is 80 to 90 per cent and consists primarily of calcitornellid, ostracods, pelecypods and oolites with the remaining part intraclasts. There are hematite or limo-nite rims on some of the intraclasts. The porosity is approximately 20 per cent, but the permeability is less than 1 md. There is no apparent orientation in the structure. Triaxial tests have been conducted to determine the variation of the physical properties of Leuders limestone in three orthogonal directions', and it is known to be unusually isotropic and uniform. Physical parameters for this rock are: uniaxial compressive strength = 9,700 psi; F = 32 and C = 2,700 psi; where + and C are Coulomb equation values (t = C+u tan +). Impact tests were run under the combinations of confining and borehole pressures shown in Table 1. Samples were dry with atmospheric pore pressure in all cases. Tests, in which elevated borehole pressures were applied, used a single layer of household Saran-Wrap to prevent horehole fluid invasion into the sample. This proved to be simple and reliable. The blunt wedge used in all the tests was 0.75 in. long and had an included angle of 60" with a 0.05-in. flat. In addition, a sharp 60" wedge was used for all confining pressures at zero borehole pressure. The chipper speed

By G. Venturello, C. Antonione, G. Della Gatta

Results from work on the effect of inferstitials on recovery and recrystallization of' very pure iron (99.995 pet) doped with nilrogen up to 400 ppm are reported. Nitrided specimens were obtained by heating the iron in a static atmosphere of NH3 + H2. The samples were cold-rolled 80 pet, subjected to a series of isochronal and isothermal anneals, and submitted to examination by X-rays, micrographs, and hardness tests. Small additions of nitrogen show a strong effect in reducing recovery of' the mechanical properties of high-purity iron. At the temperatures of. the experiments, this effect proved greater than in the case of carbon. At 400°C pure iron recovers more than 50 pet of the total hardness increase, carburized iron vecovers 25 pet, and nitrided iron only 10 pet. On the other hand. the addition of nitrogen has, similarly to carbon, a very small effect on recrystallization; the effect is, however, slightly higher than that of carbon. When the concentration Of nitrogen is above the solubility limit in a iron at the temperattue of the experiments, an increase in the frequency of nu -cleation is also observed. THE object of the present work is to improve knowledge on the effect of interstitials both on recovery and on primary recrystallization of pure iron. In fact. at present there are no available data on the effect of nitrogen on high-purity iron. The only work which at present can be somewhat related to this problem is a work of Leak et al.1 in which grain boundary internal friction at high temperature in the presence of increasing amounts of nitrogen is studied by a torsion pendulum. The present work is a continuation of a previous one2 on the effects of carbon. EXPERIMENTAL PART Preparation of the Material. Pure iron was prepared following the same methods used in the pre- vious work2 and was nitrided using controlled quantities of ammonia in an apparatus similar to that used for carburizing. The apparatus consists essentially of a gas-tight quartz tube containing the specimens. The tube, maintained at constant pressure by means of a mercury seal, is placed in a resistance furnace. For nitriding, the NH3 + H2 atmosphere with a suitable concentration of NH3 was introduced into the tube, which had been previously carefully evacuated and degassed by heating at 600°C. The hydrogen used was carefully purified by passing it through a palladium filter. The ammonia required was prepared with the following reaction: CaO + 2NH4CI —CaCl2 + H2O + 2NH3 by heating the mixture of CaO and NH4C1 in a glass flask and then collecting the ammonia in a graduated Hempel burette. For each nitriding program a given amount of NH3 prepared by this method was introduced together with the H2 into the tube previously evacuated. Nitriding of the sample was then performed at 570°C for 48 hr. After this, to ensure a homogeneous distribution of nitrogen, the samples were further heated for 72 hr at 800°C. With this method which uses a static nitriding atmosphere, carefully controlled conditions of purity are obtained. Contrarily, with the conventional continuous-flow methods, using large quantities of circulating gas, there is a greater risk of introducing impurities into the samples. Furthermore, the required nitrogen concentration in the specimen is easily predetermined and obtained. A plot of the relation observed between the initial concentration of NH3 in the gas and the quantity of nitrogen introduced into the iron samples is given in Fig. 1. The data refer to samples of 1.2-mm thickness and to the nitriding conditions previously described. Furthermore, as a comparison, the data relative to two 0.5-mm-thick samples are reported. The presence of a reservoir in the cold zone of the reaction bulb made possible the gradual dissociation of ammonia on the sample in the hot zone. Internal-friction methods were used to determine the content of nitrogen dissolved in the iron samples. Some analyses were also carried out with chemical methods. The following table, Table I, shows a comparison of data obtained with chemical and internal-friction methods. The correspondence between chemical methods and internal-friction

Jan 1, 1964

By R. V. Smith, E. J. Dewees, R. H. Williams

Before this paper was presented, the terms "f" and "v1/f in flow equations had been called "friction coefficient" and "friction factor," respectively. However, many authors have used the names for the terms interchangeably, with the result that considerable confusion has existed in the literature on flow of fluids. In an effort to establish a clear and concise terminology for these terms, the authors have designated f as "resistance coefficient" and dm as "transmission factor." Transmission factors for the flow strings of gas wells were determined by tests on wells in six fields of Oklahoma, Texas, and Louisiana. Data were collected on 14 gas wells while gas was flowing through 1 1/4, 2, 21/2, and 3-in. tubing and 51/2 and 7-in. casing. The transmission factors developed from these data were found to follow the resistance equation published by Nikuradse1 for turbulent flow in "rough" pipes with an average absolute roughness of 0.000,65 in. This average absolute roughness is believed to be representative generally of the flow strings of gas wells with the exception of those that have been exposed to corrosion or other conditions causing undue roughness. Also, use of an absolute roughness of 0.000,65 in. probably will result in transmission factors that are more representative of gas-well conditions than those in common use today, provided that the transmission factors are calculated by the methods outlined in this report. The authors believe that use of these transmission factors will permit calculation of more accurate subsurface pressures in gas wells than those in use today. Engineers use transmission factors in flow equations to compute subsurface pressures in flowing gas wells from measured wellhead pressures. These subsurface pressures are necessary for determining the productivity of gas wells from "back-pressure" tests. The methods of calculating pressures in flowing gas wells, as outlined by Rawlins and Schellhardt2 in Bureau of Mines Monograph 7, are based on the transmission factors in the well-known Weymouth formula" Natural gas engineers have realized that errors introduced by using transmission factors as given by the Weymouth formula are relatively unimportant in testing low-capacity gas wells; but they also know that such factors are important considerations in testing large-capacity wells. Accordingly, the research described in this report was undertaken to fulfill the need for more accurate means of calculating subsurface pressures in gas wells. This report is part of the Bureau's study of the flow of natural gas through pipe and commercial pipelines. Several of the conclusions regarding flow in the flow strings of gas wells were influenced by the results of the study of flow in horizontal pipelines. These instances are mentioned in the text of this report. METHODS OF COMPUTING TRANSMISSION FACTORS Methods and procedures for computing transmission factors for turbulent flow in circular pipes from test data taken on gas wells have been derived and explained in detail in a paper by Smith4. As these methods were used to calculate the transmission factors presented in this report, a summary is included. Starting with

Jan 1, 1955

By H. T. Clark

NO previous determinations of the deformation or recrystallization textures of titanium or of titanium-base alloys have been reported in the literature. The room-temperature structure of titanium is hexagonal close-packed with a c/a ratio less than 1.633. It would be expected, therefore, to have a rolling texture similar to that of other hexagonal close-packed metals, namely (0001) [1010]. Burgers and Jacobs1 have shown that zirconium, a metal isomorphous with titanium in its structure and similar in many of its properties, has such a texture with a scatter of the basal plane toward the transverse direction. This scatter is in the opposite direction from that found in magnesium by Bakarian2 but similar to that reported by Smigelskas and Barrett3 or beryllium. The rolling and annealing textures reported here for high-purity iodide titanium are significantly different from the . textures of any other hexagonal close-packed metal. All titanium used during this investigation was prepared by the iodode process." The annealed hardness of this material varied from 73 (material used for sample No. 2) to 97 Vickers hardness number. An estimate of the chemical composition of this grade of titanium has been reported by Finlay and Snyder.5 With one exception, shown in table I, the as-deposited titanium was cast into 10 to 20 g ingots in an electric arc furnace in purified argon before being rolled to sheet. The cast ingots were forged and ground until their cross-section was approximately rectangular, annealed 1 hr at 700°C in vacuum and cold rolled. Rolling was carried out in a two-high, 4 in. diam mill, using reductions no greater than 10 pct per pass. The direction of rolling was reversed after each pass, and, in order to avoid temperature effects, the sheet was allowed to cool after each pass. Unless the rolled sheet was sufficiently thin for X-ray penetration (about 0.004 in.), it was reduced to this thickness by pickling. Because of the possibility of introducing twinning or other deformation during grinding, no attempt was made to maintain uniform thickness of the sample during pickling by intermediate grinding or sanding operations. Those samples to be used for determining the annealed texture were recrystallized by vacuum annealing the cold-rolled sheet for 1 hr at 500°C. These thin samples were held between thick titanium sheets during annealing to prevent distortion. Table I outlines the rolling and annealing schedule of those samples for which photograms or texture patterns are shown. X-ray Techniques The usual techniques for determining textures were employed during this work. Molybdenum radiation was used for the transmission exposures and copper radiation for the glancing angle ones. Since titanium fluoresces under these conditions, it is necessary to employ a filter between the sample and the film. The Kß radiation filters are very satisfactory for this purpose. Sufficient grains having favorable orientation were present in both the cold-worked and in the cold-worked—500°C annealed samples to provide satisfactory patterns with the samples stationary. Because of the difficulties of comparing intensities of transmission photograms with those obtained

Jan 1, 1951

By D. G. Swarthout, J. W. Savage, R. W. Guard

The Nb-N constitution diagvam has been examined from 1100° to 1450°C at 1 atm N2 pressure. On the basis of- our work plus that of Brauer and coworkers the stable nitvide Phases are: a) a solid solutlion, basic niobium (bcc) with nitrogen contained interstitially; NbN,, x = <0.40; b) ß NhNx,x = 0.39 to 0.45; hexagonal (W2C type) (NbzN); a =3.058A,c = 4.961 + 0.001A c) y NbNx x = 0.75 to 0.80; tetragonal (distorted NaCl type) (Nb4N3); a = 4.386A,c = 4.332 + 0.001A; d) 6 NbN,, x = 0.88 to 0.91; cubic (NaCl type); a = 4.3885 + 0.0007A; e) E NbNx x = 0.92 to 1.00; hexagonal (Tip type); a = 2.958A, c = 11.272 * 0.0015A. In addition, a metastuble transition phase 6&apos; has been observed and occurs only during the transition 6 — E. 6&apos; NbN has these distinguishing parameters: NbNx,x = 0.96; hexagonal (anti-NiAs type); a = 2.94A, c = 5 .46A. The high-temperature phase fields in the system are governed by two reactions: a) 6 + Y + E, a entectoid reaction occurring at 1270" ± 20° C; b) o + N2 = E, a 2 012 1 reaction occurring at 1370" ± 20° C. As part of a study of the electronic low-temperature. properties of transition metal nitrides, a number of specimens of niobium nitride were prepared. Preliminary observations on these specimens showed several points of disagreement with data already in the literature. It was, therefore, decided to determine the constitution diagram for the Nb-N system between 1100" and 1450°C. The objective of this research was to define the temperature and composition regions of stability of the various phases and to explain the differences among previously proposed diagrams. Review of Previous Literature. The research on the Nb-N system to 1964 has been summarized by storms.&apos; Although he does not present a phase diagram, his review covers the research on the system thoroughly. One of the earliest works on NbN is that of Ascher-mann and coworkers2 who studied the superconductivity of the cubic 6 NbN. Subsequent work by Horn and ziegler,3 Cook, Zemansky, and Boorse,1 Rögener:5 Schroder6 and sellmaier7 has qualitatively confirmed the first results on superconductivity, although their methods of preparation differed considerably. The constitution diagrams proposed for the system by Brauer and Esselborn8 and Elliott9 are shown in Fig. l(a)and (b). The diagram in l(a) has been modified by more recent results in Brauer&apos;s laboratory (private communication). Although 6&apos; is shown on this diagram, Brauer has indicated that he now believes 6&apos; to be a metastable phase in the temperature range shown. The diagram of Elliott, Fig. l(b), is based primarily on the results of Elliott and Komjathy10 on ni-trided niobium strip or rod specimens examined by X-ray diffraction and metallography. It will be noted that these proposed diagrams are in conflict with respect to the temperature and composition ranges of

Jan 1, 1968

In the 100&apos; years since AIME was founded in 1871, the Institute has issued a great many publications in a variety of forms: periodicals, Transactions volumes, and special volumes or books. The following is a brief history of AIME publishing with some suggestions for proper referencing. TRANSACTIONS AIME Transactions volumes have been numbered consecutively since No. 1 was issued in 1873, including papers for the period 1871-1873. One or more volumes have been issued each year and may be divided into three general time periods: General Volumes (1873-1927), Volumes classified by subject matter (1928-1949), and the present practice, begun in 1949, of issuing three volumes per year, one each in the fields of mining engineering, metallurgy, and petroleum technology. The broad divisions of subject matter in each of these volumes correspond to the technical areas of the three constituent societies of AIME. AIME&apos;s Technical Publications, usually designated by TP number&apos;s (until the change in numbering system by the Society of Mining Engineers in 1958), may, with some exceptions, be referenced to an AIME Transactions volume. Reference to a specific volume, rather than paper number, is the preferred reference, since the volumes are the form of publication most commonly available in libraries. In many cases, over the years, the Technical Publications may also have been available in some other form, either as separates or in a periodical. General. Volumes (Vols. 1-78, 1873-1927): Until 1927 all papers eligible for Transactions were published in general volumes with no systematic attempt made to segregate the material on the basis of the technological fields to which the papers related.. One volume per year was issued from 1873 until 1912; from 1912 until 1927 from two to four volumes were issued annually. In addition to the Transactions papers, these volumes carried some of the proceedings of the business meetings of AIMS. Subject Volumes. (Vols. 79-183; 1928-1949): The material for these volumes was segregated according to subject matter, and up. to seven volumes were issued a year. In the latter part of the period, from 1934 on, there was one volume each&apos; year for the Petroleum, Institute of Metals, and Iron and Steel Divisions and-the remaining papers were grouped in various ways and is sued whenever sufficient numbers of papers had accumulated: The subject volumes containing mining engineering papers are listed in Table 1. The volumes for the period, 1936-1949 are included in this Cumulative Index. Each of the Transactions volumes carries on the binding the year of publication; this date does not give an indication of when the papers included were originally presented at meetings. The contents of the volumes usually list the meetings at which. the papers were presented. Not all papers from a given meeting necessarily are in one Transactions volume. Some of the earlier volumes do not have a number on the binding or within the volume. In 1934 numbers" were assigned to all Transactions volumes, commencing with the 1871-1873 volume as No. 1. Many of the papers published [ ]

Jan 1, 1972

By A. H. Daane, W. J. Wunderlin, B. J. Beaudry

The solid solubility of holmium in copper, silver, and gold, determined using metallographic techniques, was found to be a maximum of 0.06, 2.4, and 3.2 wt pct, respectively, nt the eutectic temperatures. The temperatures of these eutectic horizontals, determined by differential thermal analysis, were found to be 868", 787", and 778"C, respectively. The first compound on the silver-rich side of the Ag-Ho system was found to be A&Ho2. In a study by Gold et al.,&apos; on the effect of small amounts of soluble impurities on the electrical resistance and thermoelectrical properties of copper, traces of iron were shown to have drastic effects on the thermoelectric power due to the magnetic scattering of the conduction electrons. Since little is known about the state of the iron ion when dissolved in copper, Gold had hoped to repeat these experiments using certain rare earths as the magnetic scattering centers; because of the tightly bound 4f electrons it is not expected that their spectroscopic state would be affected by alloying. In such an experiment the sole role of the trace rare-earth impurity would be to magnetically scatter the copper conduction electrons without producing appreciable distortions in the otherwise pure copper matrix. Since holmium was chosen for such a study because of its high magnetic moment, it was necessary to establish precisely its solid solubility in copper. The study was extended to include the solvents silver and gold, so that an evaluation of the data using classical solubility parameters could be made. No previously reported work on the systems of holmium with copper, silver, or gold was found in the literature. Information on the solubility of other rare earths in these three metals is also very meager. The solubility limit of yttrium in copper was reported as less than 1 wt pct2 and the solubility of praseodymium in gold as 0.35 wt pct,3 while no references were found on solubility studies of rare earths in silver. EXPERIMENTAL Materials. The materials used in this investigation were distilled holmium prepared in this Laboratory, OFHC* copper, electrorefined silver (99.9 *OFHC = oxygen-free high conductivity. pct), and gold with the analyses given in Table I. Sample Preparation. Samples weighing 1 to 2 g were prepared by arc-melting the components together on a water-cooled copper plate under purified argon atmosphere. The samples, turned and remelted at least five times to ensure homogeneity, showed weight changes of less than 0.1 wt pct after melting. Samples containing less than 0.7 wt pct Ho were prepared by diluting 1 to 2 wt pct Ho alloys with the pure solvent, while samples with concentrations greater than 0.7 wt pct Ho were prepared directly from the metals. The samples were wrapped in tantalum foil, sealed in outgassed Vycor tubing under helium, annealed at the desired temperature for at least 24 hr, and then quenched by shattering the Vycor tube in cold water. Metallographic Methods. Standard mechanical polishing methods were used in preparing the silver and gold alloys for examination, while the copper alloys were electropolished using a 40 pct solution

Jan 1, 1963

By B. W. Christ, P. M. Giles

Mossbauer effect measurewents have been made on I-mil-thick foils of commercial 1 wt pct C steel and Fe-2 wt pct C alloy. The experimental method required about 3 to 5 vol pct of a phase in the nzultiphase steel sample for detection. Room-temperature Md&apos;ssbauer patterns obtained on austenitized atid quenched samples exhibit fifteen, and possibly twenty-one, lines. A sharp parama&tetic singlet and a quadrupole doublet, poorly resolued from the singlet, are attributed to austenite. Remaining lines are due to tnartensite. Accurate evaluation of austenite line paranzeters is not feasible if significant amounts of other phases such as carbides or martensite occur simultaneously with austenite. This is demonstrated by comparison of hyperfine interactions determined for austenite in multiphase high-carbon samples with those reported for Fe-C austenite in a nearly 100 pct austenitic sanple. Lines from carbides are incompletely resolced from austenite lines, as demonstrated by comparison of austenite line positions with carbide line positions calculated frow published values of hyperfine interactions. One martensite line overlaps an austenite line in the pattern for commercial 1 wt pct C steel. Results of this study suggest that the usefulness of e M6ssbauer pectroscopy for quantitatizle analysis of austenite in bulk samples of quenched and tempered high-carbon steels is restricted by poor resolution. Use of Mossbauer spectroscopy for phase identification and for evaluation of atomic and electronic structures appears quite feasible, however, The Mijssbauer effect has been widely discssed,&apos;-and e Mossbauer effect measurements have been reported on materials of metallurgical interest.7"20 In particular, it has been proposed that e Mossbauer patterns of commercial steels and laboratory-made Fe-C alloys, in the quenched condition, are composed of lines originating in two phases, Fe-C austenite and Fe-C martenite.-&apos; Evidence accumulated in this study demonstrates that three absorption lines found in the central region of the e Mossbauer pattern obtained on quenched steels are attributable to retained austenite. This interpretation is supported by parallel decreases in the intensity of these three lines caused by subambient cooling of commercial 1 wt pct C steel samples after water quenching to room temperature. A second result of this study is to clarify effects of line resolution and sensitivity in the Mossbauer patterns of multiphase steels on the accu- rate determination of austenite line parameters. Experimental line widths (full width at half height) are generally 1.5 to 3 times larger than the natural line width of 0.19 mm per sec. At least two lines, and sometimes more, from a single phase such as cementite (Fe3C), other carbides, martensite, and austenite fall in the energy band, i0.85 mm per sec. hhis band width is employed simply for convenient reference. It represents approximately the energy interval between the + 112 to 112 transitions in ferrite and is expressed as the velocity needed to Doppler shift a 14.4kev 7 ray to the aforementioned ferrite energy levels. This energy band is referred to as "the central region of the Mossbauer atttern:: in this paper. Hence, due to the large number of lines from different phases in a multiphase steel falling in a relatively narrow energy band, absorption lines from the different phases may overlap. Analysis of available data, presented below, indicates that this occurs to a significant extent for phases which commonly occur in quenched and quenched and tempered high-carbon steels. One consequence of limited resolution in the Mdssbauer patterns from multiphase steels is difficulty in accurate determination of such line parameters as position, width, and intensity. In fact, it appears that quantitative analysis for retained austenite in quenched and tempered high-carbon steels is not practical with the present experimental method. Line resolution is influenced to some extent by sensitivity. We point out below that atom or volume fractions of less than about 3 to 5 pct are not detected by the present experimental method. Thus, the presence of a multiplicity of phases does not always lead to impaired resolution. Finally, we report in this paper room-temperature MGssbauer parameters determined for austenite in a freshly quenched, commercial 1 wt pct C steel and in a freshly quenched laboratory heat of an Fe-2 wt pct C alloy. These parameters are compared with others reported in the literature. Three types of hyperfine interactions are detectable in a Mossbauer effect measurement: isomer shift, quadrupole interaction, and magnetic dipole interaction. These interactions are evidenced by one, two, and six line patterns, respectively.&apos;-4 More than one type of interaction has been reported in certain metallurgical phases thus far studied by this method. Isomer shift is the experimentally measured displacement of line position from some arbitrarily defined reference position. In the case of a multiline pattern, isomer shift is given by the displacement of the centroid (center of gravity) of that pattern from the reference position. All isomer shifts measured at finite temperatures contain a second-order Doppler effect characteristic of that temperature. The isomer shift is related to the total s electron density at the nucleus, becoming more negative with increasing s electron density. The first-order quadrupole effect arises from the interaction between the nuclear quadrupole moment and any axially symmetric electric field gradient in

Jan 1, 1969

By A. Y. Bethune, W. G. Woolf

THE hydrometallurgy of special high-grade zinc as practiced by the Sullivan Mining Co. at its electrolytic zinc plant, Kellogg, Idaho, involves an important filtration step immediately following the leaching process. By means of the filtration the heavy zinc sulphate solution is separated from the residual products which remain after the zinc calcine has been dissolved in the sulphuric acid electrolyte. Because this plant uses the so-called high-acid, high-density process&apos; for the production of First, the strength of the electrolyte (270g H,SO, per liter) results in a saturated zinc sulphate solution, having a specific gravity of 1.510 to 1.540, which must be kept warm during filtration because of its property of "seeding out" small crystals if allowed to drop much below 60°C. Second, the action of the "high" acid on zinc calcine under the temperature conditions of the leach (80" to 102 "C), although favorable to good zinc extraction, causes a considerable quantity of iron to be dissolved (8 to 18. g per liter) along with variable quantities of alumina and silica, depending on the grade and type of original zinc concentrates roasted. These three, iron, alumina, and silica, are almost completely precipitated during the neutralization of the leach (only a few. milligrams per liter of each remain in solution), so that the resulting pulp, instead of being a granular, sand-like product having a particle-size distribution dependent on the fineness of the zinc calcines leached, is in reality a slimy, chemical precipitate whose filtration characteristics constantly change depending on the amounts of iron silica, and other impurities, which are dissolved and reprecipi-tated. Third, the combination of supersaturated solution of high specific gravity plus a dense, semi-gelatinous residue creates a difficult washing problem requiring a positive displacement wash to liberate the zinc sulphate entrapped in the pulp. In a closed-cycle hydrometallurgical operation, such as practiced in this plant, the extent of washing is determined by the volum,e limitations imposed on the intermediate wash waters by the amount of "fresh" (or process) water which may be added. The volume of fresh water used for makeup purposes is limited to the amount which is lost during the closed cycle by evaporation in the leach, sulphate content of the calcines leached, moisture content of the residue, and spillage. The Burt filter as modified and improved by the Sullivan Mining Co. has successfully met and overcome these difficulties under a variety of zinc plant operating conditions since 1928. It might have many interesting applications to metallurgical fields other than that of electrolytic zinc, and its possible usefulness to hydrometallurgists in general warrants its description and discussion. The Burt filter is so named from its inventor who originated it in Mexico for pulp filtration in the cyanide process for gold and silver ores. While retaining the basic principle of Burt&apos;s earlier revolving pressure-type filter with internal filtration media, a number of modifications and improvements have been made in Sullivan Mining Co.&apos;s installation. The Burt filter may be classified as a batch-type pressure filter in contradistinction to either the conventional vacuum-type filter, which depends on atmospheric pressure to force solution through a cloth medium, or to the filter-press, which employs whatever pressure is imparted by the pump delivering the liquid being filtered. The Burt consists essentially of a hollow steel cylinder about 40 ft long, 5 ft in diameter, resting horizontally, and capable of rotation about its long axis. It is supported on one end by a hollow trunnion and near the other end by a riding-ring and roller combination. The cylinder is lined with filter units each fastened against the inside of the shell and parallel to the long axis so as to form a hollow cavity into which pulp may be charged. A specific amount of pulp is admitted to the filter and a unique valving arrangement prevents the loss of pulp while air pressure forces the solution through a canvas medium to the discharge port of each filter unit. The residue is left on the surface of the canvas inside the cavity. The remainder of the filter cycle is concerned with washing the residue free of zinc sulphate, discharging it from the Burt, and preparing the filter for the next charge. A more detailed description of Burt filter construction, a typical filter cycle, and its operating characteristics when employed on material encountered in this plant will be given in that order. Description of the Filter: Fig. 1 shows a side elevation view of a filter with riveted shell construction. Since this drawing was made shells have been fabricated by welding, instead of riveting, with complete success. Shells are lagged on the outside to retain heat. Fig. 1 shows a side elevation and plan view of a Burt filter in operating position. The 1/2-in. steel shells are lined with 3/16-in. copper sheet as protection against the corrosive action of the solution (containing about 500 mg Cu per liter) on iron, and the copper is given a thin protective coating of plastic-base paint. Fig. 2 is a view from the discharge end of the filter, with head removed, before filter units are fastened to the periphery. It shows

Jan 1, 1951

By W. G. Woolf, A. Y. Bethune

THE hydrometallurgy of special high-grade zinc as practiced by the Sullivan Mining Co. at its electrolytic zinc plant, Kellogg, Idaho, involves an important filtration step immediately following the leaching process. By means of the filtration the heavy zinc sulphate solution is separated from the residual products which remain after the zinc calcine has been dissolved in the sulphuric acid electrolyte. Because this plant uses the so-called high-acid, high-density process&apos; for the production of First, the strength of the electrolyte (270g H,SO, per liter) results in a saturated zinc sulphate solution, having a specific gravity of 1.510 to 1.540, which must be kept warm during filtration because of its property of "seeding out" small crystals if allowed to drop much below 60°C. Second, the action of the "high" acid on zinc calcine under the temperature conditions of the leach (80" to 102 "C), although favorable to good zinc extraction, causes a considerable quantity of iron to be dissolved (8 to 18. g per liter) along with variable quantities of alumina and silica, depending on the grade and type of original zinc concentrates roasted. These three, iron, alumina, and silica, are almost completely precipitated during the neutralization of the leach (only a few. milligrams per liter of each remain in solution), so that the resulting pulp, instead of being a granular, sand-like product having a particle-size distribution dependent on the fineness of the zinc calcines leached, is in reality a slimy, chemical precipitate whose filtration characteristics constantly change depending on the amounts of iron silica, and other impurities, which are dissolved and reprecipi-tated. Third, the combination of supersaturated solution of high specific gravity plus a dense, semi-gelatinous residue creates a difficult washing problem requiring a positive displacement wash to liberate the zinc sulphate entrapped in the pulp. In a closed-cycle hydrometallurgical operation, such as practiced in this plant, the extent of washing is determined by the volum,e limitations imposed on the intermediate wash waters by the amount of "fresh" (or process) water which may be added. The volume of fresh water used for makeup purposes is limited to the amount which is lost during the closed cycle by evaporation in the leach, sulphate content of the calcines leached, moisture content of the residue, and spillage. The Burt filter as modified and improved by the Sullivan Mining Co. has successfully met and overcome these difficulties under a variety of zinc plant operating conditions since 1928. It might have many interesting applications to metallurgical fields other than that of electrolytic zinc, and its possible usefulness to hydrometallurgists in general warrants its description and discussion. The Burt filter is so named from its inventor who originated it in Mexico for pulp filtration in the cyanide process for gold and silver ores. While retaining the basic principle of Burt&apos;s earlier revolving pressure-type filter with internal filtration media, a number of modifications and improvements have been made in Sullivan Mining Co.&apos;s installation. The Burt filter may be classified as a batch-type pressure filter in contradistinction to either the conventional vacuum-type filter, which depends on atmospheric pressure to force solution through a cloth medium, or to the filter-press, which employs whatever pressure is imparted by the pump delivering the liquid being filtered. The Burt consists essentially of a hollow steel cylinder about 40 ft long, 5 ft in diameter, resting horizontally, and capable of rotation about its long axis. It is supported on one end by a hollow trunnion and near the other end by a riding-ring and roller combination. The cylinder is lined with filter units each fastened against the inside of the shell and parallel to the long axis so as to form a hollow cavity into which pulp may be charged. A specific amount of pulp is admitted to the filter and a unique valving arrangement prevents the loss of pulp while air pressure forces the solution through a canvas medium to the discharge port of each filter unit. The residue is left on the surface of the canvas inside the cavity. The remainder of the filter cycle is concerned with washing the residue free of zinc sulphate, discharging it from the Burt, and preparing the filter for the next charge. A more detailed description of Burt filter construction, a typical filter cycle, and its operating characteristics when employed on material encountered in this plant will be given in that order. Description of the Filter: Fig. 1 shows a side elevation view of a filter with riveted shell construction. Since this drawing was made shells have been fabricated by welding, instead of riveting, with complete success. Shells are lagged on the outside to retain heat. Fig. 1 shows a side elevation and plan view of a Burt filter in operating position. The 1/2-in. steel shells are lined with 3/16-in. copper sheet as protection against the corrosive action of the solution (containing about 500 mg Cu per liter) on iron, and the copper is given a thin protective coating of plastic-base paint. Fig. 2 is a view from the discharge end of the filter, with head removed, before filter units are fastened to the periphery. It shows

Jan 1, 1951

By T. F. Baily

DURING the period of the War, in both this country and Canada, a number of attempts were made to make pig iron from steel scrap in the FIG. 1.-EXPERIMENTAL FURNACE. 5000 KW. CAPACITY: 150 TONS 2 PER CENT. SILICON PIG IRON PER DAY. electric furnace, and a considerable tonnage of white pig iron was produced, the silicon and manganese additions being made with ferroalloys; but it is believed that the experiments conducted at Canton, Ohio, in

Jan 1, 1930

By A. G. H. Andersen

A FEW years ago, while the writers worked on the constitution of ternary and quaternary alloys consisting mainly of iron, chromium and silicon1,2 some information on microstructures and hardness, not incor-porated in the published work, was obtained. It has not been possible to do any further work on the properties of the alloys. The information possessed is hereby presented for the interest it. may have in connection with the constitution of the alloys.

Jan 1, 1937

By L. D. Jaffe, D. C. Buffum, F. L. Carr

SINCE the temper brittleness of steels is generally considered to be a grain-boundary phenomenon¹,² it would be expected that austenitic grain size would affect temper brittleness. Several investigators"" reported that temper brittleness, as measured by room-temperature impact tests, increased as the austenitiz-ing temperature was raised. It was subsequently pointed out that conclusions as to temper brittleness based upon room-temperature impact tests are likely to be misleading.1,6 Hurlich7 used a range of testing

Jan 1, 1954

By Walter Harvey Weed

(Mexican Meeting, November, 1901.) Among the many causes of that perplexing featurc of mineexploitation, the unequal distribution of the ore, the influence of the country-rock upon the vein-contents has long beer1 accepted as an important factor in certain districts, but the general application of the theory has not been proved. It is now possible to obtain trustworthy data with which to test the theory, and either to confirm or to overthrow this time-honored

Jan 1, 1902