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By E. F. Ketterer, D. B. Collyer, A. B. Wilder

AISI constructional alloy steels are a series of steels in which a numbering system signifies the chemical composition limits. SAE (Society of Automotive Engineers) and AISI (American Iron and Steel Institute) use basically the same numbering system. The steels contain, in part, alloy additions of chromium, molybdenum, nickel, and vanadium. They are used widely in the automotive industry but have not been adopted for high temperature service. The purpose of this investigation was to study changes in microstructure observed in typical AISI constructional alloy steels in the welded and un-welded conditions after exposure for 34,000 hr at 900" and 1050" and, in several instances, 1200°F. The tensile and creep rupture properties after exposure for 10,000 hr were also evaluated. The investigation is a continuation of the work previously discussed. Little was known concerning the existence of graphite in medium or low carbon steels before 1943. It is important to note that continued exposure at elevated temperature is required in order to develop graphite in steels. Interest in the presence of graphite in steel, and also in changes in the properties of steels after long service at elevated temperatures, developed after 1943 when a failure of a welded joint of high temperature piping was associated with the graphitization of a relatively low carbon content steel with 0.50 pct Mo,8,0 Numerous investigations have beeen made in recent years studying the relationship of this type of failure to changes in properties. Attempts have been made to evaluate the performance of a number of steels, particularly in the heat-affected zone of welds. It was the unfortunate failure of a weld-heated zone in high temperature piping in the steam-power industry which focused attention upon possible failures, and upon the need for improved steels for high temperature piping service. Investigation by the National Tube Div., U. S. Steel Corp., Lorain Works, has included a wide variety of steels in an attempt to learn the effects of numerous factors and elements upon the long time performance of steels, although many of the compositions studied will never be used at elevated temperatures.1,4-7 Included were the well established AISI steel series, which offered opportunity to test moderately high carbon content steels as well as observe the effect of nickel, chromium, molybdenum, etc., upon the properties of these well known steels. The properties of the AISI steels were also studied for comparison with the previously reported properties of the Cr-Mo steels, now used by the steam-power industry.5,7 Materials and Testing Procedure The AISI alloy steels in Table I were exposed for 10,000 and 34,000 hr at 900°, 1050°, and 1200°F.

Jan 1, 1958

By J. W. Downey, M. V. Nevitt

DURING the course of the present investigation of alloy phases involving transition metals, phases were found in the systems Os-Ta, Os-W, and Ir-Ta. The (Os, W) phase was also recently reported by Raub.1 Pertinent information is given in Table 1. The approximate composition range of sta- bility was determined metallographically on arc-melted buttons that were annealed 72 hr at 1200°C and water quenched. X-ray powder patterns were obtained with a 114.6 mm diam powder camera using filtered copper radiation. The composition for (Os, W) given by Raub (66 atomic pct W) is in agreement with the composition range reported here. However, the lattice constants reported by Raub are: a0= 9.913±0.007, c/a= 0.515. The reason for the discrepancy between the lattice constants reported by Raub and those given here is not known. Acknowledgments The authors wish to thank M. H. Mueller and H. W. Knott for assistance with the X-ray diffraction work, and R. A. Morris for the preparation of the alloys. This paper is based upon work performed at the Argonne National Laboratory under the auspices of the Atomic Energy Commission.

Jan 1, 1958

By George W. Crawford, W. P. Aycock, E. W. Hough

Forty oilfield brines have been examined so far by a polarographic technique new in petroleum engineering called the "tensatnmetric method" by the team of biochemists who perfected its use in their field. Samples of brine were obtained from various oil fields in which the wells were known to be producing fluid from oil productive zones in well-known geologic formations. Most of the reservoirs from which the samples were obtained are believed to have an active water drive under the prevailing conditions of operation. The 40 samples represent brines produced front 16 different formations of various geologic ages. Graphs have been prepared of the data obtained in the testing of each sample, and the distinctive waife-like curves so obtained are characterized by reproducible profiles, called "response curves." Careful comparison of the response curves of salt water coming from different fields producing from the same geologic formation reveals that the curves are similar. The response curves of salt water coming from productive zones of different geologic formations are characteristically different. Preliminary work offers the further hope that response curves of an oilfield brine indigenous to a particular oil-bearing formation and hence representative of a particular geologic environment, such as deposit-ional and all subsequent morphological conditions, may be of value in reservoir engineering in the interpretation of surface and interfacial phenomena. For example, the wettability of the rock matrix and more specifically, the classification of productive oil-bearing strata as hydrophyllic or hydrophobic may be determinable. However, many more brines must be examined and the resulting response curves analyzed in comparison to known causal phenornena before this objective is achieved. INTRODUCTION One of the perennial moot questions in the literature of petroleum engineering is whether the reservoir rock is oil- or water-wet. Possibly an answer to this question could come from a careful examination of oilfield brines. None of the conventional methods of examining brines (chemical analysis, pH and electrical conductivity measurements, and the like) answer the question. Careful analysis of reservoir behavior observed in the exploitation of oil fields, particularly in the application of fluid injection, has been fruitful to the extent that a few reservoirs are believed to be properly classified. Physical chemistry suggests the behavior of reservoir brine and rock may be due to something in the brine in small amount. The ever increasing development and modification of theory in the general field of surface and interfacial chemistry has, and is, contributing to a better understanding of the problem, particularly as theory is verified by data. The work herein reported was begun in 1953 by Hough and Roebuck 1,2 who employed a new form of alternating current polarography, i.e., tensammetry, developed by Breyer, et a13,4 and who studied eight oilfield brines in adapting tensammetry to petroleum engineering needs. THEORY AND DEFINITIONS Tensammetry is a new technique of inquiry into surface phenomena. Specifically, a weak alternating current voltage is superimposed upon the direct current voltage applied to a dropping mercury electrode in contact with an electrolyte containing a small amount of a surfactant. The resultant alternating current can be measured and provides the experimental data for this new area of research. Under the influence of the direct current voltage, polar molecules arrange themselves in a double layer at the electrode. This double layer may be compared to a variable condenser, the capacitance of which is a function of the imposed direct current voltage. The direct current voltage determines the degree of adsorption of the surface active molecule on the electrode. Whenever the molecules are strongly adsorbed on the electrode, the capacitance of the double layer is low and the alternating current through the cell is low. Desorption occurs at some values of the direct current voltage, and at these voltages the capacitance of the double layer is high, resulting in an increase in the alternating current through the cell. The direct current

Jan 1, 1958

By John Chipman, Helen Towers

DEVELOPMENT of a simple radioactive tracer technique for measurement of the diffusion coefficient of calcium ion in liquid slag has already been reported. The investigation was of a preliminary nature designed to explore the possibilities of using radioactive isotopes and to establish a method, and no great accuracy was claimed for the results. It was shown, however, that Ca15 could be used successfully, and the values obtained for the diffusion coefficient appeared to be of the right order of magnitude. However, it was considered that a better technique could be devised for carrying out the diffusion. The experiments were, therefore, continued to find a more accurate method, to check the calcium results, and to extend the investigation to include measurements of the diffusion coefficient of silicon in the same slag. There were two flaws in the original technique. Convection was the cause of too many failures, and the interface between the two slags in the diffusion cell was curved rather than plane, probably due to a surface tension effect caused by the addition of the tracer Ca45 in the form of chloride. Two methods of overcoming these defects were tried. Since it was planned to study diffusion of the short-lived isotope Si"' also, the development of methods was restricted to those which gave promise of being reasonably rapid. Method 1—The principle was identical to that previously used with respect to the diffusion conditions, but there were three differences in technique. Temperature control was more rigid, the tracer was added to the slag as Ca45O rather than the chloride and, finally, an effort was made to translate to high temperatures the elegant method developed by Cohen and BruinV or bringing together the two liquid layers and beginning the diffusion. A master slag was melted in graphite, ground to a fine powder, and analyzed (38.5 pct Ca0-20.9 pct Al2O3-40.5 pct SiO2). The tracer was received as Ca45C12 in an aqueous solution of CaC12 + HC1. From this, calcium oxalate was precipitated, ignited to calcium oxide, and added as such to the slag to give an activity of approximately 5 µc per g. The mixture was then melted into the form of a cylinder 3/16 in. diam and about 1 in. long. A solution identical to the tracer solution without Ca45 was given exactly the same treatment. The resulting Ca40O was mixed with that slag which was to form the tracer-free half of the diffusion cell, and this was likewise melted into a cylinder of the same size. Slag cylinders, two with and two without Ca15, were set in graphite blocks as shown in Fig. 1, and the crucible was lowered into position in the fur-

Jan 1, 1958

By Ellis H. Gates

BENEFICIATION of the manganese oxide ores at Three Kids Mine near Henderson, Nev., has evolved over a period of years. Commercial application of the process is on a secure basis, and an effective working hypothesis has been formulated to help solve the problems encountered in flotation. An outstanding difference between the Manganese Inc. operation and other flotation processes is the necessity for high recovery of slime mineral values. Part of the manganese minerals in the Three Kids ore deposit occurs as primary slime or as minerals that are easily slimed by grinding. High recovery of this slime portion is essential to an economic overall manganese recovery. The aim of much of the research at Manganese Inc. was to recover these slimed and finely ground minerals by flotation. Early Agglomeration Processes: Tunbridge' in 1880, followed by Everson2 in 1886 and Cattermole" in 1904, discovered that under certain pulp conditions precious metals and sulfide minerals could be agglomerated if enough soap or oil were mixed into the pulp slurry. These agglomerated particles, Which under ideal conditions ranged from 1/16 to 1/4 in. diam, were recovered by screening, tabling, and hydraulic classification. Even flotation by air occluded in the agglomkrate particles by vigorous stirring was suggested. Cattermole nearly succeeded in getting his process into commercial operation, but it was finally abandoned, presumably because he could nat compete with the low reagent requirements of the new agitation froth process. Since Cattermole's time Christensen in 1921, Borcherdt4 in 1926, and Chapman and Littleford- in 1934 have attempted to apply the principles of agglomeration. In the light of current research at Manganese Inc. on conditioning of pulp at high energy input levels, it is interesting to note the variety of equipment such as tumbling mills, mixing drums, and shakers described by Borcherdt in his patent to produce the agglomerated particles. Ore Characteristics: Manganese in the Three Kids ore occurs as a 'complex mixture of manganese oxides commonly Known as wad. The manganese minerals have Been identified as psilorflelane, hollandite, coronadite, and pyrolusite with minor amdunts of rhodonite and rhodochrbsite. The ppincipal gangue miherals are quaktz, opal, kaolinite, montmoril-lonite, calcite, gypsum, fcelesitite, and barite. Most of the mangandse ore minerals are either porous and sponge-like in structure or soft clay-like masses composed of fine grained mineral particles approaching the size range of colloids. Consequently the ore minerals from the Three Kids mine have relatively large surface areas and high void content per unit weight. The specific area of various manganese ore samples measured at the California Research Corp. laboratories ranged from 32 to 58 sq m per g. The great surface area and high void content explains in part the unusually high reagent consumption required in the treatment of this ore. Current Milling Practice: At Henderson6 he ore is crushed to —1 in. and ground with rod mills in a closed circuit with spiral rake classifiers and cyclones. Sulfur dioxide solution is added to the pulp as it leaves the grinding circuit, immediately followed by addition of a reagent mixture of soap, oil, and wetting agent in the form of an emulsion. The reagents are initially well mixed into the pulp during their passage through centrifugal pumps to the conditioning equipment. All reagents are added prior to conditioning. The intense conditioning or mechanical stirring of the pulp, in which large amounts of power are consumed, is the principal difference between the flowsheet used at Manganese Inc. and a standard flotation circuit. As much as 38 kw-hr of energy per dry short ton of ore in a pulp containing 18 to 23 pct solids is used for conditioning. After conditioning, the pulp passes to a flotation circuit that consists of one roughing stage, a scav-

Jan 1, 1958

By H. I. Aaronson, S. M. Kaufman, G. M. Pound

WHETHER the carbides associated with bainite precipitate from the ferritic component of bainite, as originally suggested by Davenport and Bain, or from the adjacent austenite at aus-tenite:ferrite boundaries, as proposed by Hultgren, 2 remains in dispute.3-5 A recent metallographic investigation in this laboratory has shown that the bainitic carbides formed in a plain carbon hypo-eutectoid steel nucleate entirely within ferrite at higher reaction temperatures3 and in both ferrite and austenite at lower temperatures." The present investigation was undertaken to ascertain the effects of alloying elements on the nucleation sites selected by bainitic carbides. The compositions of the steels studied were as shown in Table I. Specimens of these steels were

Jan 1, 1958

By E. S. Davenport

IT is indeed an honor and a responsibility to have been selected to present the thirty-fourth in this series of Henry Marion Howe lectures, established to perpetuate the memory of a great teacher and one of America's outstanding scientists. Previous Howe lecturers have established high standards for this annual AIME event. It has been my good fortune to have enjoyed close association with five of these former lecturers; namely, Bain, Grossmann, Johnston, Sosman, and Vilella, all of whom have been prominently identified with the research activities of the organization with which I am connected. Some years ago I had an opportunity to examine a letter written by Professor Howe in 1904. This document was particularly interesting to me since I never had the privilege of personal acquaintance with Professor Howe and do not recall even having seen him during his long and active career. In view of the fact that the letter dealt, to some extent, with matters related to the subject of today's lecture, I would like to quote briefly from it. The letter is datelined, "Bad Kissingen, June 11, 1904." The salutation reads, "Dear Bradley," which suggests that it was probably addressed to Bradley Stoughton, who, I believe, was working with Howe at Columbia University at that time. The letter reads, in part, as follows: "Austenite and Martensite. I have not examined what Osmond says in his new book. His former remarks about austenite I found very confusing, indeed unintelligible. I think we can reconcile matters well enough for the present by assuming that martensite is a transition step between austenite at one end and ferrite and cementite at the other. Above critical range for steel of 0 to 1.80 carbon, austenite is normal state; below Ar1, ferrite and cementite are normal." The letter then continues with a discussion of Osmond's ideas on metallographic nomenclature, particularly his use of the terms martensite, troostite, and sorbite, including the following pointed comment: "For common purposes it seems to me unwise to drag them in, and much simpler to confine ourselves to the end stages Austenite Ferrite plus Cementite Osmond does not really know his own mind— or does not clarify his ideas to others—as to nomenclature." Thus we see that, as far back as 1904, the transformation of austenite, and the products of that

Jan 1, 1958

By D. W. Fuerstenau, J. H. Brown

The paper by Professors Sun and Mitchell illustrates the value of ultrasonics as a tool for the mineral engineer. In particular, it opens up a number of possibilities to those interested in the field of comminution. The provision of desliming technique, which is thorough as well as rapid, is a distinct contribution, but the data of the paper suggest applications beyond desliming, in that the same treatments may be useful for size determination purposes. Fig. 1 shows that a marked dependence exists between particle size and the height to which it can be elevated by ultrasonic vibrations. While the curves are only extended down to a size of about 100 u, the fact that they appear to be increasing in slope in this range suggests that the separation may be even more marked here. This, we feel, is very strong evidence that a nlethod for fine sizing could be developed to use ultrasonic waves as the separating force. Professors Sun and Mitchell indicate that floccula-ti~n will present no difficulty: "During the investigation it was found that ultrasonic waves were able to dislodge the adhering gangue particles from the min- era1 surfaces and to disintegrate the soft particles into fine sizes." Thus, it appears that the use of ultrasonic waves as the power behind a size separation process may eliminate the problem of flocculation encountered in most wet sizing techniques. It would be interesting to size a fine material under conditions in which particles are known to be flocculated and under conditions where they are known to be dispersed. Use of a sizing technique of this nature may solve several problems that have long persisted in the fine sizing field. The flocculation problem may be overcome; the continuous production of closely sized fractions may be possible with a device similar to the one described; and with photoelectric methods, rapid analyses in the subsieve sizes may be possible. In general, we suggest that this paper be followed by a study of the sizing applications of the apparatus described. We feel that such a study would not only be rewarding in providing a new sizing technique, but also that the present paper almost requires such work to complete the picture of particle motion in a field of ultrasonic waves.

Jan 1, 1958

By William L. Russell

A new instrument for measuring bulk and grain vol-urnes is described, and compared in accuracy with two modifications of Nutting's method, All three methods are reasonably fast, and in all three the probable error in the determinations of bulk volume can be kept down to about 0.1 to 0.2 per cent. INTRODUCTION The new pycnometer described in this paper is designed to give speed without sacrificing accuracy. Some time ago Russell1 described a somewhat similar appa-ratus; however, the instrument described in the present paper is more accurate. Nutting' designed the pycnom-eter shown in Fig. 1 (A and B), and Pirson3 has shown points like those of Fig. 1-D. The procedure described in this paper for using Nutting's pycnometer has been modified from that used by Nutting. CHOICE OF LIQUIDS The best liquids for measuring grain volumes are hydrocarbons or chlorinated hydrocarbons which evaporate slowly. Trimethylbenzene or mesitylene, triethylben-zene, carbon tetrachloride, and tertalin have been used for this purpose. Any of these liquids or mercury may be used for measuring bulk volume. PREVENTING ERRORS DUE TO INVASION OF LIQUID Errors due to the invasion of the porous, permeable bulk samples by the liquid of measurement may be prevented or greatly reduced by using mercury, by applying an impervious coating, or by soaking the bulk samples in the liquid of measurement until bubbles cease issuing from them. Errors are produced only by the invasion of the samples which occurs between movement when the samples are weighed in air and the moment the weight of liquid displaced by the sample in the pycnometer is determined. No error is produced by varying degrees of filling of the pore space of the samples by the liquid of measurement. The excess liquid should be wiped from the samples immediately before the weight in air W1, is determined, and they should be placed in the pycnometers immediately. OPERATION OF NEW INSTRUMENT The new pycnometer is shown in Fig. 2. It consists of two glass parts which fit together at a ground glass joint. The spaces J and D are connected by fine glass tubes E, and the space J must be larger than the space D by at least the volume of the largest sample to be tested. The projections H afford a grip for twisting when the two parts tend to stick together. The position of the sample in mercury is shown by I, and in other liquids by M. F is a permanent mark on the glass, and G is a tem-Some marker. In order to determine the position at which G should be placed, invert the instrument so that A is at the bottom, and fill space D. Place the cub K

Jan 1, 1958

By Nicholas J. Grant, Oliver Preston

PUBLICATION of data by Irmann' indicating outstanding thermal stability and elevated-temperature strength properties in a sintered aluminum powder product (SAP) stimulated interest in the strengthening of metals by means of a highly dispersed oxide phase. This material was produced by compacting, sintering and extruding a fine flake aluminum powder, resulting in a dense product containing 10 to 16 volume pct alumina, which arises from the thin oxide film on the starting powder, highly dispersed in a matrix of pure aluminum. The method of producing SAP, and the stable high-temperature properties obtained from it, introduced the possibility of developing superior materials for high-temperature service by powder metallurgy methods. The composition of the materials of this type which are presently under consideration is predominantly metallic, containing from less than 1 pct up to about 20 volume pct of the oxide. As a result, other properties of these materials, such as electrical and thermal conductivity, thermal shock resistance, and to a certain extent ductility, notch sensitivity, machinability and hot working properties, are also predominantly metallic. These alloys do not constitute, therefore, a completely new class of materials as do the cermets, but rather present a new means of modifying the properties of a metallic matrix. In this sense, SAP type alloys are more closely analogous to the alloy aging systems. While the strength properties realized in the oxide-pure metal systems at the lower temperatures are substantially less than the best attainable in the aging systems, the thermal instabilities in the latter make them of less value for use at temperature much above their optimum aging temperatures, as indicated in Fig. 1. While the means of obtaining an oxide dispersion are more difficult and costly than conventional aging processes, in the light of the as yet limited understanding of such systems there is considerable promise of improved high temperature properties arising from the thermal stability of these structures. Since the development of SAP in 1946, its properties and the properties of a series of similarAl,O,-A1 products containing from about 1 to 20 pct aluminum oxide have been fairly extensively studied and reported.'- "articular attention has been given to

Jan 1, 1958

By W. A. Krivsky, R. Schuhmann

PREVIOUS papers in this series on the thermo-•t dynamics of copper-smelting systems have presented a survey of the field and an outline of the overall program: thermodynamic studies of iron silicate slags, 2-4 and thermodynamic data for simple mattes in the Cu-S system.5 Since this program was started, an excellent summary of the whole field of physical chemistry of copper smelting was published by Ruddle. The present paper represents a further step in the study of liquid mattes, and deals specifically with the Cu-Fe-S system. The importance of the Cu-Fe-S system to copper smelting is evident from the fact that these three elements constitute 90 to 99 pct of the totalweight of most commercial mattes. In copper mattes oxygen is an important fourth component. Oxygen was rigorously excluded in the work to be described in this paper. However, the behavior of oxygen in mattes was the subject of a companion research by Lander' which will be described in a subsequent publication. Several studies have been made previously of phase equilibria in the Cu-Fe-S system,8-10 so that the ternary phase diagram is fairly well established in most regions. Also, separate studies have been made of the phase diagrams and thermodynamic properties for the three binary systems: CU-S,5,12-15 CU-Fe,11,14,17 and FeS.11,14,16,17 However, no work has

Jan 1, 1958

By F. A. Forward, A. H. Ross, J. Halpern

IN treating carnotite ores by carbonate leaching it is often necessary to subject the ore to a prior roast. Among the advantages that may result from roasting are: 1) improvement in settling and filtering characteristics of the ore; 2) destruction of carbonaceous impurities that would otherwise contaminate the leach solution and consume carbonate reagent; and 3) substantial increase in extraction of vanadium, which is usually low when the un-roasted ore is leached. Recovery of vanadium may be an important factor in processing carnotite ores, and the fact that vanadium is usually recovered in good yield by acid leaching has often been an economic advantage over results obtained with carbonate leaching. It has been found that response of an ore to carbonate leaching, following roasting, depends primarily on its composition and on the conditions of the prior roast treatment, particularly with regard to the roasting temperature, the atmosphere maintained above the charge during roasting and cooling, and the presence of certain reagents. These factors, especially the last, virtually determine the extractions of uranium and vanadium attainable by carbonate leaching, as well as the reagent consumption on leaching, whereas adjustment of the leaching conditions has only a limited influence. These variables were examined systematically to elucidate roasting and carbonate leaching of carnotite ores and to establish a treatment yielding high recoveries of both uranium and vanadium. Tests were conducted on samples of four different Colorado Plateau ores, described in Table I. Roasting Procedure: The roasting tests were conducted in an electrically heated furnace in which the temperature was controlled to +15oC. The ore (usually a 500-g charge) was ground to —100 mesh, mixed with the desired reagent, and spread in a silica tray to a bed depth of about 1/2 in. During the roast the charge was rabbled at intervals of 15 min. To provide free access of air the furnace was usually ventilated; however, in a few experiments a controlled atmosphere such as carbon dioxide or hydrogen was maintained above the charge. Leaching Procedure: The pulp, generally comprising 500 g of ore and a 2000-cc solution containing 80 g per liter of Na2CO3 and 20 g per liter of NaHCO3, was agitated in an autoclave at 120°C, under 30 psi O2. Samples were withdrawn periodically, and the solution and ore residue were analyzed. Under the conditions employed, maximum attainable extractions were generally achieved in 4

Jan 1, 1958

Extractive Metallurgy Division Institute of Metals Division Iron and Steel Division OFFICERS AND COMMITTEES W R Hibbard, Jr , President J C Kinnear, Jr , Past President John Chipman, Vice-President T D Jones, Treasurer R W Shearman, Secretary AIME, 29 West 39th Street New York 18, N Y

Jan 1, 1958

By R. W. Jigins

OPERATIONS of the Braden Copper Co. are in the Chilean Andes, southeast of Santiago. Most remote of the company communities is Sewell, a town of 12,000 people, 7000 ft above sea level at the junction of the Coya and Teniente rivers. Four miles down the Coya River is the smelter town of Caletones, elevation 4500 ft, with a population of about 3000. At the junction of the Coya and Cacha-poal rivers 24 miles below Sewell is Coya, elevation 2500 ft, location of the company's two hydroelectric plants. The principal accounting offices; steel, iron, and brass foundries; railroad shops; and major mechanical repair and fabricating shops are at Rancagua in the central Chilean valley, 44 miles from Sewell. The company owned narrow-gage railroad connects with the Chilean national railroad at Rancagua and above Coya is the only modern means of travel. El Teniente mine at Sewell is the largest underground copper mine in the world. The mill, at the portal of the main tunnel, has a capacity of 34,000 tons of crude ore daily, although production is lower during the winter beacause of electric power restrictions. When operating at capacity the mill produces 2000 tpd of copper concentrates and 32,000 tpd of tailings. Tonnage of tailings is equivalent to about 100,000 tons of pulp at normal water to solid ratio. Because the streams flowing from the Andes in the area of Braden's operations are used for irrigation, it is impossible to dump tailings directly to the river. The tailings pulp must be separated into solids and decanted clear water, and the clear water returned to the same water shed from which the original water was removed. Remaining sands and slime must be deposited in a reservoir where they will not cause trouble to farmers.

Jan 1, 1958

By E. P. Klier, Volker Weiss, George Sachs

IT has been shown that the isothermal transformation of austenite in a special steel can be modified by isothermal holding in the high subcritical transformation range.' Since this treatment potentially leads to increased hardenability, limited testing has been completed to determine if the stabilization effects observed with this treatment can be used to advantage in the heat-treating of 4340 steel. As an index of the effects of the several austenitizing treatments on the hardenability of the steel, Jominy-type hardenability tests were completed for specimens 2.5 in. in diameter and 8 in. long. Since the steel studied is to be used at strength levels where notch sensitivity is of major concern, notch sensitivity after selected austenitizing treatments has been evaluated by notch tensile tests for several specimen sizes. The steel composition and the austenitizing treatments are given in Table I. The test specimens are presented in Fig. 1. The hardenability data are given in Fig. 2 and the notch tensile properties are presented in Fig. 3. The hardenability of the steel investigated when determined by use of the standard Jominy test specimen2 as high and remained essentially unchanged for the different austenitizing treatments. For the larger test specimen, as has been shown by other investigations," the characteristic hardenability indexes are changed and it becomes possible to isolate austenitizing treatments which promote maximum hardenability. The stepped austenitizing treatment promotes higher hardenability as is indicated in Fig. 2. The evaluation of notch sensitivity for very high strength steels is best accomplished by means of the notch tensile test. The experimental conditions of the test, however, modify the notch strengths measured, and in the present experimentation an effort was made to achieve a limiting notch condition by fixing the notch root radius at 0.001 in. while the specimen diameter was allowed to increase from 0.3 to 1.1 in.* For this root radius the notch strength, 0.3-in.-diam specimen, and this trend differs from that for the larger specimens. At the highest tempering temperatures the 1.1-ip.-diam specimens yield comparable results for the austenitizing treatments compared. However, as the tempering temperature is progressively lowered below 800°F, em-

Jan 1, 1958

By H. W. Mead, C. E. Birchenall

SELF-DIFFUSION in pure gold has been studied by Sagrubsky,1 McKay,2 Gatos and coworkers,3,4 and Okkerse.5 Sagrubsky used a sectioning technique but reported results far lower than any of the others. The work seems to be carefully done, and it appears that a factor of 60 must have been omitted in his calculations or the units misstated by an equivalent amount. McKay used a surface activity method, and Gatos and Kurtz, following Gatos and Azzam, applied autoradiography to the measurement of activity on an oblique section through the diffusion zone. These two investigations agree well with each other but give results below those reported here. Okkerse employed a very careful sectioning technique. Chemical interdiffusion in Au-Ag alloys has been measured under several concentration conditions. Average values of the diffusion coefficient for the range of 0 to 18 atomic pct Au were obtained by Braune.6 since the diffusion coefficient probably varies markedly over this range, the values may not be too useful. Also, a plot of these data suggests that grain boundary contributions may have been appreciable at the lowest temperature employed. Ebert and Trommsdorf7 give average values for 0 to 9 atomic pct Ag, and Johnson8 reports average values for 45 to 55 atomic pct Au. Johnson also measured silver and gold self-diffusion coefficients in 49.2 atomic pct Au alloys, and self-diffusion in pure silver. The self-diffusion of gold in pure silver has been determined by Jaumot and Sawatsky.10 Other measurements which do not cover a range of temperature or are of low precision are not mentioned in this account since a review by Kubaschewski is available." This contribution reports diffusion coefficients for self-diffusion in gold, self-diffusion of gold in Au-Ag alloys, and chemical diffusion in Au-Ag alloys. Although it had been intended to obtain silver self-diffusion data in the alloys it now appears unlikely that these measurements can be done soon, so a table has been worked out for a self-consistent scheme of diffusion coefficients which should not be too far from the true values. Experimental Details Experiments on pure metals were conducted using fine gold of 99.99+ pct Au and silver of the same purity. Alloys were prepared by melting the two metals together in a graphite crucible in vacuo and allowing the slug to solidify in the crucible. After machining to a cylinder about 0.85 in. diam each slug formed one half of a diffusion couple. Compositions were determined later by analyzing chips taken from the extremities of the diffusion zones. The gold used in the preparation of alloys was sometimes pure gold but was normally either in the form of clean pickled alloy from previous experiments or gold recovered by oxalic acid precipitation from warm aqueous solution. Chips from the various stages of experimentation were dissolved in aqua regia and the solution taken to low bulk, diluted with water, and again taken to low bulk before diluting for the precipitation. This precipitated gold contained a small amount of silver as the only impurity detectable by spectrographic analysis. Disks for use in diffusion couples had opposite plane faces abraded on emery paper as far as zero grit, were annealed for 12 hr at 900°C in argon, and had one face of each disk polished to 000 emery paper. Radioactive gold was plated at about 2 ma per sq cm from a small volume of cyanide solution containing 1 mg of inactive gold as a carrier. Specimens , were freshly abraded on 4/0 emery paper immediately prior to plating. In the case of the active couples disks of a similarly prepared but unplated alloy or pure metal were placed on top and welded to the active disk. With the concentration couples disks of different compositions were welded. Welding was performed after a pressure of 5,000 lb had been applied at

Jan 1, 1958

By T. B. Massalski, C. S. Barett

THAT metals and alloys of the body-centered-cubic structure tend to become unstable at low temperatures is so nearly universal that any exceptions are worthy of special attention. Studies of the exceptions may disclose unrecognized examples of metastability or may shed light on the nature of some of the factors that stabilize the body-centered-cubic phase. Among the structurally analogous body-centered-cubic 3/2 electron compounds, the ß-phase in the Cu-Zn system deserves further attention for, although this phase is known to undergo partial mar-tensitic transformation on cooling below room temperature to the temperature of liquid nitrogen when the composition is less than about 42 wt pct Zn, it does not transform on cooling .when there is more than this amount of zinc present.1-4 The present authors recently found that an alloy containing 48.35 wt pct Zn could be transformed, however, if deformed severely at room temperature or lower temperatures.V his discovery led to the suggestion that the jerky flow of ß-brass single crystals6 and some of the unusual temperature variations of the yield strength and hardness are due to strain-induced transformation during the tensile tests. The present investigation is an extension of that work to cover the entire available range of compositions of Cu-Zn ß-phase alloys and certain interesting compositions of the ß-phase in the Cu-Zn-Ga system. Particular attention is given to the structure of the transformation product resulting from cold work, which is found to vary with alloy composition, and to the temperature range in which transformation can be induced in the various alloys. The composition limits of the body-centered-cubic phase in the Cu-Zn system, based on a recent review by Raynor7 and the precision determinations of Beck and Smith: are shown in Fig. la; in the ß region the alloys are disordered and in the ß region they are ordered. The rate of ordering is so rapid that a high degree of order is found in any of these alloys immediately after quenching. Experimental The nine binary and four ternary alloys of this investigation were prepared from cathode copper (99.99 pct purity), electrolytic zinc (99.99+ pct), and gallium (99.98+ pct). All alloys were cast in transparent Vycor tubing, homogenized at temperatures between 800° and 890°C, and quenched in water. Ternary alloys were cast in small amounts (-5 g) to predetermined compositions to fall along a line of constant electron concentration in the ternary system. Changes of weight during the casting operation of the ternary alloys were not greater than 1 part in 2500 from the intended nominal weights and therefore their compositions were accepted without chemical analyses. All binary alloys were cast in larger amounts (100 to 150 g), homogenized, and hot rolled after preheating to 800°C. The central portion of the rolled strip of each alloy was annealed for eight days and quenched in brine. All binary alloys were analyzed chemically. The compositions, heat treatments, and metallographic appearances of all alloys are tabulated in Table I. Various samples were subjected to heat treatment or cold work at several temperatures and were then examined metallographically or by means of X-rays. Specimens about 6x6x3 mm in size were examined metallographic ally to confirm the presence of the ß-phase after quenching. Cold work was introduced by fastening each sample between two pieces of steel, cooling the assembly to the desired temperature, and transfering it rapidly to a vise where moderate or severe compression was immediately applied. Cold working at liquid helium temperature was done by a chisel-shaped tool mounted on an X-ray spectrometer, described elsewhere.% A!! metal-

Jan 1, 1958

By S. H. Ward, R. A. Barker

THE Juniper Prospect is in Carleton County, N. B., at approximately 46º 31' north latitude, 67º 20' west longitude. During the summer of 1955 an area in west-central New Brunswick was selected for aerial electromagnetic prospecting with American Metal Co.'s helicopter-mounted equipment. Generalized, small-scale government geologic maps had suggested that this area was located along the western border of the northeast-trending granitic backbone of northwestern New Brunswick and might be underlain by the Ordovician-Silurian sediments and volcanics that are the host rocks for the recently discovered sulfide deposits of the Bathurst-Newcastle district.

Jan 1, 1958

By Robert G. Van Nostrand, John H. Henkel

TRANSIENT potentials obtained in resistivity prospecting can be separated into two classes. The first is electromagnetic, has a comparatively short time constant, and increases in relative amplitude as the electrode separation is increased. These electromagnetic transient potentials, of which an excellent theoretical treatment is given by Yost: are the result of changes in the current and can be classed as differentiated signals. The second class is electrochemical, has a comparatively long time constant, and decreases in relative amplitude as the electrode separation is increased. The electrochemical signals are generated by the current flow itself and can be classed as integrated signals. The transient potentials due to electrochemical factors are the subject of this article. The phenomenon is referred to as induced polarization. Schlumberger" was the first worker to observe induced polarization, but he was unsuccessful in attempts to apply the principles of induced polarization in electrochemical prospecting. Other workers, notably Bleil; have studied polarization and in some cases pointed out its possibilities, but no theory has been presented that describes polarization and its time dependence adequately. It is the purpose of this discussion to present the essence of a theory to geo-physicists and to show that it leads to results consistent with experimental evidence. The theory on which this analysis is based has existed in electrochemical circles since 1910."

Jan 1, 1958

By Hans Conrad, W. D. Robertson

FORMAL theories of yielding and flow have been developed to describe thermally activated plastic flow in metal crystals.'-" hey are all based on Becker's' original idea that thermal fluctuations aid the applied stress in overcoming internal barriers to flow and lead to the following relation. where j is the strain rate; C is a constant which includes a frequency factor, the entropy, the number of flow units, and the amount of strain associated with each successful fluctuation; E(T) is the activation energy associated with flow, and is a decreasing function of the applied stress, 7; k is Boltzmann's constant; and T is the temperature in OK. The various theories differ mainly in the model chosen and in the nature of the relationship between the applied stress and the activation energy. Beckerl and Orowan' suggest a relationship of the form E a(Ti — t)2, where .ri represents the stress required for flow without the aid of thermal fluctuations; Kauzmann,3 Cottrel1,5 and Seeger6,7 suggest E a(t — t) ; Fisher8 suggests E while Cottrell and Bilby4 suggest a more complex relationship between E and 7. Additional data are needed to test these various theories., esweciallv- in view of Dorn's9 ork. which indicates that the activation energy for creep is independent of the stress and strain. The present paper presents the stress-strain data derived from incremental loading of magnesium single crystals in tension and direct shear, in the temperature range of 78" to 364°K. Incremental loading was employed in order that the creep component of the strain could be determined. Stress-strain curves of aluminum10-13 and copper" single crvstals. derived from incremental loading tests, have been found to be in agreement with those obtained by the more conventional constant strain rate or loading rate tests. Two types of tests were conducted in the present investigation: 1) tests in which the temperature was maintained constant throughout the entire

Jan 1, 1958