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Tile National Research Council announces further appointments to National Research Fellowships in physics and chemistry. The object of the National Research Council in maintaining a system of research fellowships is to promote fundamental research in physics and chemistry primarily in educational institutions in the United States. Fellowships are awarded to persons who have demonstrated a high order of ability in research for the purpose of enabling them to conduct investigations at educational institutions which make adequate provisions for research: in physics and chemistry. The new appointments are as follows: In Chemistry.-Warren C. Vosburgh, of New York City, B. S. Union College, 1914, A. M. Union College, 1916, Ph. D. Columbia University, 1919. Research assistant to the Professor of Chemistry at Columbia University for the past six months. George Scatchard, of New York City, A. B. Amherst College, 1913, Ph. D. Colt tibia University, 1917. Formerly research assistant to the Professor of Chemistry at Columbia University and instructor in organic chemistry: First Lieutenant. Sanitary Corns. U. S. A.

Jan 7, 1919

By J. R. Mihalisin, J. S. Iwanski

The response of Inconel "700" to heat treatment has been studied by light and electron microscopy combined with X-ray and electron diffraction techniques. A heat treatment which vesults in low ductility for this alloy appears to be associated with the formation of MC carbide in a Widmanstdtten distribution. This type of precipitation can be suppressed by suitable heat treatment with concurrent increase in ductility. Various other phases precipitated in this alloy are also identified. RECENT studies of commercial nickel base su peralloys have demonstrated the importance of the morphology of carbide phases upon physical properties.' For example, empirical heat treatment studies applied to Nimonic "80" and Inconel "X" have resulted in prescribing double aging treatments for optimum physical properties. These treatments have subsequently been related micro-structurally to grain boundary carbide morphology.2 The purpose of this study was to obtain information about the morphology and identity of some of the phases precipitated in Inconel "700" after heat treatment. It was hoped that some correlation could be made of micro structure with heat treatment similar to that observed with Inconel "X" and Nimonic "80." EXPERIMENTAL PROCEDURE Specimens were obtained from a hot-rolled bar of Inconel "700" of the following composition: C Mn Fe S Si 0.10 0707 0.42 0.007 0.12 Cu Cr -A1 -Ti- Co Mo Ni 0.02 -14.90 TM 2.22 27.61 2.92-- Bal. Specimens were prepared in the following heat-treated conditions: (A) 2275°F for 2 hr WQ (B) 2275°F for 2 hr WQ + 2000°F for 1 hr (C) 2275°F for 2 hr WQ + 1600°F for 48 hr. (D) 2275°F for 2 hr WQ + 2000°F for 1 hr + 1600°F for 48 hr. Empirical stress-rupture studies had shown that treatment (D) resulted in optimum stress-rupture life and ductility. Treatment (C), although giving a good aging response, resulted in low ductility. Treatments (A) and (B), respresenting individual. steps in treatments (C) and (D) were added here for microstructural comparison studies. The procedure was to make an optical and electron microscopic investigation supplemented by X-ray diffraction analysis of electrolytically extracted residues. Electron diffraction studies were made utilizing selected area diffraction techniques with extraction

Jan 1, 1960

By AIME AIME

Acid Open-Hearth Manipulation.. By ANDREW MCWILLIAM and WILLIAM H. HATFIELD, ii, 279. Discussion by J. J. MORGAN, iii, 647; E. H. SANITER, iii, 648; MCWILLIAM and HATFIELD, 111, 648. ADDICKS, LAWRENCE. The Effect of Impurities on the Electrical Conductivity of Copper, iii, 559. Address of Welcome to the U. S. National Museum, Washington, D. C. By RICHARD RATHBUN, .iv, 923. ALLDERDICE, TAYLOR. Discussion of MR. ROE'S paper, The Mann¬ facture and Characteristics of Wrought Iron, v, 1091. American Mining Engineer. Discussion by ARTHUR JARMAN, iii, 641. An Automatic Stock-Line Recorder for Iron Blast-Furnaces. By J. E. JOHNSON, JR., iii, 509. Anthracite-Washeries. By GEORGE W. HARRIS, vi, 1263.

Jan 1, 1907

Jan 11, 1951

By George W. Harris

In the earlier period of anthracite-mining, much coal was wasted, both underground and in the culm-banks on the surface. Such waste is common in the development of new mining-districts, in which, as a rule, only the richest material can be profitably treated. In the anthracite-region, special causes operated to increase this evil. The mines were generally worked under 20-year leases, and royalties were paid upon such coal only as was actually marketed. The lessees consequently cared for immediate profit solely. They were not bound to win all the coal they exposed, or to leave it in such condition that their successors could win it. Nor was it their interest or duty to educate consumers in the use of their product. The market called for coal of large sizes; and such coal they furnished, throwing away the rest. Any pains taken by them to bring about a more rational use of coal by their consumers would have borne fruit, after their leases had expired, to the benefit of somebody else. A full statement of the situation was given in 1893, in the report of the State Commission, appointed in 1889 to investigate the subject.' That body included the names of Heber S. Thompson, William Griffith and the late Eckley B. Coxe.2 Its report gives special attention to the utilization of the old culm-banks.

Jan 1, 1906

By G. R. Lehman

The Inspiration Consolidated Copper Co. had an orebody at Miami, Ariz., of close to 100,000,000 tons of low-grade copper ore, and the method of mining this ore most profitably was of great importance. The selection of a method was practically limited to a "top-slicing," a "shrinkage-stope" or a "caving" method. The "top-slicing" method would give a high extraction of the developed ore, at a high mining cost, and the "shrinkage-stope" or "caving" methods a lower extraction of the developed ore, at a lower mining cost. Ore-Drawing Tests To decide on the method to be used it was necessary to know about what extraction of the ore could be obtained by the "shrinkage-stope" or " caving " methods. As no definite information regarding the,question was available at the time, C. E. Mills, the general manager, thought that some information could be obtained by experimenting in drawing ore, covered with capping, from an experimental box. Some work had already been done along these lines by W. C. Browning for the Inspiration Copper Co. and by myself for the Live Oak Development Co. The idea was to represent as nearly as possible, in the experimental box, the conditions within an area of caved stopes of caved ore all ready for drawing. That is, the area was supposed to represent a semibroken mass with the capping above it in the same condition and ready to follow the ore downward as it was drawn out of the chutes under the ore. To represent the above condition, in the experimental box, crushed ore from the mine was placed in it to a given height, and red barren capping from the mine was placed on top of the ore. The Experimental Box The experimental box shown in Fig. 1 was made of wood and glass. The glass was used for the sides so that the drawing action of the outside row of chutes could be seen and noted, the latter being cut in the center by the glass sides. The length of the box was 30 in., width 20 in. and the

Jan 1, 1917

By Paul D. Merica, R. G. Waltenberg

Although nickel was discovered and isolated as early as 1750 and its valuable properties recognized, many years passed before it was used commercially for wire, sheet, rods, etc., in the pure form. This was due partly to its high cost at that time and partly to the fact that it was not possible to refine and cast nickel into ingots sufficiently malleable to be amenable to the usual forging, rolling, or drawing processes. So remarkable was this fact, and so different from the experience at that time with metals such as copper and iron, that it has left its impress on the nomenclature within the nickel industry. To this day, furnace-cast nickel produced in such a manner as to be suitable for rolling and forging is called malleable nickel to distinguish it from the ordinary pig and shot nickel of commerce. In 1878, the firm of Jos. Wharton, of Philadelphia (which later became The American Nickel Works, a constituent of The International Nickel Co.) exhibited at the Paris Exhibition specimens of rolled pure nickel strip and of drawn nickel wire. About this time, there was considerable activity in the study of the refining of nickel and several methods were described, some of which were patented, for the production of furnace-cast malleable nickel including the use of manganese (Boed-dicker,1 Selve and Lotter2), the use of potassium permanganate (Berns-dorfer Metallwarenfabrik3) and the use of phosphorus (Garnier4). By far the most efficient method was discovered by Th. Fleitmann in 1879;5 it consisted in adding to the molten nickel, just before pouring the castings, from 0.05 to 0.125 per cent. of metallic magnesium. This soon became the recognized final malleableizing treatment for furnace-cast nickel.

Jan 1, 1925

ASSETS CAPITAL ASSETS Equity in United Engineering Society's Land and Buildings $486,792 79 Library 40,000 00 $526,792 79 INVESTMENTS Jas Douglas Fund-Schedule #2 $ 99,966 40 Life Membership Fund-Schedule #3 9,415 63 R W Hunt Medal Fund-Schedule #4 7,489 09 116,871 12 INVENTORIES Paper Account .305 10

Jan 1, 1923

[ASSETS CAPITAL ASSETS: Equity in United Engineering Society's Land and Buildings $486,792.79 Library 40,000.00 $526,792.79 INVESTMENTS: Jas. Douglas Fund-Schedule #2 $ 99,966.40 Life Membership Fund-Schedule #3 9,415.63 R. W. Hunt Medal Fund-Schedule #4 7,489.09 116,871.12 INVENTORIES: Paper Account 305.10] [ ]

Jan 1, 1925

By AIME AIME

FRIEND recently remarked that the career of Scott Turner is characterized by Work and Wild -A Ducks. To these might be added Accomplishment and Persistent Fishing. All of these elements are manifestations of his character. The diversions-hunting and fishing-are in the nature of the proverbial trolley conductor's holiday, for many of Turner's years have been spent in the outdoors, often in distant lands, as in Spitzbergen, where the ducks pictured below were bagged. The election of Scott Turner to the presidency of the Institute marks the culmination of a quarter century of membership, during the last two years of which he has been vice-president. He was born at Lansing, Mich., on July 31, 1880, and received his A.B. at the University of Michigan in 1902, with a B.S. and E.M. at the Michigan College of Mines in 1904. Since then he has been granted two honorary degrees, D.Sc. from the Colorado School of Mines, and D.Eng. from the University of Michigan, but he still prefers to be called "Scott" rather than "Doctor." Government service was not a new experience for Turner when he was appointed Director of the U. S. Bureau of Mines by Secretary Hoover in 1925, for his first employment after graduation was as Field Assistant in the U. S. Geological Survey in Oregon and Idaho. This was followed by work in Tombstone, Ariz.; then his first foreign engagement in 1905-6 as superintendent of the San Pablo Gold Mining Co. in Panama. Various field experiences followed, though there was an interlude in work of a kind that few mining engineers ever experience. This was in technical journalism, for in 1906 he was

Jan 1, 1932

By Paul C. Merritt

The story now unfolding on the Mesabi Range is more than just another chapter in the continuing history of iron mining. It is an epic of foresight, research and pioneering instinct just now culminating in the rapid growth of a new industry hardly more than ten years old. And that growth has been impressive. In the decade that has passed since Reserve Mining Co. blazed a trail as the first successful large- scale commercial taconite operation, the number of plants now existing or soon to be operating has grown to six. From Reserve's initial capacity of 3 million tons of pellets per year, total production capacity on the Range has surged to 31.5 million tons while capital investment has leaped from $300 million in 1955 to almost $1 billion today. During the past year alone, more than $500 million has been committed to these projects, an amount probably greater than that going into any other single mining area in the world. There is more yet to come.

Jan 10, 1965

By A. F. Colombo, R. T. Sorensen, D. W. Frommer

An analytical method has been developed and used in batch and continuous tests to provide initial insights into the effect of soluble calcium ion in anionic flotation of silica from iron ores. A deficiency or excess of calcium ion in pulps subjected to this type of flotation produces an impairment in flotation efficiency. Data developed in the investigation are from a single ore, but show that total calcium requirement is met from water, ore and reagent sources. In batch studies, starch additions were shown to exert no influence on the calcium level, but fatty acid and sodium hydroxide had subtractive effects. The investigation was next extended to continuous flotation testing where the general observations from batch testing were confirmed. Factorially designed experiments were performed showing that the relationship of calcium additions to flotation response was not a simple one, but tended to shift to higher additions with increased fatty acid. Nevertheless, the range of soluble calcium levels measured remained fairly constant in areas of good flotation response. It is concluded that techniques developed should be useful in removing empiricism from flotation operations in this and other systems requiring activation for success. Further development should aid in process control both through methods outlined and through investigations aimed at studying the effects of other soluble reagents. Of the major mineral commodities, iron ore was one of the last to succumb to flotation processing. Commenting on this fact, one of the speakers 1 at the convention celebrating the 50th Anniversary of flotation in the U.S.A., said ". . . in 1951 froth flotation as a means of beneficiating nonferrous minerals was a might giant and could be characterized by 'you name it, we float' - but not iron ore". This tardiness in applying flotation to iron ores was the result of a number of factors, including economics and ready availability of direct shipping ores. Even now, when the need for beneficiation can no longer be denied, proposals for flotation of iron ores are apt to be viewed with some misgivings. This disquiet results from knowledge that wide variability, which would necessitate corresponding adjustments in reagents, often exist within even a single ore deposit. Coupled with ore variability is the fact that, at present, there is no way of quickly and precisely anticipating the direction and magnitude of reagent changes required for uninterrupted production of acceptable concentrates. Despite the long delay, iron ore flotation is now practiced commercially, although the chief applications2-4 are to specular hematites having relatively coarse liberation and low slime content. In addition, the application of flotation in upgrading magnetic concentrates seems assured. However, these flotation methods do not appear applicable to substantial tonnages of fine grained, earthy, and frequently more complex semitaconites and nonmagnetic taconites. The U.S. Bureau of Mines, in devoting its attention to the semitaconite and nonmagnetic taconite class of materials, has demonstrated that anionic flotation of calcium-activated silica can be utilized with an expected high frequency of success.' Even so, it has been recognized that the flotation method is a complex one, and that the reagent suite must be carefully tailored to the feed. These conditions would be expected to offer difficulties in treating ores with the wide range of variability previously discussed. Accordingly, research was initiated to develop methods to remove much of the empiricism from the flotation operation by measuring the reagent variables within the pulp for a correlation with flotation response. A simple illustration of the technique sought would be in the well established use of pH meters to provide feedback control to reagent feeders and thereby limit acidity or alkalinity to a range producing optimum results. The first efforts in this area have been concerned with measurements of soluble calcium ion. Bureau experience in both laboratory and pilot plant over the past five years has proved that the amount of calcium

Jan 1, 1965

By J. C. Humbert, J. F. Elliott

The solubility of nitrogen in liquid pure Fe, Cr, and Ni, in liquid Fe-Ni, Fe-Cr, and Ni-Cr alloys and Fe-Cr-Ni alloys, has been measured by the Sieverts' type apparatus between 1500° and 1800°C. Tabulations and graphs of the solubility data and activity coefficients are shown. Heats of solution are reported. Interaction coefficients of the several elements in Fe. Cr, and Ni ave also reported. THE solubility of a gas in a liquid metal is usually measured by either the quenching technique or the so-called Sieverts' method. In the quenching method, 1-3 the melt is equilibrated at the desired temperature and pressure with the gas phase having a known fugacity of the gas being studied. The melt is sampled and the sample is quenched and analyzed chemically for its gas content. In Sieverts' method the melt is contained in a closed chamber. The apparent volume of this chamber, i.e. the "hot volume," is usually determined by introducing a known quantity of an inert gas having very closely the same physical characteristics as does the experimental gas. Alternatively, the experimental gas is used with an inert specimen having the same general physical characteristics as does the experimental melt. Subsequently, the experimental melt is equilibrated with the experimental gas by introducing a known quantity of the gas into the calibrated chamber. The solubility of the gas is obtained from P-V-T relationships. The quenching method suffers from' the limitation that some gas may be gained (as in the case of Cr-Fe alloys) or lost (as in the case of Fe-Ni alloys) during solidification and cooling of the sample. With Sieverts' method sampling and analysis are unnecessary. However, errors can result from the difficulty of determining accurately the "hot volume,"

Jan 1, 1961

By J. D. Verhoeven

In the past 15 years a considerable amount of experimental and theoretical work has been done concerning the onset of convection in liquids as a result of interm1 density gradients. This work, which has been doue in many different fields, is reviewed here and extended slightly to give a rrlore quantitative understanding to the probletrz of conzection in liquid metal dlffusion experinletzts. In liquid metal systems the capillary reservoir technique is currently used, almost exclusively, to measure diffusion coefficients. In this technique it is necessary that the liquid be stagnant in order to avoid mixing by means of convection currents. Convective mixing may result from: 1) convection produced as a result of the initial immersion of the capillary; 2) convection produced in the region of the capillary mouth as the result of the stirring frequency used to avoid solute buildup in the reservoir near the capillary mouth; 3) convection produced during solidification as a result of the volume change; and 4) convection produced as a result of local density differences within the liquid in the capillary. The first three types of convection have been discussed elsewhere1-a and are only mentioned for completeness here. This work is concerned only with the fourth type of convection. Local density differences will arise within the liquid as a result of either a temperature gradient or a concentration gradient. It is usually, but not always, recognized by those employing the capillary reservoir technique that the top of the capillary should be kept slightly hotter than the bottom and that the light element should be made to migrate downward in order to avoid convection. In the past 15 years a considerable amount of work, both theoretical and experimental, has been done in a number of different fields which bear on this problem. This work is reviewed here and extended slightly in an effort to give a more quantitative understanding of the convective motion produced in vertical capillaries by local density differences. The Stokes-Navier equations for an incompressible fluid of constant viscosity in a gravitational field may be written as: %L + (v?)v = - ?£ + Wv - g£ [1] where F is the velocity, t the time, P the pressure, p the density, v the kinematic viscosity, g the gravitational acceleration, and k a unit vector in the vertical direction. A successful diffusion experiment requires the liquid to be motionless, and under this condition Eq. [I] becomes: where a is the thermal expansion coefficient [a =-(l/po)(dp/d)], a' is a solute expansion coefficient [a' = -(l/po)(dp/d)], and the solute is taken as that component which makes a' a positive number. Combining with Eq. [3] the following restriction is obtained: Since there is no fixed relation between VT and VC in a binary diffusion experiment, Eq. [5] shows that the condition of fluid motionlessness requires both the temperature gradient and the concentration gradient to be vertically directed. Given this condition of a density gradient in the vertical direction only, it is obvious that, as this vertical density gradient increases from negative to positive values, the motionless liquid will eventually become unstable and convective movement will begin. The classical treatment of this type of instability problem was given by aleih' in 1916 for the case of a thin fluid film of infinite horizontal extent; and a very comprehensive text has recently been written on the subject by handrasekhar.' It is found that convective motion does not begin until a dimensionless number involving the density gradient exceeds a certain critical value. This dimensionless number is generally referred to as the Rayleigh number, R, and it is equal to the product of the Prandtl and Grashof numbers. For the sake of clarity a distinction will be made between two types of free convection produced by internal density gradients. In the first case a density gradient is present in the vertical direction only, and, since the convection begins only after a critical gradient is attained, this case will be called threshold convection. In the second case a horizontal density gradient is present and in this case a finite convection velocity is produced by a finite density gradient so that it will be termed thresholdless convection. Some experimentalists have performed diffusion experiments using capillaries which were placed in a horizontal or inclined position in order to avoid convection. These positions do put the small capillary dimension in the vertical direction and, consequently, they would be less prone to threshold convection than the vertical position. However, if the diffusion process produced a density variation, as it usually does, it would not be theoretically possible to avoid thresh-

Jan 1, 1969

By S. S. Marsden, S. A. Khan

Externally generated foam was injected continuously into short porous media. Both flow rate and pressure drop were measured. Liquid saturation was determined by electrical conductivity. Foam yuality I, expressed as the ratio of gas volume to total volume, was varied from 0.70 to 0.96. As measured with a modified fann VG Meter, apparent viscosity of this foam µa decreases with increasing shear rate but usually falls within the range of 50 to 500 cp. At a given shear rate, µa increases almost linearly with I-. When measured with a Bendix Ultraviscoson, kinematic pa is independent of V but absolute pa increases with T from about 3 to 8 cp. The effective permeability -apparent viscosity ratio ke/µa decreases almost linearly with V for porous media of high permeability, but the rate of decrease becomes less for tighter ones. The relative permeability-apparent viscosity ratio kr/µa us V data does not fall on a single line. The kr/µa ratio increases with liquid saturation in the porous medium and with surfactant concentration. Estimates of pa for foam in porous media vary from 30 to 100 cp. INTRODUCTION Although research on the development of a foam-drive, oil recovery process has been going on for almost a decade, most of the significant publications have appeared within the last several years. This illustrates well the rate at which interest in this process is accelerating. Bond and Holbrook 1 were the first to describe the use of foam to improve oil recovery in their patent of 1958. They proposed that an aqueous foaming agent slug be injected into the formation and that this be followed by gas to produce a foam in situ. Fried 2 studied the injection of foam into porous media which had already been subjected to conventional gas or water drives and found that gas could be used to drive a foam bank which would, in turn, displace additional oil in the form of an oil bank. He attributed the increased oil recovery to the high effective viscosity of foam flowing in porous media. His microscopic observations showed the importance of foam generation and regeneration within the porous medium. By injecting both air and aqueous surfactant solution, Bernard3 generated foams within the porous medium in which oil displacement was being studied. In a separate empirical test, he also measured the dynamic foaming characteristics of the same surfactants in water and/or oil. With some exceptions and for the seyen surfactants studied, there seems to be a qualitative relationship between the efficiency of liquid rlisplacrment and the dynamic foaming testtsed. This relationship was not consistent enough to eliminate the necessity of actual foam flood tests in porous media for surfactant selection. In a study basic to gas storage in aquifers, Bennett4 described the displacement of brine by foam in consolidated porous media. Among other things, he stated that the ability of a surfactant solution to foam is more important than the stability of its foam. The presence of a foam bank between the displacing air and the displaced brine improved both breakthrough and ultimate recovery. In a continuation of this work Kolb5 attributed the great reduction in surfactant solution production rate as displacement by air progressed to a decrease in relative permeability to gas. These several effects reported by both Bennett and Kolb can all be attributed to the high apparent viscosity of foam which was obviously flowing in the porous media. Bernard and Holm6 observed that gas permeability in the presence of foam was much less than in the absence of foam when both were measured at the same gas saturations. This reduction in permeability was proportionately greater for more permeable sands and sandstones than for the less permeable. Viscosities of the surfactant solution and air were used for their calculations rather than apparent foam viscosities. The foam stability increased with decreasing permeability, which was probably due to the natural regenerative properties of porous media, and the permeability reduction increased

Jan 1, 1967

By AIME AIME

DURING my senior year at college a professor said to his class that a student who failed to obtain a passing grade in that certain subject could not graduate with his class and that his diploma would be withheld until the failure had been removed. In that way for four years a diploma had been made to appear to us as the objective in attending college. We grew up to think that a diploma was the means of providing employment; consequently, a diploma could not be jeopardized and, heeding the professor's remarks, we resolved to put forth special efforts and make good. During one of our class periods this same professor digressed briefly from his prepared lecture in metallurgy and advised the boys to join a national technical society. He spoke with earnestness and sincerity. After class we students discussed those remarks. We concluded that the professor had not convinced us. We were already members of technical societies at school and saw no need of joining another. In fact, even up to that moment a society had never indicated to any of us that joining it had any relation to landing a job, and we were fully aware that joining another society meant paying out more money, for fees and dues, which money we then needed to buy food, clothes, and perhaps a new slide rule. Furthermore, we knew that joining a society was not part of the curriculum and, therefore, the diploma could not be withheld if we did not follow the advice. Our conclusion was that we would not join but would concentrate on our work that assured getting our diplomas.

Jan 1, 1936

By C. Laird, C. E. Feltner

An investigation into the effect of a material's slip character on its high strain fatigue properties has been carried out using copper and Cu-7.5 wt pct A1 as representative wavy and planar slip mode materials, respectively. In copper, the constant term and exponent in the Coffin-Manson equation, ?EpNf1/2 = const, are unaffected by the temperature of testing or the history of the metal. On the other hand, in Cu-7.5 wl pcl Al, while the exponent is invariant, the constant is increased with respect to copper and increased further with decrease in temperature. The life in Cu-7.5 wt pct A1 is double that of copper at room temperature and about four times at 78°K. Fractoflaphic studies indicate that these diffevences in life are associated with the early stages of cracking. In copper, severe surface rumpling provides crack nuclei at pain boundaries independent of' testing temperature or the history of the metal. In Cu-7.5 wt pct Al, the planar slip mode of deformation prevents grain boundary folding; crack nucleation is therefore mainly transgranular and the increase in life with respect to copper is associated with a prolonged linking-up stage of such transgranulay cracks. At the lower temperature the increased difficulty of cross slip inhibits multiplication of trans-granular cracks and retards the linking-up process, giving a further enhaancement in life. It is expected that such behavior will be found general in materials of wavy and planar slip mode, respectively. STAGE II crack propagation in high strain fatigue takes place by a repetitive process of crack tip blunting in the tension part of a fatigue cycle followed by resharpening of the crack in the compression part.1-3 This mechanism has come to be called the "plastic relaxation process".3 At very high strains (lives to failure less than 103 cycles), most of the life of a specimen is spent in crack propagation by the plastic relaxation process.4,5 Since the differences in the cyclic strain hardening behavior of metals and alloys are comparatively small in this strain range,6,7 the amount of blunting at a crack tip depends primarily on the applied strain amplitude. The rate of crack propagation in this life range is therefore nearly constant with respect to material and temperature of testing. In the longer life portion of the high strain fatigue range (l03 to 103 cycles to failure), a considerable fraction of the lives is spent in crack initiation and Stage I growth. Grain boundaries have frequently4,5,8 been found to be the sites for this growth which is also associated with a surface folding process.4'5 Such folding behavior may also be general in any material having a grain structure and capable of plastic deformation. It has therefore been suggested475 that the universality of the Coff in-Manson law,9'10 constant,* where ?Ep is the plastic strain range and Nf the number of cycles to failure, is reflected in the approximate invariance of both the crack initiation and propagation behavior. It happens that, in most investigations of the phenomena associated with failure,4,5,8 materials with a wavy slip mode have been used as vehicles for the studies, or else "normally" planar slip mode materials have been tested under conditions giving rise to wavy glide deformation, e.g., stainless steels cycled at high temperature.'' The purpose of the present investigation was to determine whether or not different cracking phenomena would occur when the slip mode of a material is planar and if the associated life to failure would be different than that of a wavy slip

Jan 1, 1968

By F. Weinberg

Lead single crystals have been deformed in tension over the temperature range of 4.2°K to the melting point. Changes in flow stress resulting from temperature cycling and strain rate cycling have been measured as a function of temperature for crystals of different orientations and purity. It was found that the flow stress ratio, after correcting for the temperature dependence of the shear modulus, decreased progressively with temperature above approximately 0.5Tm. The activation energy calculated from the high-temperature portion of the curve was found to be markedly higher than that of self-diffusion. For single glide crystals, the corrected flow stress showed an increase above 0.5 Tm before decreasitzg with temperature. This increase is attributed to static recovery occurrittg during temperature cycling. THE temperature dependence of the flow stress, based on temperature cycling and strain rate cycling, has been extensively investigated,' and on the basis of these results dislocation models of the work-hardening process have been proposed. In general, the flow stress is divided into two parts, ts, the short-range interaction term, which is only effective at low temperatures and which decreases with increasing temperature, and TG, the long-range stress term, which is independent of temperature after allowing for the temperature dependence of the shear modulus. The observations demonstrating that tG/µ is independent of temperature were generally carried out at low temperatures to minimize recovery effects. Several investigations have been reported on flow stress measurements at high temperatures2"5 which demonstrate that TG/µ does not remain constant at temperatures above 0.5Tm (where Tm is the melting temperature of the material in OK). Specifically, Hirsch and warrington3 carried out temperature cycling tests at two strain rates on single and polycrystalline aluminum up to 0.8 Tm and on polycrystalline copper. For aluminum they found that the flow stress ratio (the flow stress at temperature T2, divided by the flow stress at the reference temperature T1 in one temperature cycle) dropped progressively with increasing temperature above 0.5Tm. From the slopes of the high-temperature portions of the curves, they determined an activation energy for the deformation process of 1.6 ev (at best) which they considered was in agreement with the activation energy of self-diffusion, 1.35 ev. Calculations of the activation volume demonstrated that the deformation was not controlled by dislocation climb. They proposed a mechanism in which the rate-controlling process at high temperatures was due to the rate of move- ment of vacancies away from jogs, i.e., that of self-diffusion. Results of Lucke and Buhler4 on single crystals of aluminum confirmed this conclusion. They measured the critical resolved shear stress of aluminum over a wide range of temperature and strain rates. They found that the temperature dependence of the critical resolved shear stress was similar to that of the flow stress ratio, as determined by Hirsch and Warrington, and from their data calculated an activation energy for high-temperature deformation of 1.35 ev identical to that of self-diffusion. More recently Gallagher5 has carried out a detailed investigation of the temperature dependence of the flow stress ratio of copper, silver, and gold. In all cases, he found that the flow stress ratio, after adjusting for the shear modulus temperature change, drops at high temperatures. The activation energies he determined were found to be appreciably higher than the activation energy of self-diffusion of the material being considered. The flow stress ratio was found to be dependent on the orientation of the material, and, in addition, an anomalous increase in the flow stress ratio for copper, oriented for single glide, was observed above 0.5Tm. The purpose of the present investigation was to measure the critical resolved shear stress, the flow stress ratio, and the strain rate sensitivity of lead, primarily as a function of temperature. The results should indicate whether, following Lucke and Buhler, the critical resolved shear stress of lead has the same temperature dependence as the flow stress, and, following Hirsch and Warrington, whether the activation energy for high-temperature deformation in lead is the same as that of self-diffusion. Lead deforms as a normal fee material,6'7 is available in high-purity form, can readily be grown as single crystals, and, for this investigation, has the very considerable advantage of having a low melting point, 327°C. The observations of the critical resolved shear stress of lead have been published elsewhere.' EXPERIMENTAL PROCEDURE The experimental procedure was essentially the same as that used in the critical resolved shear stress measurements.' Single crystals of 99.999 pct (59) and 99.9999 pct (69) lead were deformed in tension with a table-model Instron in a silicone oil bath above room temperatures and in a cooled methyl alcohol or liquid-nitrogen bath below room temperatures. The test specimens were rectangular in section, 0.65 by 0.33 cm, and had a 5-cm gage length. The specimens were grown as single crystals with tapered ends, which fitted into matched tapered grips for testing. To obtain the flow stress between two temperatures, specimens were first deformed approximately 1.0 pct at the higher temperature. The test was then stopped, the load relaxed, the oil bath removed without disturbing the specimen, the grips and specimen cooled with a fan and then immersed in liquid nitro-

Jan 1, 1969

By C. Chiou, D. P. Seraphim

The effect of clustering on the superconducting properties of Al-Zn alloys has been studied by the ballistic induction techniques. The superconducting critical temperature, T,, changes when zinc-rich clusters are formed. The change in T, depends on the concentration and may be positive or negative, but always correlates with an effective decrease in the solute concentration of the alloy. Reversion after clustering effectively returns a 5 at. pct Zn alloy to the quenched state. These methods might be use&lly extended to the Al-Mg system, where X-ray data are difficult to obtain. In very dilute Al-Zn alloys, as in other tin,' indium, aluminum,2 or tantalums base solid solutions, there is a decrease in the superconducting critical temperature, Tc, roughly proportional to the temperature independent resistivity, i.e., -0.2°K per pS2cm. With increasing solute concentration, the T, generally reaches a minimum and then increases4 to a value well above that for the pure solvent. The change of T, with solute concentration follows an empirical formulation involving two constants which correlate with the scattering cross section of the impurities. As will be shown below, the Al-Zn alloys more concentrated than 1or2at. pct do not follow the empiricism, probably because they are unstable even when rapidly quenched.5 However, it seems possible to study at least the later stages of solute clustering by precise measurements of the 1', following various thermal treatments. A few experiments on quenched alloys, aged alloys, and tests on reversion are reported here. The heat treatments selected for obtaining the quenched and aged states were mainly deduced from the work of Dash and Fine.6 For the quenched state, specimens were homogenized at 480°C, quenched to -160°C, and immediately transferred and mounted in liquid nitrogen. Measurements on the superconducting properties and residual resistivities were then made at helium temperatures, after which the specimens were aged at room temperature for 3 to 5 hr, i.e., much longer than the time required for clustering to be essentially completed. The superconducting properties and residual resistivities were once again examined. To reach the reverted state of the A1-5at. pct Zn alloy, the aged specimen was heated for 5 min at 200°C and then tested as above.

Jan 1, 1963

By Marius S. Darrow, William B. White, Rustum Roy

The PbS-PbTe systen has been studied by quench-ing and D.T.A. techniques f?om 400' to 1150°C. Runs were made in evacuated silica tubes so that all equilibria are at the vapor pressure of the system. Lattice parameters of the quenched salnples , measured by X-ray diffraction, show a complete crystalline-solution series existing over a narrow temperature range between approximately 805" and 871°C. An exsolution dome extends from a maximum of about 805"C (approximately 30 mole pct PbTe) to 1 and 96.5 pet PbTe at 400°C. A narrow melting region, deternined by D.T.A., extends form 918c (mp PbTe), The shapes of the liquides and solidus curves imply the existence of a minimum at 871°C at approximately 65 pct PbTe. THe exact composition of the minimum could not be established due to the very narrow two-phase region. At compositions containing less than 50 pet PbTe, liquidus temperatures begin to increase, while the solidus remains almost flat to about 15 mole pet PbTe before beginning to vise toward the mp of PbS (1075 C). LEAD sulfide and lead telluride are isostructural (NaC1 type) semiconductors whose electrical and optical properties have been extensively studied and used in recent years. If appreciable crystalline solution exists between these compounds, the variation of physical properties with composition could be of interest. The purpose of this investigation was to determine the extent, if any. of crystalline solution, and to obtain the phase diagram for the system. To the knowledge of the authors, only three studies of the system PbS-PbTe have been reported, and, in chronological order, each investigation found an increasing amount of crystalline solution. In 1956, Yamamoto reported finding no evidence of crystalline solution between the compounds. Sindeyeva and Godov-ikov,' in 1959, found very limited crystalline solution. but only under conditions of excess tellurium concentration. Finally Melevski s3 investigation in 1963 indicated that one solid phase exists in the region from PbS to 7 pct PbTe and from 82 pct PbTe to PbTe at 886'C, with an eutectic at 55 pct PbTe at that temperature. Detailed data on the solvus boundary were not given. EXPERIMENTAL EQUIPMENT AND MATERIALS Commercially produced PbTe and PbS powders were used as starting materials. Batches of specific mole percent composition were accurately weighed and mixed in a plastic bottle, in a shaker mill. An analy- sis of impurity content is given in Table I for pure PbS and PbTe and for two randomly selected batches after the powders were mixed. Individual samples, ranging in weight from 0.2 to 0.5 g, were sealed in evacuated silica tubes which had been thoroughly washed and rinsed with acetone and distilled water. Thus all data taken were at the pressure of the system. Subsolidus relations were studied down to 400°C by heating the samples in a vertical tube furnace for 24 hr. The sealed tubes were quenched in water with quench time from the hot zone not exceeding 1 sec. Temperatures were measured by a chromel-alumel thermocouple and controlled to 53°C for most runs. The number and composition of phases present were determined from powder X-ray diffraction patterns taken at room temperature on a Norelco diffractome-ter, using silicon as an external standard. Above 850°C quenching techniques were, in general, found to be unsatisfactory, and differential thermal analysis (D.T.A.) was used to determine melting relations. The evacuated tubes were recessed about 1 cm at one end to accommodate the differential thermocouple. Al203 was used as the reference material in a similar tube containing the other side of the differential couple. For temperature measurements, a separate thermocouple was placed in the recess of the tube containing the sample to be measured, thus providing an opportunity to obtain thermal, as well as differential, analysis. All thermocouples for these measurements were Pt-Pt 10 pct Rh. Temperature and differential curves were recorded separately on synchronized strip-chart recorders. Thermocouples and recording equipment were calibrated using NaCl and gold standards, using the melting points 801" and 1063 C, respectively, which span most of the temperature range of interest. Heating and cooling rates generally were from 4 to 7°C per min. It was found, in fact. that rates ranging from 1.5 to 25°C per min did not significantly change the data obtained.

Jan 1, 1967