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By W. Jolley

Decarburized iron and Fe-3.28 pct Ni alloys were impact and tension tested in the temperature range of ambient to 4°K. It was found that alloying with nickel improves the fracture properties of the ferrite matrix. The improvement in toughness of iron alloyed with nickel is attributed to the effect of the nickel addition on the temperature and strain rate dependence of the yield stress as well as on slip behavior. The Fe-Ni alloy exhibits wavy slip when strained at temperatures down to at least 50°K. This behavior contrasts with that of the unalloyed iron where a change It is a generally accepted fact that of the common alloying elements of steel only nickel and manganese improve both the room-temperature yield strength and the notch impact properties. It has been argued for a number of years that manganese refines the ferrite grain size, the pearlite spacing, and the grain boundary carbides in medium- and low-carbon steels and thereby increases resistance to brittle fracture.''' This hypothesis recently was confirmed for a 0.04 pct C iron containing manganese, but at the same time from wavy to planar slip occurs at about 120°K. The observed lower temperature and strain rate dependence of the lower yield stress in the Fe-Ni alloy as compared to the unalloyed iron may be attributed to this difference in slip behavior. In contrast to suggestions published previously, transmission electron microscopy showed that the uniform dislocation distributions and the lack of dislocation tangles which are produced by low-temperature straining of bcc materials cannot be attributed to the absence of cross slip at these temperatures. no increase in notch toughness was observed in a decarburized Fe-Mn alloy.3 It thus appears that manganese only increases the toughness of Fe-Mn-C alloys by refining grain boundary carbides and has no toughening effect in carbon-free iron. On the other hand, the mechanism whereby nickel improves toughness has not been established. Hodge et a1.4 have clearly shown that a 3.28 pct Ni addition lowers the impact transition temperature of 0.02 pct C steel approximately 35°C when the grain size is maintained constant. Recently, Wullaert and Tetelman6 stated that nickel refined the grain boundary carbides of an Fe-C alloy and consequently increased the toughness. They also observed the previously reporteda-'

Jan 1, 1969

By Donald L. Katz

FIFTEEN years ago Dr. Manning published a paper in "Petroleum Development and Technology" on '.Fundamental Research Relating to Petroleum." He tabulated for several industries "the proportion of their present success which can be fairly attributed to the application of information and processes obtained by scientific research," giving petroleum a score of 7 compared to 100 for the electrical and coal-tar industries. Today the petroleum industry as a whole and the producing groups both have raised their score beyond the majority and are climbing toward the top. Present practices are being developed both by fundamental research and the application of the research method in field operation.

Jan 1, 1941

By H. F. Moore

This paper gives a preliminary summary of results of tests on the resistance to fatigue under reversed stresses of steel subjected to cold-working and of tests to determine the effect of rest on the endurance of steel under reversed stresses. The tests of cold-worked steel were undertaken as part of an investigation by the National Research Council Committee on Fatigue Phenomena of Metals and were made by Mr. Moore; the tests to determine the effect of rest are part of an investigation now being made by Mr. Putnam. Both series of tests were made in the Materials Testing Laboratory of the University of Illinois. The preliminary results of these tests are reported now. because it is believed that test data on fatigue strength should be available at the earliest possible moment; however, it should be clearly kept in mind that this paper gives preliminary results and is intended to encourage discussion rather than to give final conclusions. Before giving the data of the tests, the writers will explain the term "fatigue strength" as used in this paper and will discuss briefly the method used in interpreting the test data of repeated-stress tests. The term fatigue strength, as applied to a material, may be defined as that maximum fiber stress that will cause fracture of the material after the repetition of any given number of cycles of stress, each cycle involving the variation of stress from a minimum to the above maximum. The fatigue strength, then, varies with the number of repetitions occurring in the lifetime of a structural or machine member and with the range of stress for each cycle of stress. The fatigue strength will be lower for a member in which the stress is completely reversed than for one in which the stress varies from zero to a maximum. In interpreting test data from fatigue tests under reversed stress, the stresses and corresponding numbers of repetitions required for failure are plotted on logarithmic cross-section paper. In 1910, Professor

Jan 2, 1919

By D. G. Westlake

NUMEROUS hydride habit planes in zirconium, Zircaloy-2, and Zircaloy-4 have been observed by various researchers and have been compiled by Louthan and Angerman.1 While only partial agreement exists on the identification of these habit planes, there is a growing consensus that a tensile stress applied on a polycrystalline rod during slow cooling will cause the hydride platelets to lie perpendicular to the tensile axis. walters2 agrees with Louthan and Angerman who reason that "The particular plane on which precipitation will occur is the plane that will result in the maximum relief of stress by precipitation of the low-density hydride." The experiment described below was initiated to test this hypothesis on a single crystal of zirconium. A single-crystalline tensile specimen of zone-refined zirconium, designated number 13 in a previous study,3 had a square cross section with one pair of parallel faces only 4 deg from the basal plane of the hcp structure. The tensile axis was about 86 deg from the (0001) pole, 14 deg from the (1010) pole, and 16 deg from the (1150) pole. The specimen was charged to 50 ppm H by allowing reaction with the correct amount of hydrogen at 1073°K, homogenizing at this temperature for 2 hr, and cooling in the furnace. Two- surface analysis revealed that hydride platelets had precipitated parallel to the three {1010} prism planes. The specimen was heated to 673°K, in air, for 16 hr to bring the hydrogen back into solid solution, and furnace-cooled to 573°K.* It was then stressed in ten- sion at 1.2 kg per sq mm. (This produced a resolved shear stress of 0.6 kg per sq mm for glide on the prism plane with the highest Schmid factor. A higher stress would have produced significant strain at this temperature because the critical resolved shear stress for prism-plane glide in this crystal was only 1.0 kg per sq mm at ambient temperature.) The poles of the three prism planes were at angles of 14, 46, and 74 deg to the tensile axis so that an applied stress would exert normal stresses on the three planes in the approximate ratios 10:5:1, respectively. As soon as the stress was applied, the sample was furnace-cooled to room temperature. It was ground on wet Sic paper and chemically polished in 50 parts HNO3, 50 parts water, and 7 parts HF before examination. The result of the experiment was negative; i.e., the three (1010) planes were of equal importance as hydride habit planes.* It must be admitted that the ex- periment is not entirely comparable to those performed by walters,2 Louthan,5 and Louthan and Marshall6 on polycrystalline materials. They have found that some critical stress (below the macroscopic yield stress) is required for stress-orienting the hydrides. The applied stress in the present experiment was, by necessity, smaller by an order of magnitude than the critical stresses they report for the various materials. If the critical stress was related to the microstructure, one might postulate that it should be decreased by increasing the degree of perfection of the metal lattice and by increasing the grain size. But the experiment above suggests that, for the extreme case of a zone-refined single crystal of zirconium, the critical stress lies above that which one can apply without introducing gross plastic strain as another variable.

Jan 1, 1967

By Carl J. McHargue

Mechanical twins were produced in electron-beam melted columbium by high-speed impact at room temperature and by slow or fast compression at -196°C. The composition plane of the twins was { 112} and the shear direction was <111>. Notches in the twin bands often corresponded to traces of {110) of the matrix and appeared to be untwinned regions. Markings within the twin bands were interpreted as resulting from {110} slip in the twins. THERE has been much work in recent years concerning plastic deformation by glide, and the dislocation theory relating to glide has reached a relatively high degree of development. On the other hand, there have been fewer studies of deformation by mechanical twinning, and understanding of this process is far from satisfactory. This method of deformation is of interest for at least two reasons. First, it provides a mechanism in addition to glide for the relief of stresses, and, in the bcc and hexagonal close-packed metals may result in significant amounts of plastic flow. Secondly, there is the possibility that twins may act as barriers for dislocation movement, resulting in pile-ups which could nucleate cracks. As might be expected, the bulk of the literature on mechanical twinning in the bcc metals is concerned with iron. A good summary of the work done prior to 1954 is contained in the book by all.&apos; Recently the refractory bcc metals have become increasingly important. Limited studies have shown that tantalum,2,3 molybdenum,4,5 vanadium,6,7 tungsten,&apos; and columbium9-11 deform by mechanical twinning under some conditions. Alloys of molybdenum with rhenium and tungsten with rhenium show extensive deformation by twinning at room temperature.I2-l4 Most of these studies have dealt primarily with mechanical properties at low temperatures or have shown the existence of twins, and there is only a small amount of information concerning the conditions under which they form. The subject of the present paper is the formation of twins under stress in columbium with a consideration of their morphology. EXPERIMENTAL PROCEDURE The material used for these studies was taken from an ingot of columbium which had been melted twice by the electron-be am-method. The analysis of the ingot was (in ppm): B < 1, C = 10, Fe < 100, The cast ingot contained very large grains, and it was possible to obtain single-crystal prisms which measured from ¼ to 3/4 in. on a side. A few experiments were conducted on polycrystalline plate which was prepared by rolling material from the same ingot at room temperature and annealing at 1000 in a dynamic vacuum of 10-6 mm Hg. This gave a plate in which the grains had an average diameter of 3 mm. After the specimens were cut from the ingot, the six faces were metallographically polished and elec-tropolished to remove all traces of cold work. Most of the observations were made on the surfaces of the deformed specirllens without further treatment. Occasionally, etching after deformation was desirable. In these cases, an etchant of the composition 50 parts H2O, 5 parts HNO3 25 parts HF, and 10 parts H2SO4 was found to delineate the twins very well. Unless considerable care was taken to ensure the removal of all disturbed metal left by the mechanical polishing, etching failed to reveal many of the features discussed in this; paper. The specimen&apos;s were deformed either by impact or slow compression at 77°K (liquid-nitrogen coolant), 198°K (dry ice and acetone coolant), and 298°K. The impact load was delivered by a hammer except in one case where the load was delivered by a bullet. Slow compression was carried out on a hydraulic testing machine equipped with a chamber to hold the coolant. EXPERIMENTAL RESULTS It has been generally believed that the conditions favoring the formation of deformation twins are large grains, low temperature, and impact loading. In fact, Barrett and Bakish2 found twins in tantalum only after impact deformation at 77°K, and Adams, Roberts, and Smallman10 observed twins in columbium only at 20 For these reasons, the initial experiments of this study used impact loading. Hammer blows caused many bands resembling twins in single crystals a.t 77" but not at 198°K. Only a few slip lines were observed on any of the single-crystal specimens of this study—essentially all the deformation occurred by twinning. The appearance of the twins on the as-deformed surface is shown in Fig. 1. Although both Figs. 1(a) and l(b) are photomicrographs of twins taken at the same magnification and from the same crystal, they are startlingly different in appearance. Fig. 1(a) was taken from the crystal face approximately perpendicular to the shear direction, whereas Fig. 1(b) was taken from

Jan 1, 1962

By B. D. Cullity

A distribution of residual stress after plastic elongation is proposed, in which the bulk of the material is strained in compression and a very small portion in tension, This distribution is shown to account both for the X-ray observations and for the effect of plastic straining on magnetic losses in silicon steel. The regions left in compression are tentatively identified with the interiors of the sub-grains revealed by the electron microscope. THIS paper is concerned with the general problem of the nature of the residual stress which is produced in metals by plastic elongation. A particular stress distribution will be suggested which accounts for the main X-ray diffraction observations which have been made. It will also be shown that certain magnetic measurements made on silicon steel can be understood in terms of this stress distribution. X-RAY OBSERVATIONS Uniform straining of a crystal lattice (macro-strain) causes a diffracted X-ray beam to shift its position, and nonuniform straining (microstrain) causes line broadening. If a bar of metal is plastically elongated in the longitudinal x direction and then unloaded, diffracted X-ray lines are observed to be both shifted and broadened.&apos;-= Although the observed line shift indicates the presence of macro-strain, experiments have shown that no macrostrain, in the usual engineering sense of the term, exists.5"7 For example, removal of a layer from one surface of a stretched and unloaded bar does not produce curvature in the remainder of the bar 5&apos;7 Fig. 1 shows the variation of lattice strain in the x direction, as determined from X-ray line shifts, with the applied stress in the same direction. The curve ABC is the normal stress-strain curve of the material, AB being the elastic portion and BC the plastic. In the elastic region AB, the strain measured by X-rays, called the lattice strain, and the strain measured mechanically are both proportional to the applied stress, and both return to zero when the applied stress is removed. Above the elastic limit the lattice strain would be expected to continue to increase along the line BD. Actually, it increases less rapidly with respect to stress, or even decreases, as shown by BE. If the applied stress is then decreased, the lattice strain decreases along EF, which is parallel to AB. As a result, there is a compressive residual lattice strain FA after unloading. STRESS DISTRIBUTION. Since a stretched and unloaded bar does not contain macrostress, it follows that the observed line shift must be due to a special distribution of mi-crostress. Such a distribution is shown in Fig. 2, which shows the variation of the stress u, across a stretched and unloaded bar. The material is assumed to consist of two kinds of regions: regions C, stressed more or less uniformly in compression, comprising the bulk of the volume of the material and responsible for the observed diffrac-

Jan 1, 1963

By A. W. Dana, F. J. Shortsleeve, A. R. Troiano

The phenomenon of flake formation which may occur during cooling or room temperature aging of large steel sections is caused by a combination of hydrogen and stress. As such, the transformation characteristics of austenite in a particular section play a major role in the occurrence of flakes. Isothermal and continuous cooling studies demonstrated that flake formation is particularly sensitive to nature, distribution, and relative proportions of the microconstituents in the cooled sections. In the absence of transformation stresses, abnormally high hydrogen contents could be tolerated without flaking. Flakes were not found in the absence of transformation stresses. No correlation existed between average hydrogen content and flake formation where cooling stresses were low. Hydrogen in the steel was a necessary but not sufficient condition for flake formation. DESPITE a long history of laboratory and commercial investigations, the mechanics of hairline crack or flake formation in large steel sections remains unresolved. Recent publications1-5 emphasize that flaking is still a serious problem.* immediate cause of flaking is the pressure exerted by entrapped hydrogen gas that collects in small internal cavities or voids during cooling. When the temperature of steel is low enough to preclude extensive plastic flow, the cavity pressures cause local brittle fractures (flakes). 2—The microsegregation and transformation stress theory. According to this theory, flaking results from stresses arising from the volume changes accompanying the formation of martensite and/or low temperature bainite after a large portion of the section has transformed at elevated temperatures. The proponents of the hydrogen theory suggest that stresses from other sources may be additive to the stresses produced by hydrogen and may, in some cases, provide the increment of stress necessary to produce flakes. However, the critical aspect of this theory is that no stress, except that produced by hydrogen pressure, is believed to be sufficient in itself to produce flakes. For practical considerations, this means that the only safe thermal cycle is one that reduces the hydrogen content to some low critical level below which flaking will not occur regardless of the state of transformation. On the other hand, the transformation stress theory does not rule out the embrittling effect of hydrogen. This theory simply proposes that flaking does not occur in the absence of transformation stresses. With the transformation stress theory as a basis, commercial antiflaking cycles would be designed to complete the transformation of austenite prior to cooling to ambient temperatures. Both of these theories appear compatible with industrial experience. Antiflaking cycles, such as cooling at extremely conservative rates or soaking for periods of time in the upper subcritical temperature ranges prior to cooling to ambient temperatures, may allow the following: 1—diffusion of hydrogen out of the section and, as a consequence, reduction of the hydrogen content to some safe minimum value (hydrogen pressure theory) and 2—complete decomposition of the austenite at rela-

Jan 1, 1956

By M. C. Udy, P. C. Rosenthal

THE use of minute boron additions to steel has been given considerable attention in recent years. Comparisons made between boron-free and boron-containing heats of otherwise identical analysis have indicated, beyond a doubt, the potent effect of boron for increasing hardenability. The actual hardenability increase has been expressed as a multiplying factor, or in terms of the percentage of other alloying elements boron might replace, The present study presents the results of a systematic survey of. the use of boron as an addition to two types of alloyed steels and as a replacement for various percentages of molybdenum in these steels, Both cast and wrought steels of the two basic compositions were prepared. Molybdenum, because of its scarcity at the time the investigation was started, was selected as the element to be replaced by boron. Attention was also given to the effects of boron on other properties of the steels, particularly their notched-bar toughness, to investigate other advantages or limitations of this element as an alloy addition. EXPERIMENTAL WORK Steels Investigated The two basic compositions used in this survey of boron as a replacement for molybdenum are given in Table I. The cast steels were higher than the wrought steels in silicon content to improve the casting quality. [ ] Each of these base steels, both cast and wrought, was made with molybdenum contents of o, 0.10, 0.20, 0.30, or 0.40 per cent, the total comprising 20 steels. In addition, each of these 20 compositions . was prepared with boron additions in amounts of 0.0015, 0.003, and o,006 per cent as ferroboron; and in amounts of 0.002 and 0.005 per cent as two com¬mercial intensifier alloys, designated alloys A and B. The boron-treated steels totaled 100, and the entire series 120, Test Procedure Each steel was melted as an individual heat in a 50-lb., magnesia-lined induction furnace. Ingot iron scrap or mixtures of ingot iron and steel scrap were used for melting stock. Deoxidation was carried out in the furnace with o.10 per cent aluminum. The aluminum addition was

Jan 1, 1946

By N. Jaffe, J. E. Dorn

The effect of stress on the creep rate of high-purity poly crystalline aluminum in the intermediate temperature range was investigated by conducting creep tests at a series of different stresses and by decreasing the stress abruptly during the course of primary and secondary creep. Three series of decreases in stress tests were conducted: the stress was decreased in primary and secondary regions of creep at 347.5°K and the stress was decrensed in primary creep at 327°K. The results demonstrate the effects of structure and temperature on the stress dependence of the creep rate. The trends in the creep rate after a drop in stress are complicated and show that recovery takes place. The experimental results were compared with Friedel&apos;s theory for cross-slip, the experimentally determined energy for a constriction being in good agreement with the theoretical estimate proposed by Stroh. PREVIOUS investigations have shown that the ap-- parent activation energy for creep of polycrystalline aluminum, over the range from about 250° to 380°K, is approximately 27,400 cal per mole,&apos; a value that is to a first approximation insensitive to the applied stress, the creep rate, and the creep strain. Several facts strongly support the thesis that creep, in this temperature range, is controlled by the rate-determining mechanism of cross-slip: 1) Recovery of the cold-worked state can take place by a number of mechanisms prominent among which is climb and cross-slip. Astrom2 reported rapid recovery of cold-worked polycrystalline aluminum at 340° to 370°K giving an activation energy of 28,000 cal per mole and additional recovery at the higher temperatures of 455° to 478°K giving an activation energy of 36,000 cal per mole. Whereas the latter process was clearly identified with the climb mechanism, the former process. which has an activation energy in good agreement for that of creep in the same temperature range, is most likely due to recovery by thermally-activated cross-slip. 2) Single crystals of aluminum exhibit sharp slip-

Jan 1, 1962

By B. D. Lichter

In a previous paper, Oelsen, Schuermann, and Hey-nertl pointed out the possibility of obtaining complete thermodynamic functions for alloy systems from calorimetric measurements alone. Specifically, if the heat content of a heterogeneous, multicomponent system is known as a function of temperature and composition, then it is possible to derive the heats, entropies, and free energies of formation of liquid phases and of solid intermediate phases of fixed composition. The authors present equations and graphical techniques applicable to eutectic systems and systems with intermediate phases without solid solubility at lower temperatures. eijering has considered possible extension of the treatment to systems with complete solid-state miscibility at lower temperatures; however, experimental difficulties practically restrict the method to systems with very limited miscibility in the solid state. The purpose of this note is to present an alternative derivation of the heats and entropies of formation of liquid phases and of solid intermediate phases from heat-content measurements alone. Fig. 1 shows three types of phase diagram to which the analysis may be applied. If the heat content is determined as a function of composition x, at temperature T, we have quite generally and the heat of mixing of the liquid is obtained directly from heat-content measurements. If the temperature T lies in a two-phase region (solid-liquid) then

Jan 1, 1967

By Kenneth F. Whinery, John M. Campbell

Basically, the Buckley-Leverett theory involves two systems which are similar in nature but are differentiated by time. These systems may be described by the fractional flow and frontal advance equations which essentially characterize the mechanics of oil movement while being expelled from the reservoir. The fractional flow equation originally developed by Leverettl may be expressed in the more usable form The development of this equation is based on Darcy&apos;s law describing fluid flow through porous media and applies to the flow at only one point (it is a point function). For simplification, the fractional flow equation is written in the above form because the capillary forces always increase the fractional flow of the displacing phase regardless of the direction of flow or the displacing phase. If, for simplicity, the effects due to gravity and capillary pressure differences are neglected, the fraction of the displacing fluid, f, at any point in the flowing stream is related to the properties of the system by 1 Thus, it is seen that in the absence of capillary and gravitational effects, fd for a given sand and fluids varies only with saturation and pressure. The magnitude of the viscosity ratio, —a has an effective range (range of about 30) in the system where gas is displacing oil and a much smaller range for water displacing oil. In order to make the fractional flow equation more versatile, it is necessary to connect the fractional flow at a given point and saturation with time. This problem was approached by Buckley and Leverett" who developed the frontal advance equation, Eq. 3 states that the rate of advance of a plane that has a fixed saturation, Sd, is proportional to the change in composition of the flow stream caused by a small change in the saturation of the displacing fluid. It is, essentially, a transformation of a material balance equation representing the net rate of accumulation of the displacing phase within a homogeneous sand block. This accumulation is proportional to the difference between the rate at which the displacing fluid enters the sand and that at which it leaves. Eq. 3 describes the velocity with which a plane of constant displacing phase saturation advances through a porous system. Buckley and Leverett," Babson,&apos; Kern," Welge, and others have adequately discussed the basic mechanism and application of the fractional flow and frontal advance equations. APPLICATIONS OF THE FRONTAL ADVANCE THEORY TO PETROLEUM RECOVERY Two general applications of the Buckley-Leverett frontal advance theory involve the system in which the oil is being displaced by an expanding gas cap overlying the oil zone and that in which the oil is being displaced by water. Displacement by Gas in the Presence of an Immobile Water Saturation A system in which gas is the displacing phase may be thought of as having two forces effecting the displacement process. These forces are the gravitational force and that force exerted by the displacing gas. The gravitational effects control the displacing efficiency of the gas. The gravitational effect will be less at higher rates of flow, thereby reducing the effectiveness of the displacement of the oil by the gas. The more efficient displacements occur at flow rates which are less than the gravity free fall rate. Capillary forces can be neglected without materially changing the magnitude of the gas saturation. The Mile Six pool is used herein to illustrate the calculating procedures in evaluating gas drive-gravity drainage field perfomlance. These calculations represent the determination of the gas-oil contact when the distribution of the hydrocarbon pore volume is considered. Two methods

By G. R. Leverant, C. P. Sullivan

Re crystallized TD-nickel mi-2Th0,) in both coated und uncoated conditions was fatigued at 1800°F at total strain ranges varying .from 0.2 to 0.75 pct. The fatigue life of uncoated inaferal, Nf, was related to the total strain range, ?eT, by (2Nf/021AeT = 0.014. A duplex Al-Cr pack coating increased the fatigue life by about a factor of two. The cracks that led to failure in both coated and uncoated material were initiated at the outer surface, indicating that the mechanical properties of the surface layers were important in determining fatigue life. Crack propagation and subsurface crack initiation in the TD-nickel occurred preferentially at grain boundaries with cavitation at thoria particle-matrix interfaces an integral part of the grain boundary fracture process. The importance of both the grain morphology developed during thermome chanical processing of TD-nickel and the distribution of thoria particle sizes to fatigue resistance are discussed. THE fatigue properties of only a few dispersion-strengthened metals have been studied at temperatures 0.5 Tm;1,2 among these have been lead and aluminum containing oxide dispersions. TD-nickel is a material of interest for application in aircraft gas turbine engines, but little fundamental information is available on its behavior under cyclic loading conditions. In this study, the low-cycle fatigue properties of TD-nickel were determined at 1800°F with emphasis on the 101-lowing; 1) the relation of the grain morphology produced during thermomechanical processing to crack initiation and propagation; 2) the role of thoria parti-cles in the fracture process; and 3) the effect of an oxidation resistant coating on fatigue life. I) MATERIAL AND EXPERIMENTAL PROCEDURE The TD-nickel was supplied by DuPont as a 5/8-in. thick plate which had been subjected to a proprietary series of thermomechanical treatments with a final anneal at 2000°F for 1 hr in hydrogen. The composition of the material is given in Table I. At the test temperature of 1800°F, the 0.2 pct offset yield stress was 15,000 psi, and the elongation and reduction in area were 4.6 and 3.0 pct, respectively. The microstructure of this material has been previously described.&apos; Briefly, it consists of an array of lath-shaped grains, about 0.15 mm in thickness, with the long dimension of each grain parallel to the primary working direction, Fig. 1(a). The presence of very small annealing twirls, Fig. l(b ), together with the absence of extensive dislocation networks, Fig. L/C), indicated that the material was in the recrystal- Table I. Composition of TD-Nickel ThO2 2.3 vol pct C 0.0073 wt pct lex 0.01 wt pct Cr 0.01 wt pct Cu 0.004 wt pct S 0.001 wt pct Ti <0.001 wt pct Co <0.01 wt pct Ni bal lized condition. Commercial TD-nickel sheet has a similar grain size and shape, but unlike the present material is not recrystallized as evidenced by the absence of annealing twins and the presence of a well-developed dislocation substructure.4 The plate material had Young&apos;s moduli in the rolling direction of 22 x 106 psi and 13 x 106 psi at room temperature and 1800°F, respectively, indicating a texture with a strong {100}<001> component in agreement with previous observations on recrystallized TD-nickel sheet.596 The 2.3 vol pct of thoria particles were uniformly distributed although some clustering and stringering of larger particles was occasionally seen. The average diameter of the particles was 450 and the calculated mean planar center-to-center spacing was 2100Å. Two specimens were coated with a duplex A1-Cr pack coating. The coating was somewhat nonuniform from one position to another along the gage length. An area of the coating after testing is shown in Fig. 2. Electron microprobe analysis revealed the following zones in the various lettered regions indicated in Fig. 2: A) a bcc matrix of B-NiA1 with some chromium in solid solution along with a fine dispersion of a chromium-rich second phase which was probably precipitated during cooling from the test temperature to room temperature; B) fcc y&apos;-Ni,Al with some chromium in solid solution; C) porosity; D) a two-phase mixture of a chromium-rich solid solution containing nickel and aluminum and a small volume fraction of a nickel-rich solid solution having approximately the same composition as the immediately adjacent portion of region E, E) the TD-nickel substrate containing chromium in solid solution to a depth of 5 to 10 mils. As expected from the nature of the diffusion processes involved,7 the thoria particles were present only up to the layer of porosity, region C, Fig. 2. The measured thickness of the coating proper, zones A to D, after testing was 1 to 2 mils. The specimen design and testing techniques have been previously discussed.&apos; Stressing was axial and parallel to the lath-shaped grains (i.e., parallel to the rolling direction). The total strain range was controlled between zero and a maximum tensile strain varying from 0.2 to 0.75 pct. (The test at 0.2 pct total strain range was switched to load control at 1030 cycles at which point the peak tensile and compres-

Jan 1, 1970

By L. C. Brown, S. K. Behera

The diffusion rate in Ag-Sb couples is sensitive to con~pressive load with the width of Ag3Sb, the only phase present in the diffusion zone, increasing with stress up to 800 psi and remaining constant above this. Kirkendall marker experiments show silver to diffuse much faster than antimony in Ag3Sb and incipient porosity may therefore develop at the Ag/Ag3Sb interfnce restricting the transfer of atoms from the silver into the diflusion zone. Application of compressive stress reduces the tendency for porosity to develop and so increases the growth rate. In a recent paper Brown et al.1 observed a significant increase in the thickness of Cu2Te in Cu-Te diffusion couples on application of a compressive stress as low as 20 psi. Similar stress effects have also been observed in the Fe-A1,2 Al-u,3 arid cu-sb4,5 systems. It has been suggested that the increase in growth rates of intermetallic phases in these systems is due to a decrease in the amount of Kirkendall porosity with applied stress. In the present paper, results are presented of the effect of compressive stress on diffusion in Ag-Sb, together with a detailed examination of the Kirkendall effect. The Ag-Sb phase diagram6 shows that antimony has a moderate degree of solid solubility in silver, 5.7 at. pct at 350°C, but that there is essentially no solubility of silver in antimony. There are two intermediate phases— (hcp7) from 8.8 to 15.7 at. pct Sb and Ag3Sb (orthorhombic8) from 21.8 to 25.9 at. pct Sb. EXPERIMENTAL Diffusion couples were prepared from fine silver of 99.95 pct purity and from antimony of 99.7 pct purity. Both the silver and antimony were produced in the form of discs 1/2 in. in diam by approximately $ in. thick, with surfaces ground flat to 3/0 emery paper. Diffusion anneals were carried out in the apparatus previously described.1 A compressive load was applied to the diffusion couple through a lever arm system, with a reproducibility estimated to be ±10 psi. All runs were carried out in a protective hydrogen atmosphere. Following the diffusion anneal specimens were sectioned and polished and the width of the diffusion zone was measured metallographically. Composition profiles were measured using an electrostatically focused electron probe with a spot size of 10 , counting on Sb L radiation. Corrections for matrix absorptiori and fluorescent enhancement9 were not required. S. K. BEHERA, formerly Graducate Student, Department of Metallurgy, University of British Columbia, is now Postdoctoral Fellow, Whiteshell Nuclear Laboratories, Atomic Energy of Canada Ltd., Pinawa, Manitoba. L. C. BROWN, Junior Member AIME, is Associate Professor, Department of Metallurgy, University of British Columbia, Vancouver, B.C., Canada. Manuscript submitted June 14, 1968. IMD RESULTS Fig. 1 shows an electron probe traverse of a typical diffusion zone. In all couples examined only one intermediate phase was observed and the composition of this phase, 23 wt pct Sb, was in good agreement with the composition of Ag3Sb, 23 to 28 wt pct Sb. The presence of this phase was confirmed by X-ray diffraction of filings taken from the diffusion zone. The probe traverses showed no detectable solid solubility in either the silver or the antimony although the phase diagram indicates that some antimony, up to 6.5 wt pct pct Sb, should be in solid solution in the silver. However the width of this portion of the diffusion zone would be expected to be very small in view of the low diffusion coefficient in the silver, 4 x 10-l6 sq cm per sec at 350°C, 10 compared with that in the Ag,Sb, estimated as 3 x 10-8 sq cm per sec in the present work, and this region would therefore not be expected to be seen in the probe traverse. Application of stress resulted in a significant increase in the width of the diffusion zone, Fig. 2. At 350°C, the thickness of Ag3Sb increased from 250 at 0 psi to 400 p at the limiting stress of 800 psi, indicating an apparent 150 pct increase in the diffusion coefficient. Similar behavior was also observed at 400°C, indicating that the stress effect is not characteristic of just one temperature. The growth of Ag3Sb at 350°C and at various stresses is shown in Fig. 3. In every case the growth rate was parabolic indicating diffusion control. The kinetic curves all passed through the origin showing that delayed nucleation of Ag3Sb was not responsible for the stress effect and that it was a real growth effect. A series of tests were carried out in which diffusion was allowed to take place at a lower stress following an initial high stress diffusion anneal. Speci-

Jan 1, 1969

By A. H. Larson, L. G. Twidwell

DURING the roasting of zinc sulfide concentrates and by-product recovery from flue dusts, the zinc sul-fate phase may occur in various stages of the processes. In addition to zinc sulfide, other sulfide phases are usually present such as CdS, PbS, CuzS, and FeS. Consequently, the effect of these sulfides on the thermal decomposition of ZnS04 was investigated. Merck high-purity, anhydrous zinc sulfate was used as the starting material. The sulfate was heated under an argon atmosphere, at a rate of 10°C per min. With the first slight indication of decomposition as determined by gas analysis, the sample was removed from the furnace and allowed to cool. X-ray patterns showed no other phase present. It is estimated that less than 0.05 pct of the ZnS04 decomposed. The metal sulfides were also heated under an argon atmosphere to drive off any adsorbed water. The materials were then sized (-200 to +270 mesh), mixed in predetermined mole ratios, and pressed into pellets. The experimental measurement of the reaction rate consisted of purifying the argon carrier gas, continuous flushing of the heated reacting mixture with argon, and collection and analysis of the SOn product gas. The reaction system was heated to 600°C and al-

Jan 1, 1967

By M. R. Louthan, C. L. Angerman

In polycrystalline Zircaloy-2 the orientation of zirconium hydride precipitates is influenced by an applied stress during hydride precipitation; hydride platelets are oriented nearly parallel to a compres-sive stress and perpendicular to a tensile tress. 1,2 A similar effect has been observed in the Ti-H system, where precipitation of the low-density hydride platelets occurred on habit planes made energetically favorable by the application of stress. 3 Recently, stress activation of hydride habit planes in zirconium and Zircaloy-4 was also demonstrated. The hydrides precipitated on {101l), {112l} and (2131) planes in both zirconium and Zircaloy-4; however, no platelets were found near the prism-plane positions in the Zircaloy-4 samples. Investigations at the Savannah River Laboratory, using polycrystalline Zirc_aloy-2 samples, have confirmed the (101l) and (1121) habit planes but also showed that the prism planes were active hydride habit planes. Using single-surface stereographic analysis and back-reflection Laue techniques, most of the previously reported habit planes for a zirconium were observed.4"1 and one additional plane, the (1013) plane, was noted, Table I. All the habit planes observed had the form (101l) or { 112l) indicating that these planes are the habit planes for hydride precipitation in poly-crystalline Zircaloy-2. The specimens used in these studies were cut from large-grained weld areas of seam-welded tubing and were hydrided in either a static steam autoclave at 400°C and 1500 psig or in a modified Sieverts apparatus at 400°C.

Jan 1, 1967

By O. D. Sherby

In 1938, Kanter&apos; revealed that the steady-state creep rate of low-carbon iron alloys could be correlated by an activation energy expression, where the activation energy for creep, Qc, was found equal to about 90.0 kcal per mole for most of the alloys investigated. He suggested that creep at high temperatures might be controlled by some sort of solid self-diffusion process since the value of Qc was about equal to the known value for self-diffusion, Qd. Correlations were not further attempted along these lines until many years later, when new evidence2-8 was presented suggesting that Qc = Qd for many metals. This equality now appears to be established for ten metals (Al, Pb, Ni, Mg, Cd, In, a Fe, y Fe, Cu, and Au). This experimental fact prompted several investigators to postulate various mechanisms of dislocation motion which would yield an activation energy for creep equal to that for self-diffusion.7-9 Possibly the most accepted theory is that based on dislocation climb7 where a dislocation is envisioned to surmount a barrier by an atom-vacancy exchange process, thereby "climbing" from one slip plane to another. Such a model would suggest that the steady-state creep rate, i, should be directly proportional to the rate of self-diffusion, D, for a given creep stress. In order to more clearly reveal the relationship between creep and diffusion, and to eventually determine the correct model, it would be desirable to obtain data showing correlations between i and D, rather than with a comparison of the temperature coefficients, Q. It has been known for some time that the self-diffusivity of iron atoms is greatly decreased when body-centered-cubic (a) iron transforms to face-centered-cubic (y) iron. This has been ascribed to the more close-packed structure of y iron. The diffusivity ratio at the transition temperature is Da/Dy =350. Correlations of creep data for a and y iron5 reveal that the creep rates under a given stress at the transition temperature differ by about the same ratio (ea/ey 2 200). It would be difficult to reconcile these results on any other basis than that the diffusivity of atoms probably controls creep of iron in some very direct way. No other published data on other allotropic metals appear currently available for further checking such a possible correlation between i and D. Thallium transforms from a hexagonal close-packed (a) structure to a body-centered-cubic (ß) structure at 230°C (503°K) and the self-diffusivities of the two structures have been determined by shirn.10 His results are plotted in Fig. 1 where it will be noted that Dß/Da = 25 at the transition temperature. It would appear desirable, therefore, to determine the creep rates of polycrystalline a and ß thallium at the transition temperature, as well as determine

Jan 1, 1959

By T. Glen Heslop, Dennis H. Laubscher

INTRODUCTION In all cave mining operations waste is drawn mixed in the ore, hauled, hoisted and milled. This waste usually contains some mineral which partly covers some of the costs of mining and milling it, but it still re- presents a loss of profits as the production rate from the mine is matched to the mill capacity - every tonne of waste milled replaces a tonne of profitable ore. Draw control aims to reduce the amount of waste drawn and to increase the amount of ore recovered. It is also used to regulate the grade of ore flowing to the mill and in block cave blocks to prevent potential stress build- up on the major apexes above grizzly drifts. This paper summarises what has been learnt about draw control in the forty years that cave mining methods have been used in the three largest underground chrysotile asbestos mines in the southern hemisphere. The four mining methods to which draw control has been applied are: a. Block caving. b. Shrinkage with overburden caving. c. Sublevel caving. d. Open stoping. Open stoping has been included because on a number of occasions severe falls from the back and side of these open stopes have occurred. Without full records of where and when ore is blasted, when and how much ore has been drawn from each of the drawpoints, it would be impossible to analyse the migration of ore and fallen waste in the stope. Several problems peculiar to chrysotile asbestos ore bodies affect the practice of draw control. Heterogeneous fragmentation, cavities, side pressures and the interaction of stresses in the caved ore affect the migration of ore under draw. Fibre is normally not developed uniformly throughout the ore bodies, values vary from place to place but there is usually a general decrease upwards and the hangingwall contact is an economic limit. The immediate hangingwall rock frequently looks like the ore body hostrock and is difficult to recognise in a drawpoint, and cannot be used as the marker for stopping draw. During caving or shrinkage, a large proportion of fibre becomes detached from the host rock and re- ports in the fines, which migrate differently to the larger rocks. The fines are not sticky, and flow easily if loose and dry, but compacted, the fibre and rock fines con- solidate the ore. During draw the proportion of fines in the ore varies considerably, as fines either flow relatively freely between the large rocks or become trapped and compacted above large rocks or hangups. This creates a large sampling error in drawpoint grade assessments, whether done visually or by bulk sampling, unless the assessments are done frequently. The method of draw control used is to regulate the draw rate in an attempt to lower the ore-waste interface as evenly as possible, and to finally stop working the drawpoint when a calculated tonnage has been drawn.

Jan 1, 1981

By O. K. Miniato, L. Massé, K. Nobe, J. S. Aronofsky, W. F. 213-000-000-016 Seyer

MUCH work has been done dealing with the effect of mechanical stress on electrode potential in an electrochemical system. The contradictory nature of the experimental results indicates the complexity of the problem although thermodynamic considerations show that a simple relationshir, should exist. In those systems where a gas was the electromotive active substance satisfactory agreement between theory and practice has been found. Des Coudres&apos; found this to be so even when the active substance of the electrode, in this case mercury, was in the liquid state. In contrast, attempts to correlate theory and experiment for the solid state have met with a very limited success. The early workers in this field, Andrews,2 Walker and Dill3 used iron, certainly one of the most reactive of metals. Others have made use of less active metals such as copper and nickel. Recently Fryxell and Nachtrieb4 investigated the electrochemical behavior of gold and silver under both tensile and compressive stresses and concluded that it was doubtful whether true stress potentials could ever be measured. Much of the lack of success to measure the thermodynamic stress potential can be ascribed to the presence or formation of a complex film on the metal surface in contact with the electrolyte. Further, the theoretical stress potential is very small and therefore difficult to measure directly. Thus the calculated emf between a 24 B & S gage cold-drawn copper wire stressed with a weight of 1 kg and an unstressed portion of the same wire is only 2.60 X 10"7 volts. This is very small compared to that which can be produced by chemical reactions at the metal electrolyte interface which in turn can be so large as to mask completely the stress potential. Hence in this type of measurement all chemical side effects must be eliminated or reduced as much as possible. It was for this reason that the system copper-sodium chloride solution was selected for study. INSTRUMENTATION In the many preliminary experiments conducted, two major difficulties were encountered. The first was to measure the small electro-potentials to be expected and the second to obtain a suitable electrode surface. The conventional potentiometric method was found to be unsatisfactory for measuring the small emf expected. However, by using an L & N No. 2290 galvanometer having a resistance of 915 ohms consistent measurements were possible. The reference electrode was always the unstressed one made from the same sample of wire. The steady current flow was approximately 10-8 amp. Lewis and Randell5 have stated that for currents of the order of 10-8, if there is no sensible polarization, the measured emf may be taken as a reversible one. To check the galvanomenter readings an alternative method was devised to measure the potential difference between the wires. This involved a Liston-Falb d-c breaker amplifier model 10, an L & N k-2 potentiometer and a moving-coil galvanometer having a sensitivity greater than 0.1 µv (microvolt) per mm. To increase further the output voltage of the amplifier a d-c amplifier, model B. L.-932 was introduced into the circuit. This amplifier was in turn connected to a Brush recorder which had been calibrated previously by the test signals from the Liston-Falb instrument. These test voltages employed took into account the impedance of the input current. Unfortunately, this method had too low a sensitivity for measurement below 10 µv. Above this value the voltage agreed reasonably well with those obtained directly by the simple galvanometer method. The main advantage of the amplifier setup was that one did not have to wait until no deflection occurred on the galvanometer in the circuit when first exposing the wires to the solu-

Jan 1, 1959

By AIME AIME

IF the observation of our British friends is true that Americans put new records in bigness above everything else then the 150th meeting of the Institute was not the grand success it seemed to be. Just why the attendance slumped a little this year is anyone&apos;s guess, but the favourite explanation seemed to be that half the country is planning to come to the New York World&apos;s Fair this summer and that two trips from the hinterland to the me- tropolis, with another to San Francisco of course, can hardly be justified with the present condition of the stock market and the prices of the products of our mines. Certainly, some were pre- vented from coming too by the epidemic of respiratory afflictions that was rampant in February. Unfortunately. several succumbed after they had reached New York.

Jan 1, 1939

By B., Hoyaux

A first requirement for assessing the safety of a rock slope, either artificial or natural, particularly if the rock behaves in an elastic-brittle manner, is a proper knowledge of the distribution of stresses within the slope and their development with time and advancement of workings.

Jan 1, 1972