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By P. G. Shewmon

If interfacial equilibrium is maintained at the interface between a growing precipitate and the supersaturated matrix, so that solute diffusion alone determines the growth rate, the precipitate shape should evolve toward that characteristic of the dendrites found in solidification. However, this shape is rarely observed in precipitation reactions proceeding at high temperatures where interfacial equilibrium is usually felt to prevail. Thus some other stabilizing factor must enter, to keep the interface smooth. It is shown that a slow interfacial reaction (low interfacial mobility) will stabilize the interface, while transformation stresses have a IN studying the kinetics of phase transformations such as solidification or proeutectoid precipitation at high temperatures, it is customary to assume that equilibrium exists across the interface and that the rate of the reaction is determined by the rate at which heat and solute diffuse to and from the interface. In the case of precipitation, such an assumption predicts an almost infinite rate of initial growth. It is generally stated that the rate cannot be infinite and that during some initial period the rate must be determined not by solute diffusion but by an interfacial reaction, i.e., transferring atoms across the interface. The duration of this much weaker stabilizing eFfect and impurities tend to enhance instability. It is also concluded that a sets an upper limit on the wavelength of the perturbation that can give instability. Thus initially all flat or smoothly curved particle interfaces will be stable even if their growth is diffusion-controlled. Proeutectoid precipitation in the Fe-C system is considered in some detail and it is shown that the experimental results can only be rationalized if the growth rate of ferrite in steel transformations is determined by a slow interfacial reaction for all hut a few orientations between the two phases. initial period has never been clearly established, but it is generally assumed to be too short to affect any measurable results.' Several authors have pointed out that in the case of interfacial equilibrium any bump in the surface will grow out ahead of the planar interface due to the higher gradient in front of it.2j3 Thus the interface will be unstable with respect to an irregular interface with points (plates) propagating rapidly out ahead of the interface into the supersaturated phase. Recently, Mullins and Sekerka have given equations for the stabilizing effect of surface tenion.~ They found that for particles with a radius of curvature of 1 p or greater the stabilizing effect of surface tension will be completely overcome by a supercooling, or supersaturation, of as little as

Jan 1, 1965

By H. P. Leighly, J. W. Marx, H. L. Walker

A relationship between recrystallized grain size and prior deformation is predicted from elementary statistical considerations, and reasonable agreement with experiment is obtained. RECRYSTALLIZATION phenomena have received much theoretical and experimental attention, and very adequate discussions of the various mechanisms suggested have been given by Anderson and Mehl,' Cook and Richards,' and Burgers," and others. It suffices to note here that the initial concepts fitted one of two general hypotheses: I—The new crystals are nucleated within microscopic regions at which there is a concentration of internal stress, i.e., volume elements of maximum strain energy. 2—The new crystals have their inception in volume elements of minimum strain energy. In a comprehensive early review of the subject, van Arkel' considered both possibilities and came to the conclusion that hypothesis 2 was inconsistent with the experimental fact that the number of nu-cleations increased with increasing deformation. He suggested that, if allowance was made for a preliminary atomic rearrangement at the points of large internal strain, hypothesfs 1 provided the more reasonable concept. Following the initial observations of Collins and Mathewsonb nd Crussard,Y he systematic X-ray investigations of Cahn' and Guinier and Tennevin" established the existence of a polygonized structure in metals that had been cold-worked, and subsequently annealed, under conditions such that re-crystallization did not occur. This new experimental evidence by no means disproved the first nucleation hypothesis, a fact recognized by both Beck" and Cahn,10 who independently suggested nucleation mechanisms based on the idea that regions of large strain might polygonize before the bulk of the less deformed material. These mechanisms, together with others recently proposed," are dependent upon the prior existence of some degree of polygonization in the deformed material. On the other hand, a critical examination of the published data leads to the supposition that polygonization may not be the necessary precursor of recrystallization, but merely its favored energetic competitor. In regions where the lattice distortion is not too severe, the limited adjustment afforded by polygonization may permit the lattice to drop to a relatively stable low energy state in which the nucleation of a new crystal becomes improbable, even at elevated temperatures. Such structures, of course, might provide a fertile field for the growth of nuclei, if these could be introduced. In regions of concentrated lattice distortion, polygonization alone may not be able to accomplish an adequate strain reduction, and in these volume elements sufficient thermal activity permits the more drastic atomic rearrangement involved in nucleation. Completely polygonized structures are known to withstand extended heating close to their melting points," with no other effect than a slow enlargement of some of the subgrains at the expense of others. Once started, macroscopic recrystallization might be expected to go to completion in a matter of minutes under similar heat treatment. Crussard12 and his coworkers have found that recrystallization may occur in single crystals of impure (about 99.7 pct) aluminum without any detectable prior polygonization. The indication here is that large Cottrell impurity atmospheres inhibit dislocation movement, thus suppressing polygonization to such an extent that the alternative process, recrystallization, dominates the lattice restoration. Experimental studies relating recrystallization directly to stored energy have not, at the present time,

Jan 1, 1954

By R. J. Wasilewski

The variation of elastic modulus with terrzperature between -150° and 600°C has been investigated. Compounds close to equiatomic cornposition exhibit very low modulus values and very high damping near room temperature. The modulus rises steeply with both decreasing and increasing temperature. The modulus minimum and the high damping are believed to be connected with a martensitic transformation of TiNi. In bulk material this transition takes place slightly above room temperature quite rapidly and reversibly, with a hysteresis of some 30°C, depending on the Ti:Ni ratio. Oxygen impurity affects the reaction time. THE inter metallic compound TiNi has been reported to exist in an ordered CsCl (B2) structure,l-6 the homogeneity range varying rather markedly with temperature.7 Some investigators reported this compound to decompose peritectoidally to Ti2Ni and TiNi, between 650° and 800°C,3 or below,',g the latter workers also suggesting the decomposition to be strain-sensitive. Purdy and Parr were the first to report a structural transformation to a new, possibly hexagonal, structure at 36°C,7 a temperature indubitably too low to allow the significant amount of diffusion necessary for a peritectoid reaction. Mechanical-property investigations of compositions close to TiNi just above room temperature have qualitatively shown remarkable anomalies, particularly with respect to clamping,' and to a "memory" effect, that is, plastically deformed material returning to its original shape on being heated through the "decomposition" temperature.9 The original explanation of this effect—based on the apparent experimental observation of Ti2Ni or TiNi, formation in the material subjected to tensile or compressive stresses, respectivelp—does not appear plausible. It appeared more probable that the change involved may be a martensitic, diffusionless structural transformation, similar to those observed in other B2 structures such as 0 brass,'' AuCd,ll and AuZn.12 The existence of such transformation has been established recently,', although the symmetry of the low-temperature structure is not yet known. The present paper describes the elastic modulus and damping behavior of polycrystalline TiNi in both structures. EXPERIMENTAL METHOD 1) Specimens. All the specimens to be investigated were prepared from premelted electrolytic nickel and iodide titanium by nonconsumable arc melting and casting in a water-cooled copper mold. The cast billets were canned in mild steel, extruded, and swaged to approximately 0.375 in. diam. The cans were then removed by pickling or machining. Preliminary material balance checks indicated no significant weight losses on melting (less than 5 mg on a 50-g button); hence nominal compositions have been used throughout. In agreement with previously reported observations7 no single-phase material was obtained at—or close to—Ti 1.00 Ni1.00 a small amount of finely divided second phase always being present. It was found that most of the oxygen impurity was associated with this minor phase, which was identified as oxygen-bearing Ti2Ni—possibly Ti,Ni,O. The amount of this phase—at any given Ti:Ni composi-

Jan 1, 1965

By C. H. Li, R. J. Stokes, T. S. Liu

Poly crystalline silver chloride specimens having different micro structures were prepared by extruding monocrystals or precompressed powder at varying temperatures. Extrusion at high temperature (370°C) produced a Fully recrystallized equi-axed material which was brittle and fractured by simple cleavage below its transition temperature (60°C for notched specimens). Extrusion at low temperatures (down to -196°C) produced an extremely tough cold-worked material with grains elongated in the extrusion direction. This material fractured below its transition temperature (which varied from —20" to —200°C) by an intergranular mode. It is concluded that cold work increases the resistance to transgranular cleavage. Fracture is then de-flected to propagate intergranularly ouer surfaces making an angle with the tensile axis with a corresponding improvement in notch toughness. This deflection is greater for extruded powder than for extruded monocrystals because of the extremely elongated grain shape. PREVIOUS work1,' on the fracture properties of fully recrystallized silver chloride under notch impact conditions has indicated that the fracture behavior is rather invariant. Thus polycrystalline materials originating from a number of sources ranging from relatively pure Harshaw single crystals to commercial-purity powder and prepared by hot extrusion at 370°C all fracture by simple cleavage with a ductile-brittle transition at 60°C, see Fig. 1. This behavior is also typical for fully annealed single crystals and appears to be fundamental to silver chloride for the particular loading conditions and notch configuration adopted. One way in which this characteristic fracture behavior can be modified is by the dispersion of alumina particles in the silver chloride matrix.' Then, particularly when the alumina particles are in the shape of spheres, the duc tile-brittle transition is much less sharply defined and occurs over a range of temperature, the transition temperature is lowered considerably and the fracture mode changes from simple cleavage to a fibrous or shear mode. The reason for this change is believed to be partly due to the nucleation of cavities in the region of the dispersed alumina particles which influences the state of stress locally and the distribution of plastic constraint at the root of the notch. It is emphasized however that this is not the sole factor responsible for the increase in toughness. In extruded materials it is reasonable to expect that the resultant grain size, texture, and the residual cold work will be influenced by the presence of a dispersed phase. The present experiments were initially designed to determine the extent to which cold work influenced the fundamental ductile-brittle transition temperature and fracture mode of silver chloride. They were stimulated by the discovery that silver chloride could be extruded at temperatures as low as -25°C when commercial-purity powder was used and as low as -196°C when single crystals were used. This working temperature was far below that previously used (370°C) and it was found that such extruded material was exceedingly tough. The reasons for the enhanced toughness and its relation to the previous work on silver chloride-alumina compacts will be discussed. EXPERIMENTAL PROCEDURE Materials Used. Two forms of silver chloride were used in this study: i) silver chloride powder

Jan 1, 1964

By Ed L. Reed

INTRODUCTION The most efficient development of a mine plan for in-situ leach (solution) mining must be based upon an understanding and application of the basic hydrologic characteristics of the aquifer containing the mineral values. Similar knowledge of the overlying and underlying aquifers is also required. This paper summarizes the hydrologic properties of a ground water system and describes some of the more important conclusions that can be drawn from a detailed hydrologic study. Basic to an in-situ leach mining operation is the flow of fluids through porous rock from place to place. The degree to which these movements of fluids can be predicted and controlled determines to a large extent the efficiency of the ore recovery operation. HYDROLOGIC CHARACTERISTICS The principal hydrologic characteristics of a porous medium (sand, intercrystalline or vuggy limestone, fractured basalt, etc.) influencing fluid flow are: Porosity Permeability Thickness Transmissivity Storage Coefficient Water Table or Piezometric Surface Hydraulic Gradient Briefly these parameters can be defined as follows: Porosity: the void space in a unit volume of rock. Permeability: the ease with which fluid will flow through a porous medium. Thickness: the height of the formation which contributes flow to a well. Transmissivity the product of permeability and thickness. Storage Coefficient. the volume of water released from the reservoir per unit drop in head. Water Table or Piezometric Surface: the level at which water will stand in a well: the top of the zone of saturation in a gravity aquifer; the height to which water will rise above the confining bed in an artesian system. Hydraulic Gradient the direction and rate of dip of the water table or piezometric surface. A properly designed pumping test will provide numbers for transmissivity, storage coefficient and the water table or piezometric surface. Drilling records or bore hole logs provide aquifer thickness data from which permeability can be calculated. Ground elevations applied to measured depths to water enable one to calculate the direction and rate of dip of the water table or piezometric surface. Porosity can be determined from core analyses or density logs; it can be estimated from grain size distribution curves in sands or sandstones and from, microscopic examination of drill cuttings derived from carbonate aquifers. CHARACTERISTICS OF FLUID FLOW The characteristics of fluid flow that are vital to an understanding of leach mining include: Velocity Direction Flow Path Radius of Influence The velocity of fluid flow is of paramount importance in planning and managing a leach mine operation. Velocity is directly proportional to the permeability and hydraulic gradient and indirectly proportional to the effective porosity The permeability determined from a pumping test is an average value for the interval stressed; therefore, the velocity calculated from data derived from a pumping test represents average conditions. Under actual conditions discrete portions of the aquifer open to the screen may have permeabilities several times as high as the average and minimum permeabilities only a fraction as much. An injection front will be irregular to the extent that the reservoir rocks are heterogeneous An important consideration is the direct relationship of velocity to head. A reservoir which would provide a velocity of 0.05 feet per day under conditions of equilibrium would allow fluid flow of 36 feet per day under typical leaching operations, i.e. 12-foot injection head, 12-foot pumping level and 50 foot five-spot pattern. The direction of fluid flow is also vital both inside and outside the mine area. In the pattern area the direction of flow is determined by the geometry of the well field and can be approximated by mathematical modeling techniques. Outside the well field, the direction of flow is influenced by both natural conditions and the degree to which production and injection volumes are balanced. Flow directions (and velocities) are critical to an understanding of leachate excursions and their control.

Jan 1, 1979

By N. K. Chen, R. Maddin

Columbium single crystals were deformed in tension and compression. Reorientation by X-rays and stereographic projections of slip traces indicate that plane of slip may be considered as (110). The plastic behavior is shown to be quite similar to the deformation of molybdenum single crystals. STUDIES on the crystallography of the deformation process in body-centered cubic metals have been renewed recently with investigations of iron single crystals1-" and molybdenum single crystals.4 It is now apparent that too many exceptions to the rationalization based upon the ratio of absolute testing temperature to absolute melting point by Andrade5 exist to permit more serious discussion of this type of analysis. The considerations of resolved shear stress utilizing only planes of the type {ll0}, {112), and {123)³,6 permit analysis of the deformation only on the basis of those three types of planes. The suggestions made by Elam7 and by Greninger8 in which the slip process is envisioned as a composite slip on two nonparallel {110) planes can be illustrated schematically in Fig. 1. It may be seen that an unresolved trace on any plane containing a <111> direction may be accomplished by varying the number of atoms participating in the composite process. By further varying the number of atoms in each plane but keeping the ratio of participating atoms constant, jogs could be obtained in the traces and hence wavy slip lines could be produced. Vogel and Brick&apos; studied the behavior of a iron single crystals in which they suggest that the plane of glide is "non-crystallographic" and may be predicted from the intersection between the great circle joining the slip direction and specimen axis with the great circle whose zone axis is the slip direction. In a more recent investigation on iron single crystals, Steijn and Brick" suggest that the slip mechanism may be considered as made up of a type of composite slip occurring on {110} and {112} planes. Evidence for a possible composite nature of the slip process has been presented for the case of molybdenum in the form of analysis of asterism and specimen axis rotation." Definite proof of a composite slip process must, however, await good electron microscopic resolution of the individual traces making up the unresolved optical trace used in determining the acting slip plane. The present investigation was undertaken to study the behavior of columbium single crystals not only in tension but also in compression since the specimen axis migration should indicate the plane or planes of glide in the same manner that the specimen axis migration in tension indicates the direction of glide. The orientations of eleven crystals investigated are shown in Fig. 2. Specific orientations are missing (those in the vicinity of [Ill] and [001] and consequently the effect of orientation on the crystallography of deformation could not be considered. Experimental Procedure The 1/8 in. rods (7 in. long) were subjected to an axial tension in vacuo while at temperatures in the vicinity of 2000°C for 2 to 4 hr. This treatment resulted in large cylindrical grains (about ½ in. long) occupying the entire cross section. A number of these rods were used for the tension studies by observing the behavior of the individual grains. For the compression studies, single crystals approximately % in. long by 1/8 in. in diameter were cut from the rods; the ends were ground parallel. All specimens were polished electrolytically in a solution of 15 cc HF(48 pct) and 85 cc H2SO4 (concentrated) using a platinum cathode, a current density of 0.04 amp per sq cm and a temperature between 25" and 60°C.10 Orientations were obtained using a Laue back-reflection method (3 cm film to specimen distance) with a ½ mm collimator 9 cm long. For the compression specimens, a reference mark was scratched on one of the compression sur-

Jan 1, 1954

By L. Adler

Any design of a mine roof in bedded deposits which ignores differential deflections at the supports can quickly lead to dangerous overstressing. As illustrated by the typical case presented on page 1029, if one support deflects only 0.1 in. more than its neighbor, stresses 50 pct higher than anticipated will result. Previous studies1-3 have assumed that the mine roof acts like a beam clamped at both ends, with no deflection or slope&apos; at the supports (Fig. 1). Essentially this assumes:5* ?A = ?, = ?b and dA = dB = 0. However, a host of conditions can cause differential sag or deflection at one support, and even an apparently trivial deviation can have major consequences in the beam: variations in spacing, size, and material of supports; local settlement due to floor heaving or lower mine openings; non-uniformity in wedging or bolt tensioning.8 In one particular instance concrete pillars, poured in place, shrank away from the roof upon setting.&apos; When understood and controlled, differential sag becomes a definite advantage, permitting the transfer of loads from one support to another. Where one support is a bolt or prop and the other a pillar or rib, the load on the former can be reduced while the load on the pillar or rib is increased. This means two things: 1) savings can be effected by using smaller artificial supports such as props and bolts and 2) loads can be increased in the rib to induce eventual failure for longwall caving. In this last respect, another factor underlying coal bumps becomes understandable. The design of a mine roof by beam theory assumes that when a bedded formation is homogeneous, iso-tropic, and elastic, it will act like a uniformly loaded beam, fixed or clamped at both ends,6 s in Fig. 1.&apos;" These are important assumptions. The uniform load is the weight of the beam itself or its body load. For a beam of unit width, this load becomes per foot: w = yhb. w = uniform load y = specific weight, lb per ft3 h = depth or thickness of beam, ft b = width of beam, ft Since b = 1, w - yh [ 1 ] A beam fixed at both supports is statically indeterminate to the second degree, that is, two equations in addition to those for static equilibrium are required to determine the reactions at the supports. These equations result from the geometry. From statistics: ^F,= 0;RA + RB — wL = 0 [2] wU S,M0 = 0 ; MB H------------MA — RBL = 0 [3] it Using superposition in which the left support is kept intact and the right one resolved into an active force and moment, we obtain from Fig. 2:" ?b = ?m + ? b2 + ?B3 = 0 dB = dB1 + dB2 + dB3 / wU Ma RBL \ V d°=(-r+-2—r)-zr [5] Where: Subscripts refer to position on axis of beam R = force, lb M = moment, ft-lb w = uniformly distributed load, lb per ft L = span, ft 0 = slope, radians d = deflection, ft E = Young&apos;s Modulus, lb per ft" 1 = Moment of inertia about the neutral axis, ft4 Solving Eqs. 2 through 5 for the four unknown reactions, we obtain: 2 L3 Fig. 3 is obtained by plotting MA and M, vs d, and then plotting RA and R, vs d, and adjusting their scales to coincide with MA and M, vs d,. It should be noted in Eqs. 6 and 7 that as dB increases, MA increases the same amount that Mn decreases. Eqs. 8 and 9 show a similar relationship between RA and R,. Proof that MA is the maximum absolute moment occurring in the beam is as follows: where M, = moment at x wx-When where M,., = maximum positive moment Eqs. 6 and 8 into above: For small dn: MA> M,,,

Jan 1, 1960

By M. T. Hepworth, W. B. Sample

HYDROGEN solubility and linear contraction measurements were made at constant temperature on an alloy of titanium of constant oxygen-to-titanium molal ratio but variable hydrogen content. A cylindrical specimen of titanium (0.25 by 1.6 in.) containing 0.75 at. pct 0 and less than 0.03 at. pct N was cast from a master button of iodide process titanium which had been alloyed with titanium dioxide. Four vacuum fusion analyses, which were made along the length of the cylinder after the hydrogen solubility studies were made, revealed a variation of oxygen content of less than 0.02 at. pct. The specimen was introduced into a quartz furnace tube, annealed and outgassedat 1050"~ for about 1 hr, and then held at 800" * 0.5" for about 30 hr, during which latter time experimental data were taken. The leak rate to the furnace chamber was not sufficient to contaminate the specimen during the run as determined by leak-rate studies and vacuum fusion analyses for oxygen and nitrogen before and after the runs. The furnace chamber was attached to a modified Sieverts apparatus used to introduce measured quantities of purified hydrogen to the specimen. A quartz pushrod transmitted changes in length of the specimen to a Chevenard dilatometer. The push-rod passed through a vacuum grease seal to the dilatometer which amplified motion of the rod by a factor of 319. During hydrogen addition, the pushrod did not contact the specimen. Measured quantities of hydrogen were added to the specimen and equilibrium hydrogen pressures recorded as a function of hydrogen content. The solubility data, which appear in Fig. 1, agree well with a separate investigation made with a different apparatus. The solubility limit of the hcp a phase appears as an abrupt discontinuity in slope at 3.4 at. pct H. The solubility plot has been extended as a dashed line at this discontinuity in order to emphasize the discontinuity. The hydrogen content at which bcc P appears is not clearly defined. An arrow indicates solubility data were taken upon hydrogen addition. Upon reaching the arbitrary maximum hydrogen content of the run, the quartz pushrod was pressed against the specimen in order to record the change in length with hydrogen removal. A pressure of about 100 g per sq cm was required to overcome the friction of the vacuum seal in order to obtain reproducible linear contraction data. The contraction ratio ~2/1", change in length divided by original length, was set equal to zero for the maximum hydrogen content. The relative contraction of the specimen was observed upon removal of hydrogen in the following manner. The system was opened to the pumps for a few seconds and an unknown quantity of hydrogen was removed. The system was then isolated from the pumps by closing a stopcock and allowed to return to equilibrium. When the temperature returned to 800°C, the pressure stabilized, and contraction ceased, measurements of contraction and pressure were made. The hydrogen content of the specimen was then deduced by measuring the equilibrium PIydrogen pressure and referring to the solubility plot. Linear contraction was then plotted against interpolated values of atomic percent hydrogen. The justification for this procedure is the established reversibility of the hydrogen equilibrium.&apos; Uniaxial compression was assumed to have no effect on hydrogen pressure. The isothermal linear contraction data are plotted on Fig. 1. An arrow indicates data were taken upon removal of hydrogen. The solubility limits of the two phase a i /3 region can be identified by discontinuities ill slope of the dilatometric plot at 9.1 and 3.4 at. pct H, agreeing well with other studies.&apos; Dashed extensions of the plots emphasize the discontinuities. Isothermal studies of expansion made upon hydrogen addition gave curves of much smaller slope and less pronounced discontinuities. A uniaxial compressive stress tends to accentuate volume changes in going from the more open bcc phase to the hcp phase.2 Incomplete data on ex-

Jan 1, 1962

By A. L. Lee, M. H. Gonzalez, R. F. Bukacek

Experimental viscosity data for methane are presented for temperatures from 100 to 340F and pressures from 200 to 8,000 psia. A summary is given of the available data for methane, and a comparison is presented for that data common to the experimental range reported in this paper. Correlation of the data is presented, and predicted values are given for temperatures up to 460F and pressures up to 10,000 psia. INTRODUCTION The increasing ranges of temperature and pressure at which fluids are produced, transferred and processed in the petroleum and chemical industries stress the need for accurate information on physical properties, both for engineering calculation and for improving the methods used to estimate physical properties. A survey of the literature reveals that disagreements between published data on the viscosity of methane are common and that most investigations have been conducted over restricted temperature and pressure ranges. This situation made it desirable to undertake an investigation with a scope common to most of the literature data available. APPARATUS AND MATERIALS The apparatus used in this investigation was the capillary tube viscometer&apos;described by Dolan,10 with modifications introduced in the general design and operation of the instrument. It has an effective pressure range from 14.7 to 10,000 psia and a temperature range from room temperature to 400F. The design of the viscometer is based on the establishment of a manometric head between two vessels containing the test fluid and a volume of mercury. The reservoirs are connected by a capillary tube through which the test fluid flows and a tube through which mercury flows. A pressure gradient is established by elevating one of the vessels above the other, the resulting flow of mercury displacing the test fluid through the capillary. The schematic diagram of the system (Fig. 1) shows the arrangement of the equipment auxiliary to the viscometer. The density cells assembly (E, Fig. 1) was not used in this investigation since reliable data are available on methane. 23 The assembly consists of a bank of eight 316 stainless steel pycnometers. Experimental values of the density of a natural gas19 and i-butane14 samples have been obtained for pressures up to 8,000 psia and temperatures up to 340F. The methane used was obtained from the Southern California Gas Co. Mass spectrometric analysis showed a composition of 99.8 percent CH4, 0.1 percent C2H6 and 0.1 percent C3H8. EXPERIMENTAL VALUES AND ACCURACY OF DATA Determinations were carried out at several temperatures. With the temperature in the cabinet controlled at a given level, a series of runs were made at various pressures. To establish pressures lower than that obtained from the methane cylinder, it was necessary to vent the gas slowly to the atmosphere until the desired pressure was reached. The consistency of the test run time for a particular condition can be used as a criterion for the accuracy of the data. A further check is obtained by comparison of the viscosity values obtained using different driving heads. To establish the instrument&apos;s reproducibility, a large number of runs were made at three completely different conditions of temperature and pressure. Data obtained were analyzed statistically to determine the most reliable value for the variance of the experimental data. It was found that the variances of the data taken at different experimental conditions were not statistically equivalent, but they were small. The largest variance was found at 8,000 psia and 100F, where the standard deviation was 0.385 micropoise. Therefore, 99.9 percent of the data can be expected to fall within 1.15 micropoises of the population mean, except for the intervention of systematic errors in operation.

By F. W. Jessen, James N. Howell

INTRODUCTION The determination of cloud points has to date been limited to rather transparent oils, visual observation of the formation of a solid phase being the criterion for the standard ASTM D 97-47 method. The need for a quiclc and simple method for determining cloud points under dynamic conditions for opaque crude oils became necessary in a study of fundamental aspects of paraffin deposition from crude oils. PREVIOUS WORK The determination of cloud points in opaque oils by viscosity temperature curves is fairly new, Young&apos; described a method employing the capillary tube principle. No information exists relative to the determination of cloud points of crude or refined oils under dynamic conditions. Shock&apos; noticed that deposition of paraffin from crude oils took place at temperatures at or below the temperature at which a sharp inflection point occurred in the viscosity-temperature curve. This observation indicates a possible correlation between this temperature and the cloud point of the crude oil. Reistle and Vietti1 have reported that when crude oils containing small amounts of asphaltic materials were heated to temperatures sufficiently high to solubilize these materials and immediately cooled the pour point of the crude oil was lowered as much as 70°F. Sachanen\ asribes this effect to the action of colloidal asphaltenes in preventing the formation of the crystalline structure necessary to maintain the oil in a rigid state. At high temperatures, asphaltenes are peptized, and the paraffin crystals formed at these temperatures adsorb the colloidal asphaltenes on their surface thereby hindering further growth of the crystals. Reistle" found, however, that such heating and cooling of crude oils had no effect upon the cloud points. This latter work dealt with a crude oil of fixed composition, and the question immediately arises as to the effect of varying the concentration of asphaltic materials on the cloud point. APPARATUS AND PROCEDURE All viscosity measurements were made with a Bendix Ultra-Viscoson. The Bendix Ultra-Viscoson, which consists of a vibrating probe and an electronic computer. measures viscosity by exciting a thin alloy steel blade on the end of a probe by short electrical pulses in damped oscillation at 28 kilocycles. The blade vibrates longitudinally with an amplilude of less than 55 micron or 20 millionths of an inch. Energy to protlucc this excitation is generated in he computer and transferred to the probe through the connecting cable. The oscillating blade is magnetostric-tive, i.e., it is capable of transforming electrical energy to mechanical energy in the ultrasonic range. Ultrasonic waves are produced in the material surrounding the blade by the oscillating motion of the blade causing layers of the material to slip back and forth over one another at a known frequency. The electronic computer calculates the energy required to produce the sliding motion which is in turn proportional to the viscosity of the material. Actual values of viscosity times density (centi-poise X grams/cc) are indicated on the computer and a continuous D-C signal is provided which is fed into a type 153 Electronic Recorder (manufactured by Brown Instruments Div. of Minneapolis-Honeywell Regulator Co.) The liquid sample container was fabricated from a Lucite cylinder and jacketed by a Luicite water bath. Early experiments using glass and steel sample containers were not satisfactory. since the Ultra-Viscoson was apparently affected by the alterzltion of the magnetic fields surrounding the probe by stresses set LIP in the glass and steel as it cooled. The procedure for determining viscosity-temperature curves was relatively simple. The temperature ot the sample was raised sufficiently high to solubilize all paraffin and asphalts present. After heating, the oil sample was immediately transferred

Jan 1, 1957

By Mark J. Klein

The behavior of nitrogen in Cr-0.12 at. pct Y was studied in specimens of varying interstitial concentration and thermal history. It was found that soluble nitrogen can be introduced into this alloy by increasing the concentrations of either oxygen or nitrogen. For low nitrogen concentrations the nitrogen in solution is low relative to that in unalloyed chromium. However, the nitrogen in solution increases with increasing nitrogen concentration, approaching that in unalloyed chromium. When the alloy is supersaturated with nitrogen, the nitrogen precipitates readily from solution as a chromium nitride. The stress -induced relaxation of nitrogen is influenced by internal oxidation or internal nitrification of this alloy. THE addition of small concentrations of reactive elements such as yttrium have been found to enhance the low-temperature ductility of chromium.&apos; However, the mechanism by which the ductility is increased is not known. It has been suggested that this effect is caused by a drastic reduction in the concentration of nitrogen retained in solution and therefore a decrease in the number of dislocations locked by nitrogen, a factor that has been associated with an increase in ductility.1,2 However, a change in the type of interstitial precipitate induced by yttrium could also contribute to enhanced ductility of the alloy, since chromium nitride precipitates appear to be embrittling.&apos; In this regard, it has been shown that yttrium scavenges nitrogen in chromium to form YN,4 thus reducing the embrittling chromium nitride phase. However, the change in nitrogen solubility induced by yttrium and the partition of nitrogen between chromium and yttrium nitrides are not known. The object of this investigation is to study the effect of yttrium on the behavior of nitrogen in chromium to obtain information relevant to the mechanism by which scavengers enhance the ductility of chromium. EXPERIMENTAL PROCEDURES The experimental procedures used in this investigation have been described in detail elsewhere.5,6 Wires of Cr-0.12 at. pct Y, 15 cm in length and 1 mm in diam, were drawn from rods 0.6 cm in diam supplied by the General Electric Co. The grain size of the wires after recrystallization at 1150°C was somewhat nonuniform, varying from 0.006 to 0.06 mm in diam. The interstitial analysis for the wires in ppm by weight was about 160 0, 80 N, 12 C, and <2 H. Heat treatments were carried out after encapsulation of the specimens in quartz tubes containing argon. Changes in interstitial concentrations, or interstitial "loading" as it is termed in this study, were generally accomplished by annealing in oxygen, ammonia or methane at 1150°C. The internal friction was measured using a conventional torsional pendulum enclosed in an evacuated chamber. Electrical-resistivity measurements were made at liquid-nitrogen temperature.

Jan 1, 1967

By J. H. Keeler

The tensile characteristics of Zr-Fe binary alloys containing up to 5 atomic pet Fe are reported for the temperature range —195o to 500°C. A linear relation between stress at constant strain and volume fraction ZrFe2 was found. The coincidence of data from unalloyed zirconium with zero volume fraction ZrFe2 indicated little or no solid solution in IL-zirconium, in agreement with Hayes, Roberson, and O&apos;Brien.&apos; The absolute increase in strength due to particle strengthening, although decreasing with increasing temperature, was a greater percentage at high temperature. ZIRCONIUM is of interest for use in nuclear reactors because of its low neutron absorption, good corrosion resistance, and high melting temperature. The alloying of zirconium with iron has been considered as a means of increasing the mechanical strength of zirconium without seriously increasing the neutron absorption " over that of unalloyed zirconium. The Zr-Fe system has a eutectic at 934°C and 23.7 atomic pet Fe and a eutectoid at 800°C and 4.0 atomic pet Fe. The zirconium-rich end of this system determined by Hayes, Roberson, and O&apos;Brien&apos; is shown in Fig. 1. The intermetallic phase coexisting with a and ß-zirconium has been reported as Zr2Fe3,1 with a,, - 7.04A, and as ZrFe2,2 face-centered-cubic, the phase being of the MgCu, type (C-15). It was more recently agreed to be ZrFe33 and face-centered-cubic. This intermetallic phase is essentially insoluble in a-zirconium, the hexagonal-close-packed modification; and the lack of solubility makes the system particularly interesting metallurgically. The system is strengthened almost exclusively by particles of in-termetallic phase, and there is very little solid solution strengthening to complicate the analysis. The Bureau of Mines, in its survey of zirconium-base alloys,&apos; reported the tensile properties of Zr-Fe alloys made from chloride process zirconium, induction melted in graphite crucibles, and swaged at 850°C in iron sheaths. Additional data on these ZrFe alloys were given by Hayes, Roberson, and O&apos;Brien.&apos; Chubb and Muehlenkamp% have recently reported the strength of Zr-Fe alloys containing up to about 1.25 atomic pet Fe. These alloys were made from crystal bar zirconium, hot worked at 820°C, annealed at 700°C, and tested both at room temperature and at 316°C. Experimental Procedure The materials used in this investigation were high purity zirconium made by the iodide process and electrolytic iron. The composition of the zirconium as obtained by spectrographic analysis and the nominal composition of the iron are given in Table I. Alloy ingots weighing 100 g were made by are-melting under argon in water-cooled copper crucibles in a multihearth furnace."

Jan 1, 1957

By D. A. Thomas, E. S. Meieran

Tungsten wires were examined by transmission electron microscopy after drawing and after high-temperature annealing. Drawn wire consists of highly elongated grains called fibers, whose long axis is parallel to [110]. Each fiber is ribbon-shaped, with the wide dimension of the ribbon parallel to (001) and the narrow dimension parallel to (110). Furthermore, most fibers are bent about [I10] and twisted along their length. The fibers are divided into cells, which in some cases contain a platelet substructure lying on (110) planes. The misorien-tations of these platelets accumulate to allow the macroscopic twist of the fibers. During annealing, several competing reactions occur, starting at different temperatures and progressing at different rates. Among these processes are fiber-boz~ndary migration, polygonization, dislocation rearrangement, and possibly impurity segregation. The fiber-boundary migration accompanied by the formation of transverse boundaries during polygonization leads to an equiaxed grain structure although recrystal-lization does not occur. There is a relationship between the flow stress of the wires and their average subgrain width in the form sy = s0 + kyd-1/2 . Also, there appears to be a relatio&apos;nship between wire ductility and the formation of transverse boundaries during annealing at about 800°C. THERE have been many investigations of the structures and properties of tungsten wires1-4 due to their commercial importance for use as lamp filaments. The structural studies have so far been limited to optical microscope and replica electron-microscope studies. due to the difficulty of .-me- paring from wires thin foils which can be examined by transmission electron microscopy. However, this difficulty has been recently overcome,5 and it is now possible to examine tungsten wires by transmission electron microscopy as well as by other techniques. In this paper, the structure of drawn tungsten wire is described, as are the changes in the structure during high-temperature annealing. Some discussion of the relationship between structures and properties is also given. EXPERIMENTAL MATERIALS AND PROCEDURES Commercial 0.030-in.-diam doped tungsten wires drawn at progressively decreasing temperatures between about 1400° and about 800°C were examined. The composition, mechanical properties, and optical microstructures are described in detail elsewhere.&apos; All experimental materials were vacuum-annealed for 10 ot 30 min at temperatures at 100°C intervals between 700° and 2000°C. Specimens were thinned for examination in the Siemens Elmiskop I electron microscope by the method of Meieran and Thomas.5 STRUCTURE OF AS-DRAWN WIRE The optical microstructure of as-drawn tungsten wire has been described by Peck and Thomas.7 They observed that wire in longitudinal section consists of highly elongated grains called fibers whose width varies between 1 and 10 µ, while in transverse section the fibers appear to be elliptical in cross section and bent about their common [110] wire axis. They explained this unusual appearance as being due to the drawing of a bcc material with a [110] texture, and predicted that the wide and narrow planes of the fiber cross section would be parallel to (001) and (110), respectively. The fibers apparently bend about the [110] axis during drawing to maintain grain boundary continuity during drawing. Transmission electron microscopy offers a way of checking these predictions as well as providing a more detailed picture of the wire structure. Figs. 1, 2, and 3 are typical electron micrographs of

Jan 1, 1965

By J. W. Evans

ONE of the most important and frequent calculations that the extractive metallurgist is called upon to make is that of the standard free energy change of a reaction (?F°). For many reactions of metallurgical interest, the lengthy arithmetical calculations have been eliminated by the use of free energy-temperature diagrams which have been constructed by Ellingham,1 Richardson and Jeffes,2 Kellogg,3 and Osborn4 (e.g., for oxides, sulphides, halides) from critical surveys of existing data. The speed and simplicity of making calculations with these graphs make them of great practical value and, this should be stressed, in the majority of cases no greater accuracy is obtained by the individual calculations from specific heat data, entropies, and heats of reaction. With the increasing industrial application of vacuum methods to the winning of metals, notably at present magnesium and the alkaline earth metals, it is necessary to calculate low metal vapor pressures above reaction mixtures. The existing free energy diagrams usually give values where the solid and liquid metals are at unit activity. To obtain the free energy change associated with the reaction Metal (solid or liquid) = Metal (gas) it is customary to calculate this from either vapor pressure equations or from the appropriate free energy functions. This paper presents graphically the free energies of vaporization of a number of metals of economic importance which can be used in conjunction with other free energy diagrams. Certain metals have been excluded on the following grounds: titanium, tungsten, molybdenum, and platinum have very high heats of vaporization and boiling points and the uncertainty of these values arising from difficulties of high temperature measurements makes free energy values of doubtful accuracy; the data for cobalt, vanadium, and zirconium are uncertain; finally, arsenic, antimony, and bismuth could not be conveniently included. because of the presence of mixtures of polyatomic and mona-tomic vapors in the temperature range considered. Free Energy Diagram In Fig. 1, the standard free energies of vaporization per mol (?F°T) have been plotted for the temperature range 0" to 2000°C for the reaction M (solid or liquid) = M (gas) The data have been obtained from the free energy functions — (F-H298)/T for the solid, liquid, and gaseous elements and the heats of vaporization at 298°K, i.e., ?H298 (vapor). The values of these functions have been taken without change from the recent critical survey by Brewer;&apos; the bulk of this data is from Kelley7 with adjustments in the light of more recent work. Values of the function — (F-H298) /T at T = 298°, 500°, 1000°, 1500°, and 2000°K were employed. Where possible, a further independent value was obtained by using the boiling point, i.e., where ?F°T = 0. All calculations are based on the assumption that the metal vapors are monatomic and that the boiling points refer to those temperatures at which the partial pressure of the monatomic vapor above the metal is 760 mm. For the alkali metals, e.g., sodium, potassium, and lithium, diatomic gas molecules are present as minor species; details of these are discussed by Brewer." On the basis of the above values and allowing for the change in slope at the melting point, straight line graphs were constructed and extrapolated to 2000°C. The deviation from a straight line did not exceed ±500 cal, which in all cases appears less than the probable error in the ?F°T values.

Jan 1, 1954

By J. Geertsma

In order to obtain a better insight into the pressure-volume relationship of reservoir rocks a theory of pore and rock bulk volume variations is presented. The theory is independent of the shape of the pores but is restricted to isotropic porous media built up of continuous homogeneous matrix material. The main conclusion obtained from this theory is that only three elastic constants and three viscous constants are required for describing pore and rock bulk volume variations if the porosity is explicitly introduced into the treatment. In addition, reasonable approximations are introduced for various types of reservoir rock, e.g., sandstones, limestones, and shales, which lead to further simplifications of the basic formulas. In consequence there is then a further reduction in the number of deformation constants which have to be determined experimentally. It is shown how measurements of these remaining deformation constants can be performed most conveniently. Finally the application of the theory to reservoir studies is discussed and the translation of experimental results obtained in the laboratory into reservoir behavior is considered. INTRODUCTION The decline of fluid pressure in connection with the withdrawal of fluid from an underground reservoir gives rise to a change in volume of both reservoir fluids and reservoir rock. The volume variation of the reservoir rock results in a decrease of both the pore volume and the total volume of the fluid-filled formation. Whereas the variation in volume of the reservoir fluids with pressure is usually known from PVT analysis, that in the volume of the porous medium is rarely measured, as it is considered of minor importance in reservoir engineering. Nevertheless, certain experimental results&apos; suggest that in a number of cases the neglection of the variation in pore volume may introduce errors into material balance calculations of reservoirs producing above the bubble point. Only a few experimental results on the compressibility of porous rocks have been published. The compressibility of pure quartz and of calcite can be found in a paper by Adams and Williamson&apos;. Botset and Reed&apos; carried out some experiments on the compressibility of loose sands, while Carpenter and Spencer&apos; measured the compressibility of a number of consolidated sandstones, which data were supplemented by Hughes and Cooke5. Hall&apos; finally reported a number of experiments designed to study the influence of the porosity on the compressibility of oil-bearing formations, from which it appeared that, particularly in the low porosity range, the compressibility of the pore volume is important enough to be taken into account. Difficulties, however, arise in applying these experimental results to field cases. This is partly due to the fragmentary nature of the published data. Yet even if more complete data were available, the need for a theoretical background would be strongly felt. Such a background can be partially found in studies carried out by Biot,6,7 who published a theory of elastic deformations of porous materials and their influence on fluid displacement within the pores, by Lubinski8, who studied the stress distribution in an elastic porous medium neglecting pore compressibility, and by Gass-mann" who mathematically analysed the elasticity of packings of spheres. The contributions of Biot intro-duce a number of deformation constants which are impractical for reservoir rocks from an aspect of experi-mental determination. The theory developed by dass-mann is correct but difficult to read. It appeared, how-

Jan 1, 1958

By S. L. Couling, D. J-P. Adenis

i2) twinning in poly crystalline magnesium does not usually occur homogeneously but is concentrated in localized regions or bands inclined at about 45 deg to the stress axis. These bands of twinning are in many ways similar to the Luders bands seen in mild steel alzd Al-Mg alloys. Within a hand the percentage of the volume twinned may approach 100 with no twinning outside the band. Bands are not produced in specimens of grain size a3 x 10-= in. or in samples deformed at temperatures 300°F. Annealing of heavily twinned regions leads to re crystallization textures markedly different from those found in the starting material. The exact preferred orientation appears to depend on the starting grain size, the amount of compres-sive strain and the manner in which it is introduced. MAGNESIUM, with its hexagonal crystal structure, deforms plastically at room temperature by a variety of deformation mechanisms, one of the most important of which is (1012) twinning. In single crystals such twinning occurs on compression parallel to the basal plane or tension perpendicular to it. In wrought polycrystalline magnesium, such as rolled sheet, the preferred orientation is such that almost all the grains have their basal planes nearly parallel to the sheet surface. Therefore, if sheet material is deformed by cold rolling or by tension in the plane of the sheet, deformation of the grains by (1012) twinning is not favored. On the other hand, twins form readily on compression parallel to the plane of the sheet as in a compression test, on the compression side of a bent sample, or at the outer rim of a drawn cup. The first part of this paper deals with the morphology of (1012) twinning in polycrystalline magnesium. Some aspects of this subject were covered by Barrett and ~aller.&apos; Of direct bearing on the work to be reported here are the comments of Jetter&apos; in discussion to Ref. 1. He shows that Mg + 1.5 pct Mn alloy sheet when bent about a transverse axis develops a pattern of transverse bands on the surface of compression. A longitudinal section through the sheet shows that the bands are wedge-shaped and inclined to the rolling direction. The bands were identified as "outcrops of regions in which deformation is localized as the result of the reorientation brought about by (1012) twinning". The second part of the paper treats the recrys-tallization texture of the specimens twinned by compression. Magnesium deformed and then annealed generally recrystallizes with no change in orientation.1&apos;3&apos;4 This statement is true provided that the amount of (1012) twinning occurring during deformation is small. In an isolated observation, Anse15 has shown that, when deformation produces much (1072) twinning, annealing causes new maxima to appear in the pole figure. The second part of the paper elaborates on this point. I) MATERIALS AND PROCEDURES All of the experimental work to be reported was done using the commercial sheet and plate alloy AZ31B (nominal composition: 3 pct Al, 1 pct Zn, 0.4 pct Mn, balance magnesium). This alloy is available commercially in two tempers, -0 (fully annealed) and -H24 (partially annealed), and specimens of both tempers were used in various experiments. The average grain. diameter (AGD) for -0 temper 0.125-in. sheet is about 0.5 x 10- in.; where material of larger grain size was desired, anneals at elevated temperature were used to grow the grains. compression tests were made on a screw-driven "hard" machine. The specimens were clamped in a

Jan 1, 1964

By Charles S. Barrett

Recrystallization textures—thc orientations of grains after recrys-tallization—have been studied extensively not only because of their metallurgical importance but also because of the information they yield regarding the atomic movements during reerystallization. Recrystallized grains must possess the same orientations as the submicroscopic nuclei from which they have grown, and thus they offer a direet road by which experimenters can penetrate the submicroscopic realm. Many perplexing results have come of these studies, but one of the most striking has been the apparent difference in behavior between single crystals and polyerystalline grains. For example, Burgers and Louwerse have shown1 that when single crystals of aluminum are deformed by compression and are reerystallized (at 600&apos; C.) the new grains appear with orientations that are different from the orientations of the deformed crystal in which they grew; but polycrystalline specimens, on the other hand, appear to have a [110] fiber texture both before and after reerystallization and thus to retain their texture during recrystallization. This apparent difference between the habits of single crystals and small grains is the subject of the first part of the present research and has been explained by findings reported herein. A similar situation appears to exist for aluminum when elongated or drawn into wires, for single crystals alter their orientation 2,3 and polycrystalline wires retain their texture"5*" upon recrystallization after elongation (at least with high-purity aluminum), and it is possible that the explanation found in this paper for compression can be extended to cover elongatioil and other types of deformation as well. The second part of this paper deals with the theory of reerystallization textures. In the most successful theory for aluminum reerystallized after compression,1 much weight is given to the orientation of highly stressed nuclei in the deformed material. Taylor&apos;s "local distortions" arc assumed to exist along the slip planes where displacement has occurred, consisting of fragments rotated in a specific way with reference to the slip plane and slip direction; namely, about an axis lying in the slip plane perpendicular to the slip direction.1,7,89

Jan 1, 1940

By Sir Robert Hadfield

LAST year this Institute was good enough to accept some remarks by the writer regarding sound steel, entitled Plant for Hadfield Method of Producing Sound Steel Ingots, being a continuation of a research in which for some time the writer has been engaged, and full particulars of which were submitted in papers entitled A New Method of Revealing Segregation in Steel Ingots, and Method of Producing Sound Ingots, read before the Iron and Steel Institute in October, 1912. These papers gave rise to a very interesting discussion, both in England and America. This question is one of vital importance, as unless sound steel in the form of ingots is first obtained, sound steel in the finished forms of rail billets, rails, bars, sheets, and other forms cannot be expected. The working stresses demanded by modern conditions are so great, each year they probably approach nearer to the limit of safety, that without doubt those who produce steel will be compelled to pay the attention which this subject deserves. Moreover, the problem is not an insuperable one, as shown by the writer in the papers above referred to. In view of the information which has already been presented in these papers, it is not now necessary to go into details of the system advocated by the writer, except to repeat that the ingots and steel now referred to were produced by employing in the first place sound fluid steel, free from blowholes, this being poured into ordinary ingot molds, provided with the necessary feeding heads, the insulating slag medium, also charcoal and air blast or other suitable form of applying heat to the head portion of the ingot. Tile upper or head portion of the ingot is kept fluid by the intense heat generated by the air blast and charcoal, so that such fluid steel passes into the body of the ingot below the head, thus feeding and avoiding the shrinkage or piping which would otherwise occur. The result is the production of a sound steel ingot, free from blowholes, segregation and piping, and in which the waste portion, usually termed the discard, is but little over 7 or 8 per cent.

Jan 4, 1914

By Charles S. Barrett

Recrystallization textures—thc orientations of grains after recrys-tallization—have been studied extensively not only because of their metallurgical importance but also because of the information they yield regarding the atomic movements during reerystallization. Recrystallized grains must possess the same orientations as the submicroscopic nuclei from which they have grown, and thus they offer a direet road by which experimenters can penetrate the submicroscopic realm. Many perplexing results have come of these studies, but one of the most striking has been the apparent difference in behavior between single crystals and polyerystalline grains. For example, Burgers and Louwerse have shown1 that when single crystals of aluminum are deformed by compression and are reerystallized (at 600&apos; C.) the new grains appear with orientations that are different from the orientations of the deformed crystal in which they grew; but polycrystalline specimens, on the other hand, appear to have a [110] fiber texture both before and after reerystallization and thus to retain their texture during recrystallization. This apparent difference between the habits of single crystals and small grains is the subject of the first part of the present research and has been explained by findings reported herein. A similar situation appears to exist for aluminum when elongated or drawn into wires, for single crystals alter their orientation 2,3 and polycrystalline wires retain their texture"5*" upon recrystallization after elongation (at least with high-purity aluminum), and it is possible that the explanation found in this paper for compression can be extended to cover elongatioil and other types of deformation as well. The second part of this paper deals with the theory of reerystallization textures. In the most successful theory for aluminum reerystallized after compression,1 much weight is given to the orientation of highly stressed nuclei in the deformed material. Taylor&apos;s "local distortions" arc assumed to exist along the slip planes where displacement has occurred, consisting of fragments rotated in a specific way with reference to the slip plane and slip direction; namely, about an axis lying in the slip plane perpendicular to the slip direction.1,7,89

Jan 1, 1940

By J. W. Spretnak, G. W. Cunningham

A study has been made of the growth and disappearance of voids in the interface of pressure bonded copper. The formation of visible voids is primarily due to spheroidization and coalesence of microvoids produced during the application of pressure. The microvoids could be prevented from forming by the application of high pressures or by increasing the ductility of the copper. Migrating grain boundaries were found to be more effective in void removal, than stationary grain boundaries. DURING the course of an investigation on the mechanism of pressure bonding, it was found that voids formed in the bonding interface which inhibited migration of the interfacial boundary and grain boundaries in the bond region. Therefore, an effort was made to determine the nature of the voids and how they form, grow, and disappear. This paper reports the results of such an investigation. The existence of interfacial voids is not solely a characteristic of massive components of metal which have been bonded by the application of heat and pressure, but is a phenomenon which has been observed in sintering as well. Simonsen attempted to study the sintering process by hot-stage microscopy and thereupon observed the formation of interparticle porosity as sintering proceeded. It was assumed that the porosity was due to grooves created at the location where grain boundaries joined the surface of the particle. Pranatis, Castelman, and seigle2 have also observed voids along the areas of contact in wound-wire specimens used for sintering studies. They did not discuss the point in detail since this behavior was not general, but they did suggest that the voids might develop as a result of stresses along the interparticle contact area. In previous investigations on pressure bonding, workers3 have suggested that voids may exist in the region where mating surfaces are placed in intimate contact, but the existence of the voids was not verified and no attempt was made to study the growth and disappearance of these voids. Durst noted the existence of pores in roll-clad structures prepared by cold reducing two sheets to force them in contact and then annealing to improve the bond. Since his unbonded regions contained a gas which he assumed to be insoluble, he proposed a mechanism which consisted of spheroidization of the unbonded regions and a growth of the contact area, but no speculations were made regarding disappearance of the gas filled pores. One interesting comment made by Durst was the suggestion that flattened voids with sharp corners which are produced during roll bonding will have a greater driving force for spheroidization than the more rounded pores created by pressing metal powders and thus spheroidization and neck growth will occur at lower temperatures. In this study it was necessary to demonstrate conclusively that voids can actually exist in the interfacial bond area. Experimental work was then directed toward a study of the mechanism whereby the voids grow and subsequently disappear.

Jan 1, 1963