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By W. D. Robertson, A. S. Tetelman

The technique of decorating dislocations was employed to investigate deformation and fracture resulting from Precipitation of hydrogen in Fe-3 pet Si single crystals. It is shown that cracks are produced on (100) planes inside crystals, as a consequence of the precipitation of hydrogen gas, either when crystals are quenched from a hydrogen atmosphere at elevated temperatures or cathodically charged with hydrogen at room temperature. Plastic deformation in the vicinity of cracks, observed as arrays of decorated dislocations, is in conformity with the calculated stress distribution about a crack containing an internal pressure, and the observations provide information permitting a detailed analysis of the mechanics of crack growth. The fracture characteristics of crystals containing internal cracks were evaluated at 25o and -196°C and the results are related to the mechanism of hydrogen embrittlement in terms of the growth of preexisting cracks. HYDROGEN in bee iron or steel produces two characteristic changes in mechanical properties: I), a decrease in ductility (macroscopic strain at fracture) that depends on temperature and strain rate, and 2), spontaneous fracture under static load that depends on time and apparent stress. Resolution of these phenomena into the microscopic processes that combine to produce the macroscopic effects is especially difficult in the Fe-H system in which the active component cannot be directly observed and only maintained in equilibrium with great difficulty in the temperature and pressure range in which embrittlement phenomena appear. As a result of these complications, verification of the numerous hypotheses'-5 that have been proposed to explain the microscopic mechanism of embrittlement depends on self-consistency with measured changes in macroscopic properties that are averaged over the volume of a specimen. It is obviously important to obtain a more direct evaluation of the microscopic processes that combine to produce embrittlement. Accordingly, the present investigation was designed to identify and observe, as directly as possible, the microscopic effects of introducting hydrogen into a bee crystal. It was concluded from a previous investigation6 of X-ray line broadening, produced by introducing hydrogen into pure iron at room temperature, that the only effect that could be associated with the introduction of hydrogen was plastic deformation; in particular, dilation of the lattice was not observed, within ± 0.01 pet, and no evidence was found that could be interpreted to support the idea7'* that hydrogen occupies tetrahedral interstitial sites in the iron lattice. The absence of lattice dilation is consistent with the extremely small solubility of hydrogen in bee iron9,10 (0.015 at. pet at 900oC and 1 atm pressure), and the evidence of plastic deformation is consistent with the fact that hydrogen, introduced by cathodic charging, eliminates the carbon yield point.11-13 Following this investigation, the immediate problem was to devise a method by which plastic deformation could be observed directly. The technique employed by Hibbard and Dunn14 to observe the movement of dislocations during bending and subsequent polygonization of Fe-3 pet Si single crystals was adopted and modified for the present purpose to include the observation of dislocation arrays in the volume of the crystal, and their association with the fracture process. EXPERIMENTAL PROCEDURE Single crystals of a high purity Fe-3 pet Si alloy, containing 0.007 pet C, were grown in vacuum by

Jan 1, 1962

By A. M. Turkalo

IT is a well-known fact that martensitic steels show a greater resistance to brittle fracture than do pearlitic and bainitic steels. It was, therefore, thought worthwhile to investigate the mode of brittle fracture with respect to structure by studying the effect of various austenite decomposition products on the propagation of brittle fracture in steel by means of electron microscopy. Newly developed replication techniques together with the advantages of the electron microscope such as great depth of field, available high magnification and easy adaptation to stereophotography make electron microscopy very suitable for fracture studies. EXPERIMENTAL PROCEDURE An essentially plain carbon steel containing 0.56 pct C, 1.30 pct Mn, 0.02 pct P, 0.03 pct S and 0.22 pct Si was used in this investigation. The following table gives the heat treatments used to obtain the various austenite decomposition products: The resulting austenite grain size from the 870°C austenitization treatment was about an ASTM No. 7 grain size. The specimens which were 2 in. long, 1/4-in. diam bars were austenitized in a tube furnace through which argon gas was blown. The tube was not, however, air-free and the specimens were not completely oxide-free. Isothermal treatments were done in a lead bath. With the exception of the fully hardened specimen and the one as-isothermally transformed at 300°C the heat treated specimens were notched in the following fashion with a jeweler's saw. A cut about 0.08 in. deep was made perpendicular to the length of the bar. The specimen then was rotated about 45 deg and another cut about 0.08 in. deep was made. In the case of the hard martensitic and bainitic specimens, only one cut was made and the depth was not controlled. The design of the two-cut notch caused fracture to initiate at the point of intersection of the two saw cuts. The specimens were broken at -196°C in a Charpy impact testing machine. In order to hold the specimens securely in the impact machine two square pieces of mild steel were made about 5/8 in. long having the same cross section as that of a standard Charpy specimen but containing a hole 1/4 in. diam through the center of the cross-section. These adapters were slipped over the ends of the test specimen which was then secured tightly by means of set screws in the adapters. The specimen with the adapters was cooled to -196°C in liquid N,, then placed in the impact machine and broken within 3 sec. One half of the broken specimen was used for the electron microscope study of the actual fracture surface. The other half was nickel-plated and a cross section through the notch and fracture was polished for electron microscope examination. Carbon replicas of the fracture specimens for the electron microscope study were made essentially according to Bradley's evaporation technique.' Both direct carbon and two-stage carbon replication techniques were used. In the case of the direct carbon technique, a thin layer of carbon was evaporated first at an angle of about 45 deg to the mean fracture surface and then another film of carbon was evaporated normally to the fracture surface. The carbon replica was freed electrolytically.2 The specimen was made an anode in a 10 pct Nital polishing solution. It was etched intermittently by shutting off the power now and then. The freed replica was washed in 40 to 50 pct water solution of nitric acid for 10 min or so, then washed in water and picked up on a screen for examination. The two-stage carbon replication technique involved first making a primary replica of cellulose * acetate from which a carbon replica was then made. One side of a strip of cellulose acetate wet with acetone was pressed lightly against the surface of the specimen, allowed to dry and then stripped. Prior to the deposition of carbon, which was done at 90 deg to the cellulose acetate replica surface, chromium was evaporated at 45 deg. After the carbon evaporation the cellulose acetate was dissolved in acetone according to the Jaffe method3 leaving the carbon replica preshadowed with chromium for examination.

Jan 1, 1961

By David J. Mack, Chin Bea Kim

The decomposition of the Ni-Zn eutectoid at 56 wt pct Zn was studied by isothermal transformation. Its progress was followed by metallographic, hardness, and X-ray diffraction methods. Three transformation products were found: lamellar pearlite at high temperatures; an intermediate temperature structure; and martensite at the lower temperaCures. No transition structu,ves were found. THE decomposition of the Ni-Zn eutectoid at 56 wt pct Zn was stuadied as part of a long-range program of study on the eutectoid transformation in alloy systems which do not have one or more components which exhibit allotropy. Available information on the Ni-Zn eutectoid transformation is limited to that presented in connection with the determination of the phase dilagram. No systematic studies of the eutectoid were found in the literature, alkhough the microstructures of the Ni-Zn eutectoid were reported by Tamuru.3 X-ray diffraction data exist for the ß, ß1, y , and y1 phases.' EXPERIMENTAL PROCEDURE The eutectoid alloy was prepared from "A" nickel shot and Bunker Hill super-purity zinc (99.998 pct).

Jan 1, 1962

By D. L. Ritter, N. J. Grant, B. C. Giessen

Forty-six alloys covering the complete concentration range of the Nb-Rh system were examined by metallographic and X-ray methods; solubility limits of terminal ad intermediate phases and transformation and solidus temperatures were determined. There are nine intermediate phases; two eutectic, five peritectic, two eutectoid, and three peritectnid reactions were encountered. The experimental methods and the constitution diagram are described in Part I. Part 11 deals with the crys -tallography and relation of the intermediate phases. The Nb-Rh system was selected for study for three reasons: first, it was hoped that the anticipated similarity of the Nb-Rh phase diagram to the Ta-Rh1 and Ta-Ir2 diagrams treated earlier (see also Ref. 3) and to the Nb-1r4 diagram treated simultaneously would allow a crystallographic and comparative evaluation of the intermediate phases in these related systems; second, it was likely that the previous experimental methods could be carried over without significant change; and third, it was expected that the interesting mechanical properties of the a1 phase of the Ta-Rh and Ta-Ir systems would also be encountered in similar phases of the new systems, and that these phases could be investigated more closely. The phase diagram had not been treated fully in the literature; only brief surveys of some intermediate phases were found.5-7 It was attempted to cover the details of the phase boundaries, Part I, as well as to present the crystallography of the intermediate phases, Part 11. EXPERIMENTAL METHODS Specimen Preparation and Treatment. The following high-purity starting materials were used. 1) Niobium powder, 99.8 pct pure, mesh size -60 +200, from Wah Chang Corp., Albany, Ore. The analysis furnished by the supplier showed the following major impurities: Ta, <500 ppm; Zr, <500 ppm; 0, 300 ppm; Fe, 280 ppm; Ti, <I50 ppm; W, Si, <100 ppm; C, N, 30 ppm; all other impurities, <30 ppm. 2) Rhodium powder, ground sponge, 99.9+ pct pure, mesh size -80, from J. Bishop Co., Malvern,

Jan 1, 1964

By C. H. Li, R. J. Stokes

This paper compares the fracture behavior of tungsten rods in three conditions: recrystallized. recovered, and wrought. Notched specimens suhjected to a 50 in.-lb impact load showed ductile-brittle transitions at 700, 4.90°, and 440°C, respectinely. The recrystallized material had an equiaxed pain structure and jracbred by simple cleavage from a grain boundary source at all temperatures up to 700°C. The wrought and recovered material had an elongated fibrous structure and at low temperatures fractured by cleavage originating from the notch. As the transition temperature was approached cleavage was preceeded by more and more intergvanular splitting which deflected the crack front into planes parallel to the tensile axis. The enhanced toughness of wrought and recovered tungsten was attributed both to its inability to initiate cleavage because no pain boundaries were suitably oriented perpendicular to the tensile stress and to its inability to maintain cleavage because of intergranular splitting ahead of the crack. It has been appreciated for a long time in a qualitative manner that the room-temperature brittleness of fully recrystallized tungsten may be alleviated by working the material at relatively low temperatures.&apos; More recently this difference in mechanical behavior between wrought and recrystallized tungsten has been examined quantitatively by measurement of the tensile properties as a function of temperature. In these experiments brittleness has been expressed in terms of ductility or reduction in cross-sectional area upon tensile fracture or in terms of the bend radius before fracture under bending.&apos; This work has shown the existence of a fairly sharp transition from brittle to ductile behavior with an increase in temperature. The ductile-brittle transition temperature for recrystallized material is approximately 200°C higher than for wrought material. An increase in strain rate, small additions of impurity,&apos; or an increase in grain size4 shift the respective transition temperatures to higher values, but the difference between them remains approximately the same at 200°C. A number of explanations for this embrittlement by recrystallization have been given. It has been blamed either on the concentration of impurity at the grain boundaries, the increase in grain size, or the change in texture which occurs upon recrystallization. The present paper examines the effect of different heat treatments on the notch-impact behavior of commercial powder-metallurgy tungsten rods. The change in the ductile-brittle transition temperature for this method of loading and the fracture mode has been related to the different mi-crostructures produced by heat treatment. EXPERIMENTAL PROCEDURE Commercial swaged powder-metallurgy tungsten rods 1-3/8 in. in length and 1/8 in. in diameter were machined to introduce a sharp V notch 0.030 in. deep. To change the microstructure from that of the as-received wrought material some of the specimens were subjected to an anneal in nitrogen either at 1300° or 1400°C for 8 hr or at 1600° or 2000°C for 1/2 hr. The notched rods were then placed in a miniature Charpy-type impact machine and struck at their midpoint (opposite the notch) with a hammer designed to deliver 50 in.-lbs of energy. The strain rate at the base of the notch was estimated to be approximately 100 sec-1 at the instant of impact. The specimens were heated in situ to the desired impact temperature. The microstructures produced by the various anneals were studied by both X-ray diffraction and metallographic techniques. Fig. 1 reproduces the microstructures observed metallographically following a 10-sec electroetch in a 10 pct KOH solution. Fig. l(a) shows the elongated fibrous grain structure of the as-received material. Following the anneal at 1300" or 1400°C the grain structure was still elongated as shown in Fig. l(b) but the etch pits delineated dense polygonized dislocation arrays within many of the grains. Occasionally a relatively dislocation-free recrystallized grain was found growing into the matrix. The anneals at 1600° and 2000°C resulted in complete recrystallization and some grain growth. The grains produced at 1600°C were still slightly elongated as shown in Fig. l(c) whereas the anneal at 2000°C produced equiaxed grains. The changes in grain size produced the expected changes in the X-ray back-reflection patterns; there was no indication either in the as-received material or the annealed material of any preferred orientation. RESULTS a) Impact Behavior. Fig. 2 reproduces the ductile-brittle transition curves measured in the manner described in the previous section. It can be seen that under these testing conditions the as-received

Jan 1, 1964

By A. E. Gorum, I. Cornet

Fatigrle of ionic crystals has been studied primarily in magnesinm oxide. under cyclic stress dislocations move irrreversibly; they multiply; slip bands form and grow; cracks mucleate and propagnte, and failure occurs. The use of ionic crystals such as MgO is advantageorus in such investigations because they are optically transparent. Individual dislocation Intersections with {100} surfaces may be observed with a standard microscope, using etch-pit techniques. Slip, deformation, crack .formation, and fracture in MgO crystals under cyclic stress are compared with cotrresponditzg processes in metals. ThE effect of cyclic loading in metals has been studied for many years. The appearance of slip lines is readily observed and the ensuing fracture may also be seen. From these observations it is possible to predict the behavior of a material and make an educated guess as to what is happening internally, but the actual changes taking place within the structure are not readily apparent. If one could obtain a material in which the individual glide components could be observed, it would be invaluable in determining the actual slip distribution resulting from cyclic loading as well as the distribution of slip in the neighborhood of a growing crack. Such a material is magnesium oxide. Dislocation arrays may be observed by means of etch pits

Jan 1, 1961

By A. S. Koster, G. D. Rieck

X-ray experiments were carried out to show the occurrence of cylindrical texture in drawn tungsten wire. Only a small amount of (110) (110) cylindrical texture could he found in wires of intermediate thickness, i.e., of about 1.5 mm diameter. DRAWN wires of tungsten and other bcc metals like iron and molybdenum show a well-established (110) fiber texture. Now it might be conceivable that in drawing radial stresses remove the randomness of the crystallites around the [110} axis, thus giving a fiber texture of higher symmetry. In the resulting so-called cylindrical textures a specified plane normal coincides with the radius of the wire. Several authors discuss the occurrence of cylindrical textures in bcc metals. ~ieck&apos; found no cylindrical texture in drawn tungsten wires of 165 n diameter. Leber~ states that in tungsten wires of 3 mm diameter a cylindrical {100)(110) texture is developed, which is gradually converted to a normal fiber texture by subsequent drawing. He also reported a definite cylindrical texture at the surface of iron wires. Peck and Thomas3 observed a nonuniform mode of deformation of the grains in transverse sections of heavily drawn tungsten and iron wires. According to Bhandary and cullity4 a swaged iron wire has neither a perfect (110) fiber texture nor a perfect {100}(110) cylindrical texture. It is clear that the concept of cylindrical texture in bcc metals still lacks a firm experimental basis. Leber&apos;s eviden~e,~ which seems to be the strongest, rests upon qualitative interpretation of photographs. The appearance of the 110 and 200 lines on the photograph of 3-mm wire, however, can be very well attributed5 to a normal ( 110) fiber texture superimposed on random background; our Fig. 1, giving a Debye-Scherrer diagram of etched tungsten wire of 180 p, is free of cylindrical texture according to all authors, but is quite similar to Leber&apos;s diagram. It was therefore decided to use a different method of X-ray texture determination on tungsten wires of diameters where cylindrical textures may be expected.

Jan 1, 1965

By Paul A. Beck, M. N. Parthasarathi

The vecrystallization texture. formed by selective growth of random nuclei in an 80 pct volled 99.997 pct A1 crystal of initial orientation mear (123) (41.21 was found to consist of components related to the single-component rolling texture by 40 deg. rota-tiows around [111]axes. The relative-volume fractiovz of the various recrystallization-texture componezts may be accouzted for 012 the basis of the Lou) mobility of twist boundaries, if it is assumed that the mobility of the tilt boundaries also varies with their orientation. Similar results with a, aluminum-alloy cystal of the (110) [112] orientation, containing iron, silicon, and zinc, show that these solute contents do not impair the effectivezess of the oriented growth mechanism of re cry s-tallization- texture formation. In a previous investigation1,2 it was found that a sharp recrystallization texture is formed as a result of the oriented growth of random artificial nuclei in an aluminum crystal rolled to 80 pct RA, on the (110) plane in the [ 112] direction. Four recrystallization-texture components were found to occur, with orientations corresponding to 40-deg rotations around [111 1 axes of the deformation texture. Reorientations of this type were already found in earlier work,3,4 where the presence of random nuclei could be reasonably assumed, but was not rigorously documented. The same orientation relationship was found also by Lucke and Liebmann, who actually measured the orientation dependence of boundary-migration rates in the recrystallization of A1 crystals slightly deformed in tension.5,6 The occurrence in the recrystallization texture of only four of the eight crystallographically equivalent orientations of the type referred to above remained unexplained,1,2 although it was clearly not a result of the absence of suitable nuclei. Recently Burgers7 suggested that this effect may be due to the aniso-tropy of boundary mobility observed2&apos;6; it was found that the recrystallized grains of the 40-deg [111]-rotated type grow much faster in directions perpendicular to the [ 111] they have in common with the matrix than parallel to this direction, i.e., the tilt boundaries have much higher mobility than the twist boundaries. The four orientations corresponding to

Jan 1, 1962

By R. Maddin, C. H. Mathewson, W. R. Hibbard

According to conventional crystal mechanics, a face-centered cubic single crystal slips on the system {111} <110> which receives the highest shear stress in terms of the stated orientation of the stress axis of the crystal.l However, in brass, the slip process is never as simple as this conventional analysis indicates. There is always a second cooperating plane which contains the same slip direction as the primary plane.2&apos;3 There is still another cooperating slip system commonly called the conjugate system3 previously observed to function with considerable lag only after the rotation due to the action of the first plane had produced a symmetrical condition of equal shear stress on the two systems. In the 1943 Campbell Lecture,4 a slip mechanism was outlined in which the {111) planes moved step-wise in two adjacent <112> directions integrating into the <110> slip direction. "... the slipping process would be visualized as a succession of steps 30" to the right and left of the resultant, microscopically observed, slip direction; a first step setting up the twinned configuration in the single spacing involved and an ensuing slip returning the atoms to the untwinned configuration while completing a fully integrated <110> movement."4 This process is shown diagrammatically in Fig 1 which shows two close packed layers of atoms at a slip site. A movement of the full circles through the "valleys" into the adjacent sites would produce a twin configuration with respect to the open circles. The term, "twin fault," seems most appropriate to define this faulted condition of the lattice. Annealing twins in face-centered cubic metals may arise from preformed nucleii which could be described as twin faults produced by the first movement of this two stage slip process. However, it is clear that this kind of slip does not take place so as to embrace a measurable number of adjacent planes because careful X ray examination has not conclusively shown the existence of ponderable twin lamellae (as in the case of Neumann bands in the body-centered ferrite). In view of the imponderable character of these hypothetical twin faults, the search for evidence of their existence seems restricted to indirect methods. The most obvious experimental technique serving this purpose is the determination by micrographic and X ray methods of the alignment of the composition planes of annealing twins with the former slip planes in axially strained and recrystallized single crystals. In previous attempts of this sort not all of the annealing twins could be traced to slip planes known to be operative in the conventional sense and hence evidence appeared negative or inconclusive. With the discovery of additional slip systems2&apos;3 operating in conjunction with&apos; the major system of highest resolved shear stress in axially strained brass it became apparent that the simple technique outlined above might be re-employed with more gratifying results. If, on annealing single crystals of alpha brass previously strained in tension, twins are found with their composition planes parallel to all three operative slip planes and with no participation of the fourth plane there is good evidence in favor of the existence of twin faults and of the two stage slip process. Experimental Procedure and Resuits Single crystals of alpha brass of the 70-30 composition were grown by solidification from the molten state.

Jan 1, 1950

By P. E. Doherty, B. Chalmers

Subboundaries may be revealed in aluminum by the formation of pits on the surface during cooling from elevated temperatures. The pits do not form in the vicinity of high- or low-angle boundaries. They are attributed to the condensation of vacancies from a super saturation produced during coolirzg. Using the vacancy pit and Schulz X-ray techniques for observing low-angle boundaries, a study was made of the transition from the nearly perfect seed to the striated structuke characterist-ic of aluminum crystals grown from the melt. It was found that the individual striation boundaries develop by the coalescence of very small-angle boundaries, as well as by the addition of individual dislocations. Several mechanisms for the formation of striations are discussed. Evidence was found suggesting that a super-saturation of vacancies exists near a growing interface, and it is proposed that the resulting climb of existing dislocalions produces "half&apos;-loops" at the interface, which combine to form the low-angle striation boundaries. LINEAGE, or "striation" boundaries, have been studied in detail by Teghtsoonian and Chalmers 1,2 in crystals of tin grown from the melt, and by Atwater and Chalmers3 in lead. They found that single crystals grown from the melt consist of regions which are separated by subboundaries that lie roughly parallel to the growth direction. A difference in orientation of 0.5 to 3 deg exists between the striated regions; the misorientation is such that the lattice of one region could be brought into coincidence with the lattice of its neighbor by a rotation about an axis approximately parallel to the direction of growth of the crystal. They observed an incubation distance for the formation of striations which increased with decreasing growth rate. They also found that in any crystal, the sum of all rotations of the lattice in one sense, in going from one striation to the next, is very nearly equal to the sum of all the rotations in the opposite sense. A striation boundary, which is a low-angle grain boundary, can be described as an array of dislocations. If it is assumed that suitable dislocations are introduced into the crystal during solidification, the formation of striation boundaries can be explained as a result of the migration of the disloca- tions into arrays. The formation of arrays is energetically favorable since the energy of an assembly of dislocations can be reduced by the interaction of the stress fields when a suitable array is formed. This investigation presents and interprets new information concerning the nature and origin of striation boundaries in aluminum. EXPERIMENTAL TECHNIQUE Single crystals of high-purity aluminum (Alcoa 99.992 pct) were prepared by horizontal growth from the melt.&apos;&apos; The specimens were subsequently electropolished in a solution of 5 parts methanol to 1 part perchloric acid kept between -10° and 0°C in a bath of dry ice and alcohol. The current density was approximately 6 amps per sq in. Doherty and Davis9 have shown that in aluminum sub-boundaries with misorientations of not less than several seconds of arc may be revealed by the vacancy pit technique. During cooling from elevated temperatures pits form on electropolished surfaces of aluminum crystals as a result of the condensation of vacancies.11 Pits do not form in the vicinity of small- or large-angle grain boundaries, presumably because such boundaries act as sinks for vacancies. Boundaries of misorientations down to 3 sec of arc are revealed as pit-free regions, see Fig. 1. The Schulz X-ray technique12 was used to determine the angular misorientations of subboundaries. In this method, white radiation from a micro-focus X-ray tube is used to produce an image of a fairly large area of a single crystal surface. Subboundaries cause splitting in the diffracted image, see Fig. 2. Misorientations down to about 15 sec of arc may be observed with this technique. OBSERVATIONS AND DISCUSSION Figure 1 shows a striated aluminum crystal grown at 10 cm per hr etched by the vacancy pit technique. An incubation distance of about 1 cm is observed before the initiation of striation boundaries. Fig. 2 is a Schulz X-ray photograph of a striated crystal similar to that shown in Fig. 1. A large area of the crystal was studied by means of a series of photographs. Fig. 2, which is a reflection from the (100) plane, included about the first 4 cm of crystal to freeze. There is an incubation distance of about 1 cm, and a distance of about 2 cm over which the angle of misorientation builds up to its final value of approximately one degree. Some twist component can be seen in Fig. 2 at the right side of the photograph. From Fig. 2 it can be seen that the sum of all rotations of the lattice in one

Jan 1, 1962

By R. D. Reiswig, J. M. Dickinson

The 0s-Ir equilibrium diagram was determined. The diagram is of the simple peritectic type, with a peritectic temperature of about 2660°C. The solid miscibility gap is narrower than previously reported, the nearly vertical solvus lines occurring at about 42 and 63 wt pct 0s. Widmanstaetten figures resembling martensite in some of the two-phase alloys account for a previously suspected transformation. In view of the long history of use of such alloys, it is surprising that the 0s-Ir equilibrium diagram has not yet been completely determined. The boundaries of the miscibility gap in this system have been estimated to be between 24 and 39 wt pct 0s and 79 and 100 wt pct OS. It has been predicted3 that alloys of ruthenium, osmium, and rhenium with the fcc platinum metals should solidify peritectically in their two-phase regions. The metallographic examination of natural osmiridium alloys has been said4 to indicate, by the presence of a martensitic structure, the existence of a transformation or a phase separation. On the basis of superconducting transition temperature measurements, a 70 at. pct 0s alloy was found5 to be two-phase prior to annealing. EXPERIMENTAL The elemental components used in this work were obtained from several suppliers as sponge. The purities, stated by each supplier to be in excess of 99.8 pct, were confirmed in each case by a semiquantitative spectrographic analysis. The pure components were premelted in an inert-gas tungsten arc furnace with the evolution of some fume, crushed, and pickled for use as alloy melting stock. Upon arc melting to the final compositions, no fume evolution was observed. Because weight losses of the order of 15 mg or less were observed in preparing alloy buttons weighing 15 g, "synthetic analyses" were used in determining the compositions of the alloys. Alloys used in this investigation contained 15, 20, 33, 40, 42, 43, 45, 50, 55, 60, 63, 64, 66, 70, 79, and 80 wt pct 0s. Heat treatments of the alloy buttons and pieces thereof were performed in a previously described6 tungsten tube furnace under pressures of 105 torr or less. It was found that homogenization treatments on the specimens were essential to remove the severe coring which was present, a 3-hr treatment above 2300°C removing all the metallographi-cally visible evidence of coring. Following the various heat treatments, the specimens were "vacuum-quenched" by melting a tungsten fuse wire and allowing them to drop onto a water-cooled copper plate. In a few instances, specimens were quenched into molten tin for comparison, but no difference was apparent. Vacuum-quenched specimens cooled from 2400°C to below a red heat in less than 60 sec. Typical equilibration times varied from 3 hr above 2300°C to 88 hr near 1100°C. The utilization of successively longer equilibration times and the approach to equilibrium from both directions indicated that the times used were sufficient to give a close approach to true equilibrium. Heat-treatment temperatures were measured with a calibrated Leeds and Northrup optical pyrometer through a 0.120-in. lateral sight hole in the tungsten heater tube. It was known that the assumption of black-body conditions inside the 1-in.-diam by 10-in.-long tube was unwarranted. The empirical results of work with thermocouples and melting

Jan 1, 1964

By E. W. Murbach

The oxidation of uranium carbide by oxygen at various pressures, and by air, has been investigated at temperatures up to 600°C. Arc-melted and cast uranium carbide displays oxidation behavior that appears to be dependent on its treatment after melting. ccReactive" uranium carbide, which results from exposure of freshly melted material to laboratory air, ignites in oxygen at about 275° to 350°C depending on pressure, and in air at about 350°C. The product of the initial oxidation appears to be UO2+.. Continued heating produces U30,. The initial oxidation rate is poportional, roughly, to the square root of the oxygen pressure. The activation energy determined for the initial oxidation reaction is 7.1 kcal, from 400° to 600°C in 10 mm of oxygen. AN investigation of low-decontamination methods for reprocessing uranium carbide reactor fuels is being carried out at Atomics International. One of the reprocessing cycles includes oxidation of the fuel at relatively low temperature (300° to 500°C) and reaction of the product oxide with carbon at elevated temperatures (above 1500°C) to produce uranium carbide. A number of small-scale experiments have been carried out in which uranium carbide was oxidized in air and oxygen at various pressures to measure reaction rates and to obtain other information concerning the oxidation process. In initial experiments with arc-melted UC, ignition was observed at about 275°C in oxygen or 350°C in air. However, similar experiments by Neymark&apos; at 426°C in air showed no ignition. It was soon determined that the difference in oxidation behavior was due to the treatment of the UC following arc-melting. Neymark&apos;s experiments were carried out with freshly melted UC while those reported in the

Jan 1, 1963

By S. T. Wlodek

The scale md subscale reaction products were identified and their rates of formation were studied in air over the range 1600" to 2000°F (871 " to 1149°C) for periods of up to 400 hr and for hoth the solution-annealed and aged conditions. The effect of prior sltrface preparation on suhscale oxidation was also studied The general oxidation behavior of both Ni-Cr-Mo-Al-Ti type alloys was similar. A surface film of a, Al2O3, forms immediately on exposure Subsequent oxidation continued at a linear rate (QL = 55 * 5 kcal per mole) as colonies of Cr2O3 nucleated at the A12O3/gas interface Further oxidation proceeded at a paraholic rate zvhiclz could he fitted to two successive rate constants. During paraholic oxidation, and depending on temperature, the scale consisted of Cr2O3, NiCr2O4 , and TiO2 with traces of NiO. In the case of Rene 41, the activation energy of both paraholic processes was 66 * 3 kcal per mole suggesting that diffusion of cations tlzrozrgh Cr2O3 was the rate -determining process. An unusual decrease in the oxidation of Udimet 700 at 1900°F where a spinel of Ni(A1,Crh0, zuas the predominant reaction product prevented the accurate assignment of activation energies for this composition. In both alloys internal oxidation of Al2O3 commenced shortly after parabolic scaling was observed. Prolonged exposure prod7tced intemal oxidation of TiN, and in Udimet 700 a complex Mo-Ni nitride was also found. At 1900oF, the subscale reactions in Udimet 700 undergo an inversion which parallels the decrease in surface oxidation; internal oxidation ceases hut is replaced by the formation of "spherodized" 3.&apos; colonies. Surface-preparation techniqtles which introduce appreciable working, such as coarse surface grinding or grit blasting. increase the amount of alloy depletion and internal oxidation in Reni 41. The reverse is true of Udimet 700 for which electropolished or mechanically polished specimens show much more subscale oxidation than strongly worked stirfaces. The strongest commercial nickel-base alloys presently available are generic to the Ni-Cr-Mo-A1-Ti base which exploits the precipitation of Ni3(A1,Ti) as the main strengthening mechanism, while relying on solid-solution strengthening by molybdenum and chromium reinforced by the pre- cipitation of carbides to attain maximum properties. This study characterizes the oxidation behavior of Rene 41, the strongest alloy of the Ni-Cr-A1-Ti type commercially available in sheet form, and Udimet 700, whose higher aluminum and titanium content allows it to exhibit one of the more attractive combinations of high-temperature properties available in a wrought product. The scaling processes of complex, type nickel-base alloys have received relatively little attention. Malamand and vidal as well as Poulignier et al.2&apos;3 have determined the composition gradients across the metal/oxide interface produced by high-temperature oxidation and considered the effect of surface perature, Limited weight-gain data has also been published by Fere 5 for alloys of this type and Radavich6 has identified the reaction products on Udimet 500 and Inco 702 after oxidation at 1832°F. Reference can, of course, be made to the excellent reviews of Kubaschewski and Hopkins7 or Ignatov and Shamgunova8 for a summary of the data available on the oxidation of binary and ternary alloy systems which are related to the more complex alloys considered here. EXPERIMENTAL The analyses of the different commercial heats studied are given in Table I. Using the experimental procedures previously established,9 continuous weight-gain data were obtained on both heats of Rene 41 sheet (A and B) and 150-mil-thick slices of cast Udimet 700. Subscale oxidation reactions were followed by static exposure of cylindrical specimens obtained from swaged Rene 41 (Heat C) and Udimet 700 (Heats E and F). In brief, continuous weight-gain tests were performed on specimens with a surface area of 10 to 12 sq cm. These were abraded through 600 grit Sic paper, electropolished to 2p rms in an electrolyte of 10 pct H2So4 in ethanol, and lightly etched in 10 pct HCl in ethanol before final washing and rinsing in ethanol. All continuous weight-gain data were obtained in dried (-70°F dew point) flowing (1 liter per min) air to an accuracy of +0.1 mg. Subscale oxidation processes were followed by the metallographic examination of 0.5-in-diam by 1.0-in.-long specimens. After an initial center-less grinding, various additional surface treatments were employed to determine the effect of surface preparation on subscale oxidation processes. Before exposure in zirconia crucibles, all samples were lightly etched in 10 pct HCl-ethanol, washed in ethanol, and dried. The depth of internal oxidation was measured to ±0.00025 in. on unetched specimens mounted so as to provide a taper mag-

Jan 1, 1964

By C. G. Rhodes, D. Kramer

The kinetics of precipitation of transient a phase during the transformation in U-16 wt pct Mo between 400° and 550°C were studied using quantitative metallography and electrica1 resistiuity measurements. The volume percent of a phase goes through a maximum in time, corresponding to a critical degree of progress of y&apos; formation. prior to its re-solution after prolonged annealing. The fastest rate of a precipitation oc-cuvs at 500°C with a concomittant lowest peak of 9.5 vol pct a. At 450°C, 14 vol pct a, greatest fov any temperature, was observed after 24 hr witlz an associated slowest rate of formation. a precipitation at 400°C ceases after approximately 160 hr and the amount of a present remains unchanged after long times at temperature; no y&apos; was observed metallographically at this temperature. IN the U-Mo system at 16 wt pct Mo, an ordering reaction takes place below 600°C, see Fig. 1, whereupon the random bcc solid solution, y, transforms to the ordered bct phase, y&apos;."2 The new unit cell is constructed of three old unit cells somewhat distorted. While attempting to study the kinetics of this transformation it was observed that an unexpected phase was precipitating out early during the transformation anneal reaching appreciable amounts before disappearing after long times. The y&apos; appeared in the presence of this new phase and after long times constituted the whole sample. Owing to the high optical activity of this unexpected phase under polarized light, it was suspected to be the a phase. Subsequent X-ray powder pictures confirmed this belief. The kinetics of a phase formation and disappearance is the subject of this paper. EXPERIMENTAL PROCEDURE A) Alloy Preparation. Alloys for this study were prepared by vacuum induction melting normal reactor grade uranium and 99.5 wt pct Mo pellets in thoria crucibles. Two ingots were prepared, and sections of the top and bottom of each ingot were chemically analyzed for uranium and molybdenum content. The results of the analyses appear in Table I. B) Metallography. Samples of 16M were wrapped in tantalum foil, sealed in evacuated (5 X 10"6 mm of Hg) quartz capisules, and annealed at 1110"C prior to being transferred directly to the transformation temperature. They were examined metallographically after increasing times to determine the progress of the transformation at 400°, 450°, 500°, and 550°C. The samples were prepared for metallographic examination by mechanical polishing with diamond paste and electrolytic polishing with a solution of glacial acetic acid and chromic acid. Since the y&apos; phase is tetragonal, its presence can be detected by viewing the sample in polarized light. To increase the contrast between y&apos; plates, the samples were electro-etched in a 10 pct oxalic acid solution. To reveal a phase in bright field (it can be seen in polarized light in the "as-polished" state), the samples were electro-etched in a solution of citric acid and nitric acid. To determine the vol pct a phase, a variation of the one dimensional systematic point count method as described by Hilliard and cahn3 was used. The

Jan 1, 1962

By T. Vasilos, J. T. Smith

THE mechanism of pressure sintering, or hot pressing, for ceramic materials, has been investigated by several researchers.1-8 Plastic flow has been suggested as the rate-determining mech-anism1,2 while grain boundary sliding3,4 and fragmentation processess have been found controlling in other studies. Vasilos and Spriggs5,6 have reported that pressure sintering occurs by a diffusion-controlled mechanism. For the pressure sintering of metals, investigations with lead7 and with tin6 have not identified the operative mechanism during consolidation of these powders. This note reports the results of a pressure sintering study initiated to determine the mechanism controlling the densification of spherical copper powder. Temperatures of 300°, 400°, 500°, and 600°C at 2500, 5000, 7500, and 10,000 psi pressures were investigated. The copper powder for this study was obtained from Metals Disintegrating Co., Elizabeth, N.J. The minimum purity was reported to be 99.9 pct. The powder size was -325 mesh and a lineal analysis showed the average size to be less than 1 p. An alumina die body and punches were employed. Graphite spacers were placed between the copper powder and the punches before pressing. It was expected that the graphite would form carbon monoxide with any entrapped air and form a reducing atmosphere within the die cavity. This condition was generally realized during pressing although a minor amount of oxidation occurred at 500" and 600°C. The oxide particles were located randomly in the pressed samples and were not considered to influence the densification process. Calibration tests showed the temperature of the copper pellet to be about 20°C less than the die wall temperature, probably resulting from heat losses through the punches. This difference was compensated during the experimental pressing operations. The hot pressing equipment employed for this work has been described by Spriggs et a1.9 and was calibrated with a Baldwin-Lima-Hamilton load cell. Travel of the punches was monitored with a dial indicator showing increments of travel to 0.0005 in. Relative density was calculated at selected time intervals for a known copper weight, punch travel, and die diameter. The accuracy of this calculation was *1 pct. Average grain size after hot pressing was obtained by lineal analysis. Typical densification curves are presented in Fig. 1 and Fig. 2 where relative density is plotted vs log time as a function of applied pressure for the 300" and 600°C pressure sintering temperatures, respectively. The curves for 400" and 500°C were similar to those at 300°C and consequently are not shown. The curves at 300°C as well as 400" and 500°C do not show an end-point or limiting density for a particular applied pressure. At 600°C, a density in excess of 95 pct of theoretical has been reached such that further densification is extremely slow for the 5000, 7500, and 10,000 psi pressures. It is suggested that further densification at these pressure levels may be retarded or prevented by discontinuous grain growth, by entrapped gases, and by other microstructural limitations as described by Cob1e.10 The curve for 2500 psi hot pressing pressure is a straight line over the time interval although a slight change in slope may be occurring at the last time intervals. The plastic flow models,1,2 derived for hot pressing, predict the existence of an end-point (or limiting) density dependent on the yield point of the material at the temperature of interest. The yield stress of copper at a 0.005 strain level has been

Jan 1, 1965

By K. E. Nelson

The effect of thorium and zinc variations on the strength and 100-hr creep characteristics of Mg-Th-Zn-Zr alloys was investigated. Optimum resistance to creep at 650° and 700°F are attainable within a certain range of thorium and zinc contents. This range does not conform to that which develops maximum tensile properties. RAPID advances have been made during the last few years in the development of magnesium alloys for elevated temperature applications demanding high resistance to creep. The beneficial effect of rare-earth metals on the creep resistance of magnesium alloys has been emphasized by a number of publications1-13 and such alloys are now in commercial production. The use of thorium as an alloying ingredient in magnesium was mentioned by McDonald and also in two Alien Property Custodian patent applications.10,17 The initial observation of Sauerwald that thorium contributes still higher creep resistance to magnesium than is attainable with rare-earth metals has recently been substantiated.&apos;" " In fact, it has been demonstrated that the useful temperature range of magnesium alloys is appreciably extended by the use of thorium. In all cases, it was observed that zirconium must be included in the alloys in order to render them fine grained and more readily castable. Several recent publications:2-27 indicate that a still further improvement in creep resistance and a further extension of the useful temperature range can be realized by the addition of zinc to alloys. The primary purpose of this paper is to present the results of a comprehensive study of the effect of zinc on the strength and creep characteristics of Mg-Th-Zr alloys. Compositions covering the range of thorium content from M to 6 pct and zinc content from 0 to 5 pct have been investigated. The creep characteristics at 650" and 700°F reported in this paper are based on results of tests of 100-hr duration. It is appreciated that creep tests of 100-hr duration might not yield adequate data for design purposes for parts with much longer expected life. However, for the purposes of the present discussion, it is felt that the combination of stresses and temperatures used in the 100-hr creep tests have yielded a clear representation of the compositional variation of creep resistance at the temperatures investigated. Creep tests of 1000-hr duration are now in progress on a few of the most promising alloys. Preparation and Testing of Alloys The alloys studied in this intensive investigation were prepared in 25 lb capacity mild steel crucibles. The thorium, zinc, and zirconium were alloyed and poured as described in earlier publications The thorium was introduced into the melt in the form of a Mg-Th hardener," the zinc added in the metallic form, and the zirconium alloyed in the form of the commercial hardener containing magnesium and 30 to 50 pct Zr.10, 26 Fluxing practices for melting and refining were the same as for magnesium-rare-earth metal-zirconium alloys. The melts were sampled for analytical determinations and poured into separately cast 1/2 in. diameter standard tensile bars. The test bars were given a precipitation treatment of 16 hr at 600°F in laboratory furnaces. It has been shown by other tests that a high temperature solution treatment followed by an aging treatment is unnecessary for the development of optimum properties in Mg-Th-Zn-Zr alloys. The selection of 600°F as the aging temperature was based on an attempt to achieve metallurgical stability without coalescence of the undissolved phases and the attendant loss in strength. The thorium, zinc, and zirconium contents of each melt were determined chemically. The zirconium contents are reported in two parts, "soluble" and "insoluble," referring, respectively, to the portions present in the alloy which are soluble and insoluble in dilute HCl acid. Distinction is being made between these two components of the zirconium content in the alloys because it has been found that only that portion of the zirconium content which is soluble in dilute inorganic acids affects the structure and properties of the alloys. The usual impurities consisting of copper, iron, manganese, and nickel were determined spectroscopically. The analysis for each melt is listed in Table I. A description of the methods of tension and creep testing has been detailed in earlier papers. The tests were performed with the cast skin re-

Jan 1, 1954

By A. K. Mukherjee, John E. Dorn

The effects of strain rate and temperature on the critical resolved shear stress for (321)[111] slip were determined for the silver-rich CsCl type of intermetallic compound AgMg. The flow stress increased only slightly as the test temperature was first decreased below room temperature; a rapid increase in the flow stress was obtained with yet further decrease in temperature from about 250&apos; to 4OK. The effect of both the temperature and strain rate on the flow stress over the low-temperature range could be rationalized satisfactorily in terms of the Peiwls mechanism when the deformation was controlled by rate of nucleation of pairs of kinks. IN spite of the well-documented interest of metallurgists and engineers concerning the mechanical behavior of intermediate phases and intermetallic compounds, very little definitive information is available on this important subject. As recently summarized by westbrook,1 only limited and modest progress has been made thus far in elucidating the details of the mechanism of plastic deformation for the intermetallic compounds; the available information largely concerns phenom-enological descriptions of empirical observations and experimental facts, principally with reference to poly crystalline aggregates. The present report on the elucidation of the rate-controlling mechanism for slip in the bcc structure of AgMg is part of the comprehensive program of a systematic investigation on the mechanical behavior of intermetallic compounds. The intermetallic compound AgMg has a CsCl type of lattice structureZ and is completely ordered up to its melting point of 820c3 This material was selected for our present investigation because of its simple crystal structure, moderate and congruent melting point, ordered structure persisting up to the melting point, and some solubilities of the constituent elements, which could be expected to help in the growing of single-crystal specimens. Whereas previous investigations on the properties of AgMg include hardness,*"6 slip systems,7 tensile flow stress of polycrystalline specimens,&apos; and electrical resistivity,4 the current investigation will be directed principally at elucidating the rate-controlling dislocation mechanism responsible for slip in single crystals at low temperatures. It will be shown that the strain rate is consistent with a model involving the rate of nucleation of pairs of kinks by the Peierls mechanism for plastic deformation. EXPERIMENTAL TECHNIQUES Single-crystal specimens of the AgMg intermetallic compound were prepared and tested as follows: 1) A master alloy ingot of AgMg was produced by melting and chill casting the high-purity silver (99.995 wt pct) and high-purity magnesium (99.997 wt pct) in an induction furnace under a helium atmosphere. 2) Sections of the above-mentioned ingot were placed in a graphite mold containing a spherical cavity in which a single-crystal sphere of 1 in. diam was grown under helium by the Bridgman technique. 3) The operative slip systems were investigated at room temperature on a singlecrystal of AgMg, from measurements of the angles made by the slip traces on the two surfaces of the specimen, which were at 90 deg to each other. The investigation confirmed that the AgMg compound undergoes slip primarily in the (321) plane and in the [Ill] direction, but a small amount of secondary slip was also noticed in the (112) (111) system. No slip was observed in the (110) planes. 4) The single-crystal sphere, mentioned earlier, was oriented in a graphite mold containing a cylindrical cavity of 3/8 in. diam above the spherical receptable to give the angle xo = 45 deg between the axis of the cylindrical bar and the normal to the slip plane (321), and the angle AO = 45 deg between the slip direction [Ill] and the axis of the bar. Oriented single-crystal bar seeds were produced by melting, under a helium atmosphere, a polycrystalline bar in the cylindrical cavity above the oriented spherical seed and by growing an oriented single-crystal bar from the seed. 5) Finally, oriented single-crystal specimens were grown from these cylindrical seeds. 6) The cylindrical specimens were machined in a High-Tension Spark Cutting unit to give a 2-in. gage length. The spark-machined gage section was elec-tropolished in a bath containing 200 ml of H3PO4,

Jan 1, 1964

By Allan T. Gwathmey, J. Bruce Wagner, Kenneth R. Lawless

Between 250°and 550°C in oxygen pressures of 10 to 760 mm Hg, the relative oxide thicknesses formed per unit time on the (100), (111), (110), and (320), decreased in this order. The predominant oxide orientation was (001)Fe3O4 and [110] Fe304 A small amount of a-Fe2O3 which exhibited a fiber pattern was observed in all oxides except those formed at 250°c in low oxygen pressures. IN order to understand the properties and behavior of thin films, particularly their role in oxidation reactions, there is needed more experimental information on their structure, composition, and kinetics of formation on clean surfaces of known geometry. The present study was undertaken to obtain such information for thin oxide films formed on single crystals of a body centered cubic metal, iron. Crystals in the form of spheres were used in order to expose all possible crystal planes to the reactant gases simultaneously. Using this procedure the relative rates of oxidation of all planes could be estimated, and those exhibiting, maximum or minimum oxidation rates could be selected for a more intensive study of composition and expitaxy. Since the three types of information were obtained from the same experiment using a single crystal substrate, any differences between rate, composition, and expitaxy on the several planes may be attributed to the influence of the substrate structure. EXPERIMENTAL The starting material for this study was Armco iron rods, 6 in. long and 3/8 or 1/2 in. in diam. The analysis was reported to be 99.8 pct Fe, with major impurities listed as carbon 0.018 pct, manganese 0.027 pct, phosphorous 0.005 pct, sulfur 0.029 pct, silicon 0.005 pct, and copper 0.11 pct. These rods were cleaned with ether and heated in an atmosphere of moist hydrogen at 950°C for three days. The purpose of this treatment was to decarburize the iron and to provide a consistent, uniform grain size for the growth of single crystals. Crystals in the form of rods, up to 1/2 in. in diam and 2 in. long, were prepared by a method similar to that reported by Leidheiser and Buck.2 Spherical crystals, 3/8 and 1/2 in. in diam and having a handle about 1/4 in. in diam by 112 in. long, were machined from the single-crystal rods. After machining, each crystal was etched in aqueous nitric acid to remove the cold-worked metal at the surface. Before each experiment, the crystal was polished mechanically with metallographic papers through number 4/0, and electropolished in a perchloric acid-acetic anhydride mixture by the method of Jacquet and Rocquet.3 The crystal was washed in running distilled water for at least 5 min. The excess water was blotted with a soft paper tissue, and the crystal was placed in an all-glass reaction vessel (See Fig. 1). The crystal was heated at 550°C in hydrogen for at least 8 hr prior to the oxidation in order to reduce any surface oxides and to help relieve any stresses in the metal. For the structure and composition studies, flat faces were cut parallel to (loo), (111), and (110) planes on the iron crystal spheres. The orientation of these faces was checked by a back-reflection X-ray diffraction technique. The faces were within 2 deg of the desired orientation. The flat faces were treated as described above except that prior to electropolishing they were given an additional polish on metallographic felt saturated with twenty-minute levigated alumina. After the crystal was heated in hydrogen for at least 8 hr, the temperature was adjusted to the desired value, and the hydrogen was evacuated. Commercial oxygen which had been purified by successively passing through tubes containing magnesium perchlorate, Ascarite and magnesium perchlorate was admitted to the desired pressure as measured by a mercury manometer. A resistance-wound furnace surrounded the oxidation chamber, and a temperature controller maintained the temperature within ±3°C. The furnace was provided with a small window for observing the crystal. The changes in thickness of the oxide films were followed by observing the interference colors. The oxidation was allowed to proceed until the desired oxide thickness was attained on a given crystal plane. The experiment was terminated by evacuating the oxidation

Jan 1, 1962

By R. E. Cech

Metallographic observations on hydrogen-reduced nickel oxide crystals suggest that nucleation of nickel occurs at structural singularities in the oxide. The fully reduced structure contains micron-diameter, worm-like voids occupying 40 to 50 pct of the volume. The crystallographic orientation relationships between nickel oxide and nickel resulting from oxide reduction are recorded and discussed. THE process of reduction of oxide to metal is one of considerable complexity involving a chemical reduction reaction, mass transport of reducing agent to the point of reaction and of reaction product away from it, and finally a transformation whereby metal atoms released from the oxide rearrange to form a stable reduced phase. In addition, nucleation of the reduced phase affects the overall reaction kinetics. Thus far only the thermodynamic aspect of reduction has received the attention warranted by the importance of

Jan 1, 1960

By J. L. Lytton

The flow-stress recovery of high-purity aluminurn following a 10 pct tensile prestrain was studied in terms of a fractional flow-stress recovery parameter fr. The flow-stress recovery behavior was related to the dislocation arrangements using transmissiort electron rnicvoscopy. During recovery at 120° and 160°C, nearly stable strength levels were attained, the strength level for 120°C recovery being greater than that for 160°C. This stabilization of flow stress was related to the formation of meta-stable dislocation networks bounding nearly perfect cells. Both network formation and the annealing of dislocation loops were found to be recovery mechanisms, and the stronger metastable strength level joy 120°C recovery was related to a smaller average cell size. Analysis of the networks was consistent with the reaction of sets of dislocations with a/2 (110) Burgers vector to give product Burgers DURING isothermal annealing of cold-worked metals, a degree of softening occurs without re-crystallization, and the processes responsible for this change are termed recovery processes. During recovery annealing, the dislocations generated during cold work become rearranged into low-energy configurations, and as much as 50 pct of the stored energy is released."&apos; The relationship between this rearrangement of dislocations and mechanical behavior is of considerable importance, since the dislocation substructures formed during recovery provide a significant degree of low-temperature strength3j4 and can favorably alter the course of primary creep at high temperatures.4 The purpose of the present study was to relate the flow-stress recovery behavior of high-purity aluminum to the substructural modifications that occur. Electron transmission microscopy was therefore employed for direct observation of dislocation substructures at various stages of recovery following 10 pct prestrain. Several investigators5-&apos; have proposed that dislocations can become rearranged or lost during the preparation of thin foils. It was found early in the present study that the dislocation structures in the thicker regions of the foils changed in a systematic way during the course of recovery. Therefore, it is unlikely that substantial losses or rearrangements occurred during thinning. This point will be discussed in more detail later. The results of various investigators indicate that recovery processes in fcc metals can result in release of 50 pct or more of the total energy stored in the as-prestrained metal, this percentage decreasing with increasing prestrain.&apos; Alloying elements or impurities tend to increase this percentage. The release of stored energy of fcc metals during recovery appears to occur by 1) annealing of point defects if the deformation occurred at sufficiently low temperaturesg and 2) rearrangement of dislocations into low-energy Configurations.1,2In bcc metals, the annealing of dislocation loops has also been observed during recovery after prestrain,10-12 and it has been proposed that this is a recovery mechanism for unidirectionally strained fcc metals.&apos; The density of dislocations in bcc metals has not been observed to decrease appreciably during recovery,10 although the formation of regular dislocation networks has been observed. has shown that the formation of such networks can result in elimination of long-range stresses and can lead to significant release of stored energy without dislocation annihilation. It might thus be expected that network formation is a significant recovery mechanism in fcc metals, although extensive network formation has apparently not been reported in controlled recovery experiments. The formation of sub-boundaries in aluminum has been observed by various investigators13&apos;17 during recovery studies of aluminum, but the structure of these boundaries was not resolved. In this regard, it is significant to note that Bailey and Hirsch,&apos; using transmission electron microscopy, detected no network or sub-boundary formation during recovery of 99.99 pct Ag. Furthermore, Clarebrough et al.2 found no such rearrangements during recovery of copper. EXPERIMENTAL PROCEDURE The high-purity aluminum used in this investigation was obtained in the form of 0.125-in.-thick sheet. Spectrographic analysis revealed that the sheet was 99.995 pct A1 with the following weight-percent impurities: 0.001 Cu, 0.002 Fe, 0.001 Si, and 0.0004 Mg. The as-received sheet was in the heavily cold-rolled condition. The as-received sheet was cold-rolled at room temperature to 0.040-in.-thick sheet in the longitudinal direction, which was the original rolling

Jan 1, 1965