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By P. Niessen, S. J. Bercovici

RECENTLY Aust et al.&apos; proposed a model of non-equilibrium grain boundary segregation based on a vacancy gradient induced uphill diffusion process of solute to grain boundaries. According to their proposal, solute atoms which are attracted to vacancies would, during the cooling of a sample, migrate with vacancies toward grain boundaries (vacancy sinks) and thereby enhance the solute concentration in boundary regions. For solute atoms which are not attracted to vacancies no such boundary solute enrichment would be expected. These concepts were given experimental support by boundary and bulk mi-crohardness measurements of various thermally treated dilute zinc and lead alloys and also doped aluminum oxide. The underlying assumption in their work was that solute enrichment in boundary regions is indicated by higher microhardness values. From thermodynamic considerations1&apos;2 it appears that the solid-liquid solute distribution coefficient (K), defined as the concentration of solute in the solid to the concentration of solute in the liquid at equilibrium, indicates whether attractive or repulsive forces exist between vacancies and solute atoms. K < 1 indicates a solute-vacancy attractions, K > 1 indicates no, or a repulsive, vacancy-solute interaction. This note is to report on observations of different grain boundary etching phenomena in high purity zinc alloys. These phenomena appear to depend on whether a K < 1 or K > 1 solute is present. In experiments designed to measure directly the solute enrichment in grain boundary regions, samples of zone refined zinc with 0.1 at. pct solute additions were cooled from 380°C at a rate of 3°C per min. A surface layer of approximately 50 was then removed from the samples by chemical polishing. The samples&apos; surfaces were then protected by a chromating treatment such that in a subsequent etch only grain boundary regions were dissolved. The dissolved regions were approximately semicircular troughs, 10 µ in width. The grain boundaries were usually in the middle, i.e., at the bottom, of this trough. For zinc containing the K < 1 solutes cadmium and aluminum, the grain boundary was always indicated by a ridge as shown in Fig. 1. For pure zinc, and zinc containing the K > 1 solutes copper and gold, a groove at the bottom of the trough indicated the boundary position, Fig. 2., To test if these different grain boundary etching behaviors were possibly connected with the segregation process discussed above, the Zn-Cd alloy was again heated to 380°C and quenched into brine. After surface protection and etching it was found that this specimen no longer exhibited the grain boundary ridges but rather grain boundary grooves as shown in Fig. 2. It would appear, therefore, that the boundary ridge is a consequence of a process occurring during the slow cooling of the samples. From absorption spectrophotometric analysis it was found that for slowly cooled samples containing K < 1 solutes, the solute/zinc ratios of the material from the boundary trough were consistently considerably higher than the solute/zinc ratios of the bulk alloys. This boundary region solute enrichment was not observed in quenched samples. It is concluded therefore, that the boundary ridge shown in Fig. 1 is directly or indirectly connected with nonequilibrium solute segregation.

Jan 1, 1970

By T. R. A. Davey

A Survey of current and recent research and developmental work is supplemented by predictions for processes which should be developed over the remainder of this century.

Jan 1, 1970

By George W. King

The yield strength of a dispersion-hardened W-3.8 vol pct Tho,alloy, in both the recovered and recrys-tallized condition, was investigated and cornpared with that ofrecrystallized pure tungsten over the temperature range of 325" to 2400°C. It is deduced that the Orowan mechanism is obeyed in the recrystallized alloy. In the recovered alloy, a further enhancement of the yield strength results from the retained substructure which is stable up to temperatures in excess of 2700°C. Temperature and strain rate cycling tests were also performed, and the apparent activation energy for the deformation process was derived. This activation energy, - 3 ev, for the recovered and also the recrystallized alloy was about the same as that for re crystallized pure tungsten. However, the activation volume of the recovered alloy, -10-2 cu cm, was about an order of magnitude lower than that of the recrystallized alloy or pure tungsten. This fact accounts for an enhancement oj- the temperature dependence of the yield stress of the recovered alloy. A dislocation velocity exponent of about 4 to 13 was deduced frorn the strain rate cycling tests , which is in good agreement with values reported for tungsten single crystals. VARIOUS theories have been developed to explain the enhanced yield strength of a metal containing a dispersed second phase of small hard particles. These theories are thoroughly reviewed by Kelly and Nicholson.&apos; The theoretical models can be separated into two types. The first type assumes direct interactions between moving dislocations and dispersoids. One of the most widely investigated models for this mechanism is the bowing out of dislocations between the dis-persoids and their subsequent pinching off in order to bypass the obstacles. This is the well-known Orowan mechanism.&apos; The second type is an indirect effect of the dispersion because of its ability to stabilize to high temperatures the substructure introduced by cold working. In this instance, the increment in the yield strength is expected to be inversely proportional to the square root of the subgrain diameter. In the present work, a quantitative study was made of the strengthening effect caused by a thoria dispersion in a recrystallized W-3.8 vol pct Thoz alloy over the temperature range 325" to 2400°C. The results are compared with the increment predicted for the Orowan mechanism based on the calculations by ~shb~.~ In addition, the alloy was tested in the recovered state so that any additional strengthening resulting from the substructure produced during fabrication could be measured. The respective contributions can be separated in this manner, provided that the particle size distribution of the dispersion remains the same in both the work-hardened and the recrystallized state. Particle size distribution measurements showed that this condition was met in the present work. I) EXPERIMENTAL PROCEDURES A) Material Production and Fabrication. The alloy investigated is essentially the same as that reported much earlier by ~effries,~ who also found the strength of tungsten to be improved by the thoria dispersion. The procedure for producing the alloy consisted of mechanically blending a thorium nitrate solution in proper concentration with tungsten oxide (WO3) powder, followed by hydrogen reduction to metal powder. After reduction, the dispersed second phase is present as thoria (Thoz). The pure tungsten powder used for comparison was produced in the same manner except that the thoria doping step was omitted. The powders were consolidated by cold pressing and self-resistance sintering in hydrogen. The resulting ingot had a cross section about 0.6 sq in. and a density about 93 pct of theoretical. The ingot was swaged to 0.174-in.-diam rod at temperatures varying from 1650°C initially to -1200°C near final rod sizes. Two intermediate recrystallization anneals were employed during fabrication. Analysis of the swaged rods is reported in Table I. B) Electron Microscopy Techniques. Carbon extraction rrPxcas prepared by a technique reported by ~00&apos; were used to quantitatively evaluate the thoria particle size and distribution. Electron nlicrographs of extraction replicas were taken at 20,000 times but were then enlarged two to three times in printing. The areas photographed were randomly selected. A Zeiss Particle Size Analyzer (Model TGZ3) was used to count and measure the sizes of all particles present on the print. About three thousand particles were counted in determining a distribution curve. Electron transmission microscopy was used to determine the effect of annealing on the substructures of the materials. Thin foils were produced by a two-stage thinning process. The rods were first ground on emery paper to ribbons about 10 mils thick and then a jet of 5 pct KOH was used to electrolytically reduce a portion of the cross section of the ribbon. Final perforation was achieved by immersing the specimen in a 5 pct KOH solution and electrolytically polishing at a current density of about 0.3 amp cm-&apos;. The foils were examined with a Hitachi HU-11A electron microscope. C) Tensile Testing. Tensile testing was performed in an Instron Testing Machine equipped with a radiation-type vacuum furnace which operates at about 1O"S torr at temperatures as high as 2400 °C. The same furnace was used for annealing the tensile specimens.

Jan 1, 1970

By J. P. Batcha, J. Robert Denny

Since 1964. Newmont Mining Corp. has been engaged in a systematic research and development of computer techniques for a variety of mine planning applications. The general objective of this effort has been twofold: first, to arrive at a viable near-optimum plan for mining a particular orebody and, second, to decrease the financial investment by reducing the man-hours required for mine planning. Three major phases in the evolution of Newmont&apos;s computer techniques for mine planning are discernible. In phase one, the computer&apos;s ability to duplicate manual drafting and contour mapping was developed. Obviously, all recognized geologic characteristics had to be included, and consequently the development of computer techniques for the proper incorporation of structure, stratigraphic trends, and other geological features was a significant aspect of phase one.

Jan 1, 1970

By R. M. S. B. Horta, W. T. Roberts, D. V. Wilson

Evaluation of results obtained by the Harris method for inverse pole figures is discussed. Two existing analyses and a new approach are compared. In the most frequently used analysis, different reflections are accorded equal weight. A second method involves area-weighting of reflections, mainly to take account of nonuniformity of Pole distribution. In the new method, reflections are weighted according to their multiplicity factors. Intensity ratios obtained from a sample of steel sheet by the three methods are compared. INVERSE pole figures offer a convenient method of depicting the proportions of material with various orientations referred to a unique specimen axis. The technique was first applied to fiber textures, but it is now frequently used as a description of texture in sheet metal, the unique axis in this case usually being the sheet normal. The Harris method&apos; for the determination of inverse pole figures has the great merit of simplicity. It suffers certain intrinsic limitations, but provided that these are borne in mind, the results allow useful conclusions to be drawn regarding the effects of texture components on certain mechanical properties. Much thought has been given to alternative methods of texture description, aimed at eliminating the ambiguity in the simpler methods.2"6 Refinements in the method of description are obtained at the price of increasing complexity, and it seems clear that a simple method, such as that of Harris, will continue to find application. The original derivation by Harris1 has been corrected by Morris7 and later by Mueller, Chernock, and Beck.2 Since the latter reference is more accessible, it is referred to more frequently than the work of Morris. Most users of the inverse pole figure method present their results on the basis of the treatment by Mueller et al., and it is the purpose of the present communication to comment on this treatment and to suggest a simple modification to the method of presentation which enhances the meaningfulness of the results. It will be convenient first to summarize the Mueller analysis as follows: The intensity Ihkl of a hkl reflection from a textured specimen is: Ihkl=CI0AL\Fhkl\2NhklPhkl [1] where C is a constant for a given sample I, is the intensity of the incident beam A is an absorption factor. With usual diffrac-tometer geometry and a flat specimen, A is inversely proportional to the density of the specimen. L is the Lorenz polarization factor Fhkl is the structure factor for the hkl reflection Nhkl is the multiplicity factor phkl is the fraction of crystals in the polycrystal-line aggregate with any particular (nkl) plane parallel to the surface. The corresponding equation for a specimen with randomly oriented grains is lR,hkl=CRl°ARL\fnkl\2Nnklk [2] the subscripts R indicating the factors that are different for the random sample, which will, in general, have a density different from that of the textured one. The intensity ratio is hkl , c A Phkl [3] IR,hkl CR AR PR The constants are eliminated by summing over all the measured reflections ^iRMi °R AR PR ljPkkl and from Eqs. [3] and [4] T IR,hkl The only unknown in Eq. [5] is Yj phkl and before this can be evaluated, it is necessary to adopt some form of normalizing procedure. Mueller et al. assume that when a large number, n, of reflections is used, the average value of p as defined by Eq. [6] below will be unity ? = £j**l3l [6] and the final result of their analysis follows: hkl Pkkl = i I&Jf~ [7] ±y* Ihkl ^ in,hki The normalizing procedure used by Mueller et al. involves an unrealistic assumption since it gives equal weight to each of the hkl reflections. Other normalizing procedures can now be examined with a view to selecting a more appropriate one. For an infinite number of reflections, the function p can be averaged over a continuous range of orientations covering the complete solid angle 4p by the integral relation: p =1 jp(a)dQ = l [8] This is the only exact procedure, but in practice a

Jan 1, 1970

By G. R. Love, C. C. Koch

The changes in superconducting properties with aging time have been studied ,for the pecipitation reaction in a Tc-30 at. pct V alloy. Superconducting critical temperature, upper critical field, and relative critical current density were determined by ac susceptibility techniques. Aging produces changes in critical temperature of both matrix and precipitate which can be rationalized by compositional effects. maximum flux pinning (critical current density) occurs at a time during aging when subgrain boundaries are completely decorated with precipitates and the subgrain centers remain precipitate -free. The particular effectiveness as barriers to flux motion of planar defects which enclose regions of low deject density is discussed. THE precipitation of a second phase can dramatically modify the superconducting properties of type I1 super-conductors. According to Livingston and Schadler1 one might expect changes in the primary, secondary, and tertiary superconducting properties of the material. Changes in matrix chemistry caused by precipitation can alter the fundamental superconducting parameters; critical temperature, Tc, and thermody-namic critical field, Hc. The concimitant changes in electron mean free path (reflected in normal state resistivity) can affect the critical fields Hc 1, IIc2, Hc3. Finally, the presence of precipitate particles may hinder the motion of flux lines and may considerably improve the current-carrying capacity in high-field superconductors. The influence of precipitation on superconducting properties has been studied in a number of systems.2 Magnetization measurements have been used to study the influence of precipitates on flux pinning in lead-base alloys by Livingston3 and Evetts et al4 In these alloys precipitates induced magnetic hysteresis and flux trapping. The amount of hysteresis increased with the volume fraction of precipitate and decreased with coarsening of the precipitate. Jn an Al-Zn alloy5 and an A1-Ag alloy6 the initial precipitate size was presumably smaller than a coherence length and coarsening increased magnetic hysteresis5 and critical current density.6 The influence of precipitation on superconducting properties has also been studied in several of the commercially interesting Ti-Nb7-10 and zr-Nb11 alloys. The maximum in critical current density for these alloys was confined to a narrow range of either isothermal aging time" or isochronal aging temperature7 during the precipitation reaction. Thus, experimental evidence and theoretical considerations suggest there is an optimum precipitate size, spacing, and density, and a critical composition with respect to the matrix for flux pinning. What these "optimum" values might be and the relative importance of each is still not clear, although a few generalizations can be made. It is generally accepted1&apos; that particle sizes smaller than the coherence length or larger than the inter-flux line spacing are poor pinning centers. In high Hc2 materials, precipitate sizes for maximum values of critical current density lie in the range of 50 to 2000Å,9,7 and there are indications that increasing dissimilarity between precipitate and matrix produces increasing pinning force.13 Because of several interesting features of the aging reaction in a Tc-30 pct V alloy, we have chosen to study the influence of precipitation on the superconducting properties of this alloy. The physical metallurgy14 and a survey of the superconducting properties" of the Tc-V alloy system have been reported. The Tc-V phase diagram is presented in Fig. 1. At 1500°C the Tc-30 pct V alloy is in the single phase 6 field. Samples quenched from the 6-phase field have a CsCl structure X-ray diffraction pattern at room temperature and it has been proposed that the 6 structure is closely related to the bcc lattice.14 When held isothermally below the eutectoid temperature, 115O°C, the 6 phase decomposes into the CsCl and hcp phases.

Jan 1, 1970

By S. K. Tarby, A. E. Rathke

A series of 0.21 pci carbon steel melts was processed under conditions which sinzulated industrial vacuum degassing practices. The results indicated that the efliciency of carbon deoxidation was not significantly increased by vacuunz degassing at chamber pressures below 100 torr. The two common phenomena of vacuu?rz carbon deoxidation, i.e.,an unaccountable carbon loss and nonequilibrium deoxidation, were observed in this study. Oxygen from adsorbed and chenzically combined water of certain refractory structures was probably responsible for the unaccourttable carbon drop. The nonequzlibrium deoxida-tion phenomenon was adequalely correlated by a bubble nucleation )mechanism. Although the major limiting factor in oxygen removal from these melts contained in alumina crucibles could not be eslablished with certainty, there was some evidence that melt-refractory interactions were not the most imp-portant limiting factor. CONSIDERABLE attention has been given to the use of carbon in conjunction with vacuum degassing* as a deoxidation technique. An advantage of utilizing the reaction: for deoxidation purposes is that the reaction product is gaseous and hence can be effectively removed from the melt. The pressure dependency of Eq. [I] is illustrated by the expression for the thermodynamic equilibrium constant, K: where pco is the partial pressure of carbon monoxide, and hc and ho are, respectively, the Henrian activities of carbon and oxygen in molten steel. The thermodynamic aspects of the C-0 reaction in molten Fe-C-0 alloys have been investigated extensively. Theoretical predictions based on Eq. [2] indicate that, at the chamber pressures reached in most vacuum degassing units, carbon is the most effective deoxidizer that can be obtained. ~ornak&apos; has compared industrial values of carbon and oxygen contents with values calculated from theory, and has shown that on a commercial basis vacuum carbon deoxidation has not achieved the degree of success that is predicted from theoretical considerations of the C-0 reaction. The use of industrial units to determine the reason for this deviation is limited by economics and the difficulty in controlling critical process variables. Therefore laboratory-sized experiments in this area should yield valuable information. Investigations on vacuum carbon deoxidation have been made in experiments conducted under vacuum induction melting conditions where pressures in the low micron range, long treatment times, exposure to highly dynamic vacuum conditions, and relatively quiescent bath conditions have been maintained. Inve~ti~ators~~~ utilizing vacuum induction melting for the production of high-purity iron by carbon deoxidation have concluded that, under high vacuum conditions, melt-refractory interactions constantly supply oxygen to the melt. Thus, it has been suggested that refractory dissociation rather than the C-0 reaction establishes the lowest possible oxygen content of a melt. Thomas and Moreau4 and Bennett, Protheroe, and ward5 have studied carbon deoxidation of Fe-C alloys melted in magnesia crucibles under reduced pressures. The results of both studies differed considerably from those predicted by theory, and the limiting factor for lower oxygen contents was attributed to melt-refractory interactions. Because the refractory material used in both investigations was magnesia, no quantitative measure of crucible reaction could be made and the amount of carbon consumed during treatment was utilized as an indirect indication of the extent of crucible reaction. Studies concerned with the determination of the minimum oxygen content attainable in pure iron and Fe-C alloy material vacuum-induction-melted in various crucible materials have also been conducted."&apos; The suitability of a crucible refractory for use under vacuum conditions appears to depend upon the major refractory constituent, the amount and type of impurity oxides, and the composition of the melt. Meadowcroft and Elliott9 have presented a theoretical review of the type and extent of various refractory reactions which should be considered in vacuum refining. ~eadowcroft&apos;~ considered the vacuum degassing process to be dependent upon the "carbon boil" and has proposed that a part of the difference between the experimental and theoretical results for vacuum carbon deoxidation may be explained by the fact that the pco term in Eq. [2] is not the chamber pressure. Instead, the pressure necessary for carbon monoxide

Jan 1, 1970

By J. M. Davey

Lead-zinc sulphide ores at Mount Isa are currently treated at the rate of 180,000 long tons per 28 day period in the No. 2 Concentrator of Mount Isa Mines Limited. Prior to June 1966 lead-zinc ore was treated in part of the No. 1 Concentrator up to a rate of 70,000 long tons per period. Since 1955, two major changes in ore type being processed have occurred. Because of these changes, problems arising from treatment of the ore have altered and during the period several major changes in practice have been advocated and experimentally tested. Most of these flow sheets were developed with a view to overcoming one major problem in the ore. These were invariably abandoned as the Mount Isa lead-zinc ore contains a number of equally major problems all of which must be overcome in the treatment process. MINERALOGY The orebodies are situated in the Mount Isa Shale Group which is Proterozoic in age (Carpentarian System). The sediments consist dominantly of fine grained dolomitic, quartzo-feldspathic shales and siltstones. Specifically, the Mount Isa orebodies lie in the Urquhart shale formation which is characterised by sediments of high albite and orthoclase content denoting a large volcanic component. The Urquhart shales are approximately 3,500 feet thick and extend at least north and south of Mount Isa for 20 miles in each direction. In the area of the silver-lead-zinc orebodies the Urquhart shales are highly pyritic and have a relatively high carbon content. The

Jan 1, 1970

By Burt C. Mariacher

Two AIME sponsored symposia to be held during the year 1970 will examine copper, lead and zinc metallurgy in considerable depth. MBD and the Extractive Metallurgy Division of The Metallurgical Society will participate in both. Thus, the full field of minerals and metals processing including milling, smelting, and refining will be covered. Since these symposia hold special interest to MBD members, it was felt that a useful purpose could be served by devoting this column to a description of what has been arranged for the registrants.

Jan 1, 1970

By R. L. Stephenson

The effect of fabrication variables on the creep-rupture properties of TZM (Mo-0.5 pct Ti-0.08 pct Zr-0.03 pct C), Cb-TZM [columbium-modified TZM (7140-1.5 pct Nb-0.5 pct Ti-0.8 pct Zr-0.05 pct C)], and TZC (Mo-1.2 pct Ti-0.25 pct Zr-0.15 pct C) has been studied at 982º. 1093º, 1204º, and 1315°C for rupture times up to 1000 hr. The creep tests were performed in vacuum creep furnaces, employing cold-trapped oil-diffusion pumps, operating at pressures 2 X 10-7 tory. After-test chemical analyses showed no significant changes in interstitial content. The creep-rupture properties of TZM, fabricated according to current mill practice, were determined in the stress-relieved and in the re crystallized conditions to provide control data. Specimens of TZM, Cb-TZM, and TZC fabricated according to each of two experimental fabrication schedules were then tested. The schedules differed in terms of in-process annealing temperatures and warm -working temperatures. The data make several conclusions evident. Fabrication variables do indeed have a profound effect on the long-time creep-rupture properties of molybdenum alloys. Strengths of these alloys compare very favorably with those of other refractory metal alloys in the temperature range studied. FOR several years we have been engaged in the evaluation of the creep-rupture properties of promising refractory metal alloys. We consider the determination of these properties to 1000 hr at several temperatures necessary for a valid comparison. Such an evaluation indicated that the creep strengths of Mo-0.5 pct Ti and TZM (Mo-0.5 pct Ti-0.08 pct Zr-0.03 pct C) compare favorably with those of other refractory metal alloys. Tensile and recrystallization data of other investigators1,2 show an effect of fabrication variables. More specifically, those fabrication schedules which produce high strength through work hardening exhibit the least thermal stability. A similar conclusion was reported by perkins3 for Cb-TZM. This would lead one to expect that, in terms of creep, those materials showing higher strength at short times and low temperatures would exhibit lower strength at long times and high temperatures. If these expectations were fact, a substantial improvement could be made in these alloys by optimizing their fabrication schedule in terms of their anticipated service temperature. We therefore undertook a study of the effect of fabrication variables on the long-time creep properties of TZM, Cb-TZM (Mo-1.5 pct Cb-0.5 pct Ti-0.08 pct Zr-0.05pct C) and TZC (Mo-1.2 pct Ti-0.25 pct Zr-0.15 pct C). MATERIALS All materials used were supplied by the Climax Molybdenum Co. of Mich. Our original intention was to test the same heat of each alloy in different conditions. Fabrication difficulties prevented this; however, heats with nearly identical analysis were selected. The compositions of the materials used are listed in Table I. All materials were supplied in the

Jan 1, 1970

By J. R. Cahoon, H. W. Paxton

The possibility of using unidirectionally solidified, two-phase alloys as an approximation to fiber composite materials is investigated. The short-term me.chanical properties and failure modes of unidirectionully solidified A1 (rich)-Cu alloys containing ap -Proximately 0, 17.5, and 27.7 vol pct of 0 phase &apos;fibers" are determined at temperatures from 25" to 500" and compared with those obtained for conventionul SAP alloys. In a previous publication,&apos; hereafter referred to as I, the possibility of understanding some of the room-temperature mechanical properties of unidirectionally solidified castings was explored. For Al(rich)-Cu and Al(rich)-Mg two-phase alloys over a substantial range of compositions, the yield and ultimate strengths and common ductility measures were very adequately predicted from the principles of fiber strengthening4 and the analysis of ductility outlined by Gurland and Plateau." The results obtained in I suggest the possibility of using unidirectionally solidified, two-phase alloys to simulate fiber composite materials where the inter-dendritic second phase or constituent acts as the reinforcing material. Recent attempts concerning the fabrication of fiber conlposites have concentrated on producing composites with a good bond between fiber and matrix and with very long fibers so that their maximum contribution to the strength of the composite may be realized. However, these objectives are difficult to attain in practice and present fabrication processes are either extremely laborious or costly.13 The slow, unidirectional solidification of eutectics has received considerable attention as a method for producing composite materials. 5,6 This method can fulfill both of the above objectives but it is currently laborious, expensive, and has the additional disadvantage that the volume fraction of reinforcing phase cannot be easily varied. On the other hand, unidirectionally solidified, two-phase alloys, also with a good bond between the phases, are relatively easy to make and the volume fraction of reinforcing "fibers" can be easily varied by changing the average composition of the alloy. The disadvantage of the cast alloys is that the mechanical effectiveness of the "elongated interdendritic reinforcements" (EIR)* may be reduced due to their rela- tively short lengths, the w factor in Eq. [2] of I. However, if the EIR have a high strength their contribution can be considerable. For composite materials containing discontinuous cylindrical fibers of various lengths the ultimate strength is given by1 where it is assumed that the composite fractures when the fibers fail. In Eq. [I], a, is the stress in the matrix just prior to failure of the composite, Vf is the total volume fraction of fiber reinforcing constituent, Vf(l+) is the volume fraction of fibers whose lengths exceed the critical length, I,, which is defined as the shortest length of fiber in which the stress can build up sufficiently to break the fiber. af is the fracture strength of the fiber material, w is a factor accounting for the discontinuity of those fibers whose lengths exceed I,, 1-/d is the average aspect ratio of those fibers whose lengths are shorter than I,, and t is the shear stress in the matrix at the fiber-matrix interface. The factor w is dependent on the length of the fibers and also on whether deformation of the matrix occurs plastically or elastically. However, for a given length of fiber, w is smaller when elastic deformation of the matrix is assumed.&apos; It is of interest to consider the properties of simple unidirectionally solidified, two-phase alloys at elevated temperatures in view of the possibility of using suitable modifications for high temperature service. Knowledge of the creep behavior of these materials is still rudimentary (although under active investigation) and the present paper concerns itself with short time tensile properties of some alloys similar to those investigated in I (i.e., unidirectionally solidified Al(rich)-Cu alloys). Unidirectionally solidified alloys containing 5.6, 17, and 23 wt pct Cu were tested parallel to the direction of solidification at temperatures from 25" to 500°C. In the present investigation, the alloys were homogenized for 2 days at 535°C giving a matrix of homogeneous a phase (5.2 wt pct Cu) and an interdendritic constituent (EIR) which was completely Q phase (53 wt pct Cu). EXPERIMENTAL Alloys of nominal composition 5.6, 17, and 23 wt pct Cu (containing approximately 0, 17.5, and 27.7 vol pct 8 phase, respectively, after homogenization at 535°C) were prepared by melting 1200 g of A1 (99.99 pct) in a high purity graphite crucible and adding the appropriate amount of freshly cleaned copper chips (99.9 pct). The molten alloy (at 700°C) was poured into a preheated graphite mold (also at 700°C) and the ingot unidirectionally solidified by impinging water on the steel baseplate of the mold. The alloy was degassed immediately

Jan 1, 1970

By George C. Coupland

Ecstall Mining Limited, a wholly owned subsidiary of Texas Gulf Sulphur Company, is the owner and operator of the Kidd Creek Mine including the concentrator complex located near Timmins, Ontario. Canada, approximately 450 miles north of Toronto. The mine, concentrator and Timmins form a triangular arrangement with a 17-mile rail link connecting the mine and concentrator and both of these facilities 18 and 14 miles respectively by road from Timmins. A core drilling program in the spring of 1964 established the presence of a large massive sulphide orebody which was to become the Kidd Creek Mine. Texas Gulf Sulphur had been conducting an intensive search for base metal in various parts of Northern Ontario and Quebec since 1957. Of several thousand anomalies detected in airborne electromagnetic surveys, several hundred warranted ground inspection, but only one of more than sixty drilled became a commercial orebody, the Kidd Creek Mine. The geophysical exploration work has been well covered in a paper written and presented by Van Donohoo, presently a Vice-President of T.G.S., at the American Mining Congress in San Francisco in October 1969. GEOLOGY The orebody lies within a series of overturned rhyolitic flows and pyroelastics with a major peridotite intrusive to the east. The hangingwall and footwall are composed chiefly of intermediate volcanics, andesite and dacite. The southern end of the orebody appears to terminate abruptly against greywacke while the north end is bifurcated and the structure obscured.

Jan 1, 1970

By R. B. Schluter, M. M. Fine

Development of a process for winning copper from pelletized chalcocite concentrate is underway at the Bureau of Mines, Twin Cities Metallurgy Research Center. The new route from concentrate to metal by which the Bureau seeks to eliminate matte smelting and converting includes a two-stage fluid bed treatment. In the first stage, pelletized concentrate containing 32%Cu and 7% S is first desulfurized to less than 1.0% S in an oxidizing atmosphere. In the second stage, the calcine is metallized by reduction with hydrogen. Thereafter, the reduced product plus 10% CaO is routed to a smelting furnace which separates metallic copper from the gangue. Recovery and Cu content at this point are in the 97-98% range. This product must be refined to remove sulfur and iron so the metal is suitable for making wirebar copper. An important feature of the process is fine concentrate pelletization prior to fluid-bed treatment. This permits a shorter reaction time, a decrease in dusting and easier subsequent processing. In a broad sense, sulfide copper pyrometallurgy is a batch sequence in three separate vessels, i.e., a reverberatory furnace to yield matte copper, a converter to produce blister copper and another reverberatory furnace to produce fire-refined copper. Matte-smelting has remained relatively unchanged since it became a universal practice some 50 to 60 years ago. It is now serving a wide range of smelter feed materials, but many concentrates are not immediately amenable to the process. There are abundant copper resources which lack sufficient sulfur and other elements lo sustain the full chemistry involved in matte-smelting. This necessitates adding sulfur to make the product fit the process, and usually none of the sulfur is recovered. From the standpoint of pollution alone, the development of a smelting technique for low-sulfur concentrates not requiring the addition of sulfur would be a significant gain.

Jan 1, 1970

By E. I. Gordon

The electronic pickup tube is the image-to-video signal-converter or transducer in tele vision-like systems. Images may relate to visible light or IR excitation as in conventional TV systems, X-ray excitation as in some medical and production control applications, or electron excitation as in electron microscopy. The latter process is also important in some forms of light or X-ray sensitive pickup tubes as an intermediate step. In virtually all of these devices the image ends up as a stored charge pattern on a suitable target electrode and the video signal is created by periodically scanning the target with a low energy electron beam and removing the stored charge. In a major group of tubes radiation induced conductivity creates the charge pattern. In others, photoemission is used. In this paper an attempt is made to illuminate some of the device requirements placed on materials exhibiting radiation induced conductivity, some of the materials and techniques that are used, and the problems. The emphasis will be on visible light and IR sensitive targets although some attention will be given to X-ray and electron imaging. Photoconducting films as well as diode arrays will be discussed. ELECTRONIC pickup tubes find their greatest use in commercial, entertainment television, and in industrial and educational closed-circuit television. Video telephone systems, such as AT&T&apos;s PICTURE-PHONE System will become eventually the greatest user. Military use is also very important. Nevertheless the use of electronic pickup tubes in technology, science, and medicine is assuming ever greater relevance and demands the greatest diversity and perfection in the pickup tube art. Commercial television and closed-circuit television use requires visible light response, high resolution, low lag, and uniform response. Video telephone use requires the same plus extreme reliability, stability, and low cost. Military use emphasizes, in addition, sensitivity, IR response, and ruggedness. (Devices for far IR response will not be considered here.) The use of pickup tubes in medicine and biology emphasizes UV response for microscopy, X-ray response for radiology, and energetic electron response for electron microscopy. Astronomy and nuclear physics demands low light level response, storage ability, and resolution (here the tube is a successful replacement for film). The interested reader might profitably read Advances in Electronics and Electron Physics, vol. 12,&apos; 16,2 and 22A3 and 22B4 for detailed discussion of the use, properties, and technology of electronic pickup tubes. In general, because of the importance of these uses, none of the above properties will be ignored. Nevertheless attention will be restricted to only those imaging devices, called pickup tubes, using a scanning electron beam to dissect the image with a resulting video signal for conventional CRT display. However pickup tubes have become so complex that many of them include components such as image in-tensifiers which would be normally excluded by this restriction. Thus some of the other imaging devices will not be ignored entirely. We will first review the fundamental elements and physical phenomena involved in modern electronic pickup tubes, then the relevant materials and some of the material problems and then an interesting goal yet to be achieved. REVIEW OF PICKUP TUBE PRINCIPLES In all modern television systems using pickup tubes there is an interval called the frame interval, during which the incoming radiation flux is allowed to produce a cumulative effect in the form of a stored charge pattern which is a replica of the radiation image, and a scan interval during which the stored charge pattern is converted into a video signal. The frame interval bears no fixed relation to the scan interval and may be shorter or longer. In conventional, real time television the scan interval including retrace is identical to the frame interval. Integration and storage is the key to the sensitivity of modern pickup tubes, in contrast to earlier tubes such as the image dissector. At equivalent light levels and without integration, the number of photons contributing to the video signal in the image dissector is lower by a factor approximating the number of picture elements in the displayed image, a number of order 10. Statistical fluctuations in the number of contributing photons represent a serious limitation to the attainable signal to noise ratio, resolution and contrast. As a result considerably greater light levels have to be used then in targets which integrate over the full frame period. Thus the crucial elements, common to all modern pickup tubes, are the charge storage surface and the scanning electron beam which is incident on the charge storage surface at very low energy. These are shown in Fig. 1(a). The charge storage insulator is generally very thin with a thickness of several microns or less. The surface of the insulator is held near cathode potential. The backplate potential is held at cathode potential or at a small positive voltage relative to cathode. The combination of storage insulator and backplate electrode is commonly called the "target". In the absence of incident radiation flux the electron beam scans over the storage surface depositing negative charge uniformly over the scanned part of the surface by virtue of the fact that the effective secondary

Jan 1, 1970

By J. Winter, W. C. Setzer, A. J. Goldman

ANISOTROPY in cold worked tempers of commercial aluminum alloys is manifested in deep drawn products as protuberances or ears 45 deg to the rolling direction. This reflects the {123}(412) rolling texture.&apos; In fully annealed material, 0 to 90 deg ears in and per-

Jan 1, 1970

By R. M. Rose, K. A. Jones

Resistive measurements ulere made on superconducting niobium single crystals in transverse magnetic fields. Crystals were grouln in both high and ulfrahigh vacua, doped with stnall quantities of oxygen, and annealed in ultrahigh vacua at temperatures from 900&apos; to 1350°C. Maxima in the fluxoid pinr~ir~g force were observedfor the [100] and [210] directions. The increase of the critical current density with dissoved oxygen was seen to saturate at relatively low concentration. This behavior, and the variation of J, and residual resistivity (as a function of oxygen content and annealing) of both clean and dirty gassy) crystals, is seen as a consequence of the formation of clusters with (210)~b habit planes and (200)ffo common boundaries. These suboxide clusters are apparenlly stable at high temperatures and very low oxygen concentrations. It is generally known that dissolved oxygen at concentrations well below the solubility limit sharply increases the critical current density of superconducting niobium.&apos; Such a result would not be expected if Nb-0 solutions were random, not even as the result of segregation on the scale usually encountered in solid solutions. According to the Kim-Anderson theory of flux creep,&apos; the critical transport current density is determined by the pinning force Fp associated with some feature of the microstructure. As the Lorentz force. a or (J X R), of the transport current in the magnetic field approaches Fp, flux creep and then flux flow occur. The pinning force is expected to be quite small if the heterogeneity involved is significantly smaller than tte range of coherency which for niobium is circa 250~.~ Although the strain field of an individual oxygen atom in the niobium lattice is relatively large, it does not seem plausible that individual atoms could be so effective as to account for the data. Also, ~ramer~ found that straining and strain aging specimens containing small amounts of oxygen on occasion decreased the residual resistivity. A possible explanation for the above behavior may be found in the work of van Ooijen and van der Goot,= who found that annealing changed J, for niobium foils containing oxygen, and they attributed the changes to ordering of the oxygen atoms. This phenomenon has been observed by other investigators using X-ray and PROCEDURE Cylindrical 4-in.-diam niobium single crystals with axial orientations [ill], [110], [112], and [oo~] were grown from pure niobium, see Table I for analysis, in an ion-pumped ultrahigh-vacuum system using the electron beam floating zone technique. Total pressure during growth was lo-&apos;9 torr: the oxygen partial pressure was less than lo-" torr, as determined by a mass spectrometer. These crystals will be referred to as the "clean" crystals. Similar crystals were also grown in another system at a pressure of 5 X 10"6 torr. These crystals will be referred to as the "dirty" crystals. Specimens 14 in. long were cut from the as-grown crystals and one end was polished down to no. 600 carbide paper smoothness. A back-reflection Laue photograph was then taken in order to fix the crystallo-graphic directions transverse to the crystal. The critical current density J,, the current density necessary to produce a voltage drop of 1.0 pv between voltage leads placed a in. apart, was determined as a function of the magnitude and direction of the transverse magnetic field and of the oxygen concentration. The technique and experimental arrangement was essentially similar to that of Tedmon et al.&apos; In the remainder of this paper, the azjmuthal angle $ for the field H is referenced to the [ I101 direction in all four crystals, and oxygen was added in small equal increments by anodization and annealing.7 The resistivity ratio, RR, of the resistance at room ternperature to that at 4.2"K (H =7.00 kG) was determined as well.

Jan 1, 1970

By R. W. Regehr, R. A. Burmeister

Epitaxial growth of GaAs 1-xPx on germanium substrates was achieved using an open tube vapor transport system. The compositional range of 0.3 < x < 0.4 was examined. The best results were obtained with (311) orientation of the germanium substrate. The physical and chemical properties of the resulting layers were investigated using several techniques. Spectrographic analyses of the layers indicate substantial incorporation of germanium into the GaAs t-X Px layer. Evidence is presented which indicates that this incorporation occurs via a vapor phase transport process rather than by solid phase dijfu-sion. Electrical measurements suggest that the germanium thus incorporated behaves predominantly as a deep donor in the compositional range of 0.33 < x * 0.40 and has a deleterious effect upon the luminescent properties of GaAs1-x Px. The increasing technological importance of GaAs1-xPx for use in light-emitting devices has led to an evaluation of several aspects of existing growth processes. The method most commonly used to prepare GaAs1-xPx for electroluminescent device applications is vapor phase epitaxial growth on GaAs substrates.&apos;-4 In a typical electroluminescent diode structure the active region of the diode is entirely within the epitaxial layer and thus the electrical properties of the substrate are relatively unimportant since it is effectively a simple series resistance (assuming hetero-junction effects to be negligible). The use of germanium rather than GaAs as the substrate material is of interest for several reasons. First, GaAs of reasonable structural quality has been epitaxially grown on germanium4-2 and it is reasonable to expect that GaAs1-xPx could subsequently be deposited on the GaAs layer. Second, germanium substrates are readily available with both lower dislocation densities and larger areas than GaAs. Finally, single crystals of germanium are more economical than GaAs single crystals. The principal objective of the present investigation was to test the feasibility of growing GaAs1-xPx epi-taxially on germanium substrates, and to evaluate the properties of such layers with regard to electroluminescent device requirements. The approach used was to a) demonstrate epitaxial growth of GaAs1-xPx on germanium, and b) characterize the relevant structural, electrical, and optical properties of the GaAs1-xPx layers. The possibility of germanium incorporation into the grown layers was of special interest since there was some indication of this in previous studies of GaAs growth on germanium.5&apos;11,12 Although a study of the electrical properties of germanium in GaAs1-xPx was not an intent of this investigation, several features of the electrical properties of the layers grown in the present study which appear to be due to germanium are described. EXPERIMENTAL PROCEDURE The open-tube vapor transport system used for the epitaxial growth of GaAs1-xPx is illustrated in Fig. 1. This system utilizes the GaC1-GaC13 transport reaction and is similar in most respects to the larger system described elsewhere.&apos; The germanium substrates were n-type, with a resistivity of 40 ohm-cm (Eagle-Picher Co.). These were cut to the orientations of {100), {111), and (3111, and were mechanically polished and chemically etched in CP-4 (5 min at 0°C) prior to growth. In some cases, a GaAs substrate was employed in addition to the germanium. The orientation of the latter was {loo}, and they were also mechanically polished and chemically etched prior to growth. The initial composition of the deposited layer was pure GaAs. After approximately 10 microns of GaAs was deposited on the germanium substrate, the phosphorus content of the layer was gradually increased over a distance of approximately 15 microns to the desired concentration and maintained at this value throughout the remainder of the growth. Typical operating parameters used during growth are given in Table I. Selenium was used as a n-type dopant in several runs to facilitate comparison of the electrical properties of the layers grown on germanium with those of layers grown on GaAs substrates, which are usually doped with selenium. The concentration of H2Se in the gas phase was adjusted to a value which would normally yield a carrier density of 1 to 5 x 101 7 at room temperature in layers grown on GaAs substrates. The terminal surfaces of the epitaxial layers were examined by optical microscopy for structural characteristics. Laue back-reflection photographs (Cu radi-ation) were also made on the terminal surface to verify the epitaxial nature of the deposit. After these steps

Jan 1, 1970

By L. Leibowitz, M. G. Chasanov, L. W. Mishler

A drop calorimeter system is described for use in measuring enthalpies to 3600°K. Data are presented for tungsten between 2800" and 3600°K. The enthalpy of tungsten in cal per mole between 2000° and 3600°K can be represented by the equation HºT- Hº298 = - 1.7622 X 103 + 5.7772T + 8.9861 where T is in degrees Kelvin. A tabulation of com -puted values is presented for heat capacity, entropy, and free energy function. A drop calorimeter has been constructed to carry out enthalpy measurements at temperatures to 3600°K. Samples are heated by induction1 and dropped into a commercial adiabatic calorimeter, modified for this purpose. The experimental temperature is limited by the melting point of container materials and compatibility of the container and its contents. Several high-temperature drop calorimeters have been described in the literature1-5 but none has been used at temperatures as high as those in the present work; our measurements of the enthalpy of tungsten range from 2800" to 3600°K. DESCRIPTION OF EQUIPMENT An overall schematic view of the equipment is shown in Fig. 1. Power for the induction coil is supplied by a 25-kw 250 kHz Ther-Monic generator coupled to an iron core RF transformer. The Sample capsule is suspended in the work coil by 10-mil diam tungsten wires which are wrapped around a horizontal 5-mil diam tungsten wire. The horizontal suspension wire is clamped between two massive copper electrodes which are fixed in an x-y motion device that allows adjustment of the position of the heated capsule from outside the vacuum chamber. The copper electrodes are connected by flexible copper straps to a 1250-joule (5 kv, 100 pfarad) condenser bank. When it is desired to release the capsule, the condensers are discharged through the horizontal suspension wire causing it to vaporize rapidly. Very reliable and precise release of the capsule is achieved in this manner. Experiments have shown that no heat correction is required for this discharge energy. As part of the temperature measuring system, two prism holders have been incorporated in the apparatus. The upper prism holder is in the main vacuum chamber itself, whereas the lower one is in a side arm attached to the drop tube below the gate valve. The upper prism is mounted on a rotary vacuum feed-through, and may be moved under a protective shield when not in use. This prevents deposition of vapors on the prism surfaces when temperature measurements are not being made. Similarly, the lower prism is mounted on a push-pull vacuum feed-through, and when not in use may be pulled into its side tube. The prism mountings are fitted with guides and stops so that they may be moved precisely into the desired position. The aim throughout is to minimize the time the prisms are exposed to vapors from the hot samples. At the high temperatures reported in this paper, only the lower prism was used. The upper prism holder in these cases was fitted with an additional radiation shield. By using a prism and viewport, the lower surface of the samples can be observed by an optical pyrometer. The measurements discussed in this paper were obtained with a Leeds and Northrup 8622-C-S series manual pyrometer which is estimated to be accurate to 0.5 pct. Pyrometer calibrations and prism and window corrections were carried out in the conventional manner6 using tungsten strip lamps calibrated by the National Physical Laboratory, Teddington, England. Prism corrections were rechecked after each use. All work to date has been done in vacuum, and no measurable change has been observed in the prism correction below -2300°K for the upper prism and below -2800°K for the lower one. The total time of exposure of the prisms is about 50 sec per run. At high temperature, the final temperature reading is corrected by using the final A value for the prism; see Ref. 6 for details of this procedure. The calorimeter is a modified Parr Instrument Co. (Moline, lll.), Series 1230 adiabatic calorimeter with automatic jacket control. Other authors5 have used a similar calorimeter with good results. The calorimeter jacket cover and calorimeter cover are attached to the drop tube which contains a radiation shield. This shield is a gold-plated copper disc which can be operated manually from outside the calorimeter. The receiver is attached below the radiation shield and is lined with tungsten. In a typical experiment, the calorimeter and its jacket water temperatures were adjusted to 0.000°K temperature difference. The sample was allowed to equilibrate in the furnace at the desired temperature for about 20 min. The initial calorimeter temperature was then recorded, the sample dropped, and appropriate shutters closed. After about 3 min, the drop tube and receiver were filled with helium to 60 torr. The final calorimeter temperature was recorded after it had remained constant over a 5-min period. The equilibration time in the calorimeter was about 25 min. Thermistor probes are used to operate a hot and cold water supply system to maintain the jacket temperature equal to the calorimeter temperature. For actual measurements of the calorimeter temperatures, a quartz thermometer was used (Hewlett Packard Dymec Thermometer, Model #2801A). This thermome-

Jan 1, 1970

By S. Feuerstein

THE influence of environment on the mechanical properties of metals has been extensively studied and documented.&apos; Most investigations have dealt with an interaction between a particular environment and a specific metal surface and the concomitant change in bulk mechanical behavior. Typical contributing media are oxide and metal film:;, electrolytes, and other surface-active agents. In the last category fall controlled gaseous environs (i.e., pressure or vacuum). Most vacuum exposure experiments prior to 1963 were conducted at pressures s>10-6 torr and elevated temperatures, or in such a manner as to prolong the exposure (e.g., by stress-rupture, creep, and fatigue). Little attention has been given to vacuum environment effects on the mechanical behavior of metals subjected to simple uniaxial deformation at room temperature. Test times and temperatures were assumed too ineffective as far as bulk changes were concerned. Further, the contribution of surface effects to the bulk mechanical behavior of metals was considered minimal. Under vacuums of the order of 1.0- 8torr and higher, molecular densities and, consequently, the rate of monolayer formation are such that exposures from seconds to days would be required for complete gas coverage. Thus, atomically clean surfaces created under ultra-high vacuum could conceivably maintain their cleanliness for time intervals orders of magnitude greater than at higher pressures. The influence of this unusual type of environmental surface phenomenon on the short-term bulk mechanical behavior of aluminum was first observed by Krame and Podlaseck in 1963.&apos; kin equivalent effect was reported for magnesium by Williams and Nelson.3 It was concluded from these studies2,3 that vacuum and, consequently, the monolayer formation rate of the oxide, were responsible for the described changes in flow behavior. The presence of an oxide layer impedes dis- I) EXPERIMENTAL DATA: MOLYBDENUM The tensile behavior of molybdenum was investigated by the author4-6 at ambient temperature over a range of pressures from 760 to 10-10 torr. These studies revealed that the flow behavior of the bulk specimens (0.200 in. diam by 2 in. gage length) was independent of pressure on sintered (0.062 mm grain size) and arc-cast polycrystals (0.012 to 0.149 mm grain sizes) and single crystals. Since the specimens were relatively large in size, it was assumed that any flow behavior effect would be surface-limited because of the short-term deformation procedure. Strain-rate-change experiments performed to determine the activation volumes for individual specimens at 760 to 10- 10 torr further indicated that the surface flow contribution was either minimal or zero, contrary to the findings of Shen el a1.7 on aluminum. Although the flow behaviors did not change, specimen ductility did change. For the sintered material at a strain rate of 4.2 x 10-4, specimen ductility was -9 pct higher at l0- 10 torr than at atmospheric pressure (dry nitrogen). A more comprehensive investigations on this same material revealed a distinct pressure dependence, Fig. 1. Intermediate and atmospheric pressure tests were obtained by backfilling the system from l0- 10 torr with extra dry, prepurified nitrogen. Other environments (air and purified argon) were also utilized for the 760 torr experiments; the results were essentially the same as those for dry nitrogen atmospheres. Departure from the fracture strain values obtained at 760 torr takes place in the vicinity of l0-6 torr, as indicated by the scatter band; a noticeable ductility increase is apparent at l0-8 and 10-10 torr.

Jan 1, 1970

By M. J. Marcinkowski, D. B. Crittenden, A. S. Sastri

A study co.mbining stress-strain .measurements in conjunction with transmission electron microscoPy has been made with near equiatomic Fe-Cr alloys which were aged for various times at 500°C. Associated with this aging is a marked increase in deformation twinning. The outstanding feature of these twins is that they generate stress fields sufficiently great so as to give rise to spontaneous dislocation loop nucleation nearly normal to the propagating twin. This observation is in agreement with the theoretically predicted elongation of the stress field of a dislocation Perpendicular to its direction of motion as it moves near the speed of sound. Dislocation loop nucleation is more difficult in the longer aged alloys so that this energy absorption mechanism is not effective in hindering twin propagation. Since crack nucleation can readily occur near the tip of a twin, the aged alloys become extremely brittle when deformed in tension. Iron-chromium alloys in the vicinity of the equiatomic compositions become severely embrittled when aged at about 500°C. Fisher et 01.&apos; have shown that this embrittlement is related to the decomposition of the original random Fe-Cr solid solution into a chromium-rich and an iron-rich phase. In addition, Mar-cinkowski et a1.&apos; have shown that twinning becomes an increasingly more important mode of deformation as the aging time is increased. These results have been recently corroborated by the transmission electron microscopy study of Mima and amauchi . The Fe-Cr alloy thus seems ideal for verifying the predictions made in Parts I4 and 115 of this investigation where the behavior of large static or blocked twins and those of large dynamic or propagating twins, respectively, were investigated numerically. It was thus decided to measure the stress-strain curves generated by embrittled alloys that were aged for various times and to examine sections by transmission electron microscopy. EXPERIMENTAL PROCEDURE Electrolytic iron and electrolytic chromium were vacuum-melted and poured into ingot form. The composition of the resulting alloy was found to contain 46.0 wt pct Cr (47.8 at. pct), the remainder being iron. The resulting ingot was swaged above 850°C into 0.250-and 0.400-in.-diam rounds. Compression samples of 0.250 in. diam and 0.400 in. long were cut from the smaller-diameter rounds. These samples were then sealed in evacuated quartz tubes and annealed for 30 min at 1150°C to produce a uniform and equiaxed grain size of mean diameter equal to 1.73 mm. They in turn were rapidly quenched from 850°C so as to preserve the condition of random solid-solution characteristic of the elevated temperature. The samples were then aged for various times up to 300 hr at 500°C in a massive Pb-Bi alloy bath. The samples were next polished and tested in compression at room temperature as described in Ref. 6 using an Instron tensile testing machine. The strain rate used was 0.05 in. per in. per min. The remaining larger round was converted into compression specimens of 0.325 in. diam and 0.500 in. long. This larger diameter enabled wafers of sufficient size to be prepared for examination by trans-mission electron microscopy techniques after subjecting them to a suitable strain. Foil preparation is described in some detail in Ref. 6. All foils were examined in a type HU-11A Hitachi electron microscope operating at 100 kv. RESULTS AND DISCUSSION Fig. 1 shows the effect of aging at 500°C on the room-temperature stress-strain curves of the FeCr alloys. For greater clarity the origin of each curve has been displaced upward. The same origin has been used for both the 0 and the 0.1 curves. It is apparent that with increased aging times a sharp drop in load is observed at the yield stress which becomes more pronounced as aging proceeds. A loud sonic burst accompanies this drop and subsequent metallographic examination shows the sample to contain numerous twins. For intermediate aging times, a number of smaller twin bursts follow the initial large one. The total plastic strain associated with the twinning mode of deformation can be obtained by adding up the contributions AE~ from all i twin bursts, i.e., £,¦££,-, in the manner illustrated schematically in Fig. 2. The contraction of the specimen, as measured from the strip chart of the Instron, after suitably correcting for the elasticity of the machine, was converted into true strain using the assumption that there was no volume change and that the sample remained cylindrical. The dashed lines are all drawn parallel to the

Jan 1, 1970