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By Robert E. Green, P. W. Kingman

Application of a constant geometry compression test to single crystals of aluminum of selected diameters from 1/4 to 1/64 in. showed the presence of a diameter-dependmt size effect. The most pronounced effects were found in those crystals oriented for single slip, while for specimens possessing orientations in the comers of the standard stereographic triangle virtually no size effect was exhibited. The yield stress of the crystals oriented for single slip was found to increase with decrease in specimen diameter, while the strain-hardening rate was found to be lower for the smaller specimens. The experimental results are in general agreement with those of other investigators obtained from lensile tests on copper and aluminum crystals. THE earliest systematic investigation of a possible size effect on the plasticity of metals was that of no,' who in 1926 performed tensile tests on cylindrical aluminum single crystals with diameters of 3 to 8 mm. Ono concluded that the gross stress-strain curve did not show a diameter dependence, but that the resistance to slip for strains of 0.1 pet and less appeared higher for 3-mm-diam crystals than for larger sizes. Later studies of aluminum by Maddin et al2 tentatively concluded that a size effect exists, but the conclusions were again open to question because of inconsistencies in the experimental data. Wu and Smoluchowski3 had previously shown that the slip system activated in a single-crystal sheet specimen of aluminum is a function of the specimen cross section in the slip direction, but no stress-strain data were obtained. Subsequently Fleischer and Chalmers4 studied the effect of the length of the slip direction of the primary-slip system on the stress-strain curve by testing aluminum crystals with geometrically dissimilar cross sections. In the course of this investigation a size effect was indicated in rather large crystals; however, the number of these tests was small. Other investigators have indicated that a size effect in aluminum is appreciable only for diameters of 0.5 mm or less.5, 6 Size-effect studies have also been carried out on copper crystals, the most detailed being that of Suzuki et a1.7 who performed tensile tests on specimens of many diameters ranging from 2 to 0.12 mm. Suzuki found a strong size dependence in the easy-glide region, both the extent of the easy glide and the hardening rate in easy glide were size-dependent, and the size effect was found to be orientation-dependent. Suzuki's results are in agreement with the less extensive observations of Pater-sonB and those of Garstone et al.9 A size effect was found by Rebstock using tubular copper crystals.'0 Size effects have also been noted in a brass,6, 11 in cadmium,12'19 and in hexagonal crystals.14 All the previously cited works have been entirely concerned with the variation of specimen cross section. The effects of specimen length and the change of specimen geometry which results from using progressively thinner specimens while maintaining the same specimen length have been largely ignored. A theoretical discussion of the effects of specimen length and geometry has been given by Hauser and Jackson,15 who predict a grip effect on easy glide as a function of specimen geometry provided that the specimen dimensions are large compared with the spacing between the slip bands, and by Fleischer and Chalmers,18 whose analysis of grip effects resulting from lattice rotation predicts an increase in easy glide with an increase in specimen length. A study of size and geometry effects in aluminum crystals by Kitajima and shimba17 indicated increasing amounts of easy glide in specimens of increasing length and identical cross section, and nearly identical stress-strain curves for specimens of different sizes having constant length-to-diameter ratios. Since the present study is primarily concerned with diameter dependence, the following factors were taken into account: specimen material, specimen geometry, testing method, range of sizes to be tested, and possible influence of surface and volume effects. Aluminum was chosen because of the present lack of conclusive results and the seeming possibility of size effects at relatively large diameters, the

Jan 1, 1964

By James R. Holden, Frederick E. Wang

Through both single-crystal and powder X-ray diffraction methods, ten A6B23-type compounds have been confirmed to exist between lanthanides (A) (plus scandium and yttrium) and manganese (B); A = Y, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, and Lu. The formation of a compound of this type is shown to he extremely atomic size-sensitive; hence it can be classified as a "size-factorH compound. The "enveloping effect", a geometrical consideration observed in its crystal structure, is proposed as the reason for the A6B23-type compound being size-sensitive. The approximate ideal geometrical ratio of the radii R/r is 1.31 while experimentally A6B23-type compounds have a radius ratio lying within the range 1.2 to 1.4. FLORIO t al.' characterized the structure of Th6MnZ3 as fcc, space group Fm3m, with 116 atoms in the unit cell. Since then, a number of isotypic binary compounds, and recently Gd n,,' have been confirmed to exist. The fact that strontium and barium form A6Bz3-type compounds with magnesium strongly suggested the possible existence of Ba6Liz3. However, investigation3 showed the compound Ba6LiZ3 to be absent. Since both strontium and barium are group 11-a elements and are therefore "open metals",6 the nonexistence of Ba6LiZ3 can hardly be explained satisfactorily by valence-electron considerations. On the other hand, the consistent atomic-radius ratio, (R/r),* observed for the known A6Bz3-type compounds,3 strongly suggests that the formation of compounds of this type is atomic size-sensitive. Therefore, one is tempted to explain the nonexistence of Ba6LiZ3 entirely on the basis of the atomic-size difference between strontium and barium. However, this approach is not entirely without objection. Atoms are not rigid spheres and are known to vary in size within certain limits.7 Since the atomic-radius difference between strontium and barium (0.07 to 0.09A) is within these limits, it is reasonable to assume that the size difference would have a negligible effect on the formation of Ba6LiZ3. This view is further supported by the fact that the radius ratio, R/r, in other known "size-factor" compounds is observed to range widely—for example, from 1.08 to 1.45 for ABz-type compounds (C15, MgCuz type)' and from 1.37 to 1.58 for AB5-type compounds (D2d, CaZn5 type).g The present investigation was undertaken in order to find a more satisfactory explanation for the non-existence of Ba6LiZ3 and, consequently, a better understanding of the nature of the A6Bz3-type compound. The primary objectives are to confirm the previous conclusion3 that the A6B23-type compound is indeed a "size-factor" compound and subsequently to determine the atomic-radius ratio range in which the A6Bz3-type compound can exist. In order to achieve these objectives, stoichiometric A6Bz3 alloys, where manganese (B) was alloyed with various lanthanide elements (A), were selected for investigation. The atomic-radius ratios of lanthanide elements with manganese range from 1.26 for Lu/~n to 1.46 for Eu/Mn. This radius ratio range includes and exceeds the range of all previously reported A6Bz3-type compounds—1.32 for Th/Mn' through 1.38 for Sr/Li. Furthermore, the atomic-size difference between successive elements of the lanthanide series in order of atomic number) is of the order of 0.01A (europium and ytterbium are exceptions). The series of lanthanon-manganese alloy systems is ideally suited to a precise determination of the limits of allowable atomic-radius ratio for A6Bz3-type compound formation. EXPERIMENTAL PROCEDURE The lanthanide metals, in ingot form, supplied by Michigan Chemical Corp. (St. Louis, Mich.) and Nuclear Corp. of America (Burbank, Calif.), were guaranteed by the suppliers to be at least 99.9 wt pct pure (traces of silicon, calcium, and other minor constituents present on occasion, not to be more than 0.05 wt pct) as shown by spectrographic analysis. Manganese metal, in polycrystalline form, was redistilled from the commercial, chemically pure grade and was analyzed to be at least 99.95 wt pct pure. In all cases, the atom ratio between the two elements in each charge was A (rare-earth meta1):B (manganese) = 6:23 and a constant weight, 3 g, of

Jan 1, 1965

By R. L. Fleischer

IN 1925 a criterion for localized deformation in a single crystal was derived by Taylor and Elam.' They noted that for a single active slip plane the slip plane area is constant, but the direction of the stress with respect to the slip direction changes during deformation so that, when the increase in stress due to this rotation is large enough relative to the work hardening, instability occurs. (By instability is meant continued slip on the active slip plane.) The instability criterion may be written t>dt/d?/m tan2? [1] where t and ? are resolved shear stress and strain, m the Schmid factor for resolving shear stress, and ? is the angle between the slip direction and the axis of tension. The formula points out that regardless of the atomic mechanism involved, for large flow stresses and low work hardening rates, slip on a single plane—once started—should continue. The case of alloying provides a direct possibility of adjusting the parameters in Eq. [I]: As an alloying element is added to a pure metal, the flow stress is raised and the work hardening in easy glide may be either decreased2 or unaltered.3 Since flow stresses in easy glide may rise to the kg/mm2 range for alloy crystals while easy glide slopes may be less than % kg/mm2, 2 it is possible for the inequality to be satisfied. Indeed Garstone and Honeycombe3 report that slip becomes coarser with increasing stress in the easy glide range, where the flow stress would be increasing and the slope would be essentially constant. Another case where high flow stresses and low hardening rates accompany coarse slip is that of quench hardening.4 Maddin and Cottrell report that quenched aluminum crystals display slip markings resembling those of a brass. A similar effect has been observed after irradiation.'

Jan 1, 1960

By E. Hein, R. A. Dodd

The fatigue softening of prior strain-hardened poly crystalline copper has been determined by measuring changes inflow stress resulting from fatigue treatments. Tensile fatigue does not soften the metal, while the softening due to reversed stress fatigue depends on the extent to which fully reversed stressing is approached. True tensile fatigue is shown to be possible only in the case of long wire specimens. Annealing following fatiguing of strain-hardened metal shows that tensile fatigue is very effective in modifying normal recovery and recrys-tallization. OBSERVATIONS by Ludwik and Scheu,' Kenyon,' Polakowski and Palchoudhuri, Kemsley, and Broom and Ham,596 have shown beyond doubt that strain-hardened metals are softened by reversed-stress fatigue. To some extent the softening might be associated with a rearrangement of dislocations, but the results of Broom and Ham5 on the temperature dependency of the fatigue hardening of annealed copper, and those of McCammon and Rosenberg7 on the partial recovery at 100'C of fatigue-hardened copper suggest that point defects may be involved. Since lattice vacancies are the only species of point defect present in appreciable quantities in thermody-namic equilibrium, most attention has been accorded them in the various theories advanced to explain hardening and softening effects resulting from fatigue. Precise mechanisms remain uncertain, and while some effects may be due to single vacancies, defects arising from vacancy clusters may also contribute to the changes in properties. All types of plastic deformation result in point-defect formation, one frequently invoked formation mechanism involving the nonconservative motion of jogs formed by the intersection of, for example, mixed dislocations. But since fatigue deformation is thought to be a particularly effective way of forming point defects, additional mechanisms peculiar to fatigue must be sought. One possibility is that jogged loops contract during the unloading cycle to give rows of vacancies. A local high-vacancy concentration could conceivably promote polygonization and recovery by climb, and, therefore, could explain the fatigue softening of strain-hardened metals under appropriate conditions of temperature. Conversely, the experiments by Broom and Ham6 on the fatigue hardening of copper single crystals involving subsequent tensile testing of previously fatigued specimens, resulted in the observation of distinctly lowered yield points. This could be due to vacancy atmospheres associated with dislocations, possibly augmented by jogs on dislocations. In addition to the yield-point phenomenon, a post-yield hardening was observed, with a temperature-dependence resembling the friction-hardening of irradiated metals,9 this again suggesting a point-defect mechanism. An important development in this field has been the observation,10 by transmission electron microscopy, of high concentrations of prismatic loops in fatigued aluminum. By analogy with quenched aluminum filmso11 it seems certain that these loops originate in the collapse of vacancy clusters formed during deformation. Metals, such as copper, having a relatively low-stacking fault energy would tend to produce Frank sessile loops (in practice tetrahedral defects with stacking faults on all (111) planes) rather than the glissile prismatic loops observed in aluminum. The manner in which these various defects affect the different aspects of fatigue behavior has not yet been fully investigated. The present work was designed principally to indicate whether tensile fatigue gives rise to hardening and softening effects similar to those associated with reversed stress fatigue, and with the hope of providing additional information on the contribution of point defects to fatigue deformation. Despite the uncertain ty often associated with the interpretation of resistivity data, i.e., the relative contribution of stacking faults and other defects, such measurements are conveniently employed to study point defect pheno-

Jan 1, 1962

By W. H. Smith

IN connection with some recent work on the effect of impurities on the ductility of chromium, it appeared desirable to know the solid solubility of carbon in chromium. A literature survey indicated that this information was not available. Although considerable work has been done on the Cr-C phase diagram,&apos;.&apos; previous investigators have been more concerned with the structure and phase boundaries of the carbide phases than with the terminal solid solution. The phase diagram shown in Fig. 1 is taken from the work of Bloom and Grant&apos; and represents the most recent determination. As indicated by the dashed line, the a solid-solubility limit was not determined. Experimental Procedure Alloys of chromium were prepared from hydrogen-treated and vacuum-degassed electrolytic chromium plus spectrographic grade carbon. The oxygen and nitrogen content of the alloys was <0.002 pct. After melting, analysis of the alloys showed them to contain 0.02, 0.08, 0.15, and 0.55 pct C. Pieces of the alloys were heated in a protective atmosphere to various temperatures and then quenched after holding for a time sufficient to insure equilibrium. Microscopic examination of the as-quenched alloys for the presence of a second phase was used as a measure of the solubility limit. The heats were made in a multiple hearth arc-furnace using a zirconium-gettered static argon atmosphere. A zirconium melt was made before each Cr-C heat. Triple melting was used to insure ingot homogeneity as shown by microscopic examination. The alloys were prepared by adding portions of a 4.5 pct C-Cr master alloy to high purity chromium. The carbon contents listed previously were those obtained by analysis. The nitrogen and oxygen contents after arc melting were both <0.002 pct. Sections 1/8X1/4X1/2 in. were cut from the 100-g ingots and a hole drilled in one end in order to suspend the sample from a molybdenum wire. After the surface was carefully cleaned, a sample of each melt was hung in a mullite tube heated externally by a platinum resistance furnace connected to a vacuum system. The lower portion of the mullite tube was sealed to Pyrex and closed off several inches below the furnace. This was filled with sili-cone oil kept cold by circulating cold water around the outside of the Pyrex. Quenching into the oil bath was achieved by melting a fuse wire supporting the sample. It required about 4 sec for the sample to cool from 1400" to 600°C. This severity of quench was considered satisfactory to freeze-in the high temperature equilibrium. For tests made at temperatures of 900" to 1200°C, heating was done in vacuum; for tests above 1200°C, an argon atmosphere was used. The holding time employed ranged from 12 hr at 900°C to 6 hr at 1400°C. Experiments were performed at temperatures of 900°, 1000°, 1100°, 1200°, 1300°, and 1400°C. Microscopic examination for evidence of a second phase was done at X1500. Experimental Result The microstructures of a 0.08 pct C-Cr alloy as-cast and after quenching from 1300°C are shown in Figs. 2 and 3. A 0.15 pct C-Cr alloy quenched from 1300°C is shown in Fig. 4. The data obtained from the quenching experiments is shown graphically in Fig. 5. If the Van&apos;t Hoff equation is obeyed, a plot on a logarithmic scale of the mol fraction of solute vs the reciprocal of the absolute temperature should give a straight line. For dilute solutions the weight percentage can be substituted for the mol fraction without introducing any appreciable error. The Van&apos;t Hoff equation can then be written as where H is the heat of solution in calories per mol. The slope of the straight line on the log pct C vs 1/T plot gives the value of AH. Assuming that the Van&apos;t Hoff equation is obeyed, which is probably justified for the dilute solution of carbon in chromium, the heavy straight line shown on Fig. 5 represents the best fit of the data. This line was obtained as follows. On Fig. 5 the results of the microscopic examination of all alloys following quenching were plotted and designated as to whether one or two phases were seen. Below 1100°C all alloys showed a second phase on quenching. The heavy vertical lines shown in Fig. 5 therefore represent the possible range of the ter-

Jan 1, 1958

By C. A. Wert

THE solid solubility of cementite in a-iron has been investigated a number of times and there is now general agreement on the solubility of about 0.018 wt pct at the eutectoid temperature, 720°C. With decreasing temperature, the solubility falls off so rapidly and to such a low value that no data obtained by standard metallurgical methods are available below 500°C. Using a new technique, however, Dijkstral has obtained apparently accurate solubilities down to 400°C; which data agree well with previously measured solubilities in the 600" to 700°C temperature range.&apos; The present paper has in part the purpose of extending his work to still lower temperatures. Earlier work of Low and Gensamer3 on iron has established that the presence of a relatively small amount of carbon can play a tremendous role in affecting the mechanical properties. In particular they found that the yield point remained high as they reduced the amount of carbon in the iron; the yield point dropped only after the carbon content had fallen to something less than 0.003 wt pct, the point where their carbon analysis failed. It seemed desirable to the present author to see if some means could not be found to extend this part of their work. This investigation has then the additional purpose to determine the range of carbon concentration in which the major change occurs. Solubility The method used in the present work to measure small percentages of carbon in a-iron utilizes internal friction. Since this method may not be fa-miliar to the reader, the following explanation will be given (a part of this procedure is from unpublished results of Dijkstra): It is known that the internal friction associated with the diffusion of

Jan 1, 1951

By S. K. Nowak

The lithium solubility limit in solid aluminum was determined by the use of micro-graphic techniques. The solubility limit thus established was shown to be a true equilibrium by checking the reversibility of AlLi phase precipitation and dissolution around the equilibrium temperature. The experimental results fit a straight line by plotting log N(LI) against 1/T. The metallurgical reasons explaining the lack of agreement among previous investigations are discussed. THE solubility limit of lithium in solid aluminum was determined by Shamray and Saldau1 by micrography and by Grube et al.&apos; and also Voss-Kiihler- by measurement of electrical resistivity. Since the addition of lithium induces extremely small changes in the aluminum lattice, X-ray techniques could not be employed for this purpose; in fact, the addition of lithium does not cause an expansion of the lattice as might be expected from a consideration of atomic radii, but causes a small contraction from 4.040 to 4.037A3, 4 when the solvent aluminum is saturated with this element. An analysis of the results from previous investiga-tions&apos;" shows that with improvement of investigation techniques the solubility limit tends toward a lower lithium content. Again, some of the author&apos;s own experimental results on the action of atomic hydrogen on A1-Li alloys seemed to indicate that the solubility of lithium should be much lower, i.e., about 0.3 pet at 300°C: instead of 1.15 pet, the lowest published value.4 For the foregoing reasons it was decided to investigate this problem. The aluminum and the lithium used for this purpose were of the highest purity. The lithium solubility limit was determined by metallographic techniques, in particular by the use of a reagent especially developed for the purpose of revealing the AlLi phase. The solubility limit thus determined was shown to be a true equilibrium by checking the reversibility of AlLi phase dissolution and precipitation around the equilibrium temperature. All of the experimental work was carried out in 1951 at the Centre d&apos;Etudes de Chimie Metallur-gique at Vitry, France, under the direction of Georges Chaudron.

Jan 1, 1957

By R. R. Joseph, K. A. Gschneidner

The solid solubility of magnesium in the close-packed modifications of lanthanum, cerium, praseodymium, neodymium, gadolinium, dysprosium, and lutetium was determined from approximately 250°C to the eutectoid temperature by the X-ray parametric technique. The maximum solubility at the eutectoid temperature was found to be 9.4 at. pet in La, 8.2 in Ce, 9.2 in Pr, 8.2 in Nd, 14.1 in Gd, 13.5 in Dy, and 11.5 in Lu. The solubility when compared at a homologous temperature was found to increase in a smooth manner with decreasing size factor from lanthanum to lutetium. It was found that the apparent atomic radius of magnesium when dissolved in the lanthanide solvent was constant and could be accounted for by consideration of several models dealing with departures from Vegard&apos;s law. The eutectoid temperatures for the lanthanide-rich La-Mg, Ce-Mg, and Nd-Mg systems were found to be 544", 505°, and 551°c, respectively. A study of the solid solubility of magnesium in the lanthanide metals was initiated because the valency and electron egativity difference are essentially constant and favorable for solid-solution formation, and thus one could examine the effect of size on terminal solid solutions. The size factors based on metal radii range from 14.6 pet for lanthanum to 7.5 pet for lutetium. Since the electronegativity difference is small, 0.06 unit or less, application of the Hume-~othery&apos; and Darken and Gurry2 criteria for solid-solution formation indicates that the solubility of magnesium would be expected to be small for lanthanum (between 5 and 10 at. pet) and to increase as we proceed along the lanthanide series. A search of the literature revealed no data on the solubility of magnesium in the lanthanide metals except for the solubility of magnesium in cerium at 450oCA typical phase diagram for the lanthanide-rich end of the lanthanide-magnesium phase diagram is shown in Fig. 1. EXPERIMENTAL PROCEDURES Preparation of Alloys. The lanthanide metals used in the preparation of alloys for this investigation were prepared from the corresponding fluoride by metallothermic reduction techniques previously described by Daane.4 The chemical analyses of the metals used are listed in Table I.

Jan 1, 1965

By A. U. Seybolt

The solubility limit of oxygen in columbium has been determined in the range between 775&apos; and 1100°C by means of lattice parameter measurements and microscopic examination. The solubility is a function of temperature and varies, in the range given above, from 0.25 to 1.0 pct O, respectively. BECAUSE of the marked deleterious effect of oxygen upon the mechanical properties of some of the transition metals, it is desirable to know something about the solubility of oxygen in these metals. The brittleness caused by oxygen in solution is particularly marked in the case of the group VA elements, vanadium, columbium, and tantalum. The solubility of oxygen in vanadium has already been reported in an earlier paper,&apos; and Wasilewski2 has given a value (0.9 wt pct) for the solid solubility of oxygen in tantalum at 1050°C. Brauer3 in 1941 investigated the Cb-0 system up to Cb2O5, but made no real effort to investigate the extent of oxygen solubility in the metal. He made the observation, however, that this solubility must be less than 4.76 atom pct (0.86 wt pct) oxygen. This estimate was made from X-ray diffraction results on the alloys CbO, CbO, and CbO; all alloys consisted of the terminal (Cb) solid solution plus CbO, but the last alloy containing 4.76 atom pct 0 showed only three very weak CbO lines. It is surprising that Brauer, by examining only three alloys, arrived at an estimate of the solubility which agrees very well with the results to be reported herein. Experimental Procedure A columbium strip obtained from Fansteel Metallurgical Products was cut into strips, 0.020x1/2x2 in. Two holes, about 3/16 in. in diameter, were made near the ends of the strips in order to hold them against a flat steel block for mounting in a General Electric X-ray spectrometer for lattice parameter measurements. The same holes were used to hang the specimens inside a fused silica vacuum furnace tube which was part of a Sieverts&apos; gas absorption apparatus. The apparatus and method of adding oxygen gas has been previously described.1 According to the supplier, the columbium obtained had the analysis given in Table I. After degreasing the samples, approximately 0.001 in. was etched from each side of the samples in order to remove possible surface impurities from the last rolling operation. For this purpose the following cold acid pickle was found satisfactory: 8 parts HNO3, 2 parts H2O2 and 1 part HF. Various Cb-O compositions were obtained up to 0.75 wt pct O by the gas absorption and diffusion technique. After the sample had absorbed all the oxygen gas added at 1000°C, an additional 24 hr was allowed for homogenization. This treatment appeared to be adequate, as shown by the linearity of the lattice parameter-composition plot. More concentrated alloys were prepared by arc melting mixtures of Cb and Cb2O5 since it was very time-consuming to make Cb-0 alloys in the neighborhood of 1 pct O, or over, by the diffusion method. When the flat strip specimens were used, they were ready for the X-ray spectrometer after cooling from the Sieverts&apos; apparatus. The cooling rate obtained by merely allowing the hot fused silica furnace tube to radiate to the atmosphere (when the furnace was lowered) was sufficiently fast to keep the dissolved oxygen in solution. Arc-melted alloys were reduced to —200 mesh powder in a diamond mortar, wrapped in tantalum foil, sealed off in evacuated fused silica tubes, and then heat treated as indicated in Table 11. The fused silica tubes were quickly immersed in cold water without breaking the tubes after the heat treatments. The tantalum foil prevented reaction between the fused silica and the sample; there was no reaction between the powdered samples and the foil at 1000°C, but some trouble was experienced at 1100°C. At this temperature level a reaction between the sample and the foil was sometimes observed, which resulted in erroneous parameter values. Experimental Results Hardness Tests: Since most of the X-ray samples were in the form of flat strip, it was convenient to obtain Vickers hardness numbers as a function of oxygen content. Compared to the V-O case,&apos; oxygen hardens columbium much more slowly, presumably because of the larger octahedral volume in colum-bium (about 12.0 compared to 9.3Å3 in vanadium), hence, requiring less lattice strain for solution. The plot of VHN vs wt pct O is shown in Fig. 1.

Jan 1, 1955

By B. L. Dunic, Terkel Rosenqvist

rr has long been suspected that sulphur has a small but finite solid solubility in iron, but up to the present more accurate data have been lacking. The survey given by Hansen&apos; illustrates the divergence of data and opinions. Solubilities between 0.01 and 1.5 pct have been suggested, and opinions vary regarding the effects of temperature and phase transformations in iron on the sulphur solubility. The extent of solid solution and its variation with temperature might be expected to be an important factor in the occurrence of hot shortness in steel. Therefore, the object of the present investigation was to study this problem more systematically. It was furthermore hoped that solubility data for sulphur might contribute to an understanding of the factors which determine solid solubilities in general. Experimental Procedure The present work was based on the measurement of the chemical activity of sulphur in the solid solution by means of equilibrium with a mixture of hydrogen and hydrogen sulphide. When the solid solubility limit is reached, the sulphur activity in the iron becomes equal to that in the coexisting sulphide phase. A gas mixture of a controlled H,S/H, ratio was passed over pure metallic iron heated to a temperature in the range 900" to 1500". The amount of sulphur absorbed by the iron was determined by analysis, and from a plot of percentage of sulphur vs. gas composition the sulphur activity and the solubility limit were determined. As the rate of diffusion of sulphur in solid iron is very small, often several days were needed to be sure that equilibrium conditions had been established. To produce a gas flow with less than 1 pct H,S of constant composition for several days, was in itself a problem. The most satisfactory arrangement was obtained by a continuous synthesis of hydrogen sulphide from the elements. This was done in the part of the apparatus shown to the left in Fig. 1. The hydrogen used was first purified in tank batches by passage through activated charcoal cooled in liquid nitrogen under a pressure of 150

Jan 1, 1953

By Regis M. N. Pelloux, N. J. Grant

Five or six alloys each in the systems Ni-C.v, Ni-Mo, and NL-W, spaced to cover the single phase areas as well as a part of the adjacent two-phase field, were prepared as uacuum-melted alloys. Tensile tests at room temperature and stress rupture tests at 1200° and 1500°F we.ve run for time periods to give fracture in 0.1 to 500 hr. Observations mere made of solid-solution and second-phase strengthening or uleakening, coupled with studies of ductility and the role of structure on the noted behavior patterns. THE development of stable creep-resistant alloys while broad and systematic is also highly empirical. A number of simple rules have been suggestedL-" but these are based on scant data. Whereas rules for low-temperature alloy strengthening can be applied with some success in more simple systems, the extension to behavior at high temperatures (greater than about 0.4 of the absolute melting temperature) is very poorly understood and has encountered important exceptions and deviations in terms of atom size or valency effects. In particular, the occurrence of both solid-solution weakening4,5 and second-phase weakening2 at high temperatures is of interest. MATERIALS AND PROCEDURE Nickel was chosen as the base material because of its important role in current high-temperature alloy applications, because of its freedom from a phase transformation, and because of wide solubilities for many elements of interest. The selected alloys were single- and two-phase structures in the Ni-Cr,6 Ni-Mo,7 and Ni-w 8 systems. The alloys were vacuum melted and cast, utilizing high-purity raw materials, in the form of 15 lb ingots. They were readily forged into 1/2-in. bar stock (except the two highest chromium alloys). The alloy compositions are shown in Table I. Typical impurity values are: Carbon: Max 0.03 pct (except for 30 and 35 pct Cr alloys which had 0.07) Nitrogen: Max 0.005 pct (except for two of the Cr alloys which had 0.05) Sulfur: Max 0.004 pct Silicon: Max 0.05 pct Each alloy was solution treated (air quenched) to produce comparable grain size. The two-phase alloys were then overaged in an effort to produce a stable structure for testing at 1200° and 1500°F, The results are summarized in Table 11. Following the heat treatments outlined in Table 11, the bars were machined to a gage section of 1.25-in. long by 0.250-in. diam. In addition to room-temperature tensile tests, stress-rupture tests were run at 1200" and 1500°F for time periods from 0.1 to about 500 hr. RESULTS Room-Temperature Mechanical Properties—The ultimate tensile strength, total elongation, and reduction of area values for all the alloys are plotted vs atomic percent of the solute element in Fig. 1. It can be seen that for the same amount of solute element the ultimate tensile strength increases in the order chromium, molybdenum, tungsten. Elongation increases (reduction of area decreases) with increasing amounts of solute for all the solid solution alloys, the values ranging from 50 to 70 pct. The ultimate tensile strength values for the two-

Jan 1, 1961

By T. J. Koppenaal, M. E. Fine

The critical resolved shear stress of aCu-A1 single crystals has been investigated as a function of composition, testing temperature, and strain rate. The strength, and its temperature and strain rate dependency increase markedly with aluminum content. The solid solution strengthening at 4.2°K is much larger than at room temperature. The activation energy for the low temperature dislocation cutting process increases from about 0.17 ev for a 0.5 at. pct A1 alloy to about 0.50 ev for a 14 at. pct A1 alloy. This result is attributed to an increase in the width of extended dislocations due to the known decrease in the stacking fault energy. In addition, the activation volumes at 4.2 and 77°K decrease with aluminum additions. Concerning the solid solution strengthening in the 296° to 373°K range, no definite conclusions are reached, but it is suggested that subgrains and cutting of subgrains are important. In a previous paper,&apos; the authors reported that adding aluminum to copper produces two types of strengthening: a yield point effect and an increase in the lower yield stress. This behavior is illustrated in Fig. 1 by shear stress-shear strain curves of furnace-cooled single crystals of pure copper and Cu-14 at. pct A1. The yield point effect, At, was thoroughly studied previously1 and shown to be associated with short-range order. The present paper reports an investigation of the lower-yield stress in aCu-A1 single crystals as a function of composition, testing temperature, and strain rate. EXPERIMENTAL PROCEDURE Single cryski1 tensile specimens were prepared in the same manner as previously described.l Briefly,

Jan 1, 1962

By M. S. Burton, H. H. Kranzlein, G. V. Smith

The influence of up to 2 at. pct of Ni and Pt on the yield strength of mono- and polycrystalline high-purity iron has been evaluated at temperatures from + 25° to -196°C. Current theories of solid -solution strengthening fail to explain the experimental observations. The temperature dependence of yield stress was found to be less in the alloys than that in high-purity iron. The room-temperature yield stress increased with alloy content, but at —78°C the yield strength first decreased with increasing a1loy content. AS a result of many studies, a number of theories have been proposed for solid-solution strengthening. The purpose of the present study was to evaluate these theories, as applied to the solid-solution strengthening observed in Fe-Ni and Fe-Pt alloys. Of various theories of solid-solution strengthening, those of Cottrell,1,2 Fisher,3 Suzuki,4 and Mott and Nabarro5 are most prominent, and have been discussed widely in the literature.&apos;-&apos; Of the recent concepts of solid-solution hardening the work of Fleischer9 is notable. Each of these models has been applied to particular alloy systems with some success, but in general none has proved generally applicable. In many of the previous studies to assess the effects of alloy additions in ferrous systems, lack of adequate control of the purity and grain size of the materials has obscured strengthening effects, so that few comprehensive data relating composition, temperature, and change of lattice parameter have been determined. In the present investigation an attempt was made to obtain data which would be meaningful in evaluating the theories of strengthening. Materials of high purity were used to minimize extraneous impurity effects, and both single crystals and polycrystalline materials were studied to evaluate the effect of grain boundaries. Nickel and platinum were chosen as alloy additions, because both belong to the same chemical group and have the same crystal structure and valence, with markedly different atomic diameters. It appeared that some conclusions regarding atomic size effect on strengthening might be made. MATERIALS AND PROCEDURES Fe-Ni and Fe-Pt alloys containing 0.5, 1.0, 1.5, and 2.0 at. pct alloy additions were prepared from high-purity materials. The iron was supplied by the American Iron and Steel Institute from a stock of 99.98 pct zone-refined iron prepared by Battelle Memorial Institute. The minimum purity of the nickel and platinum used for alloying was 99.98 and 99.999 pct, respectively. Alloys were prepared by levitation melting, cast into cylindrical copper molds, and cooled, all under a partial pressure (0.3 atm) of purified helium. Samples were 0.375 in. in diameter and weighed 20 to 25 g. Chemical analyses of the alloys are given in Table I. A sample of unalloyed iron also was cast as a control specimen.

Jan 1, 1965

By M. E. Fine, A. A. Hendrickson

The critical resolved shear stress and the strain rate dependence of the .flow stress are reported for Ag base A1 single crystals up to 6 at. pct A1 over a temperature ralzge of 4.1° to 470°K. At room temperature the solid solution strengthening is attributed brinciballv to an increase in the dislocation density on alloying. At 42°K the alloys are relatively stronger because the dislocations widen on alloying and are more difficult to cut. In a previous paper, the authors reported the characteristics of strain aging in Ag base A1 alloys.&apos; The variation of the magnitude of the strain-aging yield drops on aging time, aluminum content, and testing temperature strongly indicated that the phenomenon is due to the Suzuki mechanism. In the present paper, the critical resolved shear stress (CRSS) and the strain rate dependence of the flow stress are reported for Ag base A1 single crystals as functions of testing temperature (4.2" to 470") and A1 content (0 to 6 at. pct). Observations on the substructure and measurements of the effect of crystal growth rate are also given. The experimental re- sults appear explainable considering that aluminum additions increase the dislocation density and dislocation width. EXPERIMENTAL METHOD The methods of specimen preparation and tensile testing were described previously.&apos; Briefly, single crystals were grown from the melt in a vacuum (1 x lom5 mm Hg), shaped into tensile samples by a combination of abrading and acid etching, annealed at 850°C in a vacuum (1 x 10" mm &Z) for several days, and furnace cooled to 200&apos;. The testing was done on a model TM Instron using friction grips and a strain rate of about 5 x 106 per sec unless otherwise noted. The various testing temperatures were obtained by immersing the specimens in the following media: 1) 4.2&apos;: liquid helium using the apparatus of G. Byrne;&apos; 2) 77°K: liquid nitrogen; 3) 200"K: dry ice and acetone; 4) 415&apos; K: ethylene glycol; 5) 460&apos; \ to 480&apos; : molten Stanalax. In the determination of the CRSS above 296&apos; K, a ratio method was used; the crystals were strained initially at the higher temperature, 0.1 pct shear strain, and then tested at 296&apos; . The ratio of the flow stress between the two temperatures was then multiplied by the average CRSS at 296&apos; K to obtain the value of the CRSS at the high temperature. (The test at 296&apos; showed a yield point resulting from strain aging; the flow stress at 296&apos; K was taken as the lower yield stress.) The ratio method, we believe, is more accurate than using different crystals since

Jan 1, 1962

By William Klement

KNELLER&apos; has recently reported that extensive metastable solid solutions may be obtained in Cu-Fe alloys by simultaneous vapor deposition. This note reports that solid solutions, apparently single -phase, can be obtained for Cu-Fe alloys containing 0 to 20 and 85 to 100 at. pct Fe by rapid quenching from the melt; the inability to extend the solid solubilities further is related to the liquid miscibility gap, Fig. 1, as for Cu-Co alloys.2&apos;3 Accurate lattice spacings of the copper-rich fcc and iron-rich bcc solid solutions have been obtained. Homogeneous alloys were prepared by casting4&apos;5 and sintering2 from elements of 99.9+ pct purity. The quenching techniques were as before,&apos; except the iron-rich alloys were liberally covered with argon while at elevated temperatures. Flakes about 1 sq mm in area were obtained and investigated with the Debye-Scherrer technique, as previously described.2,4 All X-ray work was done at 25° 2°C using filtered copper and cobalt K radiation. Relative visual intensities of the diffraction lines for the phases in the quenched alloys are shown in Table I. The lattice spacings of the fcc structure for alloys containing up to 80 at. pct Fe are plotted in Fig. 2. The variation of these lattice parameters with composition is in good agreement with the re- of cementite spots usually present (all hkl reflections are allowed) and the ease of confusing them with ferrite or martensite reflections. Copies of the report can be obtained by writing to the Materials Research Department, Rocketdyne. 6633 Canoga Avenue, Canoga Park, Calif., 91304. A copy is also available at the Engineering Societies Library, 2nd floor, 345 East 47th Street, New York, N.Y., 10017. Photocopies, either full-size or microfilm, may be purchased from the Engineering Societies Library. sults6 of Andersen and Kingsbury, Fig. 2, although there is some disagreement in absolute value. This discrepancy may be due to the different temperatures at which the X-ray measurements were carried out and perhaps to the different extrapolation procedures. Also, Andersen and Kingsbury6 state that their lattice spacings were computed relative to the wavelengths given by Siegbahn in 1933; this reference has not been found and it is assumed that the well-known 1931 wavelengths were used, the lattice spacings then being in kx units which are converted into angstroms by the factor 1.00202. There is no support for the contention that solution of iron decreases the lattice parameter of copper, as con-

Jan 1, 1965

By W. Klement

By quenching liquid alloys, single-phase solid solutions are obtained in the ranges 0 to 42.0 at. pct Co-Au and 0 to 15 and 75 to about 100 at. pet Co-Cu. Metastable solid solutions are also found in multiphase 42.0 to 49.0 and 69. 0 to about 100 at. pet Co-Au alloys. fie inability to achieve complete solid solubiliiies in Au-co and cu-co alloys is rationalized by a conszderation of the rate processes during cooling and solidification. Trends in lattice distortion and shifts in the compositions of the melting-point minima and critical points are discussed for the binary alloys of copper, silver, and gold with some of the transition metals of the first long period. By rapidly cooling alloys from the melt, a continuous series of metastable solid solutions can often be obtained for components of similar crystal structure which normally form eutectic systems.&apos; The eutectic system Au-Co, Fig. 1, and the peritectic system Cu-Co, Fig. 2, were investigated in order to determine the extent of the metastable solid solutions attainable with the present technique.* EXPERIMENTAL PROCEDURES Most of the alloys were prepared by melting weighed quantities of the elements (purity greater than 99.9 pct) under hydrogen in alumina crucibles by means of induction heating. After reweighing, the alloys were cast under argon into 1 mm diam wires. However, it was not possible to prepare some of the Cu-Co alloys with the requisite homogeneity (over about 1 mm3) in this way. For these alloys, reduced powders (purity greater than 99.9 pct) were mixed for 12 to 48 hr, pressed into compacts that were sintered at 1000º to 1050°C for 6 to 48 hr under hydrogen, and then furnace-cooled. Alloy charges of a few mm3, cut from the cast wires or chipped from the sintered compacts, were heated to 1550º to 1600°C in 30 sec in an alumina insert held within a graphite support and then ejected by a pulse of helium onto a lightly polished copper strip on the inner periphery of a rotating wheel. The

Jan 1, 1963

By H. Becke, D. Stolnitz, D. Flatley, W. Kern

Extensive solid solubilities of CdTe (zincblende-type struckre) and InTe (B37 type) in each of the rock salt-type compounds, PbTe and SnTe, have been observed. Partial phase diagrams have been determined by thermal analysis and X-ray metallography. The limiting mol fraction. X,, of the solute in the rock salt-type a phase and the corresponding eutectic temperatures, T,, are: (PbTe)l-x(CdTe)x: X,- 0.2, T, =866°C; (PbTe),-,(lnTe),: X, - 0.35, T, = 646"C; (SnTe),-,(CdTe),:X,- 0.11, T, = 784 "C; (SnTe),-,(lnTe),: X,-0.53, T, = 630°C. The lattice parameters of the a phase decrease linearly with X, even in (PbTe),-,(CdTe),, where a, (CdTe) = 6.481A > %(PbTe) = 6.459A. This is taken as proof that the cadmium atom enters an octahedral interstice of the tellurium atom sublattice; i.e., the formation of the a phase entails the direct replacement of lead by cadmium. The a, us X curve extrapolates to 6.16A at X = 1, in agreement with the value predicted for an ionic crystal of CdTe; it is also consistent with the reported lattice parameter It is well-established that the compositions of intrinsic semiconducting and semimetallic compounds conform to normal valence rules.1"5 The apparent exceptions can be explained by taking account of anion-anion covalences, as in CdSb, or of multiple cation valences, as in In Te.&apos;This empirical generalization is the basis of the chemical approach to semiconductors2 by which the properties of an intrinsic semiconductor are rationalized in terms of the ionic-covalent bonds necessary to saturate the valence-electron complement of the anion sublattice. A fundamental shortcoming of this approach is its disregard of long-range crystal interactions. It cannot, accordingly, deal with the phenomenon of charge conduction except through the use of ad hoc postulates. As an example, a crystal of CdTe would, in the valence-bond picture: be described in terms of electron pairs, each with the same discrete energy, localized between every cadmium and tellurium atom. This is, of course, contrary to the Pauli of the high-pressure rock-salt form of CdTe, corrected for decompression from 36 kbar. The free energy of formation of the a phase of pure CdTe at room temperature is calculated from the phase diagram to be +10 kcal per g-atom, in accmd with the value calculated from the transformation pressure. The standard enthalpy is +13 kcal per g-atom, and the standard entropy is +9 eu. The latter value implies the formation of extra classical particles, such as vacancies, interstitials, or nondegenerate charge carriers, but these alternatives are not consistent with the semiconducting properties and the densities of the a phase. The extrapolated values of the lattice parameters of (PbTe),-,(lnTe), and Spectively, for the rock salt-type modification of InTe. The corresponding interatomic separation is intermediate between monovalent and trivalent indium. The qualitative implications of the results are considered from the viewpoints of both valence-band theory and energy-band theory. principle, and is corrected by methods of molecular-orbital theory in which bonds are replaced by bands of molecular orbitals whose energies, E, depend upon a crystal-momentum vector, k.7 Each band is derived from a linear combination of atomic orbitals with two electrons required to saturate each molecular orbital in the band. In a crystal of N atoms containing z atoms in its primitive unit cell, there are 2 N/z states per band which lie in a region of k space bound by the Brillouin zone. In an intrinsic semiconductor, the bands can be grouped into valence bands which are normally filled and conduction bands which are normally empty. If the highest valence band and the lowest conduction band overlap anywhere within the Brillouin zone, the material is rendered semimetallic. The quantity defines the effective mass, m*, of an electron in a conduction band (or of a hole, i.e., an electron deficiency, in the valence band) and leads directly to the concept of charge mobility through the relation \x = et/m*, where e is the electron charge and t is the lattice relaxation time.

Jan 1, 1964

By H. H. Hausner, S. Storchheim, J. L. Zambrow

The solid state bonding of aluminum to nickel was studied as a function of temperature, pressure, and time at pressure. The initial results indicated that as the reaction conditions were varied, marked changes in tensile strength occurred. Plots of the log penetration coefficient vs the reciprocal of absolute temperature for various isobars were straight lines displaced from each other. THE techniques of bonding different metals to A each other include brazing, welding, welding by application of a molten phase, and solid state welding without any molten phase present. This last technique, the pressing of metals either at room temperature or at some temperature below the melting point of the metals to be joined, seems to offer interesting possibilities for bonding purposes. However, this technique has not been completely investigated, and very little is known about the diffusion phenomena which occur during solid state welding. Some previous work on the effect of pressure on diffusion1 was inconclusive. This paper is concerned with an investigation regarding the effect that the processing variables, such as pressure, temperature, and time at pressure, have in solid state bonding. The tests were made with aluminum and nickel and special emphasis was given to the strength of the bond between these two metals and to the intermetallic penetration rate during the bonding process. It seems that the effect of pressure on the intermetallic penetration is of particular importance for practical purposes and this effect was therefore studied in detail. Procedure Apparatus: The means of solid state bonding used for this study was that of the hot-pressing technique. This method requires the equipment pictured in Fig. 1 and involved the following procedure. The two metals to be bonded were placed in an aquadag lubricated 18-4-1 tool steel die, 16 in. high by 1.440 in. ID, between punches of 1.366 in. diameter made of the same material. A thermocouple

Jan 1, 1955

By W. Shockley

THIS lecture can best begin with a statement of the chief conclusion: The metallurgical industry will find profit in supporting fundamental research on dislocations. This support should be done both in their own laboratories and in universities. My lecture consists of an exposition of the basis for this conclusion. The experience on which I base it is drawn largely from two fields in solid state physics—one field is transistor electronics and the other is dislocation theory. At present the relationship of solid state physics to technology is different in these two fields. In electronics without question, the physics has led the technology. In metallurgy, on the other hand, the technology in the form of metallurgical art is far ahead of the fundamental science. In transistor electronics, physics has suggested and can still suggest previously unachieved combinations of matter that will have new and useful properties; that is, the physicist can make specific predictions. The physicist can also have some confidence that the predicted devices will actually come into existence in a matter of months or years and that they will live up to the predictions. In metallurgy, the physicist cannot to a comparable degree make predictions and have the same hope that they will lead to something new and valuable. There are a number of reasons for this difference. The first is simply historical. Transistor physics is young. It may be regarded as dating from the announcement of the transistor, in which case it is about four years old, or from the first real control of semiconductors as materials (this was accomplished largely by metallurgists, by the way) in which case it is about ten years old. Metallurgical art, on the other hand, is thousands of years old. There is no doubt that the advance of this art has been and will be hastened by a good fundamental understanding of the quantum theory of atomic phenomena. It, is too much to expect, however, that theory will soon catch up with the lead that practice has gained in a thousand years, and that theory will then point out specific pathways to better materials. It seems more probable that modern atomic theory will serve to interpret and organize information much as thermodynamics has done through phase diagrams. In this lecture, I shall emphasize an important feature common to both solid state electronics and to metallurgy. This common feature is the harmonizing principle that justifies discussing electronics and metallurgy as related topics in solid state physics. In both cases the important properties of the materials arise from imperfections. By imper- fections I mean deviations of the materials from perfect single crystals. The imperfections may be of many forms. From the point of view of utility they may be either good or bad, and a given type may be good or bad depending on circumstances. The technical material of my lecture will be divided into two parts. The first will be chiefly concerned with four types of imperfections in germanium crystals. The control of these imperfections makes possible the fabrication of useful electronic devices. A good example of such control is the junction transistor, which I shall discuss from this viewpoint later. The junction transistor, as some of you may have heard, can be used as an amplifier of electrical signals and in a number of respects surpasses what has hitherto been achieved with vacuum tubes. The second part of my technical material will be concerned with dislocations. For about fifteen years the theoretical physicist has had dislocations in mind as the most important kind of imperfection in metals. He has, however, until recently had experimental material of a highly speculative nature to back up his assertions. I am fortunate in the timing of this lecture to be able to describe some recent results that put dislocations on a far more definite basis than has been the case in the past. In fact there are now some experiments which reveal the characteristic properties of dislocations almost as clearly as experiments in transistor physics reveal the properties of holes and electrons, properties that I shall soon describe. It is this advance in the status of dislocations that emboldened me to make my initial assertion that the metallurgical industry will profit from supporting fundamental research on dislocations. Transistor Electronics In order to discuss imperfections in semiconductors, it is necessary to visualize a reference condition that may be regarded as perfect. In the cases of silicon and germanium, which find application in transistor electronics,&apos; the perfect structure is the diamond structure shown in Fig. I. In this structure, each atom is surrounded by four neighbors with which it forms four covalent or electron-pair bonds. These bonds use all of the four valence electrons possessed by each of the silicon or germanium atoms. The electronic structure of the crystal is thus complete and perfect. A crystal of silicon or germanium with a perfect electron-pair bond structure would be an insulator, In order for electrical conduction to occur, it is necessary for imperfections to arise in the electronic structure. In this lecture, I shall discuss four possible imperfections whose symbols and relationships are indicated in Table I. We shall consider first, as an example, a crystal of silicon containing an arsenic atom as an impurity.

Jan 1, 1953

By W. A. Tiller, J. P. McHugh

HE majority of liquidus and solidus surfaces in phase diagrams have been determined by the conventional cooling- and heating-curve techniques.&apos; These techniques have two main shortcomings: 1) the solidus may be in considerable error due to the difficulty involved in completely homogenizing the solid and 2) the determination of liquidus and solidus in more than a two-component system does not enable one to determine tie-lines connecting the specific equilibrium solid and liquid compositions. However, in a recent paper by one of the authors,&apos; a method was suggested whereby the liquidus and solidus surfaces plus tie-lines in an n-component system may be determined. This method utilizes a controlled solidification technique and assumes that interface equilibrium exists during freezing. The present work was undertaken with a twofold purpose; first, to determine the liquidus and solidus lines in the pseudo-binary system Bi2Te3-Bi2Se3 by heating- and cooling-curve techniques and, second, to determine the partition coefficients of Te and Se in the BizTe3-,Sex system by controlled solidifica- tion techniques. The two sets of results can be compared to test the accuracy of the controlled solidification method. EXPERIMENTAL I—The starting materials for this study were 997999 pct Bi, Te, and Se, obtained from the American Smelting and Refining Co. The compounds BizTe, and Bi2Se3 were each prepared by melting together stoichiometric amounts of the elements, followed by twelve zone-refining passes. This produced homogeneous bars of the compounds for use in the phase-diagram studies. The apparatus used to obtain heating and cooling curves is illustrated schematically in Fig. 1. The alloy samples were located in a graphite crucible placed in a stainless steel canister. The canister was supported in a heavily lagged pit furnace by a device which oscillated the canister about its vertical axis at a frequency of about 3 cycles per sec during heating and cooling-curve runs. The graphite crucible was designed to minimize the thermal coupling of the sample to the furnace. A thin graphite sleeve separated the alloy sample from the stainless steel tube that housed the thermo-

Jan 1, 1960