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By P. K. Koh, G. C. Dunn

Si-Fe single crystals in a number of selected orientations were cold rolled 70 pct and analyzed to obtain quantitative (110) pole figures. Stable end orientations were ddetermined, and the effect of orientation on deformation behavior was investigated. WHEN single crystals are cold rolled sufficiently, they rotate into end orientations that are stable or unchanged in position with additional deformation. The end orientations of heavily cold-rolled iron crystals, positioned in holes in copper to limit lateral flow and to simulate polycrystalline conditions during deformation, were determined by Barrett and Levenson.' They found that the sum of the end orientations, a pole figure for all the crystals studied, reproduced the essential features of the cold-rolled texture of polycrystalline iron. In. an investigation of Fe-Si alloys, Barrett, Ansel, and Mehl' observed little effect of silicon content on the textures of heavily cold-rolled samples. Since alloys with less than 4 pct Si are known to have the same slip systems as iron," it seems logical to expect that they would also have the same end orientations as those for iron. Whereas Barrett and Levenson in their study of single crystals were interested in the problem of the origin of the cold-rolled texture of polycrystalline iron, the present authors are more interested in the final cold-rolled textures of single crystals of Si-Fe from the point of view of their relationship to subsequent recrystallization phenomena which will be reported in another paper. Nevertheless, such points as the tendency of an end orientation not to rotate (stability), the tendency of a pole concentration to spread out, and the tendency of the crystal to widen during cold rolling become interesting separately when the initial orientations are selected already in end orientations. Also the initial orientations having a [I101 axis parallel with the transverse direction, which include the two end orientations (111) [Ti21 and (001) [110], comprise a series that needs further clarification regarding the way such crystals rotate during deformation. Finally the present use of quantitative pole figure methods* represents an advance over the X-ray photographic method employed by Barrett and Levenson in their work on end orientations. The present investigation provides information on the cold-rolling behavior of two groups of Si-Fe crystals: 1-—crystals initially oriented in recognized end orientations for iron crystals with a [I101 direction parallel with the rolling direction, and 2— crystals initially oriented with a [I101 direction 90" to the rolling direction and in the rolling plane. For the second group, there is a 90" range between the (001) [110] orientation and the (110) [001] orientation. Since the 35" portion of this range from (110) [OOl] to (111) Di2] was included in a previous investigation," only the remaining 55" portion from (111) fii2] to (001) [I101 needs further consideration. Also, since both (111) [xi21 and (001) [I101 are end orientations for iron crystals,' there might be a critical orientation* or orientation range be- • W. W. Martin and C. G. Dunno noted that (112) [Till was such a critical orientation. tween them such that early in the deformation an orientation within this critical range splits into two orientations. Upon further deformation, these two orientations rotate to produce a final texture consisting of (001) [1101 and (111) [?i2] components. The end orientations obtained are discussed in connection with the work of Barrett and Levenson, while the observed tendency for lateral flow of crystals in these orientations is treated in terms of the theory of Hibbard and Yen.' Lateral flow according to the theory increases with deviation of the plane containing the rolling direction and the slip direction from a position perpendicular to the plane of rolling. Experimental Procedure Single crystals in sheet form with preselected orientations were prepared by methods that have been described elsewhere." Three lots designated A, B,

Jan 1, 1956

By Y. C. Liu, R. H. Richman

From rolling textures of polycrystalline AgCl determined as a function of temperature, changes in the amounts of the individual textural components are correlated with temperature-dependent changes in glide geometry. The preferred orientations are influenced by the slip behavior as follows: 1) pencil glide, characterized by (110) slip directions and a greater participation in the deformation the higher the temperature, leads to a(012) fiber texture; 2) low-temperature deformation, primarily on (110) (110) systems, generates the {237}-(11, 9, 7) component; and 3) slip on {111}(110), comprising a significant portion of the room-temperature deformation, generates the {135}(211) and {110}(112) components. Typical re crystallization textures are also presented and briefly discussed. SPECIFIC relations between flow mechanisms in crystals and the individual orientations or components in deformation textures are necessary for a thorough understanding of the origin of such textures. Within each ordinary class of crystal struc- tures there is insufficient variety in the observed preferred orientations to permit direct and unambiguous correlation between flow mechanism and texture. A second approach to this problem is the correlation of textural changes with some known variation in glide geometry within one substance,1 In this paper, the latter approach is applied directly to a material in which there are distinct changes in the character of glide with changes in temperature. Silver chloride, although a nonmetal, is reported to exhibit slip,2,3 fiber textures,4 and rolling textures5,6 crystallographically similar to those of the well-studied fcc metals;7,8 in addition, there is a marked temperature sensitivity of the glide planes upon which flow occurs.3 Previous investigations of textures in AgCl unfortunately did not employ methods sufficiently sensitive to define possibly important minor components in the texture, nor did they utilize the temperature dependence of the glide systems. Thus, in order to clarify the effects of changes in slip mechanism, this paper reports a survey, using semiquantitative methods, of preferred orientations in rolled AgC1. Inasmuch as the influence of prior deformation texture upon preferred orientations after annealing is also of interest, some representative annealing textures are presented.

Jan 1, 1965

By N. K. Chen, R. Maddin

THE textures of straight-rolled and of cross-rolled molybdenum were first determined with the aid of pole figures by Custers and Riemersma.' These authors have shown that for straight-rolling, the main texture was (100) [0111 with a considerable spread about the rolling direction. After cross-rolling a second texture was obtained in which there was a [111] axis perpendicular to the rolling plane, possessing a rotary symmetry. Recently Semchy-shen and Timmons2 in their study of preferred orientation of arc-cast molybdenum sheet obtained similar pole figures. In these two investigations, polycrystalline materials were used. In the main, the textures of molybdenum in these cases are qualitatively consistent with rolling textures of other body-centered cubic metals, such as iron and Fe-Si alloys." In the present investigation, single crystals of molybdenum were deformed by rolling with respect to specific crystallographic planes and directions. Since the deformation textures of polycrystalline aggregates have been related intimately to the behavior of individual grains,4 a study of possible correlations of final textures with respect to the initial orientations of the single crystals might conceivably lead to a better understanding of the textures. Annealing treatments were carried out after deformation in order to study the recrystallization characteristics as well as the recrystallization texture. Rolling of Single Crystals Single crystals of molybdenum (about 1/8 in. in diarn x 1-in. long), grown by the method previously described,5 were cold-rolled without intermediate anneals. Except for specimens MR-1 and MR-2, which were rolled at random in the preliminary test in order to find a proper rate of reduction, all other specimens were carefully documented as to their respective orientation before deformation by means of X-ray Laue back-reflection methods. A stereo-graphic projection was constructed from which it was possible to determine a particular plane and direction to be considered for rolling. Parallel flat surfaces were then polished metallographically with respect to a reference scratch on the specimen which was mounted in sealing wax. These flat surfaces contained the plane chosen for rolling. After etching, a Laue back-reflection photogram was again made of one of the flat surfaces to determine the exact plane of rolling. The initial orientations of all the specimens (specified by two elements for each crystal, direction of rolling and the pole of the rolling plane) are summarized in Fig. 1. The specimens were mounted in plasticene between two hardened Si-Fe plates. The sandwich was then rolled down, keeping the direction constant in the case of straight-rolling. In cross-rolling (MR-10, MR-11, and MR-12) the sandwich was rotated 90" after each pass so that every first and third pass contained the same rolling direction. Specimens MR-14, MR-15, and MR-16 were compression-rolled following the manner of Barrett." In these cases the direction of the sandwich through the rolls was changed by 3" to 5" for each pass until the specimens were rolled to the desired reduction in thickness. It was found that if extreme care was exercised in rolling, i. e., the amount of deformation per pass was extremely small, the specimens could be rolled to a large reduction in thickness. The rate of reduction used, with a single exception of MR-1. was generally 0.001 in. per 10 passes. Thus, it took about 800 passes to reduce a specimen to a final reduction in thickness of 87 to 98 pct. The results of rolling are shown in Table I. Cold-Rolling Textures The final orientations were determined by the conventional Laue transmission method," using molybdenum radiation, with or without a zirconium filter. Pole figures were plotted from (1101 and (200) reflections in which three degrees of intensity— heavy, medium, and light—were determined visually. Three main types of textures have been observed from the deformed single crystals. These are: 1—a

Jan 1, 1954

By J. A. Berge, R. S. Mateer, R. G. Aspden

IN a study of the cold-rolling characteristics of iron-base alloys with 3 to 12 pct Al, the influence of aluminum content on the cold-rolling textures was evaluated. This work was undertaken to determine if binary iron-aluminum alloys possessed cold-rolling textures similar to other body-centered-cubic alloys and to contribute additional information on the effect of solute concentration on the cold- rolling textures. Gradual changes in cold-rolling textures with an increase in solute content have been observed in copper1 and in titanium.2 Iron-base alloys containing 3.0, '6.0, and 12.0 pct aluminum were vacuum-induction-melted in a magnesia crucible and permanent-mold cast. The materials used were high-purity electrolytic iron and 99.99 pct grade aluminum. Each ingot was 1 in. square in cross section by 12 in. in height. The bottom half of each ingot was soaked for 1 hr at 1000°C and rolled at 1000°C to a thickness of 0.055 in. with the long axis of the ingot parallel to the rolling direction. The strip was reheated between passes to maintain a rolling temperature of 1000°C.

Jan 1, 1960

By O. N. Carlson, H. A. Wilhelm, J. M. Dickinson

On the basis of microscopic studies, melting-point observations, and X-ray analyses, a phase diagram is proposed for the Cb-V system. A complete series of solid solutions is formed with a minimum in the solidus at 1810°C near 35 wt pct Cb. No compounds or intermediate phases were found in the system above 650°C. THERE is an ever increasing need for better structural metals and alloys for use in nuclear reactors. In addition to the normal properties of engineering structural materials, such as high temperature strength, resistance to corrosion, and fabric-abil~ty, the nuclear properties of the material must be considered. In a nuclear reactor it is important to conserve neutrons, so a material which removes these neutrons from the reaction excessively is considered to have unfavorable nuclear properties. In nuclear-reactor design the engineer must have nuclear as well as other data available on alloys in order to make a wise selection of materials. Due to the fact that many of the common structural materials have undesirable nuclear properties, it is vital that new alloys of metals having more favorable nuclear properties be investigated. Columbium and vanadium are both high melting metals, both exhibit resistance to chemical attack, and no great difficulty is encountered in fabricating them into desired shapes. With proper treatment both metals can be cold rolled extensively without failure. In addition they have desirable nuclear properties for certain types of reactors. Therefore, the alloys of columbium and vanadium should be of interest in the atomic energy program. Since an alloy-development program is enhanced by a knowledge of the phase equilibria of the components, this investigation was undertaken to establish the phase diagram for the Cb-V system. According to the Hume-Rothery rules for alloying,' the chemical similarity, crystal structure, and atomic-size factor are favorable for a complete series of solid solutions for this system. Both elements are in the same family of group V of the periodic table and thus are quite similar chemically. The crystal structures of columbium and vanadium are compatible for extensive solid solubility, since both have body-centered-cubic structures. The atomic diameters of columbium and vanadium are 2.85 and 2.62Å, respectively. This difference of slightly more than 8 pct is well within the 15 pct maximum difference allowed for extensive solid solubility. Experimental Procedures Source of Materials: Columbium powder and sheet trimmings were obtained from the Fansteel Metallurgical Corp. According to the manufacturer the metal contains less than 1 pct impurity. An analysis of the metal showed approximately 1800 ppm C in the powder while the sheet trimmings contained less than 500 ppm C. Spectrographic analysis showed minor amounts of Ca, Cr, Fe, Mn, Si, Ti, V, and Zr in both forms of the columbium. No commercial source of vanadium having the ductility and purity desired was available to the authors at the beginning of this investigation. As a result, all of the vanadium used in this study was prepared by the bomb reduction of vanadium pen-toxide with calcium employing the method reported by Long.' Yields of massive vanadium normally were about 80 pct. Chemical analysis of the vanadium prepared in this manner showed the presence of 200 to 500 ppm N and 800 to 1000 ppm C. Minor amounts of Ca, Fe, Mn, Si, Zr, Cr, and Cb were detected by spectrographic analysis. This vanadium metal was ductile and was cold rolled into 5 mil sheet. Annealing was not necessary during this rolling and the metal retained its cold-rolling characteristic after are-melting. Preparation of Alloys: The Cb-V alloys were prepared by melting pieces of vanadium sheet togethel-with columbium in the form of sheet or pellets of powder. The melting was carried out under argon in conventional arc-melting equipment employing a tungsten electrode and a water-cooled copper crucible. Each alloy was remelted three or four times, inverting the alloy after each melting in order to assure complete mixing. Alloys normally were obtained as round flat disks, weighed approximately 70 grams, and had roughly the shape of a disk 1 1/2 in. in diameter and 1/4 in. thick. Half of each alloy

Jan 1, 1955

By R. O. Williams

A recent article by Chernock, Singer, Mueller, and Beck 1 which supports the use of the integral of I sin $ d$ for comparing fiber texture data does not settle what happens to I sin ø as ø approaches zero, where I is the diffraction intensity for poles oriented 0 deg from the fiber axis. They indicate that they believe that it should approach some constant value (that is, I increases without bound) and the fact that in reality it does not was a result of the diffraction

Jan 1, 1960

By John K. Kennedy

ThE basic equations describing continuous zone-melting via the zone-void method were reported by Pfann. Using these equations, a theoretical study was undertaken in this laboratory on the effect of the variation of the significant parameters of the zone-void system. These parameters are the zone length, 1, the heater length, h, and the effective distribution coefficient, k. The object of this study was to determine the effect of these parameters on and (where a = Cp/Cf and ß = Cw/Cf, Cp, C,, and Cf being, respectively, the solute concentration in product, waste, and feed) so that, in future application of this technique to the ultrapurification of materials, the effect of 1 and h would be predictable regardless of the value of k. The basic assumptions made by pfannl were, for the purposes of this study, assumed to hold. For k < 1, the steady-state solute distribution in the stripping section and the shift in this distribution brought about by passage of a void is shown in Fig. 7 of Ref. 1. In this section the definition of k and ß precludes the possibility of ß assuming values less than unity when k < 1. In the course of this investigation it was found that computations based on Pfann&apos;s equations gave values of ß less than unity in the region 1 > k > l/h for almost all values of Ls, where Further computations showed that 6 assumes negative values when k > 1 for many values of L,, 1, and h. A check of the derivation of the stripping-section equations showed that an error had been

Jan 1, 1964

By L. B. Schmitt, N. H. Polakowski

Square bars of cold-dvawn copper, mild steel and a 2024 aluminum alloy were forced through an adjulstable gap between two hardened steel rollers by pulling or pushing. The rollers were either free to rotate or were locked in position so that conditions comparable with drawing, rolling, ad containerless extrusion could be created at will. Push or pull forces as well as roll separatirg forces were measured. Forming efficiency and coefficients of friction were determined. For- slow-rate deformation the values ot µ wrere between 0.09 and 0.14. Possibilities for further investigation are indicated. THIS work was undertaken with the aim of a) determining the principal parameters of cold drawing under simplified conditions directly, without recourse to speculative assumptions and b) comparing drawing with rolling and extrusion from the viewpoint of forces involved and deformation efficiency. Data of type a) relating forces in axially-symmet-rical drawing to die geometry. drafting schedules, material properties and lubrication conditions are abundant. Their intrinsic value is. however. limited as long as the radial die forces are unknown. On the other hand. the difficulties associated with measurement of these forces are serious as witnessed by the extreme paucity of such information."" Comparative investigations of type b) were also remarkably few and they all employed ring-shaped dies through which round bars were either drawn or pushed.2-4 Only in one case were the applied and the die splitting forces measured simultaneously.2 In order to simplify the problem, deformation under approximately biaxial conditions was adopted in the present work;. This enables both the drawing (rolling, extruding) efforts and the separating forces to be measured with reasonable ease by conventional methods. Since drawing, extrusion, and rolling can be carried out under virtually identical conditions only in a roller die. an adjustable tool of this type was constructed. The circular die profile involved a difficulty with interpreting the drawing and extrusion data. This was obviated by arbitrarily defining the angle between a contact chord and the drawing plane as the -.equivalent" die semiangle. The simplification was considered permissible since the effect of die angle was not specifically investigated. An additional conlplication was caused by the square cross section of the processed bars. This shape was selected as a compromise between the desire to have as massive as possible specimens and the capacity of the roller die. The metal was only partially restrained from spreading laterally. the flow conditions being therefore intermediate between plane stress and plane strain. On the Huber-Mises yield criterion the constrained and uni-axial yield strengths differ by up to 16 pct but the actual error due to the ignorance of the constraint factor was presumably much smaller than the maximum. In spite of these reservations it was felt that the method employed and results obtained have some merit. With certain further refinements to be indicated later, this technique can yield data perhaps more useful for checking metal forming theories than other, mostly indirect, methods. EXPERIMENTAL Materials—The metals used together with their principal mechanical properties are listed in Table I.

Jan 1, 1961

By J. Gurland

The effect of four different second-phase additions on the strength of composite alloys with a common matrix was investigated. The four compositions each consisted of 85 pct by volume of silver with additions of 15 pct of either tungsten, molybdenum, tungsten carbide, or nickel. These particular additives were chosen because of their low mutual solid solubilities with silver at room temperature, the alloys consisting essentially of a dispersion strengthened silver matrix in which the second phase is distributed randomly. Test specimens were prepared by a powder metallurgy procedure consisting of ball milling the mixed powders, compacting, and sintering at 920°C for 1 hr in hydrogen. The constituent powders were of CP quality and of particle size between 2 and 10 ?. The compacts were subsequently hot pressed at 1000 psi and 1400° in an Inconel die, coined at room temperature at 60,000 psi and finally annealed and outgassed in vacuum at 800°F. The microstructures of the alloys are shown in Fig. 1, and the microscopically observed porosity grade was A-2 or better as evaluated by ASTM Recommended Practice B 276-54. The properties of the sintered compacts are listed in Table I, and the load-deformation curves in bending are shown in Fig. 2. The samples, of rectangular cross section, were loaded at the center of 58 in. span, and the reported stress was calculated on the basis of linearly elastic behavior in order to allow the comparison of specimens of slightly different dimensions. It is apparent that the tungsten, molybdenum, and tungsten carbide alloys exhibit very similar deformation curves. The moduli of elasticity were determined from the slopes of the stress-deflection curves at small loads. The measured values agree quite well with those calculated by the strength of materials approximation proposed by Paul1 for the elastic constants of mixtures, the calculated values being 15.0, 15.0, 17.4, and 13.4 million psi, respectively, for the tungsten, molybdenum, tungsten carbide, and nickel combinations with silver. The strength of the Ag-Ni composition is appreciably lower than that of the other three alloys. The discrepancy between the two groups is accounted for by the following characteristics of deformation and failure which were observed microscopically during the tests: A) The deformation of the W, Mo, and WC alloys did not involve the second phase particles to any appreciable extent. Slip and fracture took place in the silver-rich matrix alone, although the fracture path generally skirted the particles by favoring the phase boundaries. The deformation proceeded according to the following sequence: 1) formation of small, discontinuous microcracks in areas of the matrix adjacent to a particle, 2) general slip in the matrix and extension of cracks, 3) failure of specimens by propagation of cracks through matrix. The near coincidence of the 3 load-deflection curves suggests that the nature of the second phase particles does not decisively influence the plastic behavior of composite alloys of this composition as long as the particles do not undergo any considerable deformation themselves. B) A markedly different behavior was exhibited by the Ag-Ni composition where the relatively low flow strength is associated with the low yield strength of the nickel grains. Slip in the nickel grains was first observed at a stress of approximately 10,000 psi, although failure, at a later stage, took place by the propagation of cracks through the matrix. The ductility of this aggregate, in which both components deform plastically, is appreciably greater than that of the elastic-plastic composites. In summary: 1) The measured values of the moduli of elasticity of the composite alloys under discussion are in good agreement with the "strength of materials" approximation proposed by Paul.&apos; 2) The overall plastic behavior of these particle-strengthened alloys is unaffected by the nature of the second phase particles, if the latter remain elastic. This work was supported by the Office of Naval Research. The experimental results are presented

Jan 1, 1962

By W. A. Wood, W. H. Reimann, K. R. Sargant

A study is made of the microstructural changes produced in armco and pure iron subjected to alternating torsion at amplitudes above and below the knee of the S/N curve. The aim was to identify the basic mechanisms of fatigue and to find why they should give rise to a sharp S/N knee in contrast to the type of S/N curve shown by fcc metals. It is found that the basic structural change above the knee in the iron is a pronounced cell formation in the grains, which determines irregular micro-cracks, and below the knee a dispersion of fine slip that determines a dispersed pore formation in the grains. Comparison of these changes with those in fcc metals similarly tested shows that they do not include an intermediate structural change, a concentrating of slip in narrow bands with associated slip-band cracking, that characterizes the fcc metals and accounts for their different type of S/N curve. RECENT conferences on basic mechanisms of fatigue emphasize that fatigue damage takes many forms: for example, cracking in slip bands (Thompson1), at grain boundaries and inclusions (Hempel&apos;), at precipitation zones in alloys (Han-stock, Forsythe), or at surface notch-peak effects, both hypothetical (Mott, cottrel16) and observed (Wood). Evidently it is not easy to see in this diversity a basic mechanism. At the same time the contributions suggest that some reconciliation may be possible if distinctions are drawn between three phases of the fatigue process: initiation of damage at nuclei, distribution of these nuclei, and the final macroscopic crack system. In initiation, the relevant features appear to be that nuclei may appear early, at least by 1/100th to 1/1000th of the life of a test specimen; that they may do so at many independent centers, appearing according to some observationsa as pores or voids; and that they are not necessarily self-propagating, damage spreading rather by their multiplication. In distribution, the relevant feature appears to be that they form preferentially in zones where the microstructure becomes abnormally strained (as defined more closely below). Now in these two phases the basic fatigue process should be systematic. But, at the same time, the "abnormal strains" in particular set the stage for considerable diversity in the final phase of macroscopic cracking, for where zones of abnormal strain develop will depend on what kind of fatigue deformation is applied and what kind of prior processing the test material has had. On this view it seems desirable to know what in

Jan 1, 1964

By F. E. Jaumot, R. L. Smith

Self-diffusion in zinc has been used as an instrument for comparison of the absorption and sectioning techniques as a means of studying diffusion. Single crystal as well as poly-crystal samples were used asanda the temperature range of diffusion extended from 200° to 415°C. For temperatures above 200°C, the data indicate that the results obtained from the absorption technique agree with those obtained from the sectioning technique. The effect on the values of the diffusion coefficient of electroplating vs evaporation as a means of applying the tracer was investigated and no significant difference observed. It was found that an excess or deficiency of tracer did not materially affect the results obtained from the sectioning technique, but invariably caused errors with the absorption technique. NEARLY all self-diffusion experiments and many alloy diffusion experiments have employed radioisotopes as the instrument for following the diffusion. Of the various techniques in which radioisotopes are applicable, the two most widely used are the sectioning and absorption techniques. In the former, the diffusion coefficient is obtained from a curve of log concentration vs the square of the mean penetration depth. In the latter, the diffusion coefficient is calculated from a knowledge of the decrease in activity at the surface after diffusion. In spite of the importance of knowing the reliability of the diffusion data and the widespread use of these two techniques, they had not been directly compared experimentally on the same samples. Thus, such a comparison was worthwhile. The specific system chosen for this comparison was the self-diffusion of zinc, since the metal was readily obtainable in high purity, single crystals were easily grown, and the anisotropic features of the diffusion added an additional factor of interest to the comparison. Self-diffusion in both single and polycrystals was investigated, since the possibility existed that grain boundaries and grain boundary diffusion might produce different effects for the different techniques. Also, the effects of electroplating vs evaporation as a means of applying the radioactive tracer, and the effects of applying an excess or deficiency of tracer material were studied. The general experimental procedures and the mathematical analyses of both techniques have been described previously in some detail, and only those points essential to an understanding of the present work will be discussed here. The mathematical analysis of the sectioning data requires only a knowledge of the solution of Fick&apos;s equation. where C,, is the initial concentration, C is the concentration at depth x, D is the diffusion coefficient, and p is the absorption coefficient of the solvent metal for the radiation from the solute. Having obtained F from the experiment, the value of z can be read from a plot of F vs In z, and D can then be calculated if is known. The necessity of knowing the absorption coefficient causes most of the criticism of the absorption technique. It is very difficult to measure accurately under the conditions existing in the diffusion experiment, but it is absolutely necessary, as will be indicated briefly later. Portions of this problem have been discussed in detail elsewhere." The difficulties involved in the measurement of the absorption coefficient arise from three principle factors: the physical characteristics of the absorber, the geometry, and complex radiation spectra. The first two are heavily dependent upon the third. If

Jan 1, 1957

By A. G. Rozner

TRANSVERSE rupture tests have been commonly used in mechanical investigations of brittle materials. The specimens are simple, easy to prepare, and loading presents no difficulty. Owing to the complexity of stress distribution in bending1 one can determine stresses rigorously only for the elastic range. The bend-test results, however, are at times converted into tensile-strength data, determined as maximum fiber stress. The assumption is made that for small plastic deformations the linear stress-strain relation applies. This problem was experimentally investigated by Bach3 who tested cast iron in bending and in tension and found that the maximum fiber strength obtained in bending exceeded the experimental tensile strength by a factor depending on the geometry of the tested piece. The factor varied from 1.57 for a rectangular cross section to 2.12 for a circular cross section of the tested beam. Since this work was carried out 60 years ago, the cast iron used could be expected to have been highly brittle, thus the extent of plastic deformation prior to fracture very small. We have therefore carried out a number of tests on magnesium-modified cast iron with an average elongation of -5 pct. It was hoped that the data obtained from the tests would serve as a guideline for comparing data obtained in tension and bending for brittle materials. Mechanical properties were measured at room temperature on an Instron tensile machine at a crosshead speed of 0.05 in. per min. The three-point bend test employed cylindrical bars 0.20 in. in diameter with a 1.0-in. span. For the tensile test, cylindrical tensile specimens with a gage length of 0.85 in. and a diameter of 0.160 in. were used. Results are summarized in Table I. From Table I one can see that fracture strength

Jan 1, 1965

By A. Cochardt, D. H. Feisel

HE success of the sintered aluminum powder material (SAP)&apos; in raising the maximum useful temperature of aluminum alloys has stimulated effort in investigating similar systems in which the metallic matrixes have higher melting points. Examples of such systems which have been studied are nickel-alumina,2, 3copper-silica,4 copper-alumina,4 titanium-cerium oxide,5 and 80/20 nickel-chromium,8 cobalt,= and molybdenum7 matrixes with various hardeners. Conventional precipitation-hardened high-temperature alloys are often thermally unstable in service. The original fine particles that are responsible for good strength properties grow in size at elevated operating temperatures, a process termed "over-aging." This growth of precipitated particles causes a gradual loss in strength properties. A previous paperb describes the factors that govern the process of overaging, and estimates the time required for overaging of a nickel-alloy matrix dispersion-hardened by various precipitates such as are found in current high-temperature alloys, and by alumina. These calculations indicate that nickel-base alloys hardened with Ni3Al, Tic, or TiN are quite unstable at 1340" F (727°F). Such alloys should overage within a few hours at that temperature. A nickel-base alloy hardened with alumina, on the other hand, should behave differently. It should not overage appreciably within a thousand years. It was further shown8 that the thermal stability of the oxide-hardened alloy is mainly due to the low solubility of oxygen in equilibrium with alumina in the nickel-base matrix. Since the oxygen solubility is small, little oxygen can diffuse, and structural changes require very long times. This paper illustrates the effects of time and temperature on the structural stability of nickel alloy matrixes hardened by dispersions of Ni3A1, Ni3Ti, Tic, and alumina, and of nickel-chromium matrixes hardened by alumina. Hardness measurements and metallography have been used as a measure of structural stability. EXPERIMENTAL PROCEDURE Using the best information from published phase diagrams,&apos;-l4 compositions of the Ni-Al, Ni-Ti, and Ni-Ti-C alloys were determined so as to have 5 vol pct of precipitate at 1350° F(732°C), the temperature selected to illustrate the effect of time on structural stability. Table I lists the chemical compositions of these alloys. Standard laboratory melting and alloying techniques were used in preparing ingots of the F-Series of alloys. The cast ingots, 1 3/4 in. in diam, were forged to 3/8-in. diam rods.

Jan 1, 1960

By A. Hellawell

Binary alloys of compositions intermediate between solid-solubility limits and eutectic compositions have been completely separated into primary phases and eutectic by freezing unidirec-tionally at very slow rates (10-6 to 10-5 cm per sec). The alloys examined were Pb-1 wt pct Ag, Al-20 wt pct Cu, and Al-42 wt pct Cu. The compositions and proportions were close to those expected from the phase diagrams and provided information about the solid/liquid interface at certain free zing rates. DURING the directional freezing of an alloy the solute distribution is controlled by the efficiency of mixing in the liquid,&apos;" whereas diffusion in the solid state is of negligible importance. It is known3 that mixing by convection is very efficient, but complete segregation is only achieved at very slow freezing rates4-6 or with forced stirring in the liquid. &apos; Yue9 and Yue and clark10 have previously illus- trated partial separation of primary phases in alloys close to eutectic compositions. In the present work, taking binary alloys of compositions intermediate between the limits of solid solubility and eutectic compositions, it has been possible to achieve complete separation of the primary phases by directional freezing at very slow rates. METHODS AND RESULTS The alloys concerned were Pb-1 wt pct Ag, A1-20 wt pct Cu, and A1-42 wt pct Cu. As may be seen from the relevant diagrams,11 these alloys should segregate into approximately equal proportions of primary solid solutions and alloy of eutectic compositions. Specimens, -12 cm long and 1 cm wide, were frozen in horizontal tubes by withdrawal from a furnace. The lead alloy, prepared from materials of 99.999 pct purity, was sealed into evacuated Pyrex tubes and the aluminum alloy of similar purity contained in graphite boats under vacuum. The molten alloys were seeded with some 3 cm of solid to prevent irregular initial freezing rates and the last portions to freeze were ignored. At the slow freezing

Jan 1, 1965

By J. F. Enrietto

It is shown that one cannot approximate the broad internal friction Peaks observed in the Fe-Mn-N system as the sum of a number of subsidiary Peaks and still vetain the concept of a single relaxation time. Furthermore, the approximation of manganese affectirg only nearest neighbor interstitial sites is shown to be incompatible with the experimental results. The results of this experiment show that the influence of manganese in the ferrite lattice extends over 3 to 4 atomic distances. NUMEROUS experiments have shown that the presence of relatively small amounts of substitutional alloying elements can profoundly affect the profile of the damping spectrum in the vicinity of the Snoek peak in bee metals.1-7 Dijkstra and Sladekl observed this phenomenon in Fe-Mn-N alloys where it appeared as a broadening and shifting of the Snoek peak to higher temperatures. The authors interpreted this as being the result of a superposition of two damping maxima—the normal Snoek peak, located at its usual position and having a normal half-width, and an interaction peak having a normal half-width, but occurring at a somewhat higher temperature. They prclposed that the interaction peak was caused by nitrogen atoms jumping from Fe-Mn sites to Fe-Fe sites, the Fe-Mn interstitial sites having one manganese and one iron atom as nearest neighbors, and the Fe-Fe sites having two iron atoms as nearest neighbors. They further suggested that the Fe-Mn sites had a lower energy than the normal Fe-Fe sites because of the presence of the adjacent manganese atoms. From the relative heights of the two postulated damping peaks, the dif-

Jan 1, 1962

By R. W. Gurry

In a series of charts this paper presents the composition of all gas mixtures, composed of the elements carbon, hydrogen, oxygen and nitrogen, which at temperatures from 1000° to 1800°F are in equilibrium with (1) austenite of various carbon contents, (2) iron and iron carbide, (3) graphite, (4) iron and its oxide. THIS paper presents the results of calculations made to determine the proportions of CO, CO2, CH4, H2, H2O and N2 in gas mixtures which, at temperatures from 1000" to 1800°F, satisfy, individually, the following conditions: (1) equilibrium with carbon steel of specified carbon content throughout the stable 7 iron region; (2) equilibrium with iron and iron carbide, both above and below the eutectoid temperature; (3) equilibrium with graphite; (4) equilibrium with iron and its oxide. From these data a new type of chart has been prepared which permits one to determine, from a room-temperature analysis of the furnace gas in question, the effect of the gas upon the steel at furnace temperature. Thus a guide is provided as to the carbon content which will result and as to the possibility of oxidation or sooting. All of the atmospheres commonly used in the commercial heat treatment of steel are composed of some or all of the simple constituents CO, CO2, CH4, H2, H2O and N2, and also in some cases oxygen or higher hydrocarbons. As the gas mixture is heated certain alterations in the proportions of the constituents take place, and at the temperature of the furnace the composition is, in general, not at all that of the entering gas. If equilibrium in the gas phase is presumed a calculation involving the use of certain fundamental data predicts for a certain temperature the carburizing, decarburizing, or sooting characteristics of a given atmosphere, and, upon the additional assumption of equilibrium between gas and metal, also the oxidizing ability of the gas and the ultimate carbon content of the steel. The extent to which these predictions are fulfilled will depend upon how closely the assumptions of equilibrium are realized in any particular case. Although at lower temperatures equilibrium is often not reached, there is considerable evidence indicating that above about 1000°F the approach to equilibrium in the gas phase is generally substantially complete, particularly in the vicinity of the steel which acts as a powerful catalyst in promoting reactions in the gas phase. The extent of the gas-metal reactions is commonly affected essentially by the sojourn at temperature; equilibrium with respect to carbon, for example, is accomplished simply by continuing the treatment long enough. However close the approximation of equilibrium may be in any instance, the above mentioned calculation indicates the condition of the steel at equilibrium, and at the present time this is the only basis of control of a furnace atmosphere. The effect at elevated temperature of a gas of a certain composition at room temperature upon a given steel has customarily been judged by first calculating from gas equilibrium constants the proportions of the gas constituents at the temperature of the steel, then comparing certain of these with the proportions known to be in carbon or oxygen equilibrium. This process is tedious and time-consuming, in particular because the calculation generally involves a series of successive approximations; and since some knowledge and familiarity with this type of computation are required, not everyone needing the information has been, in the past, in a position to obtain it. By making a series of equilibrium calculations, combining with fundamental data for gas-metal reactions, and plotting the results in a special way, a chart has been prepared which enables anyone

Jan 1, 1951

By D. B. Masson

THE martensitic transformations occurring in ,B AgCd as a result of cold working at room temp.. a-ture and cooling below room ten1erature have been reported by Masson and Barrett.1 These authors found that simple cooling to 127°K caused body-cen-tered-cubic AgCd containing 53.0 at. pct Ag to transform to an orthorhombic structure, while mechanical deformation at room temperature was found to induce a hexagonal structure. Furthermore, they observed that the temperature at which martensite first appeared on cooling, Ms, and that at which the transformation was complete, MI, as well as the corresponding temperatures for the reversion on heating, As and Af, could be ascertained to ± 1°K, although they report these temperatures only for the alloy containing 53.0 at. pct Ag (51.96 wt pct). In the work reported here the temperature range of the transformation on cooling was studied as a function of composition, and further consideration was given to the relationship between the original bcc structure and the transformation-induced hexagonal and orthorhomic structures. EXPERIMENTAL PROCEDURE All samples studied were in the form of annealed 300-mesh powder and were prepared from the constituent metals in the manner described previously.1 The compositions in weight and atomic pct are listed in Columns 1 and 2 of Table I. Method of determination of transformation temperature was the same as utilized previously1—measurement of the intensity of X-rays diffracted by the transformation product. A diagram of the low-temperature sample mount is shown in Fig. 1. This mount was made to fit a GE model XRD-3 X-ray diffraction unit. The powder sample was varnished to a flat surface on a copper sample holder at A. This sample holder was soldered to a brass rod, B, which was in turn soldered to a second copper rod, C. Rod C could be cooled to 78°K by inserting it into a reservoir of liquid nitrogen, D. A heater coil of nichrome wire was wound at E on the sample holder, and by varying the current through the heater a thermal gradient could be maintained along brass rod B. Sample temperatures from 78°K up could be attained and held as long as needed. The sample holder and nitrogen reservoir were insulated by Styrofoam, F, and the sample itself was protected by two radiation shields, G. The X-ray beam entered and left the sample chamber through windoys in the supporting container at H and I. Sample temperatures were measured by a calibrated copper-constantan thermocouple varnished to the sample holder just out of the beam at A. The low-temperature structure had been found to possess orthorhombic symmetry1 and the expected positions of the diffraction maxima were known. Therefore the sample was aligned in the X-ray beam and the Geiger counter of the spectrometer set to receive the most intense orthorhombic reflection without an adjacent interfering cubic reflection. This

Jan 1, 1961

By W. C. Hagel, H. J. Beattie

Phases present at 2200° and 1500°F (1204° and 816°C) were identified in sixty wrought developmental austenitic alloys possessing wide compositional variations. The bases were iron-, cobalt-, and nickel-rich as well as a base with equal parts of each. There are only two structure types previously not found in similar alloys, viz .-the Co3 W and the Fe3Al types. A molybdenum-rich monocarbide decorates dislocations with unusual clarity. Other results provide correlations between alloy composition and phas e precipitation. Grouping intermetal -lic phases into three general classes : I) geometrically close-packed, 2) topologically close-packed, and 3) bcc derivatives, the nickel base prefers the first, the iron base the second, and the cobalt base the third—each base tending to shun the other two classes. Thus, a crystal-chemistry effect previously noted by Laves and Wallbaum can he expanded for these Group VIII elemental bases. There appear to he no quaternary or higher -order structure types requiring more than three atomic species. AFTER studying aging reactions in many diverse commercial austenitic alloys1-4 as a function of detailed time-temperature variations in heat treatment, it became apparent that matrix composition influenced structure types and morphologies to a large extent. These tendencies were related4 to a crystal-chemistry effect uncovered by Laves and Wallbaum.5,6 We have now directed our efforts to exploration of the whole ternary field, covering the standard base elements—iron, cobalt. and nickel— with 10 to 20 pct Cr and moderate amounts, up to 10 pct, of the usual alloy additions. Solutioning and aging treatments were held constant with major emphasis on X-ray identification of microconstituents. The possible existence of exceptions to the Laves-Wallbaum effect, or any new phases, was sought. Phases appearing in austenitic alloys can be classified as geometrically close-packed (gcp), octahedral or nonoctahedral interstitial compounds, topologically close-packed (tcp), semicarbides, and bcc derivatives. Crystal structures of the first four classifications can be visualized as a dense packing of semirigid spheres of different sizes, while the bcc derivatives represent a less efficient packing of spheres. The Laves-Wallbaum effect involves the gcp and tcp phases. Gcp phases possess both tetrahedral and large octahedral interstices; examples are Ni3Ti(n), NiSAl(y&apos;), Co3W(E), and other ordered AB3 compounds where B atoms are smaller than A. Their precipitation is primarily intragranular, presumably coherent with an austenitic matrix, and a chief source of strengthening. Most octahedral interstitial compounds (e.g., CbC, Tic, TiN, Mo2C) have a gcp lattice of large metal atoms which accommodate small carbon or nitrogen atoms in the octahedral interstices. The compound Ti2SC, previously designated Y phase or T phase, can, with some reservation due to its partial co-valency, be placed in this category.7 The nonoctahedral interstitials (e.g., M7C3, Fe3C) represent close-packings of spheres in structures that provide larger triangular-prism interstices for carbon, since the octahedral interstices formed by chromium and iron atoms are too small. Tcp phases possess only tetrahedral interstices; examples are Laves (Fe2Ti, Fe2Cb, Fe2W...AB2), p(Fe7MO6, Co7W8.... A8B7), and (FeCr, Co2Cr3)

Jan 1, 1965

By G. Abowitz, R. B. Gordon

The velocity of sound, mass density, and thermal expansion coefficient were measured in dilute lead, tin, zinc, bismuth, cadmium, indium, and potassium amalgams as a function of composition. Measurements in the Hg-TI system extended ovev the wider range of composition, 0 to 40 at. pct TI. The sonic velocity was measured as a function of temperature. The calculuted adiabatic compressibility in all cases was found to decrease much more rapidly than would be expected on the basis of a linear variation with composition. An interpretation of the results is given in terms of changes in the Debye characteris -tic temperature of mercury on alloying and a possible change in the bonding of mercury itself. If a liquid is considered as an isotropic elastic medium, the phase velocity of a longitudinal elastic wave traveling in the liquid is given by where K is the bulk modulus, G the shear modulus, and d the mass density. G can be neglected for liquids of ordinary viscosity, i.e., approximately 1CT2 poise, because the shear stress component is relaxed essentially at once. That is, for liquids of ordinary viscosity and at frequencies of the applied stress up to several hundred megacycles, the relaxation time of the shearing process is much shorter than the period of the applied stress. Eq. [I] then reduces to The adiabatic rather than the isothermal compressibility is measured at the megacycle frequencies used in ordinary ultrasonic velocity measurements. The sonic velocity and compressibility have been determined for many organic liquids and aqueous eletroltes,&apos; and the results have been interpreted in terms of existing theories for these fluids. The velocity of sound and compressibility are important parameters in theories of the liquid state. For example, equations of state have been proposed relating the free volume of liquids to the acoustic velocity.3 Comparatively very little work has been done on the acoustic properties of liquid metals and alloys. leppa,&apos; orddon, and several other investigators

Jan 1, 1963

By B. Ramaswami, Y. Nakada, U. F. Kocks

Compression tests were performed on single crystals of aluminum, silver, gold, and a Ag-10 pet Au alloy, with height-to-width ratios from 8:1 to 1:1. As this ratio decreased, so did the amount of easy glide until, for cubic specimens of all the pure materials, it was entirely absent. Heterogeneity of deformation is proposed to he a major contribution to the explanation of easy glide in slender specimens. For comparison, one single-crystal cube of zinc was tested and showed a behavior very similar to that in tension. Beyond easy glide, tension and compression curves are very similar. It is concluded that, in this range, neither grip effects nor orientation change influence the work-hardening characteristics to any significant extent. (121) and (100) crystals of all materials had similar stress-strain curves in tension and compression, except that the stress level of the flat portion of aluminum (109 crystals at high strains mas somewhat higher in compression. These results are at variance with previously proposed mechanisms of orientation dependence by both Hosford and Kocks. The compression tests themselves are described in detail and it is shown that they are essentially frictionless and produce single slip when the crystal is suitably oriented. DEFORMATION in uniaxial compression does not necessarily give the same result as deformation in uniaxial tension, essentially because the boundary conditions chosen are practically always different. 1) The shape and size of the specimens are usually different, and any genuine effect of size on work hardening should thus influence the result. 2) The grip constraints are usually different and can vary substantially for different kinds of tests. If the compression specimen is a thin plate and the friction on the platen is large, the grip contraints are more serious than in tension and lead, in the extreme, to uniaxial strain rather than uniaxial stress. If the specimen is roughly cubical and the friction is low, the specimen is less constrained than in tension inasmuch as displacements in the contact face are allowed. 3) The orientation change of single crystals is of opposite sign in tension and in compression; it is furthermore different in detail, because the relevant orientation in a squat specimen is the normal to the contact face, whereas that in a slender specimen is the generator of the side faces.&apos; The considerable dependence of work hardening on the initial orientation in tension would suggest that the orientation change should also be very important. 4) Finally, localized deformation instabilities found in tension tests, such as necking and Lüders band propagation, are not possible in squat specimens. This is, for some investigations, a favorable consequence of the large grip influence. Even if one is not interested in any of the effects mentioned above, compression tests are often desirable just because the specimens needed are so much smaller and sturdier. For example, they have been very helpful in the investigation of latent hardening by means of alternate longitudinal and lateral compression of cubes,* and for testing

Jan 1, 1964