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By S. E. Bronisz, R. E. Tate

s-plutonium samples possessing a strong growth texture have been produced by allowing them to transform under pressure from p to a. A fiber texture with [010] parallel to the pressure axis results. The textured samples are expected to be useful in determining the effects of crystallographic orientation on the physical properties of a plutonium, and initial results of measurements of resistivity and mechanical properties are described. THE crystal structure of a plutonium1 is mono-clinic, P21/m, and many of the metal's properties should reflect the crystallographic anisotropy. Unfortunately, it has not yet been possible to grow useful sizes of single crystals of a plutonium. Therefore, few of plutonium's orientation-sensitive properties have been determined as a function of crystallographic orientation. One way to gain information about at least some of the orientation-dependent properties is to study a highly textured sample. Such samples have been produced by cold rolling a plutonium,2 but they are necessarily very small in one dimension. We have now successfully used two other techniques to produce highly textured samples, not limited to small thicknesses. METHODS OF PRODUCING PREFERRED ORIENTATION The texture is produced by causing the plutonium to transform from ß to a while under pressure. It was observed by Gardner3 that applying a compres-sive load during the transformation resulted in the formation of columnar grains of a plutonium, and Cramer4 observed a similar structure in some diffusion couples rolled in the P phase. Neither of these workers, however, investigated the subject beyond these observations. The more flexible of the two methods developed is that of compressive loading. The technique is to enclose a sample of plutonium in a die assembly before applying the load. It is possible, of course, to dispense with the die and simply press the sample between two platens. In this case, however, the unrestrained sample deforms during the pressing, making it difficult to maintain the load and to control the final sample thickness. This compressive loading technique has been used on specimens ranging from 1/4 to 3 in. diameter, with height-to-diameter ratios ranging from 5 : l to 1:6. The procedure begins with loading the sample, a right cylinder of a plutonium, into the pressing die. Plastic deformation of the sample while it is being pressed is minimized by machining the sample so that its diameter is nearly the same as that of the die barrel. Then the loaded die assembly is placed in a vacuum pressing can that fits on a hydraulic press. After a vacuum is achieved the die assembly is heated to 180°C and equilibrated. The load is then applied and the specimen and die are allowed to cool to about 40° to 50°C before the pressure is removed. The resulting sample is composed of rod-shaped a -plutonium grains, the rod axes being parallel to the cylinder axis and the pressing direction. Photomicrographs of the oriented structure are shown in Fig. 1. Although most of the specimen is composed of grains whose rod axes are parallel to the cylinder axis, a thin, peripheral layer consists of rod-shaped grains whose rod axes are perpendicular to the cylinder axis. Presumably, the highly plastic nature of p plutonium leads to approximately hydrostatic conditions during the initial stages of the P — a transformation under pressure. At this time, the grains in the peripheral layer would have grown parallel to the local force direction. During the latter stages of the transformation, the accompanying volume contraction would have eliminated the radial forces, leaving only the axial force and resulting in the growth of the observed structure. The growth texture did not form without the application of pressure. Attempts were made to produce the texture by repeating the standard temperature cycle without

Jan 1, 1965

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

The primary recrystallization textures of 11 single crystals cold rolled 70 pct were determined. The effect of crystal orientation on recrystallization behavior was investigated also and found to be large. An exception was found to the relationship that strong components of the recrystolliza-tion texture are rotated from the cold rolled texture by 30° about <110> axes, but generally this relationship was found to hold quite well. Evidence supporting oriented nucleotion was found and discussed in terms of probable active slip systems and <110> edge dislocations. THE present paper is one of a series&apos;.&apos; on recrys-tallization phenomena in cold rolled 31/4 Si-Fe single crystals and is mainly concerned with the textures produced on recrystallizing from stable end orientations. Data for the cold rolled textures of the crystals used have been reported by Koh and Dunn." Their results showed that the sharpness of the cold rolled textures varied throughout the range of stable end orientations and that the tendency to re-crystallize was related to the sharpness of the cold rolled texture, wherein the rate of recrystallization increased and the size of recrystallization grains decreased with decreasing sharpness of the cold rolled texture. In the project under consideration the cold rolled crystals involved a range of initial orientations that, together with those studied earlier,&apos; provide information on several points. The first point is whether the recrystallization texture from a (111) [112] cold rolled texture, a stable end orientation that can be approached from different directions, correlates in any way with the initial orientation before cold rolling, or whether the recrystallization texture is entirely determined by the observable features of the cold rolled texture. The second point involves a preliminary study to see if the main components of the recrystallization textures correlate with the most probable active slip systems. The third point is to determine what effect departure from slip on one slip system has on the tendency to recrystallize. Experimental Procedure Nine specimens from a previous investigation and two additional ones from thicker stock (lot D) but of similar composition to the others were used in the present work. The latter two crystals, like the nine, were cold rolled to a reduction in thickness of 70 pct and the amount of widening was determined. Depending on their primary recrystallization behavior, the cold rolled crystals were given short or long anneals at temperatures of 980°C or higher. Table I summarizes the data on initial orientations, the textures obtained by cold rolling, and the anneals given to provide samples for the present work. Fine grained specimens were thinned to 0.002 in. thickness and placed in an integrating specimen holder. Chart recordings using a transmission X-ray method and MoKa radiation were obtained for diffraction from (110) planes. This method,&apos;,3 which gives data for all of the pole figure except a central region of 30" radius, proved sufficient to give generally five, and sometimes six, of the six possible pole concentration areas of any one component of the texture. These data, therefore, were generally adequate for a positive identification of each component present. The first texture obtained for specimen B-2 was poorly defined because of too coarse a grain structure and therefore too few crystals in each component for satisfactory X-ray reflections. The same

Jan 1, 1957

By B. D. Cullity, A. Freda

It is well known that deformation by cold drawing or swaging produces a kind of preferred orientation called fiber texture in metal wires. Such textures have been extensively studied by means of X-ray diffraction, chiefly by techniques in which the diffracted X-rays are recorded photographically. This paper describes some results obtained with a new method, involving the use of a diffractometer. X-RAY METHOD Since the pole figure of a material having a fiber texture is symmetrical about the fiber axis, there is no need to present the entire pole figure. Instead, texture data can be summarized by means of a curve showing the variation of pole density along any meridian of the pole figure, if the north-south axis of the latter is made parallel to the fiber axis. The position of a pole on the meridian is specified by the angle 9 between the pole and the fiber axis (wire axis). The X-ray method1 used here to measure pole density as a function of 9 actually consists of two methods, referred to as A and B. In method a, X-rays are reflected from the wire surface. Pole densities can be measured by this method from O = 90 deg down to a limiting value which is dependent on the Bragg angle 8 and is typically of the order of 30 to 40 deg. Method B involves diffraction from the wire cross section and covers a range of 0 values from 0 up to an angle sufficient to overlap the measurements made by method A. By a combination of the two methods, a complete pole-density curve can be obtained. However, method A alone, which requires no specimen preparation other than etching, can often reveal enough of the pole-density curve to provide complete information about texture components. Both methods require that the measured diffracted intensities be corrected for changes in absorption and diffracting volume with changes in 9. A11 intensities I reported in this paper are corrected diffracted intensities; they are propor-

Jan 1, 1960

By H. S. Cannon, F. N. Rhines

IT. H. Hausner( Sylvunia Electric Products Inc., Bay-side, N. Y.)—The results reported by the authors are interesting because they contribute some information on the principles of sintering and also because of a certain practical value for the manufacture of powder . metallurgical parts in production. Pressed powder compacts are frequently sintered in a boat in several layers so that the lower layers are actually sintered under the weight of the upper layers and, therefore, are frequently deformed. The authors gave information on this deformation process by determining the effect of the load on the density. The experimental setup of the authors, however, has a disadvantage—that the sintering occurred in a cylindrical container so that the deformation was stopped in the direction of the diameter. The authors should have rather called this a study of hot-pressing than of sintering. I want to call the attention of the authors and others interested in sintering under load to the experimental work described by Dawihl and Rix.&apos; These authors sintered cylindrical compacts under a lengthwise ten-sional load of 0 to 25 g and found that the shrinkage in length and diameter changes considerably with the load, but that the volume shrinkage is affected very little by the load. H. S. Cannon (authors&apos; reply)—We wish to thank Dr. Hausner for calling attention to the experimental work of Dawihl and Rix. The fact that they found volume shrinkage little affected by varying tensional loads during sintering seems to support the contention that the forces due to loading are equivalent to and additive to the forces which cause densification. This contention is the basis of our comparison of sintering and creep.

Jan 1, 1952

By E. C. W. Perryman

The recovery of X-ray line broadening, hardness, and electrical resistivity from cold worked AI-Mg alloys has been investigated. The results, together with those from density measurements, suggest that magnesium atoms freeze in the excess vacancies formed by cold working, and that this affects the climb of dislocations during the recovery process. PREVIOUS work1, " has shown that while 1 pct Mg increases the activation energy for recrystalliza-tion, it decreases the activation energy for the recovery of mechanical properties and decreases the subgrain size both after cold working and annealing. A similar result has been reported by Varley2 for an A1-2 pct Mg alloy. With plastic deformation at high temperatures, McLean and Farmer&apos; and Rachinger have found that magnesium appears to retard the motion of dislocations and, furthermore, they find little or no effect of magnesium on the size of subgrains formed during high temperature deformation. In view of the apparent contradictions as to the effect of magnesium on subgrain size, the recovery process in Al-Mg alloys has been investigated more thoroughly by studying the annealing out of X-ray line broadening, hardness, and electrical resistivity from alloys cold worked at room temperature. Material Used—The chemical analyses of the alloys are given in Table I. Fabrication—The material used was cold rolled 20 pct at room temperature, the grain size prior to the last cold rolling operation being similar to that used in previous work; i.e., 230. The experimental procedure for annealing, determination of X-rav half-veak breadth. hardness measurement, electEica1 resistivity, and density and metallographic examination was exactly the same as previously described." Variation of X-Ray Half-Peak Breadth with Annealing Time—Isothermal annealing curves at 100°, 200°, and 250°C were obtained for material cold worked 20 pct. The half-peak breadth of the (333) Ka, line directly after cold working is shown as a function of magnesium content in Fig. 1. Only with the 2.87 pct Mg alloy was overlapping of the a, and n.. reflections observed to any appreciable extent. To separate these, Rachinger&apos;s method&apos; was used. Typical isothermal annealing curves are shown in Figs. 2 and 3 for 100" and 200°C, respectively. These curves are similar to those obtained previously for super-purity aluminum except that the

Jan 1, 1957

By M. S. Burton, G. V. Smith, A. Rosen

The kinetics of re crystallization and the effect of recovery on recrystallization of pure iron were investigated within the temperature range of 517" to 632 OC. Grain growth and activation energies were also studied. Two stages can be distinguished during recrystallization; the first is gvowth-controlled and the second is nucleation-controlled. The extent to which the first stage succeeds before the second stage begins depends on both temperature of recrystallization and temperature of recovery. The softening of cold-worked metals and alloys due to transformation of the deformed crystals to strain-free equiaxed grains during annealing is well-known, and early inestiators established that recrystallization kinetics is strongly influenced by minute quantities of impurities. Generally, it is believed that impurities decrease the rate of recrystallization and the rate of grain growth. To understand the basic phenomena of recrystallization, investigations should be on pure materials. Most of the research on high-purity materials has been on metals having the fee Bcc materials, and especially high-purity iron, have been studied only in recent years. It is known that recovery may influence recrystalliation;" however, no general description of the influence, applicable to all materials, has been presented. This paper presents results of a study of the recrystallization kinetics of high-purity iron, after 60 pct cold deformation by drawing, with particular reference to the influence of recovery on the rates of recrystallization and grain growth. From observations of these rates, conclusions are drawn concerning nucleation. MATERIAL AND EXPERIMENTAL PROCEDURE Preparation of Material. High-purity iron, prepared by zone refining of vacuum-melted electroiytic iron at Battelle Memorial Institute under sponsorship of the American Iron and Steel Institute, was used in this study. Table I gives the reported chemical analysis of the material, taken at a point near the last molten zone and thereby rep- resenting the maximum impurity level for the entire bar. Prismatic specimens, approximately 10 x 10 X 50 mm, were sawed from the 50-mm-diam bar, perpendicular to the zone-refining direction, and turned to cylindrical shape. These specimens were sealed in quartz capsules under vacuum, approximately 10"e mm Hg, austenitized at 930° C for 15 min, slowly cooled, removed from the capsules, and cold-worked in air by swaging to approximately 20-pct reduction of area. The encapsulating, austenitizing, and swaging operations were repeated two additional times, after which the samples were encapsulated, austenitized, and cold-drawn to 60-pct reduction of area. A further vacuum anneal at 630°C for 120 min and cold drawing to 60-pct reduction of area produced wire 2.8 mm in diameter. The drawn wire was electropolished to remove deformed material on the surface, after which it was sawed into 4-mm-long specimens for the recrystallization study. Microscopical examination before the final cold reduction revealed equiaxed grain structure with very fine grains in a thin layer near the surfaces of the specimen and nearly uniform ASTM 3-4 grain size in the center. Recrystallization Heat Treatment. a) Direct Recrystallization of Cold-Worked The 60 pct cold drawn iron specimens were recrystallized at five temperatures, 517, 556, 590°, 612, and 632C, in a lead bath covered with graphite (the temperature was controlled to 1°C). Specimens were treated for twelve different times at each temperature, and all were water-quenched after heat &eatment. b) Recrystallization Following Preliminary Recovery Heat Treatment. After cold working, specimens were sealed into quartz capsules under vacuum, 105 mm Hg, and recovery-annealed at 362", 400", and 440°C for 20 hr prior to recrystallization. No evidence of recrystallization was found

Jan 1, 1964

By B. N. Das, P. A. Beck

THE o phases have a complex tetragonal structure with Lo/ao = 0.52 and 30 atoms per unit cell.1 A large number of such phases are now known to occur in various binary systems of the transition elements and they exhibit the following typical features: 2,3 The composition of binary o phases is variable, ranging from approximately A4B to ABI. With only a few exceptions, in the o phases the A-ele-ment comes from the V- or Cr- group of the periodic table, while the B-elements are from the Mn-, Fe-, Co-, or Ni- group. In the first long period the corresponding o phases of the V- and Cr-series have approximately the same compositions. However, as the B-element changes from Mn to Fe to Co to Ni, the mean composition shifts monotonously toward higher A-contents.2-4 For example, if the mean compositions of the various o phases with vanadium are compared with each other, the composition shift mentioned above becomes plainly visible: V 30Mn0 80 Vo.45Feo..,, Vo .,Coo. 45 and Vo.5Nio.3. Similiar composition shifts, although not the same composition values, were observed in u phases formed by second and by third long-period transition elements.3&apos;4 This behavior, very characteristic of o phases, is in rather sharp contrast to the usually quite well-behaved stoichi-ometry of the Laves phases. In the latter, the AB2 stoichiometry predominates, with A the large atom and B the small atom.= The p phase occurs in the four binary systems of Mo or W with Fe or Co. On the basis of their crystal structure determination, Arnfelt and westgren6 ascribed to the p phase in the Co-W system the ideal composition W,Co7. Since all four binary pphases have nearly the same composition, it would seem quite plausible that some definite stoichiometry such as A6B7, might be characteristic of this phase, as AB2 is of the Laves phases. On the other hand, it has been noted,7 that the phases occur at average electron concentrations near to those at which the various cr phases are found. Also, it has been pointed out by Shoemaker and associates8 that structurally the a phases and the p phases are somewhat related to each other; both of these structures may be described in terms of suitable stackings of quasi-hexagonal layers&apos;of atoms. By studying a suitably chosen ter- nary phase diagram, one might expect to be able to find out which one of the two conditions, the analogy with the o phase or the constant ratio between the number of large atoms and the number of small atoms in effect governs the behavior of the p phase. Several isothermal sections of ternary systems containing o phases have been investigated. In all cases where two binary o phases occur, these were found to be connected b a more or less straight ternary o phase field.7&apos; &apos;10 Such elongated o phase fields were also found in ternary systems in which only one of the limiting binaries is known to contain o phase. In this manner a latent o forming tendency could be detected and the virtual composition of a "binary o phase", which does not actually occur as such was approximately determined by extrapolation. The behavior of the phases, including their composition shift, is analogous to that of the classical electron compounds, as described by Hume-Rothery.11 In order to decide whether the p phase is essentially a "size compound" like the Laves phases, where a fixed stoichiometric ratio is quite generally maintained between the "large atoms" and the "small atoms", or whether the p phase is typically an "electron compound" in the same sense as ois, it was decided to investigate an isothermal section of the Mo-Mn-Co system. The Mo-Co system12 and the Mo-Mn system13 each are known to have a binary o phase. It could be therefore expected that a ternary o phase field will connect these two binary cr-phase fields. The p phase is known to occur in the Mo-Co system. If the p phase should turn out to form an elongated phase field extending deep into the ternary system, the following considerations mighto apply. The atomic radius of manganese (1.314for C.N.12) is between the va,lues for Mo (1.40Afor C.N.12) and for Co (1.26Afor C.N.12). If it is assumed that p is a "size compound", and that Mn is substituting for the smaller Co atoms in the p-structure in the ternary system, the y-phase field might be expected to extend parallel to the Mn-Co binary line. If Mn is substituting for the large Mo atoms in the p-structure, the p-phase field may be expected to extend parallel to the Mn-Mo binary line. On the other hand, if the p-phase turns out to be an "electron compound" like o, the ternary p-phase field should extend parallel to the ternary o -phase field connecting (Mo,Mn)owith (Mo, Co) a

Jan 1, 1961

By B. D. Cullity

A distribution of residual stress after plastic elongation is proposed, in which the bulk of the material is strained in compression and a very small portion in tension, This distribution is shown to account both for the X-ray observations and for the effect of plastic straining on magnetic losses in silicon steel. The regions left in compression are tentatively identified with the interiors of the sub-grains revealed by the electron microscope. THIS paper is concerned with the general problem of the nature of the residual stress which is produced in metals by plastic elongation. A particular stress distribution will be suggested which accounts for the main X-ray diffraction observations which have been made. It will also be shown that certain magnetic measurements made on silicon steel can be understood in terms of this stress distribution. X-RAY OBSERVATIONS Uniform straining of a crystal lattice (macro-strain) causes a diffracted X-ray beam to shift its position, and nonuniform straining (microstrain) causes line broadening. If a bar of metal is plastically elongated in the longitudinal x direction and then unloaded, diffracted X-ray lines are observed to be both shifted and broadened.&apos;-= Although the observed line shift indicates the presence of macro-strain, experiments have shown that no macrostrain, in the usual engineering sense of the term, exists.5"7 For example, removal of a layer from one surface of a stretched and unloaded bar does not produce curvature in the remainder of the bar 5&apos;7 Fig. 1 shows the variation of lattice strain in the x direction, as determined from X-ray line shifts, with the applied stress in the same direction. The curve ABC is the normal stress-strain curve of the material, AB being the elastic portion and BC the plastic. In the elastic region AB, the strain measured by X-rays, called the lattice strain, and the strain measured mechanically are both proportional to the applied stress, and both return to zero when the applied stress is removed. Above the elastic limit the lattice strain would be expected to continue to increase along the line BD. Actually, it increases less rapidly with respect to stress, or even decreases, as shown by BE. If the applied stress is then decreased, the lattice strain decreases along EF, which is parallel to AB. As a result, there is a compressive residual lattice strain FA after unloading. STRESS DISTRIBUTION. Since a stretched and unloaded bar does not contain macrostress, it follows that the observed line shift must be due to a special distribution of mi-crostress. Such a distribution is shown in Fig. 2, which shows the variation of the stress u, across a stretched and unloaded bar. The material is assumed to consist of two kinds of regions: regions C, stressed more or less uniformly in compression, comprising the bulk of the volume of the material and responsible for the observed diffrac-

Jan 1, 1963

By E. P. Abrahamson II

The effect of transition elements which form binary solid solution upon the recrystallization temperature of zirconium has been investigated. All additions raised the recrystallization temperature. A correlation is obtained between the logarithm of the rate of change of recrystallization temperature with atomic percent solute and the free atom ground state electron configuration of the solute element. ThE work of Abrahamson, et al., on dilute binary solid-solution alloys indicated a correlation between the free-atom ground state electron configuration of the solute and either the brittle-ductile transition or recrystallization temperature. These studies were carried out on bcc base materials. The implication is that the outer s and d electrons of the solute are the prime determinant of the absolute rate of change of recrystallization or transition temperature. Furthermore, the limit of linearity has been shown to be a function of solute electron configuration for recrystallization in iron and vanadium. To date no Complete systematic recrystallization study of dilute binary zirconium base alloys has been made. It is the purpose of this study to note whether the change in solvent structure from bcc to hcp will influence the correlation. It was also desired to learn more of the role of the electron configuration of the solvent on recrystallization temperature. PROCEDURE All alloys were made using 99.87 pct Zr with 0.01 Cr, 0.04 Fe, 0.006 Hf, 0.003 Mg, 0.003 Mn, 0.003 N, and 0.080 0 (132 BHN). The solute elements were 99.9 pct pure. According to the published binary phase diagrams6 and metallographic examinations at X750, all alloys used were solid solutions. The alloys were arc melted and remelted six times in the form of cubic 200-g buttons under an argon atmosphere. They were then hot pressed at 950°C to 0.450 in., upset pressed to 0.350 in., and annealed at 800°C for 1 hr. The specimens were then Blanchard ground to 0.250 in., removing 0.050 in. from each side. The grain size of the material at this stage was found to be 8000 100 grains per sq mm. The specimens were then cold rolled to 0.130 in. and cold pressed to 0.125 in., yielding 50 1 pct cold work. All alloys were then chemically analyzed for the principal addition. The interstitial contents remained at the values of the starting material when checked on random alloy specimens. The rolled sheet was cut into 6.75 by 0.25-in. lengths and heat treated in a gradient furnace for 1 hr. The gradient was 250o to 900°C over the 6-in. length, recorded continuously by six thermocouples resting on each specimen. Control was 3oC, accomplished at the hot end. The recrystallization temperature was determined metallographically using polarized light. The criterion chosen was the point on the specimen showing the first recrystallized grain at a constant magnification, X200. Specimens were repeated, and the agreement was found to be 3°C. RESULTS Three different pure zirconium specimens were tested, and the recrystallization temperature was

Jan 1, 1962

By Hsun Hu, R. S. Cline

A detailed studj) of texture formation in 2 pet Al-Fe single crystals with initial orientations of approximately (111) [112], (112) [111], and (112) [111] was made by examining the textures developed on the surface and at various interior sections of the crystal after rolling to various amounts. Depending&apos; upon the initial orientation of the crystal, the surface and interior textures may differ only in sharpness, or may differ essentially in orientation. The orientation of the (111) [112] crystal does not change upon rolling up to 70 pet, but after rolling more than 90 pet a distinct component of (001) (110] orientation is developed. The texture formed in the two (112) (1111 type crystals consists of (111) (1121 and (001) (1101 components. The latter, however, is largely confined to the surface layers. The textures formed on both sides of the crystal are identical, and the texture composition profile is approximately symmetrical with respect to the central section of the strip thickness. The formation of these texture components is analyzed. DURING the past seven or eight years, deformation and recrystallization textures in rolled Si-Fe single crystals have been extensively studied by various investigators.1-7 From these studies, much knowledge on texture formation in bee crystals of various initial orientations was obtained. However, these results also raised many questions, regarding particularly the correlation between deformation and recrystallization textures, as well as the deformation texture itself of some particular crystals. To take a (111) [112] type crystal as an example, it was shown by Dunn and Koh2, 3 that this orientation does not change during deformation by rolling. This finding is consistent with the conclusion reached by Barrett and Leven-son8 with respect to iron crystals that (111) [112] is one of the stable end orientations. However, different recrystallization textures were observed by Dunn and Koh3 in (111) [112] type crystals of different initial thickness, which widened differently during rolling even though their deformation textures were identical. Another interesting example, also from the results of Dunn and Koh2&apos;3 is that of texture formation in a (112) [111] crystal. This crystal developed a two-component deformation texture of (111) [112] plus (001) [110]. Its recrystallization texture, however, was found to be predominantly (110) [001], which is related to the (111) [112] component by a simple [110] rotation. This crystal, therefore, behaved as if the other deformation texture component, (001) [110], were not present. There are also discrepancies among the results of different investigators, as well as numerous unexplained fine features of the deformation texture of crystals of various initial orientations. In order to have a better understanding of all of these points, a detailed study of deformation textures is greatly needed. One of the obvious things that has been completely overlooked in previous texture studies is the possible effect of surface texture. All past work on the texture of Si-Fe single crystals was conducted in a rather simple manner, i.e., the rolled crystals were etched to a very thin sheet; then their textures were examined by transmission X-ray techniques. For recrystallization texture studies, unless precautions are taken by etching off a sufficient amount of the surface layer before annealing, the texture developed in the interior may be affected by the surface layer, which may well have a different initial texture and which may have undergone recrystallization earlier than the interior of the specimen. Because of this effect, it is now planned to reexamine the texture of various rolled and annealed single crystals at the surface, and at various sections below the surface by using reflection techniques. In some cases, both surfaces of the rolled crystal will be examined. In one of Dunn&apos;s early papers,9 he noted that at an early stage of rolling the crystal seems to divide roughly through the middle to become a sample which in effect consists of two layers having some what different orientations. This effect has never been further explored. The investigation described in the present paper constitutes the beginning of a series of thorough investigations of texture formation in deformed bee single crystals designed to clear up some of the uncertainties which have been discussed. We have chosen a high-purity 2 pet Al-Fe alloy for this investigation. It is known that the allotropic transformation of iron is eliminated by alloying with approximately 1petAl. Such an alloy, being very similar to silicon ferrite, can be heated to the solidus temperature without phase transformation. One reason for choosing A1-Fe instead of Si-Fe for the present investigation is that we have been able to make single crystals of a vacuum-melted high-purity A1-Fe alloy by the strain-anneal method without much difficulty, but were not successful in doing so with a vacuum-melted high-purity Si-Fe alloy. For many research purposes,

Jan 1, 1962

By H. I. Aaronson, H. A. Domian

The self-diffusivity of Ag10 has been measured as a function of temperature and composition in AgMg. a CsCl-type intermetallic compound with a substitutional defect structure on both sides of the stoichiometric (50 at. pct Mg) composition. These measurements show that In D increases linearly, and both In Do and Q decrease linearly with deviation from stoichiometry. The slopes of these lines are significantly steeper in magnesium-rich alloys. Equations for the variation of Q with composition have been derived by application of the theory of random walk processes on the assumption that diffusion in compounds of this type takes place by the six-jump cycle mechanism of Huntington, Elcock, and McCombie. The favorable agreement obtained with experiment furnishes fresh support for the correctness of this assumption. A principal result of this treatment is that. although the concentration of vacancies is considerably higher in the silver sublattice than in the magnesium sublattice, the acfivation energies for movement of the magnesium sublattice vacancies are so much lower that these vacancies are responsible for effectively all diffusion of silver in this compound. A tendency for vacancies of both types to be kinetically bound to wrong atoms is also noted. THIS study was undertaken to examine the influence of substitutional defects upon self-diffusion in an intermetallic compound, AgMg, with a CsCl-type crystal structure. The CsCl structure is exception- ally simple. At the equiatomic or stoichiometric composition in a binary alloy, it consists of two interpenetrating simple cubic sublattices, each of which is exclusively populated by the atoms of one species. When atomic size and other factors are favorable, deviations from stoichiometry can be entirely accommodated by the substitution of atoms of the species present in excess of 50 at. pct on the sublattice of the other species on a one-for-one basis. Under this condition, the only vacancies present are those formed by thermal activation. The excess atoms thus incorporated into the sublattice of the minority species may be considered as substitutional defects in this sublattice. Several X-ray studies have shown that the defect structure of AgMg is entirely of the substitutional type on both sides of the stoichiometric composition.1"3 The thermodynamic investigation of Kachi indicates that, aside from a low level of thermal disorder and these constitutional defects, order is maintained to the solidus temperature. This compound is therefore a particularly useful vehicle for a study of the influence of substitutional defects upon diffusion kinetics. Other advantages of AgMg for this purpose include: the broad composition region, as much as approximately 10 at. pct on either side of the stoichiometric (50 at. pct Mg), in which the compound is stable; the comparatively low temperature range of the solidus (820°C and below),5 making diffusion anneals near this range experimentally convenient; the reasonably good machinability of the compound, permitting utilization of the standard sectioning method of radiotracer analysis; and the availability of a good tracer, A for one of the constituent species. While this investigation was in progress, Hagel and westbrooks reported data on the self-diffusion

Jan 1, 1964

By Joseph B. Darby, Paul A. Beck

IN isothermal sections of several ternary systems, the a-phase was found1 to extend in the form of a relatively narrow elongated field, connecting the U-phases that are present in the adjoining binary systems. This was interpreted in accordance with the conception that the U-phase is an electron compound and the ternary U-phase fields were shown in several systems&apos; to extend approximately in the direction of constant average d-shell electron vacancy number per atom. &apos; However, in the various isothermal sections of the Fe-Cr-Mo system" the ternary a-phase field was

Jan 1, 1958

By W. L. Finlay

Size effects in quenching steel are particularly prominent and well recognized because of the existence of a critical cooling rate separating nuclea-tion and growth transformations, as exemplified by the formation of pearl-ite, from the shear type of transformation characterizing the martensite reaction. The absence of a similar, sharply demarcating cooling rate is characteristic of precipitation hardening systems and size effects in these are correspondingly less prominent. This paper is concerned with a size effect in high-purity, precipitation-hardenable alloys which appears not to have been recognized previously. This effect is believed to result from the thermal fluctuations which inevitably occur in quenching a specimen of finite size into a cooling liquid rather than from the existence of a critical cooling rate. QUENCHING "ANOMALIES" The precipitation hardening literature contains many references to so-called anomalous quenching and aging results. By "anomalous", investigators usually meant that their alloys did not consistently harden on aging after quenching according to some anticipated pnttern: not infrequently virtually no age hardening occurred with compositions known to be precipitation-hardenable. Perhaps the most prominent series of anomalies was reported over a 15-year period by Gayler and coworkers on aluminum-copper.l,2,3,4 Working with silver-rich copper alloy, Cohen5 secured some very interesting Rockwell F hardness changes of from 1-5 Rockwell points between the first peak and valley. Fink and Smith borrowed one of Cohen&apos;s specimens and, following his heat treatment and quenching practice to the letter, secured6 very different results in which only one peak was obtained and in which the hardness level at the aging lime of Cohen&apos;s first peak was 20 Rockwell F points higher. Fink and Van Horn7 encountered serious deviations in age-hardening high purity aluminum-zinc alloys. They stated that "the discrepancies were larger than might be expected from possible experimental errors in the Brinell readings." Geisler, Barrett and Mehl8 likewise encountered anomalous hardening results in aluminum-silver alloys, securing quite different age-hardening curves from two identical specimens. They stated that "the treatments of these samples had been the same, so that the different behaviors could be attributed only to accidental variations in the quenching practice."

Jan 1, 1950

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 L. F. Pease, J. H. Brophy

A phase diagram for the Ta-Zr system is presented. The system is of the minimum-melting point type with the 0-zirconium phase decomposing monotectoidally at 785°C and 95.5 at. pct Zr. The minimum solidus temperature is 1875°C and the temperature of the top of the monotectoid loop is 1775°C. Techniques employed included X-ray diffraction and fluorescmce, electron microprobe analyses, diffusion couples, metallography, and melting-point measurements. Errors due to interstitial solutes and in melting observations are particularly common in this system, and their occurrence is discussed. SEVERAL versions of the Ta-Zr phase diagram have been reported in the literature.lm7 Williams et al.&apos; report a diagram of the minimum-melting point type with a monotectoid reaction at 800°C and 12 wt pct Ta. The minimum in the solidus occurs at 1820°C and 25 wt pct Ta, while the top of the monotectoid gap is located at 1780°C and 80 wt pct Ta. The experimental techniques employed were metallography, electrical resistance variation with temperature, dilatometry, X-ray diffraction, and direct observation of melting by the technique of Pirani and ~lterthum.&apos; Experience in the Nb-Zr phase diagram has shown that small changes in the interstitial content can cause large shifts in the positions of the phase boundaries. Small amounts of inter -stitials can cause similar changes in the Ta-Zr system and may be responsible for the wide variations in the phase diagrams previously reported.&apos;-&apos; The authors15 have found that alloys containing 0.75 wt pct 0 and 1.0 wt pct Ni with tantalum contents from 19 to 85 at. pct often contain a lamellar or cellular precipitate after annealing above 1400°C. This precipitate is very similar to that reported by pollack,12 Ralls," and Donlevy17 for the Ni-Zr system. In the present investigation, a wider variety of experimental techniques and improved alloy purity were applied to the resolution of errors in diagrams for this system as they now appear in the literature. New results have been obtained in the areas of alloy homogeneity and purity. Errors in the common techniques of direct melting observation in binary alloys have been demonstrated. In the commercially important high-tantalum region, the more accurate metallographic method of solidus determination has been employed. EXPERIMENTAL PROCEDURE Nominal analyses of the materials employed are given in Table I. The zirconium was low hafnium reactor grade iodide crystal bar, and the tantalum was in the form of high-purity sheet. Powders were impossible to use because of gas content. Alloys were melted on a water-cooled copper hearth, with a thoriated tungsten-tipped nonconsumable electrode in 2/3 atm of Zr "gettered" argon. Alloys were

Jan 1, 1963

By J. T. Norton, N. J. Grant, I. S., Servi

Coarse grained high purity aluminum was tested in creep at temperatures of 400° to 1200°F to develop subgrain structures. Measurements of subgrain size, distribution, and rotation were made from X-ray diffraction patterns. Subgrain size and distribution were checked metallographically and the size was compared with average slip band spacing. The slip family was determined for several specimens. THE interest and research recently evident abroad in the role of subgrain formation and polygon-ization as a contribution to the creep of metals at elevated temperatures is deserving of greater attention in this country. Such metallic subgrains can be defined as macroblocks existing within the grains. The general observation has been that the macro-blocks which belong to the same grain have a maximum difference in orientation of a few degrees. In spite of the considerable amount of work that has been done since Jenkins and Mellorl observed the "division of existing crystals into smaller units when deformation occurs at an annealing temperature," the subject of subgrain formation is only now receiving truly active discussion and investigation. The existence of subgrains has been revealed by metallographic methods, as in the work of Jenkins and Mellor,1 and by X-ray methods, first applied to this problem by Homes.&apos; Hirst3 and Calnan and Burns4 applied the back-reflection Laue technique to the study of coarse grained specimens. Wood et al.5 and Greenough and Smith&apos; examined the ring obtained with a back-reflection camera for the study of fine grained specimens. In addition to the above, the transmission technique was used by Wood.6 A special technique was developed by Guinier and Tennevin8 in order to improve the resolution. Metallographically, the subgrains have been observed directly on the surface of deformed specimens by Wood et al.,3 or have been made evident on repolished surfaces by applying a suitable etching reagent. The latter technique, first suggested by Lacombe and Beaujard,9 was then improved by Wyon and Crussard.10 Subgrains can be formed in single crystals after small amounts of bending followed by heating after this cold work, or during deformation at elevated temperatures. The first phenomenon was analyzed by Cahn11 for the simple case of pure bending followed by annealing. Cahn suggested a mechanism of subgrain formation based on the dislocation theory and called this phenomenon "polygonization." He extended this mechanism to the more complex case of local bending, such as the bending which may occur when a polycrystalline specimen is deformed in tension. Cahn&apos;s suggestion was later found quite consistent with the results obtained by Dunn and Daniels." An explanation has been presented recently regarding the formation of subgrains during deformation at elevated temperatures by Chang and Grant.&apos;" In general, there are two schools of thought on the subject. One, according to Wood et al.,5 is that subgrain formation is a mechanism of deformation which is operative under certain conditions in the same way that the slip process is the mechanism of deformation which is operative under other conditions. The boundaries between the subgrains undergo a viscous flow which contributes substantially to the deformation of the material. The second, according to Cahn,13 Wyon and Crussard,10 and Chang and Grant,18 is that subgrain formation is the effect of simultaneous deformation and annealing and is,

Jan 1, 1953

By Laurence Pellier

Electron microscopical studies were made of the effect of sensitization at 1200oF on a Type-.104 stainless steel with high carbon and low nitrogen and oxygen contents, after solution annealing and after cold working. The loci of the carbide precipitates in the early stages of sensitization were followed in dry stripped plastic replicas. Some observations were made by direct electron transmission on thinned films. Intragranular dislocations showed a high degree of stability through the annealing necessary to produce sensitization. I HE present work was undertaken to determine the effect of sensitization, at 1200°F, for 1/2 hr, on the electron microstructure of a Type-304 stainless steel with high carbon, and low nitrogen and oxygen contents, after solution annealing and after cold working. Many electron microscopical studies of sensitization of 18-8 stainless steels have already been made. Most of them utilized extraction replicas, from which the morphology and composition of the precipitated carbides could be established.&apos;-" ry stripped replicas were seldom used for such studies, although it was demonstrated that they are applicable, in general, to EurveYs of the general microstructure of many alloys&apos; and, in particular, to the observation of precipitated carbides in austenitic stainless steels.3

Jan 1, 1963

By H. H. Podgurski, Hsun Hu

Large cryslals of high-purily iron (99.996+ pcl) cannot be obtained by the usual strain-ameal technique. Repealed phase transformation by thermal cycling prior to crilical deformation improves the capabilily of cryslal growith but fails to yield satisfactory crystals. Imperfect columnar crystals can be produced by the phase-transition method. The addition of a small amounl (0.005 wl pet) of nilrogen IT was reported&apos;-4 that for metals of very high purity the usual procedures of the strain-anneal technique fail to produce large crystals. This was eliminates practically all the difficulties in crystal growth by the normal strain-anneal procedures. An actual example is presented, showing that most parts of a strip have been converted into a large crystal by this method. The addition of nitrogen, which can be removed from iron with less difficulty, is believed to be more desirable than carbon additions for the same purpose. thought to be due to the strong tendency for recovery in the high-purity metals: hence the critically strained matrix undergoes polygonization instead of recrystallization upon annealing for crystal growth. Talbot1,2 succeeded in overcoming this difficulty by adding 0.03 to 0.04 pct C to high-purity iron before critical deformation. followed by annealing in hydro-

Jan 1, 1965

By Nicholas J. Grant, H. C. Chang

TRANSCRYSTALLINE fracture surfaces of the cleavage type have been examined by microscopy and X-rays for several metals.&apos; These investigations revealed that the fractured surfaces were not flat and invariably had cleavage and other deformation markings on them. On the other hand, the study of inter crystalline fracture surfaces has been limited. Perryman, in a recently published paper on the inter crystalline fracture of ß-brasses,&apos; found that a thin layer of heavily deformed metal was invariably associated with these surfaces. Furthermore, the thickness of this layer was found to depend on the orientation of the grain boundary surface with respect to the applied stress. The mechanisms of grain boundary sliding and intercrystalline fracture have been presented in two previous papers,which described certain aspects of the deformation of a 20 pct Zn-A1 alloy. It is the purpose of this paper to present some observations on the structure of intercrystalline fracture surfaces and to correlate the structure of such surfaces with the mechanism of intercrystalline fracture. Experimental Techniques—The high purity 20 pct Zn-Al alloy was generously supplied by the Research Laboratories of the Aluminum Co. of America. Two sizes of specimen were used; the first had two parallel flat surfaces of dimensions 1x0.17x0.09 in. and the second was round with a 0.25 in. diam. A grain diameter of 1 to 3 mm was obtained by annealing the specimens at 1000°F for 24 hr. The specimens were then air cooled. The specimens were subjected to creep at 500°F and 2300 psi. The rupture times ranged from % to 3 hr, with one room temperature tensile test. It has been mentioned previous1y" that the intercrystalline fracture surfaces of this alloy, when tested under the conditions given above, are sharply defined. In the optical examination of the fracture surfaces, whenever possible, magnifications of at least X250 were used. The locations of the regions examined, both optically and by X-rays, were selected to give several fracture surface orientations with respect to the stress axis and to the specimen surfaces. This was possible for the X-ray studies since the grain diameters were large compared to the X-ray beam. A film to specimen distance of 3 cm, a 1 mm pinhole and Cr radiation were used for the Laue back reflection pictures.

Jan 1, 1957

By R. G. Aspden

The cold rolling and annealing textures were studied for 3 pct Si-Fe grains initially (001) [hkl]. A concentration of (001) [loo] primaries were observed only in the annealing textures of crystals initially having [loo] within 8 deg of the rolling direction. Eke annealing textures of the (001) [I101 cold rolling textures were sensitive to the initial orientation of the grains. Single crystal data were used to explain the formation of (001) [loo] in poly-crystalline malerial. CUBE texture formation in 3 pet Si-Fe sheet occurs during the final high temperature anneal. Its formation is dependent on the proper distribution of (001) plane primaries with reference to the rolling direction&apos; and on the growth of these primaries by secondary recrystallization. The selective driving force for these primaries with (001) within 7 deg of rolling plane is derived from the difference in surface energy between the annealing atmosphere and the crystallographic planes exposed at the surface of the sheet.&apos;-= The alignment of [loo] directions of (001) secondaries with the rolling direction is required for optimum magnetic characteristics7 and is dependent on processing.&apos; A high degree of alignment has been observed when the final cold rolled texture has a strong (111) [ll2] type component3 and the normal grain growth texture prior to secondary recrystallization has components with a [loo] parallel to the rolling direction and planes from (001) to (110) parallel to the rolling plane.1,3,8,9 Generally, this (001) component is much weaker than the (110) component. The growth rate of (001) plane primaries to secondaries has been found to be independent of the orientation of the primaries with reference to the rolling direction, i.e., the secondaries have the same degree of alignment of [loo] directions with the rolling direction as the (001) primaries.&apos; Hence, the rolling and annealing textures of individual grains or single crystals are of interest in understanding the development of the (001) [loo] secondary recrystallization texture. (001) components have been observed in the annealing textures of cold rolled grains initially having a [loo] parallel to the rolling direction and an (001) rotated up to 30 deg from the rolling plane. Crystals initially near the (001) [loo] orientation when rolled under the influence of constraints imposed by neighboring grains form deformation bands and ro- tate in both directions toward (001) <110>.10,11 Deformation bands have been reported also for crystals initially with an (001) within 1 deg of the rolling plane and a [loo] within 1 deg of the rolling direction when rolled as a free single crystal.12 These crystals have weak recrystallization textures and contain near an (001) [loo] component.10-12 When near (001) [loo] crystals are rolled as free single crystals no deformation bands form and the crystals rotate by a single rotation toward (001) [110]. Recrystallization after a 70 pct cold reduction yielded near an (001) [loo] component13 and after a 90 pct cold reduction an (001) [I201 component." Crystals initially near (210) [001] had a texture after a reduction of 70 and 84 pct which was similar to the (111) [li2] but rotated 10 to 15 deg in the transverse direction. These crystals recrystallize to (210) [OOl] or (410) [001] and contain an (001) [loo] component.10,13 An (001) component has not been detected in the normal grain growth textures of other single crystals. Crystals initially having orientations between (110) [001] and (111) [ll2] have a cold rolled texture of principally (111) [ll2] .10>16 Other crystals with a [I101 parallel to the cross direction rotate to (111) [112] and/or (001) [110] stable end orientations. Crystals initially having from (001) [110] to (111) [lie] retain this orientation after cold rolling.15 The cold rolled textures having [I101 directions parallel to the rolling direction had components in the annealing textures related to the deformation textures by 25 to 30 deg rotations about common (1 10) poles. Cold rolled textures of the (111) (112) type recrys-tallized to (120) [001] or (110) [00l]. The purpose of the present work was to further the understanding of the alignment of [loo] directions of (001) secondaries with the rolling direction. The cold rolling and annealing textures of grains initially (001) [hkl] were studied. These data were applied to the formation of (001) [loo] by secondary recrystallization. PROCEDURES AND EXPERIMENTAL TECHNIQUES The (001) poles near the sheet normal and rolling direction are given in Fig. 1 for the 10 grains studied. Each of these grains was located in the center of a polycrystalline specimen approximately 25 mm wide and 50 mm long. The lower case lettered grains, a through dl were about 1.2 mm in diam and near the (001) [loo] orientation. Specimens containing these grains were from a commercial 3 pct Si-Fe alloy with the principle orientation of (110) [001] as obtained by impurity inhibition of growth with manganese sulfide inclusions.17,18 Upper case lettered grains, A through F, were about 6 mm in diam and had (001) planes near the rolling plane and [hkl] di-

Jan 1, 1963