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By W. A. Backofen, A. T. English

The kinetics of re crystallization were determined metallographically for a 3-1/4 pcl Si-Fe rapidly compressed at temperatures of 710° to 911°C, and held for various times at the working temperature. As in re crystallization following cold wwk, the time for re crystallization was reduced by increased temperature and strain. Nucleation occurred chiefly at grain edges, although other pre-existing interfaces, notably inclusions, also served as nucleation sites. The importance of intragranular nucleation to grain refinement in hot working is pointed out, together with some possible techniques by which nucleation might be induced within the grains. The observed isothermal growth rates are quite accurately described by the equation G = 4 x 10-'/t (cm per sec), independent of temperature and strain at all but the shortest times. Changes in G during recrystalliza-tion can exceed two orders of magnitude. It is argued that release of stored energy associated with lattice defects cannot adequately explain the time dependence. A suggested alternative involves processes of solute segregation and desegregation in the unrecrystallized matrix and at the moving boundary, respectively. EFFORTS to improve hot-working practice are hampered by an incomplete understanding of the fundamental metallurgy involved. Research directed at establishing the required basic foundation falls into two categories, the first concerned with measurement of mechanical properties under the conditions of high temperature and strain rate which characterize such processing, the second focused on structure and its relation to the deformation conditions. Rossard,' Rossard and Blain,2 and Hardwick and Tegart have conducted many high-speed, high-temperature torsion tests on various metals. One of their objectives was interpretation of stress-strain curves in terms of the structures of specimens rapidly quenched following interruption of twisting. They showed that appreciable hardening occurred in the early part of the test, and that this hardening reflected the concurrent development of an increasingly dense substructure within the grains. The detailed nature of this substructure was observed to depend on the ease of polygonization which, at least in fcc metals, varies with the stacking-fault energy.= By holding specimens after interruption but before quenching, the nucleation and growth of new grains could also be studied. Some success has been realized in relating the microstructure of hot-rolled steel to its temperature:strain rate:strain history with such testing.' The same general observations have been made by others investigating rolling4f5 and drop-hammer forging.~-~ Incident to these experiments, some efforts were made to determine the kinetics of re-crystallization as well as the velocity of the migrating boundaries. The results have been largely qualitative, owing to difficulties of interpreting hardness measurements5 and microstructures. The work described here was undertaken to obtain more quantitative information from tests on a material having suitable metallographic properties, and, in this way, to provide further insight into the fundamentals of this practically most important kind of deformation processing. I) MATERIALS AND EXPERIMENTAL TECHNIQUES Materials. Electrolytic etching of a Si-Fe alloy reveals dislocations and substructure in unrecrystallized grains.8'9 This unique characteristic makes possible a precise determination of the extent of recrystallization. For that reason, it was the material selected for all experiments in the present work. The two particular alloys that were used are identified in Table I. A major difference between "A" and "B" is the number of inclusions, as noted in the table. Most of the experiments were made with material "A". It was received as hot-rolled plate 1 in. thick, sawed to 2-in. widths, hot-forged at 1200°C to 5/8-in. rounds, and finally annealed in a mechanical vacuum at 1000°C for 24 hr. The result was substructure-free grains of mean diameter 0.05 cm.*

Jan 1, 1964

By S. F. Reiter

The paper presents isothermal recrystallization curves for 0.08 and 0.15 pct C steel at subcritical temperatures following small amounts of plastic deformation. The effects of deformation, temperature, and aging on nucleation and growth rates ore described. The free energy of activation for grain boundary migration in steel is given. SEVERAL excellent reviews of the literature have appeared concerning the recrystallization of metals.'-' The present investigation follows the approach advanced by Mehl, Stanley, and Anderson,6-7 in which the rate of recrystallization was analyzed in terms of N, the rate of nucleation, and G, the rate of growth of recrystallization nuclei. Two lots of low carbon, capped steel of the analysis given in Table I were studied. Each lot consisted of a 150 lb coil which had been hot rolled to 0.083 in. and then cold rolled to 0.042 in. at the mill. Strips 0.930 in. wide were sheared perpendicular to the rolling direction. Both steels were normalized before studying their recrystallization characteristics. The strips were cleaned, painted with a magnesia-acetone paste, and made into packs of equal weight, wrapped in 0.002 in. copper foil. The packs were placed in a salt bath at 900°C for 30 min and air cooled. A relief anneal followed in a second salt bath for 15 min at 650°C. The relief anneal was found necessary from early tests in which a longer incubation period and slower rate of recrystallization were observed in relief-annealed lot A steel than in similar material which was strained and recrystallized directly after being normalized. This effect, which indicates the presence of transformation and/or cooling stresses in steel air cooled from above the A, temperature, has also been observed by Samuels8 and Masing.9 Figs. 1 and 2 show the microstructure of lot A and B materials and illustrate the rather uniform No. 8 ASTM grain size produced by this heat treatment. Winlock and Leiter10 observed that strip specimens which had their sharp edges removed elongated more uniformly than those which were not polished. Similarly, when the sheared edges were removed on a belt grinder, it was found in the present investigation that such samples recrystallized more uniformly than did unpolished strips. Therefore, all strips were carefully rounded prior to their extension. The approximate strain limits for the production of large recrystallized grains are from 6 to 12 pct extension." It was found that for the purpose of this investigation, 8 and 9 pct elongation were suitable deformations. The strain rate employed was 0.01 in. per in. per min and produced a yield point elongation of 4 pct. Winlock and Leiter found that mild steel of No. 8 ASTM grain size gave the same yield point elongation when extended at 0.012 in. per in. per min. All of the lot A and B strips extended in tension developed a straight, stretcher strain line at each grip when the upper yield point was reached. The lines were parallel and made an angle of 55" with the edge of the strip. They approached each other with increasing strain and met near the center of the sample at the end of the yield point elongation. Immediately thereafter, a small drop in load was observed and then the load increased in a regular manner with increasing extension. The grips were initially 8 in. apart. After extension, the 6 in. gage length was carefully cut into 1 in. samples. The remainder of the strip was discarded. After a flash pickle in hot 50-50 hydrochloric acid, six samples, each of which had been taken from a different strip, were placed in a basket and submerged in a lead pot for isothermal recrystallization. Although no recovery effect was observed, strain aging did occur after extension. Therefore, samples were always recrystallized within 24 hr after their cold deformation. After recrystallization, the samples were etched with a solution comprised of one part by volume of nitric acid with three parts of water. Bromide printing paper was exposed directly at low magnifications and later used with a mask to measure the desired quantities. First, the average diameter of the largest grain visible in each sample was determined using dividers. Next, the number of recrystallized grains per unit area was counted and recorded as n. Then, for each sample, the combined area of the recrystallized grains was measured by transcribing the grain outlines to standard graph paper. Many determinations of the area of the recrystallized grains were repeated five times and indicated a standard error that was not greater than 25 pct. The average area for six samples was divided by the area of the mask to yield the percentage recrystallized. Recrystallization of 0.08 Pct C Steel The progress of recrystallization at 670°C after 8 pct elongation of lot A steel is shown in Fig. 3, a through f. The shapes of the growing crystals are approximately equiaxed, as is assumed in the

Jan 1, 1953

By Y. C. Liu, W. R. Hibbard

Based on pole figure data and microstructural observations, the re-crystallization orientation found in a copper strip previously cold-rolled 99.5 pct from a single crystal with an initial (110) [112] orientation may be described as: a 30° rotation, clockwise and counterclockwise, about octahedral poles of the cold-rolled texture such that all four poles function at a low annealing temperature (400°C) and only three of them function at high temperatures (500' to 1050°C). The relative intensity of deformation stresses on various slip planes can be correlated with the choice of poles affecting the rotations found in the recrystallized orientations. ROTATIONAL reorientation about the poles of densely packed crystallographic planes is an important characteristic of secondary recrystallization" in face-centered cubic metals. Some evidence has also been interpreted to show that such a rotational relationship also exists in the primary recrys-tallization process." In an investigation of the crystallographic relationships in the recrystallization process, several aspects of the experimental procedure should be considered. With cold-rolled poly-crystalline metal as the initial material, pole figure analysis leaves many ambiguities as to whether or not simple indices can be assigned to adequately represent its orientation. The rolling texture does not consist of a single texture. Minor deformation textures are usually present. In all cases, twin textures are present. The presence of both minor and twin deformation textures influences the recrystallization texture. In order to study the recrystallization mechanism, a more precise knowledge of the history of the material before recrystallization is necessary. Tensile deformation of a single crystal usually produces residual stresses which are concentrated at slip bands. Since the exact nature and orientation of these potential nuclei sites cannot be experimentally evaluated, the tensile deformation of a single crystal was not considered adequate. From the work done by Barrett and Steadman6 n copper, it appeared that cold rolling of a single-crystal specimen with an initial (110) [112] orientation would yield a specimen which fulfills the conditions required for the present investigation, namely a highly preferred single rolling texture with relatively homogeneous stress distribution. By investigating the recrystallization texture of this material, additional details of reorientation during recrystallization might be obtained. The purpose of this paper is to describe such an investigation. Experimental Procedure Copper used in the present investigation was cathode sheet with a purity of 99.94 to 99.97 pct. A copper single-crystal specimen, 1.15x0.8720x0.5322 in. (thickness) was cut from a cylindrical crystal which was grown in a Bridgman furnace.' The cutting was accomplished on a horizontal milling machine operated at a very slow speed to obtain a (110) plane in the rolling plane and a [112] direction in the rolling direction. The disturbed surface was removed by electrolytic polishing in dilute orthophos-phoric acid (H3PO4) with a specific gravity of 1.14, and a current density of about 1 to 2 amp per sq cm. A 3-min polishing was needed to eliminate the disturbed surface causing Debye-Scherrer rings and a 45-min polish produced a surface which yielded sharp rounded Laue spots. It was estimated that about 1/16 in. of metal was removed from the original cut surface. The final orientation of this specimen before rolling was about 2" from the (110) plane in the rolling plane with a [112] direction aligned in the rolling direction. It is possible that a small amount of strain was still present in the cube despite the fact that the Laue spots seemed very sharp. It is doubtful, however, that this would be an important factor after a subsequent rolling reduction of 99.5 pct. This copper specimen was rolled on a laboratory rolling mill with two highly polished rolls 37/8 in. in diam in the following manner: 0.010 in. per pass to 50 pct reduction, 0.005 in. to 70 pct, 0.002 in. to 85 pct and, finally, 0.001 in. per pass to a 99.5 pct reduction. Specimens, about 1 in. sq with the rolling edges intact, were cut from the rolled strip by the electrolytic method previously described, after the strip

Jan 1, 1954

By A. Szirmae, Hsun Hu

The early stages of recrystallization in a 70 pct cold-rolled Si-Fe crystal of the (110) (0011) orientation were studied with a Siemens electron microscope. Orientation studies based on electron-diffractzotz. patterns confirm the results of previous texture analysis. The driving energy for recrystallizatior and the critical radius for growth were calculated from the dislocation energy and the energy of the subgrain bourzdaries, and it was found consistent with the observed size of the recrystallized grains. The recrystallization characteristics of crystals with different initial orientations are discussed. The recrystallization of cold-rolled (110)[001] crystals of Si-Fe has been widely studied by various investigators.1-4 Their results on both deformation and annealing textures are in good agreement. The rolling texture after 70 pct reduction consists mainly of two crystallographically equivalent (111) [112] type textures and a minor component of the (100) [011] type. The latter is derived from the deformation twins, or Neumann bands, which are formed during the early stages of deformation and later rotate to the (100) [011] orientation upon further rolling reduction. Between the two main (111) [112] type textures, there is some orientation spread, because of which very low intensity areas appear in the pole figure. If these very low intensity areas are considered to be a very weak component in the texture, then a (110) [ 001 ] orientation may be assigned to them. When this rolled crystal is annealed at a sufficiently high temperature for recrystallization, the texture returns to a simple (110) [001]. The purpose of the present investigation was primarily to seek a better understanding of the recrystallization process by using the electron transmission technique. The (110) [0011 type of crystal was selected because orientation data for it are well known from previous studies with conventional techniques. Direct observations on the recrystallization of such a crystal have also been made by using a hot-stage inside the electron microscope, and the results will be reported in another paper. MATERIAL AND METHOD A single-crystal strip of the (110) [001] orientation was prepared from a commercial grade 3 pct Si-Fe alloy by the strain-anneal technique.= The strip was approximately 0.014 in. thick, and was rolled 70 pct at room temperature to a thickness of 0.004 in. Specimens were cut from the rolled strip and were annealed in a purified hydrogen or argon atmosphere. They were then electrolytically polished in a chromic-acetic acid solution to very thin foils. Best results were found by polishing first between two narrowly spaced flat cathodes with the specimen edges coated with acid-resisting paint, followed by polishing between two pointed electrodes until a hole appeared in the center as described by Bollmann.6 It was found that a thin transparent film always formed along the thin edges of the polished specimen. This film was then removed by rinsing the specimen very briefly in a solution of alcohol with a few drops of HF or HCl. RESULTS AND DISCUSSION 1) The Deformed Crystal. From the electron-diffraction patterns taken at various areas of an as-rolled specimen, the texture components as deduced - from ordinary pole-figure analysis were confirmed. Over most of the areas where orientation was examined, a (111) pattern with a [112] direction parallel to the rolling direction was obtained. This corresponds to the main deformation texture of the (111) [112] type. In a few areas the diffraction pattern was (100) [Oil], corresponding to the minor-texture component derived from the Neumann bands. The (110) [001] orientation, which corresponds to the very weak intensity area in the pole figure, was found infrequently. A typical example of the deformed matrix having the (111) type main texture is shown in Fig. 1, where (a) is the microstructure and (b) is the diffraction pattern taken from that area. It was also frequently observed that in other areas more or less continuous rings of weaker intensity were superimposed on the simple (111) diffraction pattern, suggesting the presence of a wide range of additional orientations. Other evidence indicated that the recrystallization characteristics are different in these two different types of areas. The hot-stage observations which provide this evidence will be discussed in another paper. AS shown in Fig. l(a), numerous dislocation-free areas of very small size are embedded in the "clouds" of high-dislocation density. This indicates that the deformation of a single crystal, even after a rolling reduction of 70 pct, is far from uniform on a micro-

Jan 1, 1962

By N. K. Chen, C. H. Mathewson

Recrystallization of aluminum single crystals after plastic extension is carefully studied in relation to the structure of the deformed matrix. The shapes of the new grains are analyzed with regard to slip planes and to the presence or absence of deformation bands. A mechanism by which the orientations of the grains are related to the parent lattice is described. EXPERIMENTS previously reported&apos; have been extended to develop some of the characteristics of the new crystals which are formed on annealing axially strained crystals whose deformational characteristics had been documented with special care. Thus, the presence of deformation bands affects the growth contours of the crystals, some of the strained crystals produced single crystals anew, and some, polycrystals, on annealing, while others merely "recovered" or "polygonalized" after the 600°C annealing treatment generally adopted in these tests. In the matter of orientational relationships between new crystals and the strained matrix, the present experiments have added little to previous experience, which had demonstrated great variety in the range of orientations encountered and no simple theory or correlation. For example, there has been ample evidence for the predominance in various face-centered cubic metals of a favored orientational relationship; viz., a rotation of 30° to 40° around a <1ll> axis, between grains growing in a matrix with a strong single orientation texture and the matrix itself.&apos;-&apos; This reorientation has been interpreted by various investigators in support of both the "oriented nucleation" and the "oriented growth" hypothesis. In the case of axially extended single crystals of aluminum, no general relationship, such as the one stated above, can be used to correlate the orientations of the recrystallized grains with that of the original crystal. Thus, Carpenter and Elama and Burgers and Basart7 were content to assume that the orientational relationships so developed were random in nature. Mathewson, however, in the Campbell Lecture of 1943 "rgued on the basis of <112> slip that a complex strain, chiefly characterized by rotation around a variable axis in the slip plane combined with a principal rotation around the pole of the slip plane, could be responsible for such devious relationships. Nevertheless, owing to the limited data now available dealing with orientational relationships between new grains and the single crystals strained in tension from which they have recrystallized, no adequate examination of the above generalization could be made. Here, there is the disturbing preliminary condition that any desired orientational relationship may be expressed by means of two rotations about mutually perpendicular axes, so the process lacks a certain critical flavor and any successful choice of axes meeting certain theoretical requirements could be replaced by another differently selected pair. With this reservation clearly in mind the process of double rotations, as previously indicated, was used to relate the orientations of the single crystals which grew out of the strained single crystalline matrix and was construed as certain evidence in favor of the theory of incongruent shearing action proposed by Mathewsons as a necessary element in the (111) slip process with close-packed metals. There is here

Jan 1, 1953

By F. V. Lene, E. J. Westerman

The recrystallization behaviors of two extruded and cold-drawn experimental sintered aluminum powder alloys, containing 1.75 and 3.0 pct Al2O3 by weight, were compared with that of extruded and cold-drawn commercially pure alumirzum. The kinetics of recrystallization of the alloys are described semiquantitatively. For the alloy containing 1.75 pct A l203 the rates of nucleation and of growth were also semiquantitatively determined. THE most striking property of aluminum alloys strengthened by a dispersion of Al2O3, the so-called SAP alloys, is their stability at elevated temperatures. One of the manifestations of this stability is their resistance to recrystallization after they have been cold worked. Most of the commercial grades of either the Swiss SAP or of Alcoa&apos;s Aluminum Powder Metallurgy Products have not been recrys-tallized after cold working, even when they are heated for a long time at a temperature near the aluminum melting point. Lenel, however, observed that the dispersion strengthened aluminum alloys with a larger spacing between the oxide particles than that of most commercial grades would recrys-tallize.1 It appeared to be of interest to further investigate the mode and kinetics of recrystallization of these alloys, and to compare their recrystallization behavior with that of commercially pure aluminum. Because homogeneous deformation of these SAP alloys in tension did not provide sufficient cold work to induce recrystallization, they were cold worked by wire drawing; the nonuniformity of this deformation unavoidably complicated the interpretation of the recrystallization studies. EXPERIMENTAL DETAILS Extrusions—Two types of sintered aluminum powder extrusions were used in this study. One type, designated AT-400, was produced from Reynolds atomized aluminum powder consisting of spherical particles averaging 3µ in diam and containing 1.75 wt pct of Al2O3. This powder was very similar to the R3M powder from which extrusions were previously prepared with an average spacing of 0.9µ between oxide particles.2 The second type, designated MD 2100, was produced from Metals Disintegrating Co. flake powder containing 3.0 wt pct of Al2O3, with an average flake thickness of 0.8µ. The average spacing between oxide platelets in MD 2100 extru- sions was 0.45µ.2 Powder compacts of 3/4-in. diam were extruded at 1000°F into 0.097-in. diam (AT-400) and 0.093-in. diam (MD 2100) wires by methods previously described.3 In order to compare the recrystallization behavior of sintered aluminum powder extrusions with that of wrought commercially pure aluminum 3/4 in. rod stock of 1100 F aluminum was extruded at 1000°F into 0.102-in. diam wire. Wire Drawing—Tungsten carbide dies were used for the AT-400 and 1100 F alloys. They had an included angle of about 15 deg and reduced the wire area approximately 7 pct per pass. Steel dies with an included angle of 11 to 13 deg and an average reduction per pass of 10 pct were used for drawing the MD 2100 alloy, because drawing this alloy through the carbide dies produced overdrawing defects. Heat Treatment—The cold-drawn wires were cut into small samples, and the deformed ends were etched off. The samples were each wrapped tightly in a single layer of aluminum foil, and individually isothermally annealed in a lead bath. Metallography—The modes and kinetics of recrystallization were determined by metallography. Mounted and polished specimens were anodized in a solution of 1.8 pct HBF4;4 examination under polarized light clearly revealed their grain structures. The recrystallized grains were generally much larger than those of the unrecrystallized matrix, and could clearly be distinguished because they alternated between maximum and minimum light reflection when the microscope stage was rotated, while the unrecrystallized matrix had a comparatively homogeneous "salt and pepper" structure. The fractional recrystallized volumes of the dispersion hardened alloy wires were determined by cutting and weighing of recrystallized and total transverse areas on photomicrographs. The recrystallized grains in the 1100 F alloy were too small to be cut out individually; therefore a combination of cutting and lineal analysis was used in this case. RESULTS AND DISCUSSION Modes of Recrystallization—The modes of recrystallization of the three alloys varied widely. In the 1100 F alloy nucleation and growth started in the region midway between the center and the surface;

Jan 1, 1961

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 F. J. Plecity, J. T. Michalak, W. C. Leslie

Isothermal recrystallization and grain growth in zone- and vacuum-melted irons and Fe-Mn alloys, up to 0.60 pct Mn, were studied in the range 480° to 650° C, after 60 pct cold reduction. In initial stages, rate of grain growth and rate of recrystallization of iron decrease with time. The recrystallization is typical of a growth-controlled process, and rate of growth is determined by the extent of recovery. Mn decreases rates of growth and of recrystallizatzon. The recrystallization process changes at about 0.30 pct Mn and nucleation may become time-depetzdet~t. In recent years, considerable effort has been expended in determining the effects of solute elements on recrystallization and boundary migration in fcc metals. The results have indicated that the effects produced by single solute additions are dependent upon both the element added and its concentration.&apos;-&apos; In contrast, there have been very few attempts to determine the characteristics of recrystallization and boundary migration in high-purity bcc metals, especially after heavy deformation, and the effects thereon of single solute elements.9-11 This study was undertaken to determine the recrystallization characteristics of various "high-purity" irons and the effects of manganese additions at two levels of base purity. It was hoped that the information obtained would improve our understanding of the recrystallization of pure metals and aid in formulating a theory for the effect of solute elements. The interest was not entirely academic, for the annealing of low-carbon steels, which is of very great commercial importance, is but poorly understood. MATERIALS The compositions of the irons and iron-manganese alloys used are listed in Table I. The zone-melted iron and Fe-Mn alloys were made by Battelle Memorial Institute. Iron S-1 was arc-melted in a water-cooled steel mold in an argon atmosphere. The ingot was forged into a bar, then given two horizontal zone-refining passes in an alumina boat. Iron V-4 was treated in a similar manner, but was not zone-refined. The iron for the zone-melted Fe-Mn alloys was induction melted in vacuum in MgO crucibles and cast into alumina molds. The ingots were forged into bars, machined to shape, and a groove milled down one side of each. The best available electrolytic Mn was placed in the grooves, and the bars were zone melted. The vacuum-melted Fe-Mn alloys were induction melted in this Laboratory in MgO crucibles and poured into cast-iron molds. Iron V-5 was purchased from National Research Corp. in the form of a small vacuum-cast ingot. The low-carbon steel was made by induction melting in air at the U.S. Steel Corp. Applied Research Laboratory. The history of the materials prior to the final cold reduction differed; these details are given in the Appendix. The penultimate grain size of the principal materials was kept in the range ASTM 2 to 4, except for the low-carbon steel. PROCEDURES The cold work prior to the final recrystallization anneal was kept constant at 60 pct. It is known that rolling procedure can influence the kinetics of recrystallization of ironI2; therefore, all specimens were rolled in one direction only, between clean,

Jan 1, 1962

By F. J. Plecity, J. T. Michalak, W. C. Leslie

W. M. Williams (McGill University)-The authors are to be congratulated on completing this detailed investigation of recrystallization behavior. The present writer has recently completed some research at the University of Toronto on the recrystallization and grain growth behavior of a number of "pure" irons, and he would like to take issue with the authors&apos; contention that recrystallization cannot be followed by means of hardness measurements. Two series of specimens of Ferrovac E, a com- mercially available iron, were annealed to complete recrystallization at 525" and 620" C, measurements being made both of Rockwell hardness and of volume percent recrystallized as a function of annealing time. Good correlation was found between these two quantities and, following the earlier practice of Cook and Richards for copper, hardness measurements were used in an extensive investigation of recrystallization. No anomalous behavior was observed as a result of this practice. Specimens which showed complete softening always showed, (metallographically and by X-rays), completely re-crystallized structures. These observations do not, of course, detract in the least from the results of the work under discus-

Jan 1, 1962

By Bruce Chalmers, D. C. Larson

Aluminum crystals with longitudinal-axis orientations of (111) . (110), and (100) were deforined in tension and annealed. The conditions of deformation were controlled so that the re crystallization nuclei originated in either the heavily deformed regions at saw cuts {artificial nucleation) or in the lightly deformed matrix (spontaneous nucleation). The artificial-nucleatioln experiments showed that in lightly deformed (110) and (100) crystals low-angle twist boundaries are most mobile, while in (111> crystals and heavily deformed (110) and (100) crystals high-angle tilt boundaries with near (111) rotations are favored. The spontaneous-nucleation experiments showed the existence of preferred orientations in the (111) crystals. The nonrandomness of the grain orientations is quantitatively determined through a comparison with the results which would he obtained from a randowl set of grain ovientations. PREVIOUS recrystallization studies have been performed on single crystals deformed in tension.1 7 The crystals used in these studies usually had random tensile-axis orientations and the extent of deformation was not a primary consideration. The present study concerns the recrystallization of single crystals with tensile-axis orientations of (Ill), (110), and (100). The emphasis of this work is on the influence of the tensile-axis orientation and the degree of deformation on both the nucleation and growth processes. The multiple-slip orientations were chosen because secondary slip or slip intersection promotes nucleation.1,5,8 These crystals recrystallize at lower strains than the crystals which are oriented for single slip. Also, the greatest variation in deformation behavior is exhibited by the multiple-slip orientations. The stress-strain curves for crystals with tensile-axis orientations of (111) are higher than the stress-strain curves for poly-crystals, and the stress-strain curves for crystals with tensile-axis orientations of (100) are lower (at large strains) than the stress-strain curves for the crystals which deform initially in single slip.g The recrystallization nuclei originated in either 1) the homogeneously* deformed matrix of the crys- tals or 2) the heavily and inhomogeneously deformed regions at saw cuts. The nuclei will be referred to hereafter as spontaneous and artificial nuclei, respectively. The two terms do not imply a difference in the nature of the nuclei; they imply simply a difference in the mode of introduction of the nuclei. During spontaneous nucleation very few (always less than ten) grains nucleate, while during artificial nucleation large numbers of grains nucleate. Only a fraction of the artificially nucleated grains penetrate very far into the deformed matrix during annealing. The grains that penetrate the farthest into the deformed matrix will be referred to as the dominant grains. EXPERIMENTAL PROCEDURE The thirty-five crystals used in this investigation were grown from the melt in milled graphite boats at a rate of 1.6 cm per hr. The crystals had dimensions of approximately 6 by 12 by 80 or 6 by 6 by 80 mm and the aluminum was of 99.992 pet purity. The as-grown crystals were annealed at 610°C for 24 hr and furnace-cooled. They were then heavily etched and electropolished in a solution of five parts methanol to one part perchloric acid. The crystal orientations were obtained by back-reflection Laue photographs and were accurate to ±2 deg. The tensile-axis orientations were (loo), (110), and (111). Two of the side faces of the (111) crystals were (110) lanes. The (110) crystals had both {100) and {110) side faces and the (100) crystals had (100) side faces. The crystals were deformed at a strain rate of 0.003 per min. Shear stress and shear strain were obtained by multiplying and dividing the tensile stress and strain, respectively, by the Schmid factor, m. For the (111) crystals m = 0.272 and for the (110) and the (100) crystals m = 0.408. The Schmid factor is effectively constant during deformation for all orientations. The deformed crystals were sawed into 1-in.-long specimens while the crystals were totally enclosed in a graphite boat. The sawing was performed very carefully in order to limit the plastic deformation to the sawed regions. The specimens were electropolished in the solution mentioned above to remove the sawed-end deformation as well as controlled amounts of surface material. A special stainless-steel grip was used to hold the specimens during the electropolishing treatment. The gripping faces were flat, with no teeth, to prevent the introduction of extraneous de-

Jan 1, 1964

By D. Harker, W. E. Seymour

CERTAIN alloys of iron and nickel, when rolled and annealed, possess a preferred crystal orientation: (001) in the rolling plane and [loo] in the rolling direction, when recrystallized at 850" to 1050°C after approximately 98 pct cold reduction. Since the preferred orientation makes a direction of easiest magnetization coincide with the rolling direction, these alloys, especially a 50 pct iron in nickel alloy, have found wide application in the electrical industry&apos; for choke coils and special types of transformers. The rate of the recrystallization reaction was studied at temperatures ranging from 500° to 600°C. The heat of activation for the reaction was calculated from the observed rates, and crystal orientation determinations were made before and after re-crystallization. A vacuum melted iron-nickel alloy* analyzing 49.6 pct nickel, 0.018 pct carbon, and 0.30 pct manganese was used for the experiments. The alloy was cold-rolled 98 pct into strips 1/2 in. wide by 0.002 in. thick. Specimens 1 in. long were sealed under a vacuum (approximately 10-8 mm Hg) in 1/2 in. ID pyrex glass tubes. For heat treatment these tubes were fastened to Nicrohm wires and submerged in a molten salt bath controlled to ±2°C. (The maximum measurement error was within 3°C.) The time at temperature was varied logarithmically from one sample to another, and runs were made at 500°, 525", 550" and 575°C. A molten lead bath was used for a run at 600°C which was controlled to the same accuracy. To determine the extent of recrystallization after a particular time at a given temperature, a method was used suggested by the work of Decker, Asp, and Harker.3,4 This method employs an X-ray spectrometer whereby X rays are diffracted from crystallites whose diffracting atom planes are parallel to the rolling plane of the specimen. The intensities of the diffracted rays are measured by a Geiger counter. The counter can be rotated through a range of angle, and can be motor driven through this range at a speed of 2" per min. The measured intensities are plotted vs. angle by a potentiometer recorder. In a 50 pct iron-nickel alloy it was found that only (200) reflections were obtained from the rolling plane with recrystallized material, and that only (220) reflections were obtained from the rolling plane with unrecrystallized material. No other reflections were obtained under these conditions over a range of Bragg angle of 0 to 45" using either type of specimen. As a consequence, the intensity of the (200) reflections from the rolling plane was taken to indicate the amount of recrystallized ma-terial present in a specimen, and the corresponding intensity of the (220) reflections was taken to indicate the amount of unrecrystallized material present. To insure flatness and proper alignment of the reflecting specimen in the spectrometer, the sample was laid in a slot 1/2 in. wide x 0.001 in. deep which was machined in a 3/4x2x1/2 in. steel carrier. The specimen then was taped down with cellophane tape. This steel cradle was mounted vertically in the specimen holder of the spectrometer so that the bottom edge of the carrier rested against a horizontal shoulder. Intensity data used in plotting the percent of recrystallized material vs. time at temperature were obtained by directly counting the diffracted beam of nickel filtered copper Ka radiation used throughout the work. The X-ray spectrometer was employed also in obtaining pole figure data to be used for orientation determinations. At the beginning of this investigation a transmission pole figure holder was used." As a thickness of 0.002 in. of this alloy was found to be opaque to the copper Ka radiation, it was necessary to reduce the thickness of the pole figure specimen. A cold-worked sample was etched in a 50 pct HCl solution for 5 min and was found to transmit a

Jan 1, 1951

By P. A. Beck, Hsun Hu

It has been known for many years that in cold drawn polycrystalline aluminum the recrystallization texture is practically identical with the deformation texture.l,2,3 V. Goeler and Sachs4 stated that in cold rolled polycrystalline aluminum, too, the deformation texture is retained upon recrystallization. This behavior was interpreted by Dehlinger9 as an indication that each recrystallized grain inherits the orientation of the matrix in which it grew. However, Burgers and Basart showed6 that in deformed aluminum single crystals the orientation of the recrystallized grains strongly deviates from that of the matrix. Barrett demonstrated8 that even in deformed polycrystalline aggregates the local orientation within each deformed grain changes on recrystallization. No explanation has as yet been offered of how the aggregate texture can be retained, while the local texture is everywhere changing. According to Burgers and Louwerse6 the orientation change on recrystallization in compressed and rolled aluminum single crystals corresponds to a rotation around [112] axes lying in the active slip planes and perpendicular to active slip directions. This orientation change was rationalized by them on the assumption that the orientation of the recrystallized grains is determined by the orientation of the available nuclei, and that these nuclei are small fragments of the deformed crystal, rotated in the deformation process. Barrett pointed out,? however, that these assumptions were by no means proven, and that the total volume of material necessary for the nuclei is so small, that it must be available in any orien- tation whatever. It is, therefore, unlikely that an "oriented nucleation" theory could satisfactorily explain the orientation changes in recrystallization of a deformed crystal. Furthermore, in contradiction to Burgers and LOU-werse&apos;s conclusions, Barrett&apos;s results for the orientation change could be best expressed in terms of rotations around. [Ill] axes. Thus agreement is lacking not only in the interpretations but apparently even in the experimental results contributed by the various investigators. The orientation relationships on coarsening* in a highly oriented polycrystalline matrix were first investigated by Burgers and Basart.5 They produced a fine grained highly oriented matrix by the recrystallization of a compressed or rolled single crystal of aluminum, and studied the orientation relationships in three successive generations of crystals: the "deformation texture" in the single crystal, the recrystallization texture, and the coarsening texture. Burgers24 showed that the preferred orientation of each successive generation was almost always widely different from that of the preceding one, but that the coarse grains often approximately reverted to the orientation of their grandparent, the deformed single crystal. This observation, and the idea that the orientation of the coarse grains is determined by that of the available "nuclei," led to the concept that the coarse grains are nucleated by the remnants of the deformation texture.12,15 On the other hand, Bowles and Boas16 found, in a carefully conducted experiment, that in recrystallized fine grained copper of cube texture coarse grains grow in orientations which can be derived from the orientation of the recrystallized matrix by rotation around a [lll].] direction: the coarsening texture here does not appear to be related in any simple manner to the original rolling texture from which the cube texture had been obtained by recrystallization. It may be assumed that in a recrystallized material, even with a strong texture, there always are present some grains of practically any orientation. These may serve as "nuclei" for the coarse grains, provided that the conditions are favorable for their growth. The existence of a coarsening texture may be considered as an indication that grains with certain relative orientations with respect to the preferred orientation of their neighbors can grow much faster than others. This "oriented growth" theory was briefly suggested by van Arkel, as early as 1936,13 and it was mentioned by Burgers." Recently, C. G. Dunn produced direct

Jan 1, 1950

By I. L. Dillamore

A purely geomentrical analysis based on oriented-growth relationships is presented to derive annealing-texture orientations in bcc metals from their- known deformation textures. The analysis takes as its starting point a description of- the bcc deformation texture and follows previous work on fcc metals in considering pvobable nurleation sites for recrystallization and the textural limitations on grains growing into a deformed matrix. The analy-sis accounts for the prominent and the minor coinponents of the annealing textures formed from two the deformation textures and can account for the ob-sem:ed temperature dependence of the annealing texture of bcc metals. THERE have been a number of investigations of annealing textures in bcc metals but few attempts to relate these textures to the deformation textures. This has been largely due to the lack of definition of both annealing and deformation textures, neither of which shows sharply defined orientations. It is, however, necessary to get a better understanding of primary recrystallization textures in bcc metals in view of increasingly exacting demands upon the quality of steel sheet for drawing purposes and as a necessary step towards the control of textures through processing. An analysis is presented here which relates annealing textures to deformation texture, by a purely geometrical method. This takes as its basis the oriented-growth theory of recrystallization and makes some reasonable assumptions regarding the make-up of bcc deformation textures and the limitations on growth relationships in bcc metals. Detailed information on this latter point is not available at the present time, and the present analysis may need to be streamlined or extended when such information is at hand. It is felt, however, that despite these limitations the analysis provides useful results and a valuable aid towards understanding the effect of processing variables. 1) BCC ROLLING TEXTURES Different workers have used a variety of descriptions for the texture developed in bcc metals by rolling. For the present purpose it will be assumed that two different deformation textures can be obtained: 1) a texture containing a major (112)[li0] component and a minor (001)[1i0] component for which increasing deformation causes the (001)[li0] component to increase at the expense of the (112)[li0] component, as suggested by Dillamore and ~oberts&apos; (this is the texture predicted to arise starting from randomly oriented material); 2) a t~xture containing the above components and (111)[110] and (ii1)[112] components. This texture could arise from a material with an initial (110)[001] or (iil)[112] texture. It is well-known that the (ll0)[001] orientation rotates to (ii1)[112]that on roll-

Jan 1, 1965

By C. A. Stickels

The preferred crystallographic orientations developed during recrystallization of polycrystalline electrolytic iron sheet, cold-rolled 90 pct, were ivestigated. Recrystallization at 500° or 565° C for relatively short limes produces a texture which is similar to the rolling texture. A duplex partial fiber texture, significantly different from the rolling texture, is found when the annealing time is increased. Recrystallization at 700°C also produces a sequence of textures with increasing annealing time. In order of their appearance, these textures are: 1) the duplex partial fiber texture found at lower temperatures, 2) a four-component texture "near {322}(296)", 3) a {112)(110) +(111)(110) texture, and 4) a two-component "near {554)(225)" texture. Secondary recrystallization, or discontinuous grain growth, accompanies the development of the latter texture. However, the "near {554} (225)" texture was nol observed when secondary recrystallization occurred under other conditions. All of the ideal orientations found in recrystallization textures can be accounted for by the growth of minor components of the deformation texture. IN recent years there has been increased interest in improving the drawability of metals by controlling the preferred crystallographic orientation of the sheet.1-l3 Since more low-carbon steel is drawn than any other material, considerable attention has been focused on the properties of sheet steel. Efforts to improve drawability through texture control have been hampered by the lack of any published systematic study of the recrystallization textures developed in iron annealed below Acl. The purpose of the present work was to supply some of this missing information, specifically, the recrystallization textures obtained by isothermal anneals of polycrystalline iron, cold-rolled 90 pct. LITERATURE REVIEW—DEFORMATION TEXTURES Barrett14 reviewed and summarized the investigations of rolling textures in iron and low-carbon steel prior to 1952. The texture of heavily deformed iron (rolled 90 pct or more) is described as consisting of two partial fiber textures. The dominant fiber texture (designated here as fiber texture A) has a (110) fiber axis in the rolling direction and includes the orientations (001)[110], {112}( 110), and {111}(110). The secondary texture (designated here as fiber texture B) is described as having a (111) fiber axis in the sheet normal direction, and includes the orientations {111)( 110) and (111)(112). Since the publication of Barrett&apos;s book, there have been two detailed studies of the deformation texture in polycrystalline iron. In both instances, the more sensitive diffractometer methods of pole-figure determination were used. Bennewitz15 studied the cold-rolling textures developed in polycrystalline low-carbon steel and a 3 pct Si steel. He determined (110), (2OO), and (222) pole figures for specimens reduced 30, 50, 60, and 90 pct and analyzed his results in terms of partial fiber textures. He distinguished three stages in the development of the final deformation texture. 1) Grains rotate to form two incomplete fiber textures, with (110) fiber axes inclined 30 deg to the sheet normal toward the rolling direction (fiber texture B). After 50 pct reduction, the highest density of poles is near an ideal orientation {554}(225), the two components of which are members of this duplex fiber texture. 2) With increasing amounts of reduction, grains rotate about the former fiber axes toward ideal orientations of the type {112)( 110) (common to fiber textures A and B). 3) Finally, grains rotate about their ( 110) axis in the rolling direction, clockwise and counterclockwise from the orientations {112}(110). This produces the range of orientations from (111)(110) to (001)(110) commonly found in the rolling texture of heavily deformed iron (fiber texture A). No significant difference was found between the deformation textures of low-carbon and silicon steels. A few years earlier, Haessner and weik16 had determined (110) pole figures for carbonyl iron rolled to 30, 60, 80, and 90 pct reduction in thickness. heir data agree quite well with the more complete data of Bennewitz, but a somewhat different description of the evolution of the deformation texture was given. The appearance of (110) poles in the transverse direction is ascribed to a (100)[011] component rather than "near {554}( 225) " components, and the (110) fiber axes of fiber texture B are described as located 35 deg rather than 30 deg from the sheet normal. Both of these studies agree that the secondary texture present in heavily rolled iron, the duplex fiber texture B, has (110) fiber axes and not a single ( 111) fiber axis normal to the sheet, as

Jan 1, 1965

By Y. C. Liu, W. R. Hibbard

An aluminum single crystal cold-rolled from (110) [1121 essentially retains its initial orientation after 99.6 pct reduction in thickness. The orientation of the recrys-tallized grains of this material can be described in terms of crystallographic rotations about principal poles of deformation texture. DURING the study of the recrystallization of a copper single crystal cold-rolled from a (110) [112] initial orientation, the orientation of the re-crystallized grains could be derived by a 30" rotation of the orientation of the cold-rolled matrix about its <111> poles.&apos; The present investigation was undertaken to extend the work done on copper&apos; to an aluminum crystal also cold-rolled from a (110) [112] initial orientation. Experimental Procedure The procedure of this experiment was similar to that reported for copper.&apos; An aluminum (99.998 pct) single crystal rod* 1 % in. in diameter was grown in back-reflection technique.&apos; The specimen (1.20x 1.004x0.6787 in. thick) was then rolled along the [112] direction. The final thickness was 0.0028 in., giving a reduction in thickness of about 99.6 pet. Specimens were cut from the rolled strip with scissors, and approximately in. of disturbed metal was removed with Tucker&apos;s reagent. The rolling edge remained intact. The specimens were sandwiched between two graphite plates and annealed in a lead or lead alloy bath which was electrically heated. Pole figures were constructed using the techniques previously described.&apos; Specimens were electrolytically polished4 and etched with 47 pct HNO8, 50 pct HC1, and 3 pct of 48 pct HF. The electrolytic polishing method and etching reagent employed for aluminum specimens were not entirely satisfactory and the microstruc-tures could not be studied in any detail. Results and Discussion The octahedral pole figure of cold-rolled aluminum strip is plotted in Fig. 1. The <111> poles spread in the transverse direction approximately 8" for the highest intensity areas. The spread in the transverse direction can be related to a rotation about two <110> directions lying in a plane containing the rolling direction and rolling plane normal. The two <110> directions and a scale of rotation for the <111> poles are shown in Fig. 2. The amount of rotation is consistent for three of the four <111> poles, about 35" to 40". The discrepancy for the fourth pole is believed to be due to limitations of the film technique. Alternate inter-

Jan 1, 1956

By C. J. Bechtoldt, H. C. Vacher

Quenched alloys, prepared by powder metallurgical techniques, were examined by microscopic and X-ray diffraction methods. The compositions and heat treatments were chosen so that the chromium and nickel solvuses could be determined and a range of composition and temperature, in which a eutectoid had been reported, could be explored in small intervals. The results showed no evidence of eutectoid reactions having taken place. ALLOYS containing iron, chromium, molybdenum, and nickel are extensively used in high-temperature applications. In order to provide basic information on the solid-state reactions that occur in such alloys, the National Bureau of Standards is engaged in an extensive study of the equilibrium phases in the binary, ternary, and quaternary systems involving these four metals. Attention was directed to the chromium-nickel system because a review of the literature showed conflicting data. A recent compendium1 of the constitution of binary alloys gives two diagrams for the chromium-nickel system, one a simple eutectic and the second a diagram showing a eutectoid and a eutectic. The eutectoid was the result of an allotropic transformation in a high-temperature solid-solution form of a chromium-rich phase called 0. The approximate temperature and composition of the eutectoid was 1200°C and 30 at. pct Ni. In the preliminary study, at the Bureau, no transformation was indicated in the chromium-rich phase of ternary and quaternary alloys in which chromium and nickel were major components. Similar results have been reported from time to time in the literature,2-8 In consequence of this situation, a systematic study was made of the constitution of heat-treated chromium-nickel alloys using metallographic and X-ray diffraction methods. The compositions of the alloys were selected so as to determine the boundaries of the chromium-rich and the nickel-rich phases and to explore in small intervals the ranges in composition and temperature in which the eutectoid had been reported. The results of this study are reported and discussed in the present paper. EXPERIMENTAL PROCEDURES Materials, Alloys, and Heat Treatments—The alloys were prepared by a powder metallurgy technique similar to that used in earlier work.9 Analyses of the materials used are given in Table I. Powders were mixed using a vibrator in 30-g batches of predetermined composition; 2-g pellets were made from the mixture by compacting at room temperature in a 1/2-in. diam mold under 60,000 lb per sq in. pressure. The pellets were sintered in dry hydrogen for 10 days at 1300°C. At the end of the sintering treatment the specimens were quenched in water, which caused a pale green film to form on the chromium-rich alloys and thin black scale to form on the nickel-rich alloys. The pellets after sintering were approximately 1/2 in. diam by 3/32 in. thick. The purification train9 was modified by inserting a tube of titanium turnings, heated at 700°C to increase the efficiency of the removal of oxgen and nitrogen. It was found in the earlier work that the sintering treatment lowered the carbon, oxygen, and nitrogen contents of chromium-rich alloys to 0.01, 0.01, and 0.004 wt pct, respectively, and that there was a loss of chromium. In order to ascertain the extent of this loss, the chromium contents of certain alloys were determined chemically. They included those alloys used to determine the parameter-composition curves and those of critical composition, used to determine the chromium-solvus microscopically; these analyses were made on samples after the final heat treatments. The mixed powder values for the chromium content of those alloys that were not analyzed were adjusted to conform to a smooth curve based on the chemically analyzed values for

Jan 1, 1962

By A. H. Daane, W. J. Wunderlin, B. J. Beaudry

In an earlier study at this laboratory,&apos; the authors investigated the solid solubility of holmium in copper, silver, and gold, and also the melting point of the first eutectic on the noble-metal-rich side in these systems. In a more recent study of the solubility of rare-earth metals in gold at this laboratory. Rider, Gschneidner, and McMasters2 noted that the reported eutectic temperature in the Ho-Au system was lower than the corresponding eutectics in systems of dysprosium and erbium with gold. A redetermination of the eutectic temperature in the Ho-Au system with the same alloy used in the original study showed the eutectic temperature to be 810°C instead of 778°C as originally reported. (The eutectic temperatures in the Ho-Ag and Ho-Cu systems were also redetermined and were found to be 795" and 864°C compared to 787° and 868°C, respectively, which were reported originally.) Since this large change in eutectic temperature made the solubility data appear questionable, new alloys were prepared, heat-treated, and examined metallographically. The procedure of sample preparation and heat treatment used in the original work&apos; was followed except longer heat treatments were used ranging from 7 days at 600°C to 6 hr at 900°C. The results obtained are shown in Fig. 1. There is good agreement between the two studies in the maximum solubility of holmium in gold. Since the slope of the solvus is less pronounced in the present study, the extrapolation to 550°C shows a solubility of 1.6 wt pct Ho in gold compared with 1.0 wt pct in the original work. Since additional data were obtained and longer heat treatments were used in the present study, the larger value is believed to be more accurate. The authors wish to express their appreciation to P. Rider and K. A. Gschneidner. Jr., for bringing this discrepancy to their attention, and also to D. Thompson for assisting in the present study.

Jan 1, 1965

By W. G. Pfann

Formation and slow solidification of a molten zone in a homogeneous ingot produces a discontinuity in solute concentration at the boundary of the zone and a gradient of concentration within the zone. By using two solutes, one a donor, the other an acceptor, step or graded pn barriers can be produced. EXPLOITATION of the difference in concentration between a molten solution and the solid which freezes from it is continued in this paper. The normal segregation which results from this difference has been used for purification&apos;.&apos;2 and for pn barrier-formation in semiconductors."4 By means of traveling molten zones this difference has been used to effect multistage separations and to eliminate segregation in ingots." a It will be shown here that by means of stationary molten zones this difference can be used to produce discontinuities in concentration. In particular it will be shown that a pn or npn barrier can be made by the simple act of melting and refreezing a portion of a block of semiconductor, provided that the block contains proper concentrations of a donor and an acceptor in solid solution. Assumptions The operation of melting and slow refreezing will be called remelting and the interface between liquid and solid at the start of refreezing will be called the remelt bormdary. While remelting may be done for various shapes of starting crystal and remelt zone it will be assumed that the remelt zone is cylindrical, its length being measured in the direction of freezing, which is normal to the remelt boundary, and

Jan 1, 1955

By S. J. Hruska

Rate expressions for the formation of two-and three-dimensional nuclei on foreign substrates are developed, taking into account previously neglected contributions to the standard Gibbs free energy of formation of critical nuclei. The temperature dependence of critical super saturation data predicted using these expressions is in accord with data for cadmium on copper and sodium on CsCl. EXPERIMENTAL data on the heterogeneous nuclea-tion of metal crystals from the vapor phase1&apos;2 exhibit the temperature dependence predicted by a nucleation rate equation derived by Pound et al.3 In their treatment, the critical nuclei are visualized according to the Volmer4 model as cap-shaped (three-dimensional). Accordingly, it seems desirable to compare these data with a nucleation rate equation which is derived on the assumption of disk-shaped (two dimensional) nuclei. Further, Lothe and Pound5 have recently shown that the standard Gibbs free energy of formation of these critical nuclei contains a contribution which has heretofore been neglected. Thus it is necessary to re-examine these nucleation data using a rate equation which contains this contribution. The van&apos;t Hoff isotherm relates n(i), the concentration of nuclei of critical size i (i = number of atoms), to nil), the concentration of adsorbed single atoms: where standard Gibbs free energy of formation of critical nuclei given by is temperature insensitive and is the bulk free energy change/volume of transformed material], T = substrate temperature and k = Boltzmann&apos;s constant. Previously,3 was determined by considering only the contributions of bulk and surface free energies in transforming i atoms from the population nil) to a cluster of i atoms. It has been shown5 that this procedure does not take into account the free energy contribution arising from the multiplicity of sites, q, where the clusters can be situated. If this contribution, -kT In q/n(l),is added to iG3 [Note that this increases n(i) by a factor q/n(l).] Since the above does not affect the remaining terms in the rate expression of Pound et al., the details are referred to their paper. The resulting nucleation rate is If the experimental AGV and T values at some common value of are employed, a plot of vs T(ln C3/l + In p&apos;) should yield a straight line of slope k/B<p and intercept . The corresponding plots for / = 1 nucleus per sq cm sec and C3 = 1018 are shown in Figs. 1 and 2 for cadmium on copper1 and sodium on CsCl2 and the values of obtained therefrom are entered in Table I. It is apparent that the data yield reasonable straight lines with about the same scatter as found using the equation of Pound et al. When the configuration of minimum free energy for a nucleus is a circular monatomic layer, the standard free energy of formation is

Jan 1, 1963

By A. J. Griest, A. P. Young, P. D. Frost

A study was made of the effect of ß grain size on the tensile ductility of a-ß titanium alloys haet treated to strengths in the range 165,000 to 180,000 psi. It was concluded that the primary cause of $ embrittlement is the large grain size which is obtained so rapidly in many a-ß titanium alloys when heated into the ß field. It was also found that grain-boundary a and acicular intragranular a in the microstructure are not necessarily detrimental to the tensile ductility if the prior ß grain size is sufficientlv fine. BETA embrittlement occurs in a-ß alloys when the finish hot-working or stages of the subsequent heat treatment have been done at temperatures in the ß field. In order to avoid this embrittlement, for-gings must be finished at temperatures under the ß transus. For better workability, it would be desirable to forge at temperatures in the ß field. For this reason, research has been conducted to determine the cause of ß embrittlement. Although ß grain size has been considered as a possible contributing factor to ß embrittlement, only limited research has been done to evaluate its effect. The effect of addition elements on ß grain growth in unalloyed titanium has been studied by Liu.&apos; Complete mechanical property data, however, were not obtained for correlation with grain size. Ogden and coworkers2 have investigated the effect of both a and ß grain size and grain shape in Ti-Cr-Mo alloys. Their data indicated that tensile ductility was relatively insensitive to ß grain size at annealed strength levels (140,000 psi ultimate). No study has apparently been made to determine the relationship between ß grain size and ß embrittlement in a-ß alloys heat treated to high strength (180,000 psi ultimate). The high-strength condition is that in which ß embrittlement is particularly severe. Beta grain size is not easily varied through the use of a range of annealing times and temperatures in the ß field, because of the rapidity with which ß grain growth occurs. Short-time heating techniques are needed to obtain the smallest ß grains. EXPERIMENTAL PROCEDURE In this research, the experimental procedure was as follows: 1) Tensile and microimpact specimen blanks were resistance heated to produce a range of ß grain sizes. 2) The tensile and microimpact blanks were then solution-treated in the a-ß field and aged to produce predetermined ultimate tensile strengths in the range 165,000 to 180,000 psi. Tensile and impact ductility were then correlated with a grain size for constant strength levels. Materials—The alloys Ti-6A1-4V, Ti-4A1-4Mn, and Ti-16V-2.5Al are representative of the heat-treatable a-ß types in which ß embrittlement can be severe. The compositions and ß transi of the heats studied are given in Table I. The Ti-16V-2.5Al heat was melted and fabricated to 1/4 in. round at Battelle; the other alloys were obtained as 1/4 in. round rolled from commercial heats. The micro-structures of the as-rolled alloys were fine a-ß mixtures. This structure is typical of titanium alloys hot-worked extensively in the a-ß field. Resistance-Heating Treatments to Establish ß Grain Size—For direit resistance heating, a 1/4-in.-diam s~ecimen was heated with a 3000-watt transformer rated for 1000 amp with adjustable secondary voltage. The apparatus included a spray quench fixture. Both heating and quenching periods could be automatically controlled. For temperature measurements, 28-gage Chromel-Alumel wires were tack-welded to the specimen at its midpoint. A high-speed recorder-controller was used to control the heating cycle.

Jan 1, 1960