Search Documents

By B. Ramaswami

INTERNAL oxidation occurs readily in silver due to the rapid diffusion of oxygen in silver.' It has a marked effect on creep in polycrystalline silver2 and raises the critical resolved shear stress in single crystals of silver.3 However, the effect of oxygen on the work-hardening parameters of silver is not known. It is the aim of this paper to describe the effect of internal oxidation on the work-hardening characteristics of single crystals of silver and an Ag-0.1 at. pct A1 alloy. The materials used were: 99.99 pct Ag from Handy and Harman and 99.993+ pct A1 from Alcoa. Single crystals, 6 mm by 6 mm in cross section of silver and Ag-0.1 at. pct A1 of mo.5 orientation, i.e., the orientation with the Schmidt factor m = 0.5. were grown by the Chalmers technique.4 One set of specimens, referred to herein as oxidized specimens, was annealed at 940°C for 24 hr in a muffle furnace, in air, and furnace-cooled to room temperature. Another set of specimens, referred to as nonoxidized specimens, was annealed in oxygen-free helium at 940°C for 24 hr and furnace-cooled over a period of 7 hr to room temperature. The annealed single crystals were tested at room temperature in a floor-model Instron testing machine. The results are presented in Figs. 1 and 2. A

Jan 1, 1965

By Goldye Leeds, Marian Balicki

A SURVEY of literature reveals the scarcity of experimental evidence relating to work hardening and reannealing of silver.'-'" With the exception of the well-known X-ray investigation of silver and other metals by W. A. Wood? the effect of progressive cold working has not been studied. The determination of thermal stability of silver in the work-hardened state by means of isochronal or isothermal annealing has been confined apparently to very high reductions only. In the survey made, no study was encountered which endeavored to produce a complete picture of the changes in various properties due to cold working and subsequent reannealing. To fill these gaps and to assemble data that could be used for the determination of activation energies and of frequency coefficients of primary recrystallization, a systematic experimental approach, which was developed by one of the authors, has been applied to pure silver. Material and Processing The silver used was Handy and Harman fine silver, with a spectroscopic analysis at the testing stage of Cu, 0.0001 to 0.001 pct; Te, 0.0001; Pb, Si, Ca, Mg, and Mn, traces. The material was supplied in the form of a rod 0.406 in. diam and was converted into test samples according to the procedure condensed in Table I. It should be mentioned that air annealing was adopted to simulate industrial practice, though it was realized that annealing in a neutral gas or in a vacuum would be preferred. The usual precautions have been taken to eliminate any structural changes and property changes resulting from the storage of the samples prior to annealing or testing. Thus the wires were kept at the fully annealed stage, and the final wire drawing, which produced the desired degree of work hardening, was done just prior to the final annealing or testing. During the short waiting period, the samples were kept in a thermosflask filled with ice. Even with these precautions some strain-age-hardening or self-annealing could occur. To test such a possibility, wires of different reductions were prepared in the manner adopted and portions of them were immediately tested. The remaining portions were similiarly tested after different periods of storage, both at room and melting-ice temperature. Within experimental error, all samples obtained from a wire of a given percentage of reduction yielded identical values. This result qualified the material for further tests and interpretations, because it showed that either strain-age-hardening and self-annealing were absent, or that these effects fully balanced each other. The final annealing was carried out in an electric resistance furnace automatically controlled to within a 10°F. It was realized that the temperature fluctuations were greater than desired for this type of work. TO diminish the errors due to fluctuations of temperature, the hot junction of the thermocouple was placed as close to the samples as possible; the time of soaking was reduced to 15 min; and the number of samples annealed at different temperatures was increased. It will be seen from Table I that some tests were performed on the same material at rising temperature. These will be discussed elsewhere. Room temperature testing was limited to the determination of some of the mechanical properties that are known to be additive in a degree sufficient to be used for indirect study of the kinetics of the reannealing process, Tensile tests, carried out on a manually operated J. Camillon machine, accurate to within permitted the determination of the ultimate stress (U.S.1 and of the 2 in. elongation, (A,). The proof stress (d,e) has been determined from a series of bend tests carried out on a Tinius Olsen Stiffness Tester by using the offset method. This involved accurate determination for each sample of load-angular deflection curves, finding a

Jan 1, 1952

By E. J. Dulis, A. Kasak, R. C. Westgren

The potential of uirought tungsten- and tantaluw-rich alloys of the W-Ta-Mo-Cb system was investigated for high-strength structural applications above 2500° F. Appreciable strengthening of tung-sten and tantalum—essentially attributable to solid-solzction effects—was obtained with binary, ternary, and quaternary alloys. Tensile strengths as high as 67,000 psi were achieved at 3000 OF. ThE quest for wrought structural materials which possess good strength properties at temperatures above 2000°F has led to a considerable research effort during the past decade. In addition to exploring the potential of various high-melting-point refractory metals (such as molybdenum, columbium, tantalum, and tungsten) for very high-temperature structural applications, alloy-development programs have been undertaken to achieve greater strengths than could be achieved with unalloyed refractory metals. The methods of strengthening refractory metal alloys have included both solid-solution and dispersion strengthening. General relationships among the relevant properties (melting point, recrystallization temperature, and high-temperature strength) of refractory metals indicate that the highest strengths at temperatures of 2500°F or higher would be obtained with tungsten-or tantalum-base alloys. Therefore, the present investigation was undertaken to determine the high-temperature strength potential of solid-solution strengthened alloys based on the binary system W-Ta; to effect further strengthening, minor additions of molybdenum and columbium (at the 6 and 12 pct levels) were made. The portion of the W-Ta-Mo-Cb quaternary alloy system of interest is shown schematically in Fig. 1. The component metals—W, Ta, Mo, and Cb—have a bcc structure at all temperatures, and their binary systems are mutually completely soluble.' Complete solid solubility in the W-Ta-Mo and W-Ta-Cb alloy systems has been demonstrated,' and, therefore, it was expected that the quarternary alloys of the system would also exhibit complete solid solubility at all temperatures. In the virtual absence of contamination by interstitial elements, all the alloys would be truly solid-solution strengthened. Twenty specific compositions of this investigation included binary, ternary, and quaternary alloys of the W-Ta-Mo-Cb system as well as unalloyed tungsten and tantalum. The compositions are shown in Table I. EXPERIMENTAL PROCEDURE Consumable-electrode vacuum-arc melting with ac power was used to produce small laboratory-sized, cylindrically shaped ingots (1-1/4 in. in diameter and 2 to 3-1/2 in. long) of the twenty compositions. A furnace was specially constructed to melt as many as four electrode rods simultaneously into molds lined with tungsten or tantalum sheet. High-purity rods of tungsten, tantalum, molybdenum, and columbium were used for consumable electrodes; the diameter of each rod was determined by the desired weight percentage of the component metal in a given alloy. The details of the construction and operation of the melting furnace will be discussed in another p~blication.

Jan 1, 1964

By S. Andrew Kulin, L. Kaufman

A general treatment of the broadening of X-ray double-crystal spectrometer rocking curves due to distributions of tilts and strains has been carried out. The results of this treatment have been applied to the case where dislocations in a crystal give rise to both tilts and strains. On this basis it is found that the rocking-curve halfwidth due to imperfections in the crystal, ßC , increases with increasing Bragg angle, 8. These considerations predict linear relationships between & and tan2 , and ßCand tan 8, for Gaussian and Cauchy distributions of dislocations, respectively. The zero intercept of the ßC us 8 curve, which is a measure of the degree of imperfection of the crystal, is found to depend directly on the distribution rather than the number of dislocations. In addition, the slope-intercept ratio for the ßc - ? curve has been calculated for both the Gaussian and Cauchy distributions. Experimental determination of the - 8 curves for a series of copper single crystals prepared by the Bridgeman and Czochralski methods yields results in agreement with the calculated slope-intercept ratio for a Cauchy distribution of dislocations. CERTAIN X-ray techniques have been used to study the perfection of single crystals. Gay, Hirsch, and Kelly have considered the spreading of spots into arcs on Debye-Sherrer rings due to imperfections. The Double-Crystal Spectrometer has also been applied to this problem.2 The characteristics of Double-Crystal Spectrometer Rocking Curves have been described in the literature by various workers.2-4 By assuming a random spacing of dislocations which give rise to a Gaussian distribution of misorientations relative to some mean orientation in a crystal Gay, et al.,1 arrive at the conclu- sion that the most probable misorientation is given by where h is the spacing between dislocations, and 8 and are the relative misorientations of neighboring regions. If ßC is the halfwidth of the rocking curve (the width at one-half the peak intensity) due to dislocations in the crystal then5

Jan 1, 1960

By C. M. Schwartz, J. R. Bridge, D. A. Vaughan

THERMAL expansion coefficients of a uranium were originally reported' on the basis of X-ray diffraction measurement of lattice constants at 25°, 300°, and 650°C. These data have been reproduced by Katz and Rabinowitch.' CuK radiation had been used in this work, with consequent crowding of the patterns. Considerable overlap of the back-reflection lines was observed as the temperature was raised. Subsequent reexamination of the data led to the conclusion that errors had resulted from failure to obtain unequivocal indexing of the high angle reflections at elevated temperatures. The measurements have been repeated, using FeK radiation, which provided sufficient dispersion to assure proper indexing of the reflections, at each temperature level. The unit cell dimensions were re-determined at ten temperatures, from 25" to 650°C. Schuch and Laquer easured the macroscopic contraction from room temperature down to —253°C, and reported a negative value from —210" to —253°C; they suggested the possibility of the occurrence of a phase change. In the present work, the lattice constants of uranium have been measured down to —253°C, to test this hypothesis. Filings were prepared from a single piece of pure uranium bar stock. They were carefully cleaned with a magnet and pickled in nitric acid to remove traces of iron from the file. They were then annealed at 600°C in a sealed evacuated silica tube. The annealed filings were pickled in strong nitric acid to remove any oxide layer, washed in water and alcohol, quickly dried, and sealed in evacuated thin-walled silica capillary tubes. If properly sealed, the sample could be heated to the a-ß transforination temperature without significant buildup of the diffraction pattern of oxide. The high temperature X-ray diffraction camera was modified from the design of Hume-Rothery and Reynolds.' The thermocouple used to record the specimen temperature was calibrated from lattice-constant measurements of a standard silver specimen, using the Hume-Rothery and Reynolds values for silver over the temperature range from 25" to 700°C. Temperatures were reproducible to 210°C. Temperatures to —210°C were attained by passing precooled gas over the sample. The gas from the cooling train was directed over the sample capillary tube and thermocouple by means of a chimney of 1-mil polystyrene. The 36-gage Cu-constantan thermocouple had been calibrated by

Jan 1, 1957

By Robert E. Green, Kenneth Reifsnider

A microscopic X-ray diffraction technique was employed for the simultaneous study of the behavior of several families of lattice planes, whose local orientatiotz changes are manufestations of internal distortions resulting from specimen deformation. Photographs taken using aluminum were single crystals 1/64 in. In diam are presented which illustrate the appearance of various types of deformation- or growth- induced structural variations. Slip and lattice bending were detected in tensile tests for strains as small as 0.1 pct. Evidence of deformation bands, lineage structure, and void formation wns also shown. AmONG the most important methods of studying internal stresses in metals is the utilization of various X-ray techniques. The general subject of X-ray metallography has been treated in a most excellent manner by Taylor,1 and the use of X-rays for the direct observation of imperfections in crystals has recently been reviewed in an article by Newkirk2 and in the book edited by Newkirk and Wernick.3 Since the inception of metallographic X-ray analysis, there have been numerous technological developments and refinements, each with its particular advantages and disadvantages and, acrording to these, its particular applications. X-ray diffraction techniques can be divided into two general categories, that of X-ray diffraction microscopy and that of X-ray diffraction macroscopy. In the former are included such methods as those of Berg-Barrett, Lang, and Schultz2,3 which are concerned with microscopic imperfections such as dislocations. The second category includes all work concerned with the study of the condition of a crystal lattice structure as indicated by the marroscopic detail in its diffraction patterns. An example of this is the study of the diffraction manifestations of inhomogeneous plastic deformation as manifested by formation of deformation bands and inhomogeneous lattice rotations. The method used in the present investigation was an X-ray diffraction macroscopy technique. The geometry and analytical aspects of the method were similar to those of Julien and Cullity.4,5 The source was collimated with a single slit in a manner simi- lar to the "parallel beam'' method of Barth and Hosemann6 except that a continuous spectrum of radiation was employed. The apparatus produced large-beam transmission Laue patterns of thin cylindrical aluminum-wire crystals, which were deformed either in tension or torsion. Although the conventional X-ray target and interposed slit were not capable of the high resolution obtainable with a fine-focus X-ray source as employed in a microfocus apparatus, resolution was a secondary consideration in our technique, and was sacrificed to obtain sufficient intensity along a sizable length of the specimen. By using a grid indexing technique similar to that of Barth,7 we were able to study several diffraction lines from various planes simultaneously. The results of these tests give additional information with regard to the inhomogeneous deformation of single crystals, and the indexing procedure used provides a correlation between portions of the test specimen and portions of a diffracted beam. EXPERIMENTAL TECHNIQUE The experimental arrangement used is shown schematically in Fig. 1. A source of continuous X radiation from a vertically mounted Machlett X-ray tube possessing a copper target and operated at 20 kv and 10 ma was passed down a horizontal lead tube 80 cm long which terminated in an adjustable vertical brass slit. The slit opening was adjusted to correspond with the diameter of the test specimen. In front of the brass slit it was possible to place a screen wire mesh, one horizontal strand of which was a lead wire which served as a fiduciary mark, the screen itself serving as an indexing system as will be described later. Behind the screen was the test specimen which consisted of an aluminum single crystal wire 1/64 in. in diameter and 3 in. long. These 3-in.-long crystals were cut from

Jan 1, 1965

By A. J. Jacobs, G. Katz

MANY of the studies of intermetallic compounds containing uranium were performed during the early 1940's under the aegis of the Manhattan Project. Subsequently, much of this work was declassified and published after 1949. In some instances this early work, completed with relatively impure materials, represents the only source of X-ray diffraction powder data available in the literature. In the case of the intermetallic compound U,Fe some discrepancies in the powder pattern exist in the literature. Since this compound has been prepared in this laboratory, it is believed that the publication of the indexed powder pattern would help clarify the conflict in the literature. In studies of the U-Fe system, Gordon and Kauf-mannl and Grogan and Clews2 independently reported the intermetallic compound U,Fe in 1950. The crystal structure was described by Baenziger, Rundle, Snow, and Wilson3 in 1950. It is isostructural with U,Mn, U,Ni, and U,Co and crystallizes in a body-centered tetragonal lattice. The lattice constants determined by Baenziger et al. are: giving an X-ray density = 17.7 g cm-3 for 4 mol per unit cell. The compound used in this study was prepared by melting a stoichiometric mixture of the constituent metals in an argon-arc furnace using a nonconsum-mable tungsten electrode. Before the argon of 99.98 pct purity was introduced into the furnace, it was passed through CaC1, to remove water vapor and afterwards through a stainless steel tube containing calcium turnings heated at 600°C for the removal of nitrogen and oxygen. The purity of the uranium used was better than 99.9 pct and that of the iron was 99.97 pct. Before and during melting a zirconium getter was used to further purify the argon atmos-

Jan 1, 1962

By C. Altstetter

THE work herein reported is restricted to the carbides which occur in quenched and tempered AISI 43XX steels with carbon contents up to 0.40 pct and silicon additions of up to 3 pct. In view of the instability and extremely small size of the carbides formed at low tempering temperatures, the technique for successfully preparing specimens for X-ray diffraction will be outlined. The alloys listed in Table I were obtained through the courtesy of the United States Steel Corp. in the form of 1/2-in. rounds forged from 100 lb. induction furnace heats (except for 4337 which was a commercial heat). The stock was normalized and then swaged and drawn to 15 mil wire with anneals at 1200F between passes. The wire was austenitized for 45 min in evacuated vycor capsules and quenched into iced brine with simultaneous smashing of the capsule. Tempering was done in air with a water quench after tempering. The carbides were extracted in a simple cell using a solution of 1M KC1 and 0.5 pct citric acid with an initial current density of 0.1 amp per sq cm. One end of a short length of wire was immersed in the solution, and the current at constant voltage was noted as a function of time. After about an hour the current dropped sharply because of the decrease in specimen cross-section. At this point it was found that the dissolution could be stopped and that the very fine wire which then resulted was just large enough to permit handling of the extracted precipitate still clinging to it, yet so small that it diffracted and absorbed only a negligible amount of the X-radiation. This rod of residue with a convenient handle of undissolved wire was rinsed in distilled water. alcohol, and acetone. Then it was dipped in a thin solution of cellulose-acetate cement and dried in vacuum. The resulting specimen was straight, uniform in density, easily handled, but most important, was completely sealed and never exposed to air. Furthermore, the residue had never been subjected to strong acids or rough handling such as in the extraction-replica technique or in the complete extraction to a powdered residue. It was found that improperly coated specimens were pyrophoric, turning to oxide with a dull red glow as they were exposed to air and yielding patterns of Fe2O3 and Fe3O4. The steels containing 3 pct Si were especially difficult to prepare for this reason. The specimens were put in a 57 mm Straumanis camera with double pinholes or slits and irradiated with filtered-chromium radiation. Readable patterns were obtained in less than an hour. A preliminary finding of some note was that for both tempered and as-quenched specimens of steels 4337 and 4337 (1.5 Si). M23C6 patterns were found along with the patterns of other constituents of the residues. This result was somewhat surprising in that previous investigators had reported that this carbide did not appear in a 0.38 pct C, 0.48 pct Mo steel1 or in chromium steels of less than about 10 pct Cr.2 Although the total amount of carbide-forming alloying elements is less than 2 pct, due to their mutual interaction and the action of the plastic deformation in promoting equilibrium, this carbide was able to form even in the steel containing 1.5 pct Si. M23C6 was not detected in the 4337 (3.0 Si) steel and the lower-carbon steels were not investigated in this condition. It is very likely then that the steels studied herein underwent a fourth stage of tempering during the anneals at 1200°F. This result has significance in that even a small amount of undissolved M23C6 in a low-carbon, low-alloy steel would exert a large effect on its hardenability. Its presence would also influence the mechanical properties by decreasing the carbon content of the matrix. Annealing in vacuum for 1 to 4 hr in the austenite field removed all traces of MZ3C+ The results on carbide precipitation during tempering, summarized in Table I, are in agreement with those of Klingler et al.3 for the higher carbon steels. For the AISI 4337 steels it is noteworthy that in the steels with added silicon the E carbide persists to longer times and higher temperatures and that silicon delays the formation of cementite. The results for the lowzr-carbon steels parallel those of the higher-carbon grade. The appearance of E carbide in the AISI 4315 is significant. There is considerable disagreem-nt in the literature as to whether this carbide forms in the tempering of steels containing less than about 0.2 pct C. Following the detection of E carbide in a 0.18 pct C plain-carbon steel,4 its occurrence in a steel containing chromium and molybdenum should be expected. The fact that the low-carbon steels have the same carbide-precipitation sequence as the high-carbon steels has bearing on the larger problem of the exact tempering reactions in all steels. Following the suggestion of Roberts et al.,' the first stage has been generally assumed to result in a metastable equilibrium of c carbide and martensite of about 0.25 pct C. From this it was concluded that a steel having less than 0.25 pct C should then be under-saturated with respect to c carbide and should not precipitate this carbide upon tempering. In view of the experimental findings of c carbide in steels hav-

Jan 1, 1962

By J. P. Boisseau, C. N. J. Wagner, E. N. Aqua

An analysis ulas made of powder-paltern peaks from cold-rolled polycrystalline copper and from copper powders, compacted into briquets (1 in. diameter) with pressures up to about 106 psi. Powder-pattern peaks from both contact faces were measured with a diffractometer and CuKa radiation. Laltice-parameter measurements indicate the presence of residual stresses in the bulk specimen of the order of a - -10 kg per sq mm after 93 pct reduction in thickness, and give some evidence for the occurrence of deformation stacking faults (probability a - 0.003) in both bulk and powder samples. Fourier analyses of the line profiles were carried out on the (111) - (222) and (200) - (400) Pairs of reflections. The particle sizes decrease rapidly with increasing deformation and reach asymptotic values of De (111) = 550A and D, (200) = 350A at about 25 pct reduction in thickness or 80,000 psi pressure for compaction. The anisotropy of the particle sizes indicates the presence of microtwins and stacking faults on (111) planes. The rms strains increase also with deformation and reach limiting values of 2 x 10-3 in the [100] direction and 1 x 10-3 in the [Ill] direction at a distance L = 100A normal to the reflecting planes. THE diffraction of X-rays in cold-worked, polycrystalline, fcc metals and alloys yields Debye-Scherrer patterns in which the individual (hkl) lines may show a broadening, a shift, and an asymmetric shape.' These effects can be explained by the fragmentation of the small, coherently diffracting domains, the presence of residual elastic strains in the lattice, and the formation of stacking faults. X-ray studies of stacking faults in fcc metals and alloys have been methodically performed during the last few years, but so far most of the investigators dealt with cold-worked powder specimens obtained by filing.2-8,10-19 In such specimens, the crystals are randomly oriented and the average elastic strains are assumed to be zero, so that the observed peak shifts are due to stacking faults only. The agreement between X-ray diffraction theory1,20 and experiment is generally good. On the contrary, cold-worked, polycrystalline bulk specimens (after wire drawing, rolling, plastic deformation by tension or compression, etc.) contain residual elastic strains, which may not average to zero in the surface of the specimen and show very strong preferred orientation of certain lattice planes (texture) parallel to the specimen surface. Nonzero elastic strains also produce peak shifts, the magnitudes of which depend upon the crystallographic orientation of the reflecting lattice planes in elastically anisotropic materials as well as on the type of plastic deformation and which have to be taken into account when measuring stacking-fault probabilities in deformed bulk specimens.21-23 The purpose of the present investigations was to perform a detailed X-ray analysis on a bulk specimen of a fcc metal deformed by rolling at room temperature and on powder of the same material deformed by compaction, and to compare these results with those previously obtained on cold-worked filings.18 Pure copper was chosen for this study since it is known to produce only a small quantity of stacking faults by filing at room temperature.3,16,17,19 The residual elastic strain in the surface of the bulk copper should be the predominant factor determining

Jan 1, 1965

By F. von Gemmingen, E. J. Fasiska, L. Zwell

EARLIER studies of the dependence of creep on structure1 and of the dependence of creep rupture on creep behavior2 did not include detailed discussion of the phases present in the specimens under examination. It is of interest to determine the nature and amounts of such phases present since it is well known that these are dependent on composition, heat treatment and creep conditions.3 This investigation has therefore been undertaken to identify these constituents and to determine their relative amounts. This report presents the results of this investigation and describes an improved "extraction replica" technique developed in the course of the work. The composition of the Type 316 austenitic stainless steels studied in this investigation is given in Table I. The specimens were solution treated at 2000°F for 1/2 hr and water quenched. Those specimens subjected to prestrain at room temperature Methods for extracting precipitate particles from materials for electron and X-ray diffraction analysis have been described by Fisher,4 Smith and Nutting: and Booker and coworkers.6'7 Electrolytic extraction methods have been described by Andrews and Hughes.8 The first two methods have been used at this Laboratory, but have not proved satisfactory for many problems requiring X-ray diffraction analysis. It has been difficult to remove the replicas or to avoid tearing them during removal. These difficulties are overcome by backing the replica with a water-soluble plastic such as Dupont 51-05 Elvanol (polyvinyl alcohol). The backing increases the thickness of the replica so that it can be mechanically stripped from unloosened particles without folding or tearing. This procedure eliminates the stripping of wet replicas, which usually have a low tear strength. By stripping replicas after drying, it is possible to extract partially loosened particles which otherwise would remain imbedded in the metal. The modified method is as follows: after the specimen is polished, it is etched for 60 min in modified glyceregia consisting of 30 ml glycerol, 7 ml nitric acid, and 4 ml of hydrochloric acid. The sample is then washed, air dried, and coated with a 20 pct Baker and Adamson 1611 collodion (85 pct amyl acetate by volume) film. After the collodion film is dry (about 15 min), the sample is again etched in the modified glyceregia for 50 min, washed with isopropyl alcohol (to prevent dissolving the collodion) and air dried. A very thick coat of polyvinyl alcohol (about 50 pct solution "Elvanol Dupont 51-05" in water) is poured over the sample and is permitted to dry for about 24 hr. The composite film containing the precipitates is then stripped from the specimen and floated, polyvinyl alcohol side down, in water (at about 50°C) until the polyvinyl alcohol dissolves. This usually takes about 15 min. Should any of the polyvinyl alcohol remain on the replica, it does not give a crystalline diffraction pattern and therefore does not hinder identification of the precipitates. The extraction replica, floating in water, is picked up on a glass fiber and mounted in the Debye-Scherrer camera for X-ray diffraction analysis. Concentration of the etchant, and also etching time, had to be increased for several of the samples. Fig. 1 shows two extraction replicas taken from different areas of spec. M74-37; X-ray analysis showed a strong diffraction pattern of M23C6 and a medium one of u phase. A

Jan 1, 1962

By J. B. Cohen

In an investigation of the microstructure of shock-loaded metal specimens1 C. S. Smith found that there was little distortion of grain boundaries or change in external dimensions, although the hardness corresponded to that produced by severe rolling. Furthermore, the hardness of individual grains was independent of the deformation structures present; grains with no markings were as hard as those heavily populated with markings. These markings which resemble twins do not appear in copper until high shock-loads of the order of 200 kb are applied. It appears that due to the high velocity of a shock wave and its sharp front, heavy deformation takes place on a submicroscopic scale. In this work an attempt was made to examine this deformation, particularly at a load below which macroecopic markings appear. The broadening of 200 and 400 diffraction peaks was examined from the face of a poly crystalline sample normal to the direction of the shock wave. These peaks were chosen because the elastic constants in copper are such that residual strains would be greatest in the <100> directions; hence, the strain-broadening contribution to these peaks would be large in comparison to other sets. Also the broadening due to stacking faults and microtwins would be greatest with this set.2 A complete Fourier analysis of these peaks was made, as described by warren,&apos; using the Stokes correction with peaks from an annealed sample.3 With the aid of the U. S. Army Ordnance Corps EDVAC computer and a curve matching program, sixty sine and sixty cosine coefficients were obtained for each peak. The last of these was about 1.5 pct or less of the largest coefficient, indicating good representation. Transverse sections from a 1.5 in. rod of as-drawn electrolytic tough-pitch copper were reduced in cross-sectional area about 50 pct by cross rolling. Disks 1.5 in. in diam were recrystallized at 275 °C for 30 min and then at 300°C for the same time. The faces were polished and deeply etched in nitric acid to remove 25 mils. The grain size was 0.02 mm. Laue back-reflection patterns indicated the sample was well recrystallized. The two diffraction peaks from this sample were recorded on a Norelco diffractometer using filtered copper radiation. Peak intensities were kept less than 600 cps to assure linearity of the counter and circuitry. This sample was then placed between two rods of the same material and diameter. The top rod was 2.25 in. long and the bottom rod 1 in. long. (In

Jan 1, 1961

By W. P. Evans, R. W. Buenneke

Warren and Averbach&apos;s multiple order, Fourier method was applied to solid specimens of SAE 1045 steel. The material was hardened to three hardness levels and specimens of each hardness were shot peened to three intensities. Particle size, root-mem-square strain, mean strain, md macro residual stress were determined for each. Microstrains caused by either hardening or peening varied markedly over microregions. In general, increasing the hardness or peening intensity increased the rms strain and decreased the particle size. Similar effects were observed by varying hardness and peening intensity independently. At a Rockwell hardness of C 50, peening had little effect on line broadening, but both mean strain and macro residual stress increased. Mean strain was independent of column length. Induced macro residual stress by peening was affected most by initial hardness, but not by specific peening intensity. The purpose of this work is to establish the state of residual strain and particle size by X-ray diffraction in hardened and cold-worked plain carbon steel and attempt to relate these X-ray measured parameters to fatigue performance. X-ray line broadening (and its micro implications), along with X-ray residual stress (and its macro implications), may be basic indicators of the inherent fatigue resistance of the material. X-ray line broadening is caused by variable lattice strains and small particle size. Both are a result of plastic deformation which accompanies hardening or cold working processes. Therefore, X-ray line broadening is a good measure of both. warren1 has recently reviewed the Warren and Averbach2,3 Fourier analysis of line broadening. Strain and particle size effects can be separated because broadening due to particle size is independent of order of the diffraction peaks, while broadening due to strain is not. Microstrain is obtained as a root-mean-square strain averaged over discrete distances within the crystals causing diffraction. These distances are quite small, varying from 10 to 10081, and may be interpreted as the gage length over which the strains are averaged. Because of their variable nature, the X-ray line is broadened. The plot of rms strain vs distance (or column length) within the specimen gives a measure of their variability. Small particles also cause X-ray line broadening as already mentioned. A particle is interpreted as a region within a crystal or grain which diffracts X-rays coherently. This region is one of given orientation and may be bounded by a small angle grain boundary, dislocations, a twin boundary, or a stacking fault. The present work covers measurement of X-ray line broadening and macro residual stress on an SAE 1045 steel, quenched and tempered to various hardnesses. Various amounts of cold working were produced by shot peening the surfaces to various Almen intensities. Particle size, root-mean-square strain, and mean strain were calculated from the Fourier coefficients of the X-ray diffraction profiles in a direction normal to the peened surface. No effort was made to separate the various causes of particle size broadening. Macro residual stresses were reported in directions parallel to the peened surface. I) X-RAY METHOD The Fourier coefficients were determined for the 110 and 220 X-ray profiles. They were corrected for instrumental broadening by the method of Stokes,4 using an annealed reference specimen of similar geometry presumed to be free from broadening due to small particles and distortions. The nth Fourier cosine coefficient, A,, is related to a particle size coefficient, Ap, and a distortional coefficient, ADn, by the equation:

Jan 1, 1963

By R. E. Ogilvie, E. T. Peters

The X-ray Kossel-line method has been used preaioz~sly for measuring lattice parameters to accuracies of 1 part in 100,000.5 A second application of this method is described for determining the crystallographic orientation of a randomly positioned single-crysta1 spherical volume that can he as small as 50 µ in diameter, within accuracy limits of ±1/2 deg. The theory, experimental procedure, and interpretation of Kossel-line patterns and an experimenta1 verification of the predicted orientation relationship of the cph k and fee a Cu-Si phases are presented. This orientation relationship can be described as (111)a, (00.1)k; [110]a [11.0]k. In addition, the lattice parameter of the a phase was found to he a. = 3.62154 ± 0.00014Å. The Kossel-line method when used in conjunction with electron microanalysis is shown to he capable of providing a complete chemical and structural analysis of a given crystal. THE most easily accomplished methods for determining the orientation of a single crystal are variations of the Laue X-ray diffraction method. Although certain materials can be oriented to within ± 1 deg accuracy by observation of exterior macroscopic features, such as etch pits, cleavage faces, or growth features, the Laue method is generally preferred for routine laboratory application. Both back-reflection and transmission patterns are coordinated by appropriate reference charts and are plotted in terms of reflection plane poles (normals) on a stereographic projection. Orientation is deduced by relating the pole distribution (which is fixed by the crystallographic symmetry of the specimen) to two specified external reference directions. The Laue method has several limitations. 1) Orientation can rarely be determined to better than ±l deg accuracy. Principal errors involve inaccuracy in specimen-to-film distance, measurement confidence of individual Laue spots, and stereographic plotting. 2) Because of the indeterminacy of the X-ray wave length diffracted to a given spot, it is not possible to determine supplementary crystallographic data, such as interplanar spacings and lattice parameters. 3) The method is generally limited to specimens of cubic symmetry or to specimens of high symmetry and known structure. 4) The relatively large cross-sectional area of the incident X-ray beam generally precludes the measurement of relative grain orientation in a polycrystalline material.* _____ Several of these limitations can be overcome by application of the Kossel-line method, which has been previously employed for precision lattice-parameter determinations.&apos;-= For this method, a point source of divergent monochromatic X-rays is generated within the crystal by means of an incident electron beam. The divergent X-rays which fulfill the Bragg law are diffracted by the specimen and are recorded on a film placed either in transmission or back reflection. Analysis of the film yields a direct measurement of orientation and lattice-spacing values to an accuracy of ±1/2 pct. As analyses can be obtained from spherical specimen volumes as small as 50 µ in diameter, the method provides a means for structural analysis of second-phase or impurity precipitates within a given matrix. The primary limitation of the Kossel-line method is the requirement for an electron microanalyzer or similar apparatus capable of producing a finely focused electron beam. This paper is designed to present the theory, experimental procedure, and geometrical interpretation of Kossel patterns. The experimentally determined orientation relationship between the k and a phases occurring in the Cu-Si system and a precision measurement of the a lattice parameter are presented as a practical application of the method. THEORY OF KOSSEL LINES Divergent X-ray beam photography utilizes an effective point source of characteristic X-rays which, when diffracted from a single crystal, form numerous diffraction and absorption cones that are recorded on film.7 The cones generated from a source lying within the crystal are called Kossel lines.&apos; Although the X-ray scattering from a divergent point source contained within a crystal is described in terms of Laue dynamical theory,9 the directions of the diffracted spectra can be ade-

Jan 1, 1965

By J. A. Berger, R. J. Towner

The pjPocesses of polygonization and subgrain growth were followed in slightly stretched 99.99 pct A1 single crystals heated for cumulative times at 400°, 500°, and 600°C. Changes in sub-grain size and boundary angle were determined from measurements on X-ray micrographs. CAHN1, 2 studied polygonization in stretched and heated aluminum single crystals of 99.99 pct A1 using various techniques, including etch pits, Laue patterns, and a slight restretching of heated specimens to reveal small changes in lattice orientation by the direction of new slip lines. He found that kink bands, which had well-defined boundaries lying in a plane perpendicular to the slip direction (at least in the early stages of deformation), formed during stretching. Also, he noted that bending occurred about the <211> axis lying in the (111) slip plane perpendicular to the <110> slip direction. His studies of polygonization were largely confined to the kink bands rather than to the weakly bent matrix regions between bands. The minimum temperature required to bring about polygonization was established at about 450 "C. Guinier and Tenevin used a focusing Laue X-ray diffraction technique to study polygonization in aluminum single-crystal specimens of 99.99 pct purity. Stretching the crystals 5 pct in tension caused a widening of the focused Laue spots. After heating for 4 hr at 450°C, their method revealed no change in the specimen. Above 450°C polygonization was detected and further annealing near 600°C led to subgrain growth. They concluded that the orientation of the crystal relative to the axis of deformation had no marked effect on polygonization. Gay and Honey-combe4 using an X-ray microbeam technique found that polygonization did not occur in a stretched aluminum crystal heated at 250oC, although some decrease in the yield strength occurred. When the temperature was raised to 475oC, the asterism became broken up as a result of polygonization. Honeycombe5 noted that reflections on X-ray mi-

Jan 1, 1961

By Ganesh P. Mohanty, James J. Wert

THE brittleness of the intermetallics usually render their deformation studies at ordinary temperatures using conventional techniques inadequate. On the other hand, although X-ray line broadening measurements is not a complementary technique, it provides a means for gaining limited but useful information on the cold worked state of these materials. In the present instance, a study of the effects of cold work in the lead telluride intermetallic compound was carried out by analyzing the diffraction profiles of the deformed and the corresponding annealed samples. An ingot of PbTe was prepared by induction melting high-purity lead and tellurium in a quartz crucible under an atmosphere of argon. After homo-genization, the ingot was ground to -325 mesh at room temperature, and using a polished die the cold- worked powder was pressed into the form of flat faced briquets for diffraction measurements. A spectrometer with 0.125 deg per min scanning velocity, CuKa radiation, pulse height analyzer, and a proportional counter were employed in the X-ray measurements, and the powder peaks were collected from the sample in fully cold-worked state and after it had been annealed to relieve the effects of cold work completely. For reliable estimates of the peak extremities, small angular ranges where the tails merged into the background were point counted. Fourier inversions of the experimental peaks were carried out in an IBM 705 computer using the procedures introduced by stokes.&apos; Both the cosine and sine components of the Fourier series were used to take into account any peak assymetry arising

Jan 1, 1963

By D. Geiselman, A. G. Guy

Single cvystals were grown from high-purity magnesium containing known amounts of nitvogen in the range 0.0008 to 0.0048 wt pet. Crystals of known ovientation were tested in tension in an Instron ma chine to determine the yield strength and to obsevue wheather a yield point occurred. Slowly cooled crystals or those given a solution heat treatment did not show a yield point. However, crystals that were aged following a solution treatment showed a yield point for all of the nitrogen contents studied. It was concluded that nitrogen caused the yield point by the Cottrell mechanism. NITROGEN has been shown to produce sharp yield points in single crystals of cadmium, zinc,2&apos;3 ß-brass,4 and iron,5,6 as well as in polycrystalline iron7 and molybdenum.8,9 Since magnesium has a structure similar to zinc and cadmium, it seemed reasonable that magnesium should also exhibit a sharp yield point provided it contained sufficient nitrogen. Bobalek and Shrader10 reported a total nitrogen content of 0.002 to 0.0065 wt pct in com- mercial magnesium alloys, an amount well in excess of that required by theory. However. magnesium differs from cadmium and zinc in that it forms a stable nitride, Mg3N2, which has a standard free energy of formation of -95,480 cal per mole at 25" c." If rather than being in solid solution, the nitrogen were predominantly combined as the nitride, it could not act to produce a yield point. This type of behavior is the basis for the elimination of strain aging and a yield point in steel by the addition of strong nitride formers such as titanium,12 columbium,13 aluminum,14 vanadium,15 and boron.16,17 Thus, there appeared to be factors both favorable and unfavorable to the production by nitrogen of a sharp yield point in magnesium, and the purpose of this investigation was to determine the actual behavior of magnesium crystals containing known amounts of nitrogen.

Jan 1, 1960

By Joachim J. Hauser

Experiments on latent hardening were peyformed by compressing single crystals along a direction perpendicular to the tension axis. The slope and length of easy glide in the tension test were found to depend only on prior deformation in the same slip plane. Prior deformation on a different slip plane changes the stress level of the resulting stress-strain curve. The yield points appearing upon reloading after prior extension and unloading were related to the end of easy glide. SEVERAL researchers have studied the latent hardening due to deformation of a crystal by slip on a slip System after prior deformation. These experiments can be divided into those in which the prior deformation was on the same plane as the subsequent and those in which the two deformation processes were in different planes. In the former category are the experiments of Buckley and Entwistle,1 Parker and washburn,2 and Haasen and Kelly.3 The latter case has not been studied systematically; it was the main purpose of this investigation to produce this type of latent hardening and explain the results in terms of the existing theories of work hardening. In general, tension producing slip on a certain slip system can be preceded by tension, transverse compression or longitudinal compression, each with predictable dislocation movement and intersection. The intersection of dislocations can lead to glissile or sessile jogs, Cottrell-Lomer locks and other sessile dislocations. The effect on the stress-strain curve could depend on which combination of the former mechanisms is operating. Haasen and Kelly3 have studied the yield points which occur in aluminum and nickel single crystals upon reloading after prior unloading in a tension experiment. They attributed this effect to the anchoring of dislocations occurring during unloading. As Cottrell and stokes4 have shown that dislocations cutting through the "forest" could only lead to reversible changes, they attributed the anchoring to the formation of sessile dislocations during unloading. However, different kinds of sessile dislocations could be formed during unloading, and it was the purpose of this experiment to determine whether Cottrell-Lomer locks are responsible for the yield effect and for the end of easy glide. The case where a longitudinal compression is followed by tension along the same axis is commonly referred to as a Bauschinger test. This type of effect was studied by Buckley and Entwistle1 on aluminum single crystals and by Parker and washburn2 on zinc single crystals. In such a test, the tension and the compression activate the same slip plane with opposite slip directions. The use of sideways compression in the present experiments permits the activation of different types of slip systems and the study of their effect on the easy glide region and on the transition between the elastic and easy glide region. The theory of seeger5 for the flow stress in fee materials is applied to explain the latent hardening. EXPERTMENTAL PROCEDURE All the single crystals used in this investigation had an axial orientation close to <210>, called the "0.5" orientation. This is the orientation for which the tensile axis is 45 deg from both the slip plane and the slip direction. The single crystals were grown from the melt under a helium atmosphere using milled graphite boats,=at a rate of 8.6 mm per min. The silver used in the experiment was 99.98 pct pure. The single crystals had a square cross section about 0.9 by 0.9 cm and a length of 14 cm. The orientation of the specimen was determined within ±2 deg by the Laue back-reflection method. The specimens were annealed at 940&apos; ± 2°C in a helium atmosphere for 24 hr and then furnace cooled over a period of 7 hr. The specimens were electropolished in a solution of 9 pct KCN in water. The specimens were tested in a soft-type tensile machine (the load is prescribed) up to 3 pct strain. The stress was increased continuously at approximately 30 g per mm2 per min. The strain was measured over a 5 cm gage length with a mechanical extensometer employing an optical lever. The strain and stress were measured with accuracies of i 2 X 10-5 and ± 2 g per mm2, respectively. The remainder of the stress-strain curve up to 20 pct strain was obtained in a hard-type tensile machine (the strain rate is prescribed). The strain and the stress were measured in that machine with an accuracy of ±2 pct. The compression tests were performed in the hard-type machine using accurately machined steel blocks without lubrication. The blocks were used so as to apply a uniform compression over a length of 13 cm. The strains were measured on the hard-type machine and with a micrometer.

Jan 1, 1962

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

A yield point effect attributed to short-range ordevi?g (SRO) occurs in Cu base Al. At at 296°K varies with heat treatment, decreasing as the annealing ternperature is raised .from 433Oto 598°K. Davies aid Cahn&apos; observed a corresponding decrease in SRO. (523 °K anneal, measured at 77°K) is approximateZy proportional to the variations of A7 with strain rate and testing temperature are also Consistent with the idea that is associated with SRO. A preliminary investigation of the tensile properties of a Cu-Al single crystals showed the presence of a rather strong yield-point effect (drop in flow stress after initial yielding). The object of this research was to investigate its origin and behavior. a Cu-Al alloys are particularly interesting because diffuse X-ray scattering measurements by Davies and Cahn,&apos; Houska and Averbach,&apos; and Borie established the presence of short-range order. The degree of local order may be changed with heat treatment.&apos; cottrel14 suggested that the presence of local order might result in a yield-point effect, and thus the possibility exists here for experimentally ascertaining the importance of short-range order with respect to yield points in these alloys. Since a 12 pct difference exists between the atomic sizes, elastic or Cottrell locking5 must also be considered. Further, Howie and swanne have shown that the stacking fault energy of copper is reduced by aluminum additions. The width of extended dislocations should thereby increase. hus the conditions appear attractive for Suzuki locking.&apos; Finally, the possibility of stress-induced order at dislocations, schoeck locking,&apos; must also be examined, EXPERIMENTAL PROCEDURE Alloys up to 14 at. pct Al were prepared by induction melting high-purity (99.999 pct) Cu and (99.996 pct) Al in a graphite boat under a dynamic vacuum of 5 X 10o mm of Hg. After homogenizing the ingots at 900°C for at least 24 hr under vacuum, they were rolled with intermediate anneals to strips 1.55 mm thick. Single crystals 10 in. long were grown by lowering strips, contained in a split graphite mold sealed in fused quartz at 5 X lo-&apos; mm of Hg, through a single coil induction heater at a constant rate of 1/2 in. per hr. Tensile specimens 1.25 in. long were cut from the single crystal strips and reduced cross sections about 0.7 in. long and 3.0 to 3.5 mm2 in area were introduced by filing and abrading.8 To remove the worked portion about 10 pct of the cross-sectional area was removed by etching. Back-reflection Laue photographs of a filed and etched specimen were taken before and after annealing at 900°c for 24 hr. Small, well defined Laue spots were obtained with no visual difference in the two photographs. Further, specimens with and without the reduced sections began yielding at about the same stress. Hence, for our purposes, filing and abrading did not affect the structure of the specimens. Each single crystal specimen was annealed at 900° c in vacuum for at least 24 hr and furnace cooled; while cooling through the range of 250o to 200°c, the rate was about 55°C per hr. Orientations were determined by the usual back-reflection Laue

Jan 1, 1962

By R. Grierson, R. N. Parkins

The m.echanica1 properties, at high lzomologous temperatures, of the intermetallic compounds InzBi and Mg17A112 were measured as a .function of temperature, applied strain rate, previous thermal and mechanical history, and composition. Mgl,Al12 was investigated ilz compression, whereas Zn,Bi was investigated in tension. A decrease inflow stress with increasing strain was observed jor both alloys. The results obtained are discussed in terms of the dislocation-multiplication processes in these materials. MANY intermetallic compounds are reported to undergo a brittle-ductile transition at high homologous temperatures.&apos; There is evidence in the literature that some of these compounds exhibit a large yield drop when plastically deformed.&apos;j3 Both of these forms of behavior are shown by the covalent elements germanium and silicon4,5 and also by certain ionic compounds.8 The present work is a study of the deformation, at high homologous temperatures (>2/3 Tm), of two intermetallic compounds, In2Bi and Mg17Al12. InzBi has a disordered hexagonal structure7 (c/a = 0.598) and a solubility range of 32.3 — 33.2 at. pct Bi.8 It has a melting range from 72° to 89°C. Mg17Al12 has an ordered bcc (A12 type)7 structure and exists over the range 50 to 60 at. pct Mg8 with a melting range from 437° to 462°C. We have been unable to find any reference to previous investigations of the mechanical properties of BiIn,. Novikovg has reported that cast samples of Mg17A112 show ductility, when bend-tested, at temperatures above 380°C. EXPERIMENTAL Ingots of In2Bi and Mg17Al12 were melted under an argon atmosphere and cast, in situ, in a graphite crucible. The materials used were of 99.99 pct purity. The alloys prepared contained 66.9 at. pct In in the case of In2Bi and 58.4 at. pct Mg in the case of m17A112. The ingots were homogenized and then extruded. Two-in.-diam Mg17Al12 ingots were extruded at 375°C to give 3/8-in.-diam rod. The rate of formation of this rod was 0.25 in. per min. One-in.-diam InzBi ingots were extruded at 20°C, using a rate of 1 in. per min, to give 1/8-in.-diam rod. In both cases the extruded rod had a recrystal- lized, fine-grain, structure. (For Mg17Al12, d = 11.2 µ; for BiIn2, d = 22 µ.) Mechanical-property determinations were made in a hard-beam machine, in tension in the case of In2Bi and in compression with Mgl7Al12. The tensile tests were on specimens having a gage length of 1.1/2 in. and a diameter of 1/8 in. The compression tests on Ml7A112 were on specimens of 3/8 in. diam by 3/8 in. high and the ends were coated with poly-tetrafluorethylene to minimize friction. RESULTS In2Bi. Fig. 1 shows, particularly at the higher applied strain rates, that In2Bi exhibits a marked yield drop as the deformation increases to about 2 pct, after which the material shows neither hardening nor softening up to 15 pct strain. The magnitude of the yield drop, the stress in the region of flow under constant stress (the stress plateau), and the 0.5 pct proof stress were all dependent upon the applied strain rate according to an expression of the form

Jan 1, 1965

By H. Conrad, K. Janowski, G. Stone

The available data on the dynamics of plastic flow of sapphire indicate that the deformation rate in the temperature range .from 900° to 1700°C can be expressed either as A number of investigators1-10 have established that sapphire deforms plastically above 900°C, the most common mode of deformation being slip on the basal plane in the [1120] direction. Under certain conditions and at temperatures above 1500°C, slip

Jan 1, 1965