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By S. Feuerstein, J. M. Galligan

SURFACE effects in the deformation of metal single crystals have been noted by a variety of workers.&apos; A large majority of these experiments have used surface roughening or a second chemical constituent at the surface. We performed the following experiment to see how the presence of a fine polycrystalline layer influenced the stress-strain behavior of single crystals of zinc. Spherical single crystals oriented for single slip were acid-machined into cylindrical dumbbell-shape shear specimens having a gage length of 3.2 mm and a cross section of 20 sq mm. The crystals were then deformed varying amounts at the surface of the gage section with emery paper. Following this treatment, the crystals were heated for approximately 8 hr at 200°C. This resulted in a polycrystalline surface layer, with an observed grain size of approximately 1/10 mm in diameter. Deformation of these crystals was undertaken at 78°K in pure shear, the shear direction <1120> lying in the basal plane. The deformation apparatus has been described elsewhere.2 The presence of a polycrystalline layer markedly raises the first observed plastic deformation, as can be seen from Fig. 1. This yield stress is then followed by a region of low work hardening comparable to that observed in shear tests on similar untreated zinc single crystals. However, the extent of easy glide is quite seriously curtailed, and is followed by a more rapid increase in work hardening, reminiscent of Stage II observed in the deformation of fcc crystals. The higher yield can probably be attributed to the difficulty of penetrating the grain boundaries by dis locations from sources interior to the boundaries. If we associate this yield stress with this breakthrough, then we might expect that more dislocations would be trapped in the crystal than is normally the case. If there is an increased density of trapped dislocations, this could lead to an increase in the amount of trapping with increasing strain, giving a larger strain hardening in the crystal. Although other explanations can be given, it is quite tempting to characterize the region of increased work hardening as a manifestation of Stage II-type deformation. This seems reasonable if the polycrystalline layer is quite efficient in holding up a large number of dislocations. In zinc crystals, since it is well-known that the slip distance can be as large as the specimen dimensions, one would only expect to entrap a large number of dislocation with very large crystals or by applying surface layers. If this interpretation of increased strain hardening is correct, it might present a method of studying Stage II in single crystals of zinc. This research was supported, in part, by the Office of Naval Research (1959). The encouragement and stimulation given by Professor E. R. Parker is gratefully acknowledged.

Jan 1, 1965

By William V. Kotlensky

PYROLYTIC graphite may be represented by a stack of overlapping, wrinkled sheets with the graphite basal planes more or less parallel to the deposition surface. Previous work1" has described two stages in the deformation above 2600°C produced by applying a stress parallel to the deposition surface. The first stage occurs at deformations less than about 15 pct and involves dewrinkling accompanied by basal-plane slip and basal-plane reorientation. The basal planes are not perfectly

Jan 1, 1965

By A. T. Churchman

The deformation modes of rhenium have been identified as those typical of the hexagonal metals, titanium, zirconium, and beryllium whose c/a ratios, in common with rhenium, are less than ideal for close packing. Slip is observed on (1010), (1011), and (0001) planes and twinning on (1121), (1122), and (1012) planes. The very high rate of work hardening is believed to be associated with intersecting partial dislocations on two (1010) systems which can combine to form sessile barriers. If the stacking fault energy is low, as postulated by Seeger, these barriers should be strong and not easily bypassed by cross slipping. Such an explanation could also account for the very small temperature dependence of the yield stress which was observed. RHENIUM is interesting scientifically as a member of the group of high melting point hexagonal metals: titanium, beryllium, and zirconium with a c/a ratio less than that for ideal close packing. Unlike them, however, it work hardens at a very high rate. This rate is greater and continues to a much higher degree of deformation than for nickel, normally considered to have a high rate of work hardening. This paper presents experimental observations on the modes of deformation of rhenium and, by comparison with other hexagonal metals, some speculation on the cause of the high work hardening. MATERIALS Johnson, Matthey rhenium powder of both 99.9 pct and 99.5 pct purity, see Table I, was compacted at 10 tons per sq in., part sintered at 1350°C in vacuo, and finally arc melted in a "gettered" argon atmosphere arc furnace to produce small buttons. Little difference was observed in the as-cast hardness or working down behavior of the two purities suggesting that either silicon and potassium do not have a significant effect on the working properties of rhenium or they were lost during arc melting. SPECIMEN PREPARATION The cast structure was broken up by cold-rolling with inter-stage annealing at 1600o or 1800°C in a vacuum high-frequency furnace using a tungsten susceptor. Strip for tensile testing was taken from two thicknesses of material 0.011 and 0.064 in. The former with intermediate anneals at 1800°C had a grain size of 900 grains per sq mm, while the latter with inter-stage annealing at 1600°C had a grain size of 3600 grains per sq mm. A coarse grain size was obtained by secondary recrystallization in a half button cold-worked by 30 pct reduction. Annealing times of from half an hour to several hours at 2200° to 2600°C in a "gettered" argon atmosphere arc furnace1 resulted in grains of up to 2 mm diam.

Jan 1, 1961

By S. R. Dunbas, D. C. Jillson, E. A. Anderson

THE present work was undertaken to furnish information, lacking in the literature, on the deformation mechanisms active in pure titanium at room temperature. Since it was started, Rosi, Dube, and Alexander&apos; have indicated that slip can occur in coarse-grained (2 to 6 mm diameter) titanium on the {1010} and {1011} planes and twinning can take place on the {1072}, (1122) and (1151) planes. Liu and Steinberg,&apos; working with titanium flakes produced by fused salt electrolysis, found evidence of twinning on the {1032$, {1121), {1122}, (1123}, and (1154) planes. The crystals used in the present work were substantially longer (up to nearly 2 in. in length) and possibly purer. Production of Large Crystals It was the purpose of this part of the work to provide single crystal or large grain specimens for use in the deformation studies rather than to study the mechanism of crystal growth. Accordingly, all further exploratory studies on methods were abandoned when it was found that cold-rolled bars sealed in vacuo in individual Vycor tubes and given three or more cycles of 4 hr at 1200°C and three to five days at 850°C, gave large grains. Eighteen specimens about 0.2 in. square x 2 in. long yielded 33 useful grains, ranging from Va in. to nearly 2 in. in length, with an agreeably wide range of orientations, Fig. l. The 0.25 in. thick strip from which the starting specimens were cut had been reduced 67 pct on 18 in. diameter rolls from a scalped, hot-forged (959" to 1000°C), arc-melted, iodide titanium ingot. Thc bar was at room temperature, but the rolls were at 200°C. Reductions of about 0.03 in. per pass were used. The bar was cut into four segments, each of which was rolled in a somewhat different manner. No effect on the growth of large grains was noted. The composition of the titanium, determined on turnings from the ingot scalping operations, is given in Table I. The Rockwell A hardness of the ingot was 26. The standard starting specimens, about 1/4x1/4x2 in., were milled on all four sides, hand polished on 280 and 400 mesh emery papers, etched for 3 min in a 50 HF-50 glycerine solution, rinsed, and dried in alcohol and ether just before sealing them in Vycor tubes. The average specimen weight was 7.5 g, and the tube volume was 6.5 cc. A vacuum of less than 1 micron pressure was applied. The specimen tubes were placed in an evacuated Inconel muffle to minimize the danger of collapse of the glass tubes at temperature. In practice the specimens were first heated to 1200 °C for 4 hr and then transferred fairly quickly to an 850°C furnace where they were held for three to five days. This cycle was repeated at least three times before the specimens were cooled, removed from the tubes, lightly polished and etched on one surface for examinstion. Those in which large grains had not developed were resealed in Vycor and returned to the cycling. Satisfactory specimens (about one out of every four cycled) were polished with emery paper on all four side;, then metallographically polished using ctchinz between wheels to remove distorted metal and, finally, given a very light etch to reveal the grain boundaries. This was necessary because the surface was roughened by the sublimation of titanium under high temperature vacuum conditions. Specimens were identified by TiXl numbers using supplementary letters to designate specific grains.

Jan 1, 1954

By L. T. Lloyd, H. H. Chiswik

The operative deformation elements in a-uranium single crystals under compression at room temperature have been determined as a function of the compression directions. The deformation mechanisms noted may be arranged with respect to their frequency of occurrence and ease of operation in the following order: 1 — (010)-[I001 slip, 2—{130} twinning, 3—{~172} twinning, and 4bunder special conditions of stress application, kinking, cross-slip, {.-176) twinning, and (011) slip. The composition planes of the (172) and (176) systems were found to be irrational. Cross-slip was shown to be associated with the major (010) slip system, coupled with localized interaction of slip on the (001) planes. The mechanism of kinking was found to be similar to that observed in other metals in that it occurred chiefly when the compression direction was, nearly parallel to the principal slip direction [loo] and was associated with a lattice rotation about an axis contained in the slip plane and normal to the slip direction: the [001] in the uranium lattice. The resolved critical shear stress for slip on the (010)-[100] system was found to be 0.34 kg per mm2 In a single test it was shown that under compression in suitable directions twinning on the (130) also occurs at 600°C. DEFORMATION mechanisms of large grained polycrystalline orthorhombic a-uranium have been studied by Cahn.1 A major slip system identified as the (010) with a probable [loo] slip direction and a minor slip system on the (110) planes were reported; the slip direction of the minor system was not determined. The twinning systems that were identified experimentally included the (130) and the irrational (172) composition planes; observations of other traces which were not as frequent and which did not lend themselves to positive experimental identification led Cahn to postulate on the basis of indirect evidence that twinning also occurred on (112) and (121) planes. In addition to the foregoing slip and twinning mechanisms, Cahn also observed kinking and cross-slip in conjunction with the major (010) system; the cooperative cross-slip plane was not identified. The availability of single crystals to the present authors has enabled them to check these results, particularly with reference to the doubtful mechanisms and the preference of operation of any one mechanism in relation to the direction of stress application. The tests were confined to compression only, primarily because of experimental limitations imposed by the size and shape of the available crystals. The tests were performed at room temperature except for one crystal compressed at 600°C. The compression directions were chosen to obtain a representative coverage of one quadrant of the stereo-graphic projection. To test the existence of some of the deformation elements that were reported by Cahn, but were not found in the present study, several additional crystals were compressed in specifically chosen directions considered most ideal for their operation. Experimental Techniques The single crystals were obtained by the grain coarsening technique described by Fisher? They grinding and polishing on rotating laps, with final surface preparation performed in a H3PO4-HNO3 electropolishing bath. A typical crystal readied for compression is shown in Fig. 1; their dimensions were rather small and depended upon the testing direction. Crystals isolated for compression in a direction close to the [010] axis, which lay roughly parallel to the longitudinal axis of the polycrystalline rod, were about 3 to 4 mm long and 5 mm2 in cross-section, while those prepared for compression in other directions were smaller. Most of the crystals were free from twin markings and showed no evidence of Laue asterism. Several crystals, however, contained twin traces prior to compression; these were identified prior to compression so as to clearly distinguish them from those initiated during deformation. The origin of the twin markings prior to deformation may be ascribed to two sources: thermal stresses and specimen handling during isolation and preparation. Two other types of imperfections in the crystals should be mentioned: inclusions, which were probably oxides or carbides. and three of the crystals contained a small number of spherical included grains (<0.01 mm diam), which were remnants of unabsorbed grains from the coarsening treatment. The volume represented by these imperfections was small, and their presence presented no difficulties in the interpretation of the macrodeformation processes during subsequent compression. Two compression fixtures were employed: crystals A, B, C, E, and G were compressed in a hand-operated screw-driven jig whose compression platens were designed to minimize axial rotation;

Jan 1, 1956

By E. J. Rapperport, C. S. Hartley

I TTRIUM is a close-packed-hexagonal metal with a c/a ratio of 1.5712.1 This low c/a value prompted a cursory examination of the deformation modes to obtain more data on the deformation characteristics of hcp metals with subideal c/a ratios. The chemical analysis of the arc-melted stock from which the specimen was cut is given below in Table I.

Jan 1, 1960

By K. E. J. Rapperport, C. S. Hartley

The only slip system observed in zirconium crystals deformed at 77", 575", and 1075OK was (1010) [1210] with a critical resolved shear stress in tension of 1.0 kg per sq mm at 77°K; 0.2 kg per sq mm at 575 °K; and 0.02 kg per sq mm at 1075 OK. The active twin planes were {1012}, (1121}, (11221, and (11233) with varying temperature dependence. A detailed analysis for the slip direction using Laue spot asterism is appended. NeARLY all metals of the hexagonal close-packed structure exhibit basal slip, i. e.,(0002)<1120>- type slip. This is true of magnesium,&apos; zinc,&apos; cadmium,3 beryllium,4 titanium,= yttrium,6 and rhenium.Many of these such as titanium 5&apos;8-&apos;0beryllium,4&apos;" magnesium, and zinc13&apos;14 display other slip modes even at room temperature, and nearly all have been reported to slip on other systems under particular loading or temperature conditions of testing. As is shown in this paper, basal slip was not found at any of four test temperatures from 77" to 1075°K in hexagonal close-packed zirconium under the simple loading conditions of tension and compression, even though in one case the resolved shear stress on the inactive (0002) <llgO> system was twenty-five times higher than the critical resolved shear stress on the active (1010) [1210] system. This result is consistent with prior studies on the active deformation processes in zirconium deformed at room temperature. &apos;&apos;-I7 SPECIMEN PREPARATION A) Material—The zirconium used in this work was of two types: 1) as-deposited reactor grade crystal-bar, and 2) arc-melted and forged reactor grade crystal-bar. Typical chemical and spectrographic analyses of these materials as received, and after hydrogen removal and crystal growth are given in Ref. 17. Crystals of type 1) above have the letter prefix (A) and those of type 2) have the prefix (B) throughout this paper. B) Crystal Growth— he zirconium was machined into rectangular parallelepipeds about 0.2-in. scl in cross section and 2 in. iong. These were hand polished through 4/0 abrasive paper, electropolished, given a hydrogen removal anneal, and subjected to long-time anneals at 840 °C in vacuo to produce usable crystals.&apos;7 A second technique used to obtain large crystals was to cycle the samples two or three times between 1200" and 840°C, allowing them to remain at the higher temperature for about 4 hr and at the lower temperature for 5 days.17 These techniques yielded some grains which occupied the entire cross section of the bar and were as long as 3/4 in. C) Orientation Determination—After the growth of large crystals by thermal cycling, the samples were repolished with extreme care through 4/0 abrasive paper and electropolished. Metallographic examination after polishing showed the surfaces to be free of visible deformation traces. Standard Laue back-reflection X-ray techniques were used to find the crystallographic orientations of selected large grains with respect to a specimen face and edge. Fig. 1 shows the stereographic projections of the stress axes for the crystals used. The sharpness of the spots on the Laue photographs indicated that the crystals were of good quality. EXPERIMENTAL METHODS Nine crystals were deformed in tension at 77"K, nine in tension and five in compression at 300°K in previous tests,17 fifteen in tension at 575"K, and eleven in tension at 1075°K. All specimens were stressed by load increments. After a predetermined load was applied, the specimen was removed from the loading appratus and metallographically examined for deformation traces. An attempt was made to initially stress each bar so that some crystals slipped a small amount and others not at all. This was done to bracket the critical resolved shear stress. One bar of special orientation (B-11) was repolished and annealed at 1075°K for 1 hr after lower temperature deformation, before final deformation at 1075°K. In the other bars the loading by increments, followed by metallographic examination, was continued until the surface distortion would interfere with analysis, or until fracture. One example of a crystal pulled to fracture is shown in Fig. 2. This photograph shows a crystal (B-14C) which was pulled at 1075°K and failed by slip on two (10i0) planes. The approximate orientation of this crystal is illustrated in the figure. Specimens were deformed at 77°K in liquid nitrogen on a tensile machine using an insulated bucket with an internal hook to accept a clamped specimen.

Jan 1, 1961

By R. M. Brick, F. L. Vogel

THE elementary mechanism of deformation in the body-centered cubic metals has been a subject of dispute for many years. If the problem were merely that of designating the crystallographic plane or planes of slip, the solution would have appeared long ago. However, there must be greater differences in the deformation behaviors of the body-centered and face-centered types than the differences in their lattices would suggest. The lines of slip formed on the polished surface of a strained face-centered cubic metal conform to glide over a single plane of the crystal. Slip in body-centered cubic iron, however, is frequently observed as curved and forked lines which could not possibly define a single plane of atoms. This alone is sufficient reason to expect different modes of deformation to operate in the two lattice types. The literature in this field now has generally accepted the proposition that {110), {112), or (1231 planes will act as slip planes in iron. It is essential that the experimental evidence supposedly supporting this proposition be critically examined. Taylor and Elam1 in 1926, using relatively small single crystals, determined the operative slip systems by measurements of the distortion of a grid engraved on the specimens prior to deformation. Their results indicated that shearing had taken place in the close-packed direction on a plane adjacent to or coinciding with the plane of maximum shear which contained the slip direction. This led the authors to propose a theory of noncrystallographic or banal slip. The authors considered an alternate rationalization of banal glide. Slip on two (1101 planes or possibly two {112} planes containing the same <1ll> direction could produce the wavy slip lines. By employing plane segments of varying widths, the integrated plane could take any position in the <111> zone. They rejected this explanation, however, feeling that the preponderance of evidence was against it. Taylor&apos; continued the investigation of the plasticity of the body-centered cubic lattice on ß brass. He reasoned that the resistance to shearing of a given plane in the zone of the slip direction was a function of the angle between the glide plane and the closest (110),: P F=—cose sine cos(X —?) [1] where F is the resistance to shear; P, the axial load at yielding; A, the cross sectional area; e, the angle between slip direction and load axis; x, the angle between plane of maximum shear containing the slip direction and the (101) pole; and ?, the angle between observed glide plane and the (101) pole. Differentiating Eq. 1 and rearranging, dF — = tan(x-?) d? [2] F which expresses the variation of the shear resistance with the angle $. Integrating this equation between the limits 0 and ? yields In F/F0 = ?0?tan(x— ?) d? [3] Here, F, is the resistance to shear of the (110) plane and F is the resistance to shear of a plane $ degrees from the (110). Thus, the variation of shear resistance with $ can be calculated from an experimentally measured x vs $ relationship. Fahrenhorst and Schmid8 sed several methods, none of them involving direct observation, to determine the glide system in ferrite. They determined the variation of critical resolved shear stress with

Jan 1, 1954

By M. S. Abrahams

Germanium has been rolled in the temperature range of 700o to 800°C. The thickness has been decreased by as much as a factor of four, from a thickness of 0.032 in. to a thickness of 0.008 in. For deformations below 60 pet, the true strain per pass is found to be a constant; from the temperature dependence of this slope, an activation energy of about 2.5 ev is obtained. This energy agrees with that for dislocation climb in germanium . For reductions greater than 60 pet, complete rings are seen in the Lave photographs, new grains are observed in the microstructure, considerable softening occurs, and the hole mobility is very low. This evidence indicates that the recrystallization of gertnanium has occurred. GERMANIUM has been deformed in many ways1 including tension, compression, torsion, and bending since Gallagher2 first described its plastic nature at elevated temperatures. All of these studies indicate that the glide plane in germanium is (111) and that the glide direction is (110). Rolled germanium specimens were used by Kolm, Warekois, and Kulin3 in their X-ray study of deformed semiconductors, but no information is given on the rolling itself. The present experiments deal with the rolling of germanium at various temperatures and for different orientations. In all previous deformation studies, the phenomenon of recrystallization (i.e., the transformation of a single crystal into a polycrystal) in germanium has not been observed4 despite relatively large deformations at elevated temperatures. The proposed reason4 for this was that sufficient energy could not be stored in the deformed germanium lattice. In contrast to the earlier studies this work will present evidence indicating that recrystallization occurs in germanium during rolling at an elevated temperature. I) EXPERIMENTAL PROCEDURE A) Test Specimens. The samples used for rolling were in the form of rectangular parallelepipeds measuring 0.3 in. long, 0.06 in. wide, and 0.035 in. high. They were cut from an undoped single-crystal ingot of p-type germanium with a resistivity of 24.4 ohm-cm, a Hall mobility of 2300 sq cm v-&apos; sec-l, and a hole concentration of 1.1 x 1014 cm"3 at room temperature. The surfaces of the specimens were metallographically polished prior to rolling. The initial dislocation density of the samples was about 10&apos; cm-&apos; as determined by etching in CP4. Two different specimen orientations were used. In the first case, the direction of rolling was parallel to (251), the surfaces in contact with the rolls were of the form (1021, and the normal to the third face was parallel to (211). The corresponding di-

Jan 1, 1964

By W. D. Robertson, R. E. Reed-Hill

DEFORMATION of magnesium crystals in a direction parallel to the basal plane has a special significance as a result of the preferred orientation characteristic of cold worked and recrystallized polycrystalline magnesium sheet and extruded rod in which the basal plane tends to lie in or near the plane of the sheet or the axis of a rod. The principal objective of the present study is a determination of the modes of plastic deformation in magnesium single crystals in this orientation. Evidence for nonbasal slip in magnesium has been presented by a number of authors. Schmid and Was-serman&apos; indicated that pyramidal slip on {1011} < 1120> or {1012} <1120> could occur above 225°C. Bakarian and Mathewson2 stablished that the slip system {1011} <1120> operates at high temperatures and that 225°C was a lower limit for pyramidal slip. The latter authors also showed that the critical resolved shear stress for {1011} slip was 400 g per sq mm at 330°C, while that for basal slip was 66 g per sq mm at the same temperature. Thus, at 330°C basal slip should be expected for all orientations except those in which the stress axis lies almost in the basal plane. More recently Burke and Hibbard3 oserved pyramidal slip at 25°C, when the stress axis was 6" to the basal plane and 14" to a <1120> slip direction. The critical resolved shear stress for pyramidal slip was 52 g per sq mm, which is only slightly greater than their value for basal slip (46 g per sq mm). Chadhuri, Chang, and Grant4 have observed non-basal slip in creep tests with polycrystalline specimens in the temperature range 250" to 350°C. The observed slip bands, which were extremely irregular in appearance, can be explained in terms of cooperative slip on {1011} and (1010) planes which have a common slip direction. Prismatic (1070) slip in polycrystalline magnesium was observed by Hauser, Landon, and Dorn.5 It was found to occur at low temperatures (78" and 195°K) and it was accompanied by cross slip in which the cooperating plane was the basal plane. Since prismatic slip occurred only at regions of high stress concentrations, the critical resolved shear stress could not be determined. Experimental Procedure The present work was performed on crystal specimens which were all cut from the same large single crystal. The original cylindrical crystal, 0.5 x 7 in., was grown in a Bridgman type furnace in which the temperature gradient was moved past the stationary crystal in the manner described by Jillson6 and Burke.&apos; High purity magnesium was furnished by the Dow Chemical Co. with the following spectro-graphic analysis in weight percent: 0.003 pct Al, <0.01 pct Ca, 0,002 pct Cu, <0.001 pct Fe, 0.008 pct Mn, <0.001 pct Ni, <0.002 pct Pb, <0.01 pct Si, <0.001 pct Sn, and <0.01 pct Zn. The large crystal was cut into four cylindrical pieces about 1.5 in. long. A flat surface parallel to the basal plane was made by hand grinding with lubricated metallographic paper on one side of each cylinder. In order to prevent bending in subsequent cutting operations, the crystals were supported by

Jan 1, 1958

By H. C. Chao, L. H. Van Vlack

Small MnS inclusions with known crystallographic orientations were placed inside powder compacts of low-carbon steel. After the metal was axially campressed with negligible end friction, the deformstions for the metal and the inclusions were compared. The MnS inclusions deformed more when the [100] direction was aligned with the compression axis than when the [111] direction was parallel to this axis. The deformations of the inclusions in the two principal radial directions were equal for each of the above orientations. Inclusions with [110] compression alignments did not deform with radial symmetry. The relative deformation of the inclusion and metal was closely dependent upon the relatiue hardness of the two phases. The relative deformation of the two phases was not sensitive to the rate of deformation. RECENT studies by the authors1.&apos; suggested that the plastic deformation of MnS in steel would probably be highly sensitive to the orientation of the inclusions and to the temperature of the metal. This paper reports an investigation of these factors upon MnS behavior within steel. Manganese sulfide (MnS) possesses an NaCl-type structure and typically has extensive (l10) {110} slip as a separate (noninclusion) crystal.&apos; A secondary slip system, ( l 10) { l l l}, has also been observed where the major slip system is restricted. In general, MnS inclusions must be rated as a highly deformable second phase.3 The amount of sulfide deformation varies, however, with several composition and processing factors. Some of these have been only partially assigned. For example, it is known that minor amounts (<0.01 pct) of silicon within free-machining steels will increase the amount of MnS deformation,4 but the mechanism of the added deformation can only be surmised at the present. Manganese sulfide and steel have sufficiently comparable deformation characteristics so that slip which is started in steel may be continued through the sulfide inclusions and back into the steel if the crystal orientations are favorable.5 A more detailed discussion of previous work on the plastic deformation of NaC1-type crystals and on the plastic deformation of inclusions within a metal is given in Chao&apos;s work.6 EXPERIMENTAL PROCEDURE The manganese sulfide which was used in this study was prepared by previously described methods.&apos; Single crystals of MnS, both as cleavage cubes and as spheres, were oriented within steel powder compacts so that the desired crystal directions were parallel to the direction of axial compression. A four-stage hydrostatic compaction procedure was used and involved the following steps. In the first stage part of the powder was placed in a metal die 1 in. in diameter with a thick (1 in. OD, 5/8 in. ID) rubber liner which had one end plugged. The steel powder was hand-rammed, making it as dense as possible before placing a carefully sized MnS crystal (either as a sphere or as a cube) near the center. The crystal was oriented with the chosen direction vertical; viz., [001], [011], or [111], with the aid of a X10 microscope. A pair of tungsten wire threads 0.020 in. in diameter was inserted along the side of this (&apos;core compact" to locate the desired plane after the compression tests. After the crystal was positioned in the center of the die, more powder was added and carefully rammed by hand. The die was then capped with a rubber plug of the same hardness and thickness as that of the liner. The whole assembly as shown in Fig. 1 was compacted by a ram load of 54,000 lb (about 70,000 psi). In the second stage a smaller, 3/4-in, rubber-lined die was used to give a stress of approximately 120,000 psi. The above process was repeated with the initial compact serving as a core for a larger compact. The final product after sintering was a cylinder 1 cm long and 1 cm in diameter, having a density of 7.54 g per cu cm. This was close to the theoretical density since the metal contained a non-metallic phase. There was no evidence of MnS deformation during the hydrostatic compaction or subsequent sintering. Elevated-temperature hardness data were obtained by procedures previously described.2 Compression tests for inclusion deformation utilized the cylinders which were described above. The critical problem in these tests was the lubri-

Jan 1, 1965

By R. M. Rose, D. P. Ferriss, J. Wulff

Single crystals of tantalum were grown by multipass zone melting in an electron beam apparatus. Tension tests of these crystals at 4.2 x 10&apos;* per sec-gave a resolved louler yield stress of 7300 psi at with a chisel edge; total uniform deformation increased from 1 to 2 pct at 77°K to over 20 pct at 300°K. This, and slip traces, indicated that deformation is more inhomogeneous at lower temperatures. Deformation occurred exclusively by slip in <III> directions, on planes in the <111> zones. Cross slip was frequent, particularly for those orientations where the resolved shear stress on the cross system was comparable with that on the primary plane. The existence and magnitude of the upper yield point were found to be sensitive to orientation. This effect was related to the circumvention of dislocations which were "locked" by interstitial atoms, by double cross slip, or composite slip, of screw dislocations. Prestrainirg at 300°K did not remove the upper yield point in subsequent tension at 77°K. Also, this treatment was found to cause yield points, where none existed for the unprestrained material. This behavior was also rationalized in terms of the circumvention mechanism. The mechanical properties of polycrystalline tantalum have been investigated by several workers,1"4 and may be summarized by pointing out the following features: a) Sharp rise of yield stress with decreasing temperature below room temperature. b) Response to strain aging at 300" to 400"C. c) Yielding with upper and lower yield-point phenomenon at and below room temperature. d) Low strain hardening below room temperature. e) Reluctance to twin except at very high strain rate. Furthermore, tantalum is ductile at ordinary strain rates as low as 4.2"K.&apos; This feature, in particular, makes tantalum unique among the high melting point, bee transition metals of Groups V and VI in the periodic system. Therefore, a more fundamental and detailed knowledge of the low-tempera- ture deformation of tantalum is required. Since high purity and the absence of grain boundary effects make such a study most productive and unambiguous, the method of electron beam zone melting was selected for the preparation of test specimens. This technique has the further advantage that crystals may be seeded in order to obtain any desired orientation. EXPERIMENTAL The electron beam zone-melting equipment was constructed as a modification of that described by Calverley, Davis, and Lever? All crystals were made by three passes of the molten zone at 4 mm per min to achieve an optimum purity commensurate with economy of time and material. Table I reports the chemical analyses of the starting and refined metal. It will be noted that there remain some 50 to 70 wt ppm of interstitial elements, while all substi-tutional elements have been removed by evaporation. Tungsten is picked up by evaporation of the cathode filament wire. Crystal seeding was normally successful within 3 deg, and the orientation of all crystals are given in the standard stereographic triangle in Fig. 1. Tensile bars were prepared from the crystals by centerless grinding to the shape in Fig. 2. Specimens were then electropolished to remove 10 pct of the diameter in order to remove worked material and to prepare a metallographic surface for subsequent deformation trace observations. All specimens were held in the split bushing grips as indicated in the cross section view of Fig. 2. All tests were made at a strain rate of 2 112 pct per min in an Instron testing machine.

Jan 1, 1962

By J. E. Burke, A. M. Turkalo

IN 1923 Desch¹ pointed out that the grains in a metal which is anisotropic with respect to its thermal coefficient of expansion would contract differently upon cooling, and that the stresses developed might approximate the plastic strength of the metal. More recently Boas and Honeycombe2-5 studied the behavior of several metals upon thermal cycling and observed that the stresses developed in arlisotropic metals are great enough to produce slip lines in individual grains and a roughening of the specimen surface. This phenomenon they have named "thermal fatigue." The mechanism they propose involves essentially a kneading of the grains, the deformation being alternately in compression and tension in a given grain as the temperature is changed in one direction and then the other. The present work was undertaken to investigate the possibility that an additional mechanism might operate to produce plastic deformation during thermal cycling—a "thermal ratchet" that depends upon a combination of grain boundary flow to relax the stress that develops between differently oriented grains upon raising the temperature and transcrys-talline slip to relax the oppositely directed stress which develops on lowering the temperature. Thus, thermal cycling should produce a nonreversible distortion such that certain grains will change shape differently from their neighbors with a simultaneous displacement being produced at the grain boundary. Temperature Dependence of Grain Boundary and Grain Strength The critical resolved stress for the initiation of slip in metal grains is only mildly affected by temperature." For example, in cadmium it decreases from 0.15 to about 0.05 kg per sq mm when the temperature is increased from 20° to 458°K and further temperature increase causes little further decrease. On the other hand, the work of KG1 indicates that the grain boundaries behave in a viscous fashion that can be described8 by the expression: t = BVexp(Q/RT) [1] t is the shearing stress on the boundary; B, a constant; V, the flow rate at the boundary; Q, the activation energy for grain boundary flow; R, the gas law&apos;s constant; and T, the absolute temperature. Eq 1 indicates that the stress necessary to cause a given grain boundary flow rate, V, decreases rapidly with increasing temperature. The value of the constant B is such that at sufficiently low temperature and ordinary strain rates deformation will occur preferentially by slip rather than by grain boundary flow. There is considerable evidence to indicate Consider the bicrystal shown in Fig. 1. In grain 1 the slip plane lies 45 " to the boundary while in grain 2 the slip plane is 90" to the boundary. The coefficients of expansion of the grains in a direction parallel to the length of the crystal are a1 and a, with a, > a2 for the orientations shown. The sequence of events that can occur upon heating and cooling this specimen is illustrated schematically in Fig. 2. Initially there is assumed to be no stress in the specimen (A). Upon heating, grain 1 attempts to become longer than grain 2, but is constrained by grain 2. Thus grain 1 is loaded in compression and grain 2 is loaded in tension, and a shearing stress is present across the boundary (B). As the temperature is increased, the stress will build up, and finally grain 1 will be plastically deformed by slip, since the greater stress is resolved on its slip planes. Any further heating will result in more slip and the stress will remain constant until some temperature T* is reached where the stress can be relaxed by grain boundary flow.† At this relaxation temperature (C) a step will appear between grain 1 and grain 2. Further heating above T* will cause grain 1 to become relatively longer, but no stress will appear because the grain boundary is too weak to support the stress (D). Upon cooling again, at T* (E), the grain boundary will again be able to support a shearing stress, and upon cooling further, grain 1 will be loaded in tension and grain 2 in compression (F). When the decrease in temperature below T* is sufficient to impose the critical shear stress upon the slip plane of grain 1, it will be stretched by slip.

Jan 1, 1953

By N. J. Grant, H. Brunner

This paber is concerned with the determination of equations relating elongation to the amount of shear taking place both along grain boundaries and in slip planes of poly crystalline aggregates during creep. Certain discrepancies with previously used equations are pointed out. Grain boundaries were observed to become serrated during creep, but it is shown that this does not necessarily prevent further grain boundary sliding. Direct obser-vations of subgrain boundary ingration lead to the conclusion that this migration facilitates sliding along serrated grain boundaries. It is bointed out that the state of stress at triple boints is still unknown. MOST of the mechanisms of deformation contributing to elongation are shear processes, such as slip, kinking, grain boundary sliding, and twinning. For quantitative investigations of individual deformation mechanism it is necessary to know the equation which permits the calculation of speci-tnen elongation from measured amounts of shear. This calculated elongation must then be compared with the observed total elongation. The authors&apos; special interest concerned grain boundary sliding during creep. Although this subject has already been investigated quantitatively by McLean,&apos; Rachinger,&apos; and Fazan, Sherby, and Dorn, calculations indicated that none of the equations used thus far to relate shear with elongation were sufficiently well founded. A basic study of this relationship was thus made and the results of this study (which do not entirely agree with those previously used) are presented. Most of the ideas set forth apply not only to grain boundary sliding but to other mechanisms of shear as well. THE SPEAR-ELONGATION RELATIONSHIP Basic Models—The relationship between shear and elongation is trivial in the simplest case of shear, which is shown in Fig. l(a). The vector A; designates the displacement across the shear interface, and Au, and Aut are its components parallel and normal to the tensile direction, respectively. It is evident that the specimen elongation due to shear is equal to the longitudinal component of the shear vector, and it should be noted that the normal component does not contribute to the elongation of the specimen (there are, of course, two normal components in a three-dimensional model). The model shown in Fig. l(b) may be applied to mechanical twinning and to subgrain boundary tnigration. In this case the width (h) of an already existing shear band increases by the migration of an interface, but the shear angle y (angle of mis-orientation in the case of a subgrain boundary) remains constant. The geometrical relationships indicated in Fig. l(b) permit this case to be reduced to the one shown in Fig. l(a). For the resulting elongation A6 we find: where AV/V = fraction of the volume of the specimen swept by migrating interfaces , and 1 = length of specimen. Thus, assuming for example that the angle of mis-orientation is 1 deg, and that P = 45 deg, we find that the specimen elongates 0.87 pct of its length if the entire volume of the specimen is swept once by such a subgrain boundary. An example of deformation by migration of subgrain boundaries is shown in Fig. 2. The specimen shown was repolished after 9.8 pct creep strain and the test then continued for another \ pct. Since the shear vector has, in general, a component normal to the surface, subgrain boundary migration results in the formation of an inclined band delineating the region swept by the subgrain boundary. These inclined bands become clearly visible when observed with oblique illumina-

Jan 1, 1960

By W. C. Thurber, C. J. McHargue

THE deformation textures of metals have been extensively studied because of both the practical implications in metal fabrication and the fundamental insight into the behavior of the metal during deformation. Most studies have been concerned with pure metals or solid-solution alloys and relatively little attention has been directed toward more complex alloy systems. Barrett&apos; and Brick2 have summarized work on multiphase systems in terms of the relative ease of deformation of the phases. Thus, if the phases are deformed about equally, each develops its usual texture for the particular fabrication process. This behavior has been reported for Ag-Cu and Cd-Zn alloys3 and 62-38 brass.4 A dispersion of hard particles in a softer matrix interferes with the normal reorientation of the matrix lattice during deformation, thus distorting the texture or in some cases preventing its development. Increasing the amount of carbon in steel has been observed to increase the randomness of the ferrite5 and almost random textures have been reported for A1-12 pct Si eutectic alloy wires.6 It has also been noted that if the second phase is platelike, deformation causes the platelets to line up in a common direction. The present work concerns a quantitative study of the deformation textures in aluminum-uranium alloys containing 5 or 13 wt pct U. Alloys in this composition range are characterized by a pure aluminum matrix in which the intermetallic compound UA14, is dispersed. From a fundamental standpoint, this system affords the opportunity for studying the effects of a dispersed phase on texture development in an essentially pure metal matrix. Further, these alloys are commonly used as fuels for nuclear research and testing reactors, and a knowledge of the preferred orientation may be useful in evaluating physical and mechanical properties as well as response to fabrication. The deformation textures in sheets of aluminum (99.996 pct), Al-5 pct U alloy, and Al-13 pct U alloy were determined for reductions in thickness of 90 pct by cold rolling. The texture in an alloy rod of the latter composition which had been extruded at 455°C was also determined. It can be readily ascertained from the aluminum-uranium phase diagram that the 5 pct U alloy is hypoeutectic and contains 7.3 wt pct (3.4 vol. pct) UAl4. The 13 pct U alloy has the eutectic composition and contains 18.9 wt pct (9.4 vol. pct) UAl,; however, because of nonequilibrium solidification conditions, the typical eutectic microstructure was not developed. The alloys were prepared by open-air melting in graphite crucibles. The slab castings were cropped and cold reduced 90 pct in thickness on a two-high mill. The slabs were reversed after each pass. Although the uranium-bearing alloys exhibited edge cracking, they could be cold rolled to the desired thickness. Small coupons 1.5 by 0.75 by 0.1 in. thick were sheared from the center of the rolled plate with a major axis parallel to the rolling direction. To obtain a specimen of sufficient thickness for machining of the X-ray diffraction specimen, three coupons were laminated into a single three-ply sandwich with a suitable adhesive. Adhesives which could be cured at room temperatures were selected in order to prevent recrystallization during bonding. Bondmaster M-648 (Rubber and Asbestos Corp.) was used for the pure aluminum laminate and Armstrong A-6 (Armstrong Products Co.) was used for the alloys. The alloy for extrusion was cast in a cylindrical graphite mold! cropped and machined into a 3-in. diam by 4-in. long billet. This billet was preheated to 455°C, upset to 3.125 in. diam, and extruded on a 700-ton hydraulic press at a speed of 6 fpm through a flat-face, 1-in. diam die. The rod was quenched with a water spray as it emerged from the die. Pole-distribution data were obtained using the diffractometric method described by Jetter and Borie.7 A spherical X-ray diffraction specimen of

Jan 1, 1961

By M. N. Shetty

LARGE copper whiskers (-100 p) of 11111 orientation were tested in a floor-model Instron testing machine, at liquid nitrogen temperature. (Testing methods will appear elsewhere.) Whiskers deformed by twinning after some initial deformation. A load-elongation curve at the onset of twinning is reproduced in Fig. 1. Twinning was confirmed by taking a back-reflection Laue picture, using a slit colli-mator, which showed distinct splitting of reflections. The tensile stress reached just before twinning is about 1.4 x 107 g per sq cm (-7.0 x106 g per sq cm—resolved shear stress) which drops to 1.2 x107 g per sq cm (-6 x 106 g per sq cm—resolved). This twinning stress is about five to ten times larger than the value for bulk single crystals of copper deformed at 77°K (-106 g per sq cm—resolved). Twinning models based on Cottrell-Bilby&apos;s pole mechanism are discussed in detail by Venables.&apos; In the present work a mechanism based on the idea of failure of a Lomer-Cottrell barrier by recombination will be proposed. An L-C barrier may fail either by recombination or by dissociation.3 Fig. 2 provides the necessary information. It shows that the stress necessary to break such a barrier is about 1.8 x 107 g per sq cm by recombination and 4 x 107 g per sq cm by dissociation at 77°K. The twinning stress reached by whiskers is comparable to the stress level required for failure of an L-C barrier by recombination. (Stroh himself points out that his calculations should not be taken too literally.) We consider a segment of the L-C dislocation which has recombined (AB in Fig. 3) over a length to form the total dislocation which then glides in the

Jan 1, 1965

By W. N. Roberts

Hadfielcl steel has been studied by transmission electron microscopy to determine the microsl.rtic-ture of the cold-worked material, which has been a subject of controversy for many years. The presence of fcc deformation twins in specimens deformed in tension, by hamnzering, and by explosive -shock loading at room temperature lzas been established by electron diffraction. No evidence of a mar tensite was detected in any of the speciwens. Small amounts of E martensite were idenLified in the hamnleved specimens. DESPITE numerous researches on Hadfield steel since its discovery in 1882, there is still disagreement on the nature of transformations in the cold-worked material. Collette el al.,&apos; using X-ray and electron diffraction, have found evidence for stacking faults, E martensite, and a martensite in Hadfield steel deformed in tension at room temperature. Nishiyama and Simizu,&apos; using electron microscopy, have found stacking faults and E martensite in hammered Hadfield steel. White and Honeycombe have concluded from X-ray diffraction that Hadfield steel remains fully austenitic even after severe cold work at -196 Previous work by the author, indicating the presence of a, martensite in deformed Hadfield steel, was in error due to a faulty interpretation of the electron-diffraction patterns. Various workers,5&apos;7 over the years, have speculated on the presence of deformation twins in Hadfield steel, largely from such circumstantial evidence as the persistence of slip bands with repeated polishing and etching, the presence of serrations in the stress-strain curve, and the absence of evidence of a martensite by X-ray measurements. The advent of electron-transmission microscopy and se- lected-area diffraction has made possible the positive identification of fine deformation twinning. PROCEDURE For tensile tests, standard ASTM specimens of 2-in. gage length, ground from 0.12-in. Hadfield steel sheet, were solution-treated at 1050°C for 30 min in a salt bath, to avoid decarburization, and water-quenched. The grain size was about 0.01 sq mm. Chemical analysis of the steel after heat

Jan 1, 1964

By R. Maddi, I. R. Kramer

The delay time for the initiation of slip was studied in single crystals of a brass, aluminum, and ß brass. A delay time for slip was found in ß brass when the specimens were tested below room temperature; however, one was not found for a brass or aluminum. A general theory for the existence of the brittle transition temperature is proposed. A LTHOUGH a considerable amount of effort has A been devoted to the study of the deformation and fracture of single crystals, the vast majority of the work was concerned with static tests or with tests carried out at relatively slow strain rates. The necessity for the study of a possible incubation time for slip becomes apparent when the various theories which have been postulated for the elucidation of the mechanism of slip are considered. The existence of an incubation period would strongly indicate that slip occurs by a process of nucleation and growth; whereas the absence of an incubation would present rather convincing evidence that slip occurs by a cataclysmic process. In addition to shedding light on the process of plastic deformation, an understanding of the early stages of plastic deformation may be helpful in finding an explanation for the brittle behavior of the body-centered metals under certain conditions. It is well known that these metals, such as iron, molybdenum, tungsten, ß brass, etc., will become brittle as the test temperature is lowered or the strain rate is increased. In spite of the fact that this subject has received considerable attention since the turn of the century, no adequate theory exists today which explains the phenomenon. In the ductile temperature range the metal breaks with a "fibrous" fracture after considerable slip has taken place. In the brittle temperature range the metal fails essentially by cleavage on the {loo) planes: however, some plastic flow is always present even in the most brittle fractures. It is possible, as will be explained later, to ascribe this brittle behavior to the length of the incubation time for slip. Clark and Wood,&apos; using polycrystalline metals, showed that a delay time existed for the yield point in mild steels and that the delay time depended upon the applied stress. These authors stated that the delay time was observed only with those materials for which the stress-strain curve showed a definite yield point. In their work only the mild steel specimens exhibited a delay time at the yield point, while the other materials studied-type 302 stainless steel, SAE 4130 normalized steel, SAE 4130 quenched and tempered steel, 24s-T aluminum—did not show a delay time. These authors&apos; in an extension of their work, found that as the temperature was lowered the delay time was increased. It is, then, the purpose of this investigation to measure or to set an upper limit on the delay time for plastic flow in single crystals of a brass, aluminum, and ß brass. The delay time will also be studied as a function of temperature. The incubation time may be measured by determining the length of time the specimen will support a stress without slip occurring when the stress is greater than the static critical resolved shear stress. In order to accomplish these measurements use was made of a pendulum which was so designed that a single crystal specimen could be placed at various positions along its length. When a pendulum is struck by another pendulum of the same length, an elastic wave is transmitted down the bar with the velocity of sound in the material and is reflected from the far end of the bar. The reflected wave then travels back and unloads the stress until it reaches the impacted end of the bar and the two pendulums separate. The length of time that the specimen is subjected to the stress is equal to the time it takes for the stress wave to travel twice the distance from the specimen to the end of the bar. The stress applied to the specimen is governed by the velocity of impact of the two pendulums. The stress at which the specimen first suffers plastic: deformation was determined in these experiments by examining the specimen under the microscope for the first appearance of slip lines and by measuring the residual strain after each impact. In these experiments the critical resolved shear stress was approached from the low stress side and no attempt was made to determine it exactly. To determine it exactly, it would have been necessary to find that stress at which slip would have just started. However, since the stresses were increased in rather small increments the critical stress is believed to be approached rather closely, as will be seen from the experimental results. The critical stress will be taken as the highest stress obtained before the onset of plastic deformation. The stresses

Jan 1, 1953

By R. Maddi, I. R. Kramer

C. S. Roberts (Dow Chemical Co., Midland, Mich.)— In this study we have seen another example of how modern electronic instrumentation can be of great value to metallurgical research. The authors have shown much ingenuity in their experimental work. However, I wish to point out that anelasticity theory tells us that we must be cautious when we use pulse methods for measurements which are to be correlated with knowledge of static stress-strain behavior. The basic stress calibrations used by the authors depend on the use of static moduli combined with the pulsed strains. No recognition of a possible modulus defect has been indicated. The general agreement of critical resolved shear stresses may indicate that a

Jan 1, 1953

By I. R. Kramer

The delay time for single crystals of iron, zinc, and pre-strained aluminum was measured under conditions of high-speed deformation. The delay time of aluminum was found to be affected by the orientation of the crystal. Under the dynamic conditions employed, tile calculated "activated volume" term appears to be very small for the three metals studied. IN a previous paper,1 it was shown that under dynamic testing conditions at 78° K, there was a delayed yield in single crystals of aluminum and copper which had been cold-worked prior to testing. The experimental results also indicated that the delay-time effect was not due to the interaction of dislocations with impurity atoms or vacancies, but rather to a dislocation-dislocation interaction since aluminum which has not been prestrained shows no delay-time phenomenon. In this paper, some data are reported on the effects of orientation on the delay time of aluminum single crystals; the delay time of zinc single crystals saturated with nitrogen and the delay time of iron single crystals also were measured. EXPERIMENTAL PROCEDURE Aluminum (99.997 pct) and zinc (99.999 pct) crystals, 1/2 in. in diam and 8 in. long were grown by the Bridgman technique. The iron single crystal was supplied by Dr. R. Maddin. The zinc crystals containing nitrogen were prepared by melting high-purity zinc in a graphite crucible and the nitrogen was introduced by additions of ammonium chloride. The liquid zinc was then drawn up into glass tubes of 1/2 in. diam and allowed to solidify. The rods were cooled to room temperature before the transfer to the mold for conversion into single crystals. The orientation of all specimens was determined by the Laue&apos; back-reflection technique, Fig. 2 and Table I. To prepare for the delay-time measurements, the crystals were cut with a fine jewelers saw and the ends carefully machined. The specimens then were electrolytic ally polished to remove the cold-worked metal, mounted in a special fixture and hand-lapped. As a final step, the crystals were annealed in evacuated tubes. Specimens of aluminum crystals, Nos. 24 and 26, were compressed 0.5 and 2 pct, respectively, in the direction of the later impact. The zinc specimens were aged at 50°C for 15 min, In the case of iron, only two specimens could be obtained. To obtain sufficient data, it was necessary to resort to a reaging treatment. After each delay-time test, the specimens were aged at 65° C for 100 min. This treatment, according to Clark,2 is sufficient to restore the original delay time. It is believed that although the specimens were plastically deformed approximately 10-4 pct, after each test the delay-time values are reliable. The delay-time measurements were made in an apparatus similar to that described previously.&apos; Single crystals approximately 1 in. long and having a diameter of 1/2 in. were placed in a pendulum which consisted of a bar 1/2 in. in diam and 8 ft long, designed with a crystal holder to accommodate the specimen at low temperatures. The crystal was held at a position 2 ft from the front part of the pendulum. This portion of the apparatus was supported on a fine molybdenum wire. A projectile bar of the same diameter and length comprised the other portion of the apparatus. This bar was supported on

Jan 1, 1962