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By R. M. Hudson

A study has been made of the decarburization of low-carbon sheet steels at temperatures from 1100" to 1475°F in mixtures containing hydrogen, nitrogen, water vapor, and in some instances carbon monoxide. Decarburization occurs principally by the reaction C (in steel) + H20 = CO + H2 and follows a first-order rate law. The decarburization rate appreciably increases with an increase in temperature up to about 1325°F, but the increase in rate is small with fur- Use of a dry hydrogen atmosphere results in a relatively slow decarburization of steel and use of a wet hydrogen atmosphere results in relatively rapid decarburization. It is now generally recognized' that the reaction C (in steel) + H2O = H2 + CO [l] accounts for most of the decarburization that occurs in wet hydrogen-containing atmospheres. The present article is concerned with the decarburization of low-carbon sheet steel in H2-N2 atmospheres ther increase in temperature. The limiting rate of decarburization can be predicted from a knowledge of the solid solubility and diffusivity of carbon and this rate is approached as the water-vapor content of an atmosphere is increased. Hydrogen contents above about 8 pct are beneficial only in that they permit higher levels of water vapor to be used without oxidation of the steel. A buildup of CO in the atmosphere lowers the rate of decarburization. containing various amounts of water vapor and carbon monoxide. The effectiveness of these atmospheres and the influence of temperature on decarburization rate will be considered. EXPERIMENTAL WORK The chemical compositions of the three steels used in decarburization-rate studies are listed in Table I. Steel A was a commercially hot-rolled rimmed steel that was cold-reduced at the Laboratory to furnish specimens 0.025, 0.041, and 0.059 in. thick. Most of the experiments in which this steel was used were made on the 0.041-in.-thick material. Steel B and Steel C were cut from 0.010-in.-thick commercially cold-reduced coils that were

Jan 1, 1963

By A. S. Nowick, A. E. Roswell

Anelastic measurements of atomic mobility in an Ag-Zn substitutional solid solution, make possible a study of the rate of decay of lattice defects frozen into the alloy by quenching. A WIDE variety of experimental evidence has accumulated recently in support of the belief that atomic mobility or diffusion in face-centered cubic lattices occurs principally through the movement of lattice defects, as contrasted to a mechanism by which two or more atoms directly exchange lattice positions. The most direct evidence, summarized in a recent review,' includes the Kirkendall-effect measurements and anelastic measurements on quenched alloys. Theoretical calculations' have focused attention on the lattice vacancy as the defect probably responsible for diffusion in the common metals. Later calculations3 have also shown the possible importance of combined pairs of vacancies in producing diffusion. The only defect that has been considered seriously, in addition to the vacancy and combination of vacancies, is the "interstitialcy" (an atom which has left its normal lattice position and entered an interstitial position) ; the calculated energy of formation of an interstitialcy in a close-packed lattice is too large to permit a reasonable probability for the occurrence of this defect In view of these calculations it may be tentatively concluded that the defects producing atomic movements are single or multiple vacancies. Anelastic measurements of atomic mobility in substitutional solid solutions provide a valuable method for the study of lattice defects. By means of this method it was first demonstrated' that defects may be frozen into a lattice by rapid quenching from high temperatures. (It was subsequently shown6 that resistivity measurements may also be capable of detecting the presence of frozen-in defects.) A summary of the principles involved in these anelastic measurements will now be presented. The anelastic method is based on a relaxation phenomenon in substitutional solid solutions, first discovered by Zenera in a brass and subseauentlv investigated extensively in a series of Ag-zn solid solutions.' This relaxation effect may be observed in the usual way either dynamically, as a peak in

Jan 1, 1954

By F. R. Brotzen, A. R. Troiano, E. L. Harmon

Precipitation processes leading to drastic property changes are a frequent occurrence in titanium alloys containing large amounts of the retained high temperature P phase. In order to establish the kinetics and nature of these precipitation processes, a series of Ti-V alloys was studied. Time-temperature-transformation diqgrams were obtained for 12.5 and 15 pct V-Ti alloys. These diagrams consisted of two intersecting C-shaped curves: one in the high temperature region for the euilibrium transformation P +u+P, and another at lower temperatures depicting the formation of the meta-stable transition phase, o. Presence of the transition phase retarded the precipitation of the equilibrium a phase. Deformation of retained P resulted in the formation of the o phase. Reversion and retrogression phenomena of the transition phase were observed. A negative temperature coefficient of resistance was found in quenched alloys containing from 15 to 20 pct V. CERTAIN titanium-base alloys can be heat treated to produce appreciable changes in properties. For example, remarkably high hardness values may be obtained by aging or isothermal quenching treatments. Most of the information available to date on the hardening of titanium-base alloys has been systematized recently in an article by L. D. Jaffe.' It was pointed out by that author that the hardening was the result of the decomposition of the retained j3 phase to the equilibrium constituents, a and p, and that this decomposition had many of the characteristics of an age-hardening reaction. Recent work by Frost et al.' 3 has contributed much to the fundamental understanding of the hardening mechanism in titanium-base systems. These authors established the presence of a transition phase in the transformation from j3 to a + j3, which they designated o. The transition phase, in their opinion, was at least partially responsible for the hardening and embrittling effects which accompanied low temperature aging. The present investigation of the mechanism and kinetics of the hardening reaction was carried out for the Ti-V system. Ti-V alloys were ideally suited for a study of the decomposition of j3, since age hardening was known to occur readily in this system." Moreover, no intermetallic compounds occur in this system, Fig. 1, thus simplifying the interpretation of the results. Material and Procedure Alloys containing 12.5 and 15 pct V were prepared by Battelle Memorial Institute from iodide titanium furnished by Watertown Arsenal and vanadium of 99.8 pct purity. Ingots of 8 Ib each were prepared by arc melting in an inert atmosphere with a tungsten electrode and water-cooled copper crucible. Each of the ingots was melted once, forged at 1600°, and rolled at 1400°F. Following this, the ingots were remelted, forged, and then rolled to % in. sq bars, which were subsequently grit blasted, pickled, and wire brushed. Another set of alloys containing nominally 17.5 and 20 pct V was produced by the Research Div., New York University. These alloys were arc melted in an inert atmosphere in lots of 20 g each. Heat-Treating Procedure: Whenever feasible, specimens were heat treated in high vacuum resistance furnaces at pressures below 5x10." mm of Hg. Aging and isothermal quenching treatments were generally carried out in salt baths. Specimens were not attacked by the salt, provided the tempera-

Jan 1, 1956

By J. E. Harris, J. A. Whiteman, A. G. Quarrell

The graphitizing reaction has been studied in a number of Fe-C-Si alloys in the temperature range 550° to 725°C. The TTT relationships exhibit "C" curve behavior except where nuclei, either foreign or graphite itself, are present before the start of the reaction. It is suggested that the rate -controlling process is diffusion of carbon through ferrite. For the reaction to proceed at the observed rate it is calculated that the matrix surrounding the particles must deform plastically; experimental evidence for this deformation is presented. It is well-established that the decomposition of austenite to pear lite occurs at a maximum rate at an intermediate temperature.l-5 This "C curve" be- havior, which has been reported in a number of other systems,5-10 is a consequence of the relatively low rate of nucleation of the pearlite at small degrees of undercooling of the austenite. The cemen-tite phase in the pearlite is, in turn, metastable with respect to graphite and if steels are held for prolonged periods at elevated temperatures decomposition of the pearlite occurs. It is difficult to predict the shape of the subcriti-cal graphitization TTT (time, temperature, transformation) diagram for, in this case, undercooling does not occur. However, the free-energy change for the reaction does decrease with increasing temperature" (Fig. 1) and it is thus anticipated that the rate of nucleation will fall as the temperature approaches that of the eutectoid. In addition, a decreasing growth rate with increasing temperature is predicted in some circumstances with pure Fe-C alloys. However, apparently similar conditions exist for first-stage graphitization in the austenite range (malleabilization) but no evidence for C curve behavior has been presented in the extensive liter-

Jan 1, 1965

By J. D. Mote, J. E. Dorn

This investigation was undertaken to study the effects of piledup arrays of dislocations on inducing slip, twinning, and fracturing in magnesium bicrystals. A series of variously oriented bicrystals of magnesium having a vertical grain boundary were prepared and tested in tension. It was found that piled-up arrays of dislocations at the grain boundary could, under appropriate conditions, induce slip, twinning- and cracking. The results that were obtained substantiate, at least qualitatively, the general dislocation mechanism for transmission of strain across grain boundaries and the Petch-Stroh concept of fracturing. WHEREAS single crystals of magnesium generally exhibit extensive deformation, coarse-grained poly-crystalline magnesium at subatmospheric temperatures fractures after a few percent elongation.' Although a small amount of ductility is obtained, several features of this fracturing are characteristic of typical brittle behavior. Over a rather broad temperature range the fracture stress is insensitive to the test temperature and the fracture stress increases linearly with the reciprocal of the square root of the mean grain diameter. The course of fracturing is predominantly intergranular, but small fragments of adjacent grains frequently adhere to the fractured surface.2 The brittle behavior of polycrystalline magnesium is attributable to the limited number of facile deformation mechanisms it exhibits at low temperatures. For a general deformation of a randomly oriented polycrystalline aggregate, each grain must exhibit at least five independent mechanisms of deformation to permit accommodation of the imposed deformation from grain to grain.= Although minor amounts of prismatic slip occur in corners of grains where stress concentrations are known to be high, glide in polycrystalline magnesium at low temperatures takes place almost exclusively by basal slip.' The common type of twinning, which takes place on the (1012) pyramidal planes, can under the most favorable orientations, lead to a. strain of only 6.9 pet; the contribution of twinning to the tensile strain would indeed be much less than this in a randomly oriented polycrystalline aggregate of magnesium. Since the three mechanisms of basal slip are coplanar, they are equivalent to only two independent mechanisms, a number insufficient for a general deformation. Consequently, once the permissible twinning has taken place in conjunction with basal slip, no further plastic deformation is possible because of interference to slip at the boundaries of dissimilarly oriented grains. At this stage brittle fracturing takes place due to high stress concentrations at the juncture of slip bands with the grain boundaries; the predominance of intergranular fracturing in magnesium, in preference to transcrystalline fracturing which is prevalent in zinc, has not yet been rationalized. A more atomistic description of the plastic behavior and fracture characteristics of magnesium follows from the analyses made by stroh4 on the stresses induced by piledup arrays of dislocations. Slip first takes place by dislocation motion in the most favorably oriented grains. As the dislocations approach the boundary of a dissimilarly oriented adjacent grain they begin to form an array of dislocations with its attendant stress field. Piledup arrays of screw and edge dislocations introduce high localized shear stresses at the spur of the array; piledup arrays of edge dislocations also induce high tensile stresses localized in the vicinity of the grain boundary. Whereas the shear stresses can induce slip to take place, the tensile stresses, if sufficiently high, can cause fracturing. The localized shear stress will be relieved if sufficient numbers of mechanisms of deformation become operative in the original and the adjacent grain to permit accommodation of the dislocations in the grain boundary. In this event a ductile behavior will be obtained. But if the number of deformation mechanisms is insufficient for complete migration of dislocation arrays into the grain boundary, the tensile stresses due to the edge components of piledup dislocation arrays will continue to increase with increasing applied stress until fracturing takes place. Whereas face-centered-cubic metals have a sufficient number of mechanisms of slip for accommodation of dislocations in their grain boundaries to exhibit ductile behavior, hexagonal-close-packed metals, in general, do not. Consequently, hexagonal-close-packed metals are usually brittle except when conditions such as alloying or temperature permit facile slip by a number of mechanisms. The arguments presented above suggest that the mechanical behavior of magnesium depends on whether or not dislocation arrays in adjacent grains can enter the grain boundary. When such accommodation is possible, ductile behavior is expected; but when such accommodation is impossible, fracturing will ensue. To further test the validity of these arguments it was considered advisable to study the

Jan 1, 1961

By N. S. Stoloff, M. Gensamer

The effects of temperature, grain size, and magnesium content on the strength and ductility of cadmium were studied in the range -269° to 23 °C. A sharp drop in ductility between -140° and -190°C marked a transition in fracture mode from ductile shear to inter gvanular fracture. The addition of up to 15.35 wt pct Mg in solid solution raised the transition temperature, and for two compositions produced basal cleavages. The relatively high ductility of unalloyed cadmium at cryogenic temperatures is attributed to temperature independence of the yield stress and the absence of dislocation locking. ALTHOUGH numerous studies have been made of the mechanical properties of cadmium single crystals,1-5 no comprehensive investigation of deformation and fracture in polycrystalline cadmium has been carried out. This investigation was initiated to determine the mechanisms of deformation and fracture in polycrystalline cadmium, and to attempt to correlate these mechanisms with the behavior of other metals of hexagonal close-packed structure. A second objective of this work was to determine whether the slip systems and mode of fracture of polycrystalline cadmium could be altered by reduction of the axial ratio, which is 1.886, through alloying. Dorn and co-workers' have been able to induce prismatic slip in magnesium through alloying to reduce the axial ratio. Single crystals of cadmium are so highly ductile that glide strains of 400 pct are observed at room temperature, and 80 pct at -269°c.l Failure in every reported case is by necking down and shearing off of the crystal. Cleavage in cadmium single crystals has never been observed. Magnusson and aldwin reported a ductile to brittle transition for polycrystalline cadmium at about —160 C for specimens tested at a strain rate of 0.05 in. per in. per min in tension. However, even at -196° substantial ductility was retained. The transition temperature was strain rate dependent, impact loading at 19,000 in. per in. per min raising the transition temperature to about -85°C while leaving the low temperature ductility unchanged. No information was given on microstructures or fracture mode, nor were stress-strain characteristics reported. In the present investigation, tensile tests were carried out on polycrystalline cadmium and solid solution Cd-Mg alloys to determine flow stresses, work-hardening behavior, fracture strength, and fracture ductility. Variables employed included temperature, alloy content (and c/a ratio), and grain size.Some compression data also have been obtained for comparison purposes. I) EXPERIMENTAL PROCEDURES A) Polycrystalline Cadmium. Two purities of cadmium were employed in this investigation. Cadmium of 99.95 pct purity was supplied by Belmont Smelting and Refining Co. Cadmium of 99.99+ pct purity was supplied by American Smelting and Refining Co. Threaded cylindrical tensile specimens were machined to give approximately a 1/2 in. long straight gage section with a reduced diameter of about 0.110 in. Specimens were heat treated in evacuated pyrex capsules in the range 140" to 290°C to produce desired grain sizes. All specimens were polished in a solution containing 320 g Cr03 and 20 g NaS04 in 1000 cc of H20. Occasionally this solution caused staining of the specimen, in which case a further polish with a solution of one part HN03 and two parts H202 in two parts ethyl alcohol was employed.' Tensile testing was carried out on a screw-driven Instron machine, at a constant rate of crosshead movement, which for most tests was 0.01 in. per in. per min. Load vs time, and therefore load vs total strain, were recorded. Temperatures from -196" to -40°C were obtained by passing nitrogen gas through a copper coil immersed in liquid nitrogen, and then feeding the gas into a jacket around the specimen. Tests at -269°C were carried out in a helium cryostat, at a crosshead rate of 0.1 in. per in. per min, with specimens of 1 in. gage length. Compression specimens were tested in a jig similar to one designed by ilman. The jig was mounted on the under side of the Instron crosshead. Load was transmitted by means of a rod connected to a movable part of the jig at one end, and the load cell at the other end. A downward movement of the crosshead applied a compressive load to the specimen.

Jan 1, 1963

By Robert Corcoran, George Wiener

A study of the orientations and microstructure of 3 pct Si Fe alloys after deformation and recrystallization has been made. The components found after deformation agreed with recently published work on single crystals, being primarily (001) [110], (111) [110], and (111) {112}. A pronounced effect of temperature of recrystalliza-tion was found on microstructure and orientation. Low temperature recrystallization was interpreted in terms of low angle boundaries which resulted in the retention of a large amount of the deformation texture. High temperature recrystallization was interpreted in terms of high angle boundaries which gave rise to new components. No simple angular relation between the deformation and high temperature recrystalliza-tion textures could be detected. DEFORMATION and recrystallization behavior of 3 pct Si-Fe has been the subject of scientific investigation for many years. The fact that it is a single phase body-centered-cubic alloy from room temperature to the melting point permits study over a wide range of temperature without the complications of phase transformations. There is an important commercial interest in this material as well, since it is widely used in the electrical industry. In the present work the deformation and recrystallization behavior of poly crystal line silicon iron has been studied with the primary purpose of evaluating the effect of a second phase impurity on both processes as well as the effect of temperature on the recrystallization characteristics. With regard to deformation, the emphasis has been placed on a study of the crys-

Jan 1, 1957

By H. W. Knott, M. H. Mueller, P. A. Beck

The rolling and recrystallization textures in 300°C rolled uranium sheet were investigated using a Geiger counter diffractometer with the modified Schulz reflection technique. Seven sections of sheet material were used in order to obtain sufficient data for quantitative pole figures by the reflection technique. A special integrating specimen table was used for obtaining and recording the data automatically. The rolling texture was described in terms of several "ideal orientations" in which the stronger orientations have either the (1103 or (010) poles in the vicinity of the rolling direction. The recrystallization texture of the sheet uranium was also described by several "ideal orientations" which are somewhat different, except in one case, than the as-rolled "ideal orientations." RESULTS of an X-ray study of the deformation texture in rolled uranium rods were reported by Harris' in which a concentration of (010) and (110) poles was found in the rolling direction. More recently Seymour," Mitchell 'and Rowland,3 and Adam and Stephenson4 reported results obtained on uranium sheet rolled under various conditions of tem- perature and amount of reduction. Since the results of Seymour as opposed to those of the two other groups of investigators are not in full agreement, it seemed justifiable to publish the present data, obtained concurrently with the previously mentioned investigations.'-' The results with rolled and re-crystallized uranium sheet were also included in the paper, since they appear to be more complete than the only previously published texture data on recrystallized sheeL3 In the present investigation great care was taken to maintain complete separation of the reflections from different crystal planes, even in cases where the 20 angles differed from each other by less than

Jan 1, 1956

By H. W. Schadler

Single crystals of tungsten, which were grown by electron bombardment floating zone refining, were strained 2 pet in tension and bending at 298°, 77°, and 20°K to determine the modes and crystallography of the plastic deformation of these temperatures. At 77° and 20°K plastic deformation occurs by slip on systems of the type (011) [111] and by twinning on (112)-type planes. For crystals strained at 298°K, deformation occurs by slip in [111] directions on either (Oil)- or (112)-type planes. CURRENT models for the initiation of brittle fracture in crystalline materials are based on a knowledge of the details of their plastic deformation.1 Body-centered cubic tungsten exhibits brittle failure at temperatures below about 500 °K yet the modes and crystallography of its plastic deformation have not been studied below 1000°K. In 1924, Goucher2 reported that tungsten single crystals with a total impurity content of less than 0.01 wt pet deformed by slip on the (112) [111] system in the temperature range 1000° to 3000°K. He also observed (001) [010] slip in one crystal which was constrained by the presence of a large fissure. According to Barrett3 tungsten also deforms by twinning on the (112) plane in the [111] direction, but he gives no details on the tendency for twin formation or the temperature range in which twinning occurs. Therefore, as a necessary part of a study of the factors influencing the brittle fracture of tungsten, the modes and crystallography of the plastic deformation were determined at 298°, 77°, and 20°K. Tungsten single crystals, grown using the electron-bombardment zone-refining technique first described by Calverly,4 were deformed to between 1 and 2 pet plastic strain in tension and bending. The surface offset resulting from slip or twinning was observed with an optical microscope to determine the crystallography of the deformation. The existence of twins was proven by the standard polishing and etching technique; and the crystallography of dislocation motion was followed using the dislocation etchant described by Wolff.5 Some observations on the fracture characteristics of tungsten single crystals are included. EXPERIMENTAL TECHNIQUES Growth, Purity, and Perfection of the Crystals-Several years ago Calverly, Davis, and Lever4 dem-onstrated the feasibility of growing tungsten single crystals by the electron-bombardment floating zone-refining technique, and Carlson6 showed that crystals produced in this way had a high degree of purity and were ductile at room temperature. Tungsten single crystals produced by this technique in equipment similar to that described by Carlson were used in this study. The starting material, a powder metallurgy product, was obtained in the form of a swaged 1/8-in. rod from the General Electric Wire Plant in Cleveland, Ohio. The crystals were grown from this material in a vacuum of 10"4 mm of Hg by passing a molten zone 1/8 in. long down the rod twice at a speed of 3 mm per min. At this zone speed

Jan 1, 1961

By S. Floreen

Measurements have been mode of the effects of tempering and austenitizing heat treatments, the work-hardening characteristics, and the effects of test temperature and strain rate on the properties of a low-carbon Fe-18 pet Ni martensitic alloy. In many respects the alloy behaved quite similarly to cold-worked iron. One notable quality was the excellent ductility at temperatures as low as 20°K. Many of the qualities of the maraging steels could he related to the properties of the Fe-Ni matrix. THE 18 pet Ni maraging steels have demonstrated that unusual combinations of strength and toughness may be obtained by age hardening a low-carbon Fe-Ni martensite matrix.' These properties must, to some extent, reflect the properties of this Fe-Ni matrix, and therefore an understanding of the properties of this matrix is a prerequisite to a complete understanding of the steels. There have been several recent studies of Fe-Ni-C martensites, but not much attention has been paid to alloys with very low carbon contents. At low carbon levels the crystal structure of these alloys is essentially bee.2 Electron transmission microscopic examination of a 20 pet Ni binary alloy showed martensite platelets separated by low angle boundaries.3 Plastic deformation of the low-carbon alloys has been shown to proceed by wavy glide.4 The hardness of these martensites is typically RC 28, and their yield strengths are 70 to 80 kg per sq mm.2, 5 Their ductility is excellent. Room-temperature tensile elongations of 18 pet and reductions of area of 70 pet have been observed in an Fe-18 pet Ni binary alloy.5 These observations have provided a qualitative understanding of the flow characteristics of these alloys. To date, however, no thorough study of their properties has been made. In particular, it is not known to what extent the deformation characteristics of low-carbon martensites are similar or dissimilar to those of pure iron or other bee metals. The present work was undertaken to provide more detailed information on the flow characteristics of a low-carbon Fe-18 pet Ni martensite. PROCEDURES, RESULTS, AND DISCUSSION Materials. A 40-lb heat of the Fe-18 pet Ni alloy used in this study was made by vacuum-induction melting. The charge materials were electrolytic iron and electrolytic nickel. A carbon boil was used to achieve deoxidation. After the boil the heat was refined by additions of 0.1 wt pet Ti and Al. These additions are commonly used in the maraging steels to keep the carbon and nitrogen contents in solid solution at a minimum. After casting, the heat was

Jan 1, 1964

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