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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' 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,' 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 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 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 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 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 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

By L. B. Harris

Continuous cyclic unloading during tensile work hardening of polycrystalline zinc at room temperature enables specimens to sustain greatly increased extension. Such enhanced ductility is associated with creep-type extension, during which the cyclic component appears to promote relaxation of internal strains. It is possible to trace the transitions from tension, through enhanced cyclic extension, to fatigue and relate the observed behavior to simpler types of deformation. DISTINCTIVE deformation behavior has been shown to occur when loading includes both cyclic and unidirectional components. For aluminum and copper extended by a sequence of progressively biased strain reversals, coffin1 observed greater fracture ductility and lower flow stresses than during monotonic tension. This may be compared with the reduction in hardness obtained from conventional fatigue softening. But fatigue softening is accompanied by enhanced fatigue life,&apos; whereas Benham3 found that fatigue life was reduced when copper continuously extended during axial load cycling. The corresponding specimen elongation, for large cyclic load amplitudes, was greater than during normal tension. Under different conditions, Bendler and wood4 found that torsional fatigue initiated extension in copper under low tensile loads previously in equilibrium with the specimen; fatigue life was again reduced. Thus there is a type of cyclic softening which is associated with reduced fatigue life and which occurs when the cyclic loading is accompanied by a unidirectional strain component. Further, the fracture ductility or extension obtained from the unidirectional component can exceed that obtained in the absence of cyclic load. Specimen extension was not initiated by axial fatigue at small load amplitudes;3 hence Benham&apos;s work distinguishes between fatigue at large and small amplitudes, the former often being linked with unidirectional deformation because of similarities in strain Structure. The initiation of tensile extension during torsional fatigue,4 however, occurred with small amplitudes. Comparable changes in behavior have been ob- served during creep. kennedy&apos; found that combined cyclic and creep stresses on lead at 32°C increased the rate of elongation over that for simple creep, the consequence being a reduction in creep life. It was also demonstrated that small cyclic stresses applied after creep deformation initially increased recovery, but that prolonged application produced only normal fatigue hardening. It is clear that physical properties can be changed by interaction between the cyclic and unidirectional deformations, but owing to the number of different ways in which the deformations can be combined and the large number of possible variables for each combination, trends of behavior become easily obscured. One definite conclusion is that enhanced ductility or increased extension can be obtained by cyclic action, and it is this process that has been investigated for the tensile test by measurements of the extra tensile strain produced by the addition of a cyclic tensile component. EXPERIMENTAL PROCEDURE Material. Specimens were 99.99 pct Zn wire of 1.6 and 2.0 mm diam. Mean grain diameter was 0.02 mm, sufficiently small to give a ductile necked-down fracture under all loading conditions. All experiments were conducted at an average temperature of 20°C. Normal Tension. Unidirectional tensile curves at different strain rates were obtained from an In-stron testing machine, on which load-time curves were recorded autographically, using gage lengths of 5 and 10 cm. Straining was at constant cross-head velocity, and quoted strain rates are with reference to initial specimen length. Measurements of total elongation under simple tension were also made on the tensile machine that had been modified to incorporate an added fluctuating load. Combined Tension and Rapid Cyclic Load. An electromagnetic vibrator was coupled to the elastic beam of a Hounsfield ensometer- and driven sinus-oidally from a power amplifier at frequencies from 20 to 360 cps, the flexible connecting links on the tensometer being replaced by rigid fixtures to eliminate lateral vibration in the specimen. One end of the specimen was pulled by the normal extension drive of the tensometer while the other end, fixed to the elastic beam and vibrator, was subjected to rapid oscillations of load. It was thus possible to apply cyclic load to a tensile test without altering the rate of extension of the specimen

Jan 1, 1964

By J. E. Dorn, L. A. Shepard

LOW and Gensamer&apos; demonstrated a number of years ago that the yield point phenomenon in mild steels was associated with the presence of fer-rite soluble carbon or nitrogen. More recently the yield phenomenon in body-centered-cubic metals containing interstitials was rationalized by Cottrell&apos; in terms of a simple dislocation model. Interstitial atoms interact with dislocations in two ways; they cause not only local expansions but induce local tetragonality in the lattice. Consequently, interstitial~ interact with the hydrostatic tension and shear components of the stress about dislocations. They tend to migrate toward the expanded regions of edge dislocations and to assume sites that relieve the shear stresses of screw dislocations. Thus, a dislocation saturated with solute atoms constitutes a lower free energy state than that obtained when the dislocation threads through the average composition regions of the matrix. A greater stress will be required to separate the dislocation from its atmosphere than to move the dislocation through the matrix. This factor gives rise to the upper yield stress, which is required to unleash a series of dislocations in a localized region. This local yielding is propagated across the specimen to form a thin band of plastically deformed material known as a Lueder&apos;s band, making an angle of about 45" to the stress axis. Once the band has formed, deformation continues at the lower yield stress by the spreading of the Lueder&apos;s band in the direction of the applied stress. Undoubtedly the spreading of Lueder&apos;s bands at the lower yield stress is accomplished by the high stress concentrations at the band fronts, which serve to induce continued unlocking of new dislocations in advance of the migrating band fronts. Cottrell and Bilby have shown that the dependence of the yield point on temperature can be deduced by assuming that thermal fluctuations aid the stress in unlocking small dislocation loops from their solute atmospheres. Once a loop that exceeds a critical size has been nucleated, the entire locked diqlocation is released and can migrate. Fisher4 simplified this analysis by assuming that the locking forces were short range, so that if the dislocation loop were displaced only one Burgers vector from its atmosphere, it would be unlocked. Applying his model to the special case of delayed yielding under a constant stress of the order of the upper yield strength, he demonstrated that the delay time 7 for yielding should depend on stress and temperature according to where A and B are constants, G is the shear modulus, and u and T are the resolved shear stress and absolute temperature, respectively. Cottrell and Bilby, Fisher, and Fisher and Rogers&apos; have shown that the above deductions are at least in qualitative harmony with the experimental facts. A number of investigators5-0 have shown that the yield point phenomenon can also be induced in sub-stitutional alloys of face-centered-cubic metals. In general such yield points are not as pronounced as those encountered in body-centered-cubic metals containing interstitials. The yield point phenomenon in these materials is usually enhanced by prestrain-ing at low temperatures and aging at intermediate temperatures. Undoubtedly the yield point phenomenon induced by strain aging substitutional alloys also results from locking of dislocations. But the locking of dislocations in substitutional alloys of face-centered-cubic metals differs somewhat from interstitial locking of dislocations in body-centered-cubic metals. Substitutional elements in face-centered-cubic lattices cause only radial displacements of the adjacent lattice points. Consequently, only the edge components of dislocations can be locked by the mechanism suggested by Cottrell. Additional locking, however, can be obtained by the Suzuki mcchanism.10 In face-centered-cubic metals, dislocations exhibit lower energies when they are present in the

Jan 1, 1957

By F. N. Rhines, B. H. Alexander

MUCH attention has been directed to the effects of grain size upon the properties of alloys, but there has been scant study either of the conditions that determine the pattern and dimensions of den-drites in metal systems, or of the influence of their shape and size upon the overall properties of cast-ings. The aim of the research that is about to be described has been to investigate the effect of vari-ous factors upon the mode of formation of dendrites in alloys by measurements of the distance between adjacent dendrite arms (dendrite spacing). Early investigators, including Grignonl and Tschernoff,2 showed that a metal dendrite is com-posed of a tree-like system of stalks and branches arranged in a simple geometrical pattern. North-cott and Thomas3 demonstrated that, in the face-centered cubic solid solutions of copper-base, these stalks and side arms all lie in (100) directions in the crystal. Several investigators, including Sauveur and Chou,0 Sauveur and Reed,&apos; and Martin and Mar-tina have reported that the addition to steel of alloy-ing elements, such as nickel, chromium, and molybdenum, not only makes the dendrites easier to reveal by etching, but makes them coarser. The latter authors8 proposed that the coarsening of the dendrites is roughly proportional to the increase in the temperature range of freezing, caused by adding the alloying elements. Sauveur and Chou6 showed, in addition, that the dendrites are coarsened by a decreased rate of cooling of the casting. Measurement of Dendrite Arm Spacing Among the physical conditions that could be ex-pected to have an influence upon the dendrite arm spacing, that appears in a cast metal, are: composi-tion, rate of freezing, crystal structure, and type of constitution. The relationships obtaining between these variables and the dendrite dimensions have been examined, in the present research, by measur- ing the arm spacing in a wide variety of alloys, listed in tables II through VI. Alloy compositions are recorded in the tables by showing the symbol of the major metal followed by the percentage and symbol of the alloying agent; thus, "Al-10Ag" is an aluminum-base alloy containing 10 pct of silver. Although none of the alloys were analyzed, an im-pression of their degree of purity may be obtained from that of their component metals given in table I. Five hundred grams of each alloy was made by melting in small clay-graphite crucibles in an elec-tric muffle furnace. After alloying the temperature was adjusted to 50" to 75°C above the liquidus and the melts were poured into cast iron molds, at room temperature, the molds having a wall thickness of 1 in. and a cavity 11/2 in. sq in cross-section. Each ingot, thus cast, was sectioned at mid-height and the sectioned surface was polished and etched for metallographic examination. Dendrite spacing meas-urements were made at three positions, namely, ad-jacent to the mold wall, midway between the wall and the center of the ingot, and at the center (desig-nated e, m, and c respectively, in the tables). A typical series of microstructures is presented in fig. 1. For each measurement, the average was taken of the dendrite spacing of several grains covering a zone about 2 mm wide. Only those grains which had a major dendrite axis nearly in the plane of polish were selected in order to eliminate corrections for orientation differences from grain to grain. Although the dendrite spacings were measured to the nearest thousandth of a millimeter, the values listed in the tables are thought to be significant only to the nearest hundredth of a millimeter. The larg-est difference in readings found, when various ob-servers rated the same specimens, was 0.012 mm; the largest difference between corresponding meas-urements upon duplicate specimens was 0.027 mm.

Jan 1, 1951

By W. G. Lidman, H. J. Hamjian

&apos; I HE fabrication of many materials from powders involves a sintering process. A mass of powder will sinter because of the excess free energy over the same mass in the densified state caused by the higher total surface area of the powder. An understanding of the kinetics and mechanism of sintering should assist in improving the properties of such materials. The present investigation conducted at the NACA Lewis laboratory deals with the sintering of chromium carbide. Dry sintering (sintering at a temperature below the melting point) was divided into two stages by Shaler:&apos; the first stage, during which the particles preserve much of their original shape and the voids are interconnected, and the second stage, during which densification occurs and the pores are isolated. The mechanism of forming interfaces between particles, or welding together of particles, has been investigated by Kuczynski2 and may be described by any one or a combination of the following mechanisms: viscous flow, evaporation and condensation, volume diffusion, or surface diffusion. The mechanism by which pores are closed or eliminated (densification) during sintering, is of interest. Grain growth observed during sintering may be attributed to the variation in the surface energies of individual grains, causing some grains to grow at the expense of others. Grain boundary migration occurs presumably by a diffusion process, therefore the rate of grain growth would be expected to increase exponentially with increasing time and temperature. Thus, for practical sintering times of less than 1 hr, a certain minimum temperature may exist at which major structural and property changes will occur. Densification and kinetics of grain growth during sintering under pressure of chromium carbide were investigated to provide additional information which will aid in describing more accurately the sintering process and the mechanisms involved. This material was selected for this study because of the current interest in high strength, oxidation resistant refractory materials, such as carbides, which are sintered to produce solid, dense materials from powders. Sintering under pressure is a process where the heat and pressure are applied to the compact simultaneously, specimens for this work were prepared by sintering under pressure at different temperatures and for various time periods. Experimental Procedure Preparation of Specimens: Chemical analysis of the commercial chromium carbide used in this investigation was as follows: Cr 86.19 pct, C 12.14 pct, and Fe 0.2 pct. X-ray diffraction powder patterns gave characteristic diffraction lines of Cr3C2 crystal structure. Powder particle size was determined microscopically and the average initial particle size was 6 microns with 85 pct between 2 and 10 microns. Specimens sintered under pressure were formed in graphite dies3 heated by induction. Sintering temperatures were measured with an optical pyrometer by sighting into a 3/8-in. hole drilled 1 in. deep at the midsection of the graphite die. A load of approximately 1 ton per sq in. was applied to the powder. The die assembly was heated in 20 min to the highest temperature (2500°F&apos;) at which no increase in grain size could be observed, and less than 2.5 min were required to heat from this temperature to the maximum temperature (3000°F). Sintering temperatures and times for the specimens of this investigation are indicated in Table I. Analysis of Specimens: Specimens polished with diamond abrasives were etched to reveal the grain boundaries with a 1:1 mixture of 20 pct potassium hydroxide and 20 pct potassium ferricyanide heated to 160°F. Representative areas of each sample were photographed at 1000 diameters. The largest diameters of all well-defined grains were measured, but only the measurements of 15 of the largest grains were averaged in order to determine an index of grain size on the assumption that they were among the first to begin growth. Densities were determined from differential weighing of the samples in air and water. The reported density values are considered correct within ±0.01 g per milliliter. Results and Discussion Metal compacts have exhibited grain growth when sintered at temperatures about two-thirds of the absolute temperature of their melting point.&apos; Grain growth also occurs during the sintering of chromium carbide and is illustrated by the micrographs shown in Fig. 1. These micrographs were prepared from specimens sintered for 90 min at temperatures ranging from 1371°C (2500°F) to 1648°C (3000°F). Average grain size and density measurements of specimens investigated are presented in Table I. The relationship between grain size and sintering tem-

Jan 1, 1954

By L. A. Geoffrion, R. H. Perkins, J. C. Biery

Densities of cerium metal and several lour-melting binary cerium alloys were measured over the range 25° to 800°C. A rolumeter, using NaK as working fluid, was used to obtain the data. The cerium, Ce-Co, Ce-Ni, and Ce-Cu alloys all exhibited an increase in density on melting, while a Ce-Mn alloy expanded on melting. FOR the proper design of a nuclear reactor, the change in density of the fuel with temperature must be known. This is especially important in a system utilizing molten fuel, such as LAMPRE (Los Alamos Molten Plutonium Reactor Experiment), since a relatively large change in density usually occurs during the solid-liquid transition. The fuel for LAMPRE is a Pu-2.5 wt pct Fe alloy with a melting temperature of 410°C. However, limitations in reactor design with this fuel have led to consideration of other plutonium-containing alloys for use in future generations of this type of reactor. Several ternary alloys containing plutonium and cerium as two components have satisfactorily low melting points. The system that at the present time appears to be most acceptable is Pu-Ce-Co; it exhibits little change in melting temperature with wide variation in plutonium concentration. Other alloys that have received some consideration contain nickel, copper, and manganese as the third constituent. The proposed fuel alloys are difficult to handle experimentally in the 25" to 800°C temperature range since they oxidize readily, react with many solvents, and contain a poisonous fissionable material. In addition, in this temperature range the alloys pass through the solid-liquid transition. Several techniques are available for measuring the densities and volume coefficients of expansion of solids or liquids. However, the only apparatus that appears suitable for measuring expansion coefficients over this temperature range and through the phase transition is a volumeter. In a volumeter, the indicating medium must be essentially inert to and insoluble in the material being studied. It must also possess a low vapor pressure over the operating temperature range, and its coefficient of expansion must be accurately known. One material that is satisfactory in nearly all of these respects is the alloy Na-78 wt pct K, which melts at -10°C and has a vapor pressure of 860 mm Hg at 800°C. This relatively high vapor pressure at 800°C requires an overpressure of an inert gas to prevent boiling. While a volumeter is capable of determining accurately the volume coefficients of expansion of materials, it cannot be used for absolute density measurements. Therefore, a density determination at a known temperature must be coupled with the volumeter measurements to give all the desired data. The weight-loss technique using immersion in bromobenzene at room temperature proved to be satisfactory. The preliminary work that was done on this experimental program involved developing and calibrating the equipment, and measuring the densities and volume coefficients of expansion of cerium and some low-melting binary cerium alloys. The complications that are caused with the introduction of plutonium into the system were avoided until the equipment was proved to be satisfactory and until experience was gained in its operation. It is this first phase of the experimental work that is described in this report. DESCRIPTION OF EQUIPMENT AND OPERATING PROCEDURE The NaK volumeter is shown schematically in Fig. 1. Basically, the equipment consists of two weld-sealed stainless-steel containers of nearly identical volume. One container holds a tantalum crucible and the specimen being measured; the other contains a tantalum crucible and a tantalum specimen used as a control reference material. To avoid temperature gradients, the bombs are located in a copper block inside the furnace. Stainless-steel capillaries of equal length and volume connect each stainless-steel container to a glass viewing capillary. The stainless-steel containers, stainless-steel capillaries, and a portion of the glass capillaries are filled with NaK (22 wt pct Na-78 wt pct K). The NaK/gas interface in the glass capillary is viewed with a cathetometer which is accurate to *0.5 mm. The cathetometer readings are used to calculate the volume changes of the samples during a run. This volumeter is basically the same as that described by F. Knight in Plutonium 1960. 2 However, changes in equipment design and operating procedure were made to eliminate some major operating difficulties. These changes are summarized below. 1) In filling the manometer with NaK, gas was frequently entrained in the system. Evacuation of the system before filling failed to eliminate the en-

Jan 1, 1965

By W. J. Helfrich, R. A. Dodd

Binary aluminum solid-solution alloys containing various amounts of silver, magnesium, and zinc were prepared by careful directional solidification, and the hydrostatic and X-ray densities were compared. With the exception of the Al(Ag) alloys, the X-ray densities were consistently greater than the hydrostatic measurements, in agreement with earlier observations by Ellwood. In contrast to Ell-wood&apos;s interpretation in terms of vacant lattice sites associated with Brillouin zone effects, a tentative explanation based on the existence of solidification microshrinkage was favored. This hypothesis was confirmed by an examination of Al(Zn) alloys prepared by vapor diffusion of zinc into aluminum. The hydrostatic and X-ray densities were now in very close agreement, and it was concluded that the filling of Brillouin zones in aluminum solid-solution alloys does not necessarily result in the formation of defect structures containing an excess of vacant lattice sites. ThE existence of defect structures of the vacancy type in alloys in which the excess vacancies have an electronic rather than a thermal or mechanical, and so forth, origin is well recognized. Examples of incomplete lattices of this type are to be found in the Ni-Al,1-3 Fe-Ni-A1,4 c~-Ni-Al,5 Fe-Cu-Al,= and Co-A17 systems. These defect structures are of a special kind in that the intermediate phases possess an ordered atomic arrangement or superlattice, and in some instances the vacancy concentration may be unusually large, e.g., at 45.25 at. pet Ni in NiA1, approximately 8.8 pet of the lattice sites are unoccupied. Ellwood8-10 has reported similar defect structures in the aluminum solid solution alloys of the Al-Zn and A1-Mg systems and in alloys of the Au-Ni system." In Al(Zn) the (apparent) vacancy concentration rose, somewhat irregularly, to a maximum of about 2 pet vacant sites at 25 at. pet Zn, while in Al(Mg) the (apparent) vacancy concentration increased continuously to 1.7 pet at 15 at. pet Mg. An explanation in terms of Brillouin zone overlap was attempted, although Pearson12 has pointed out the difficulty of reconciling the observations with zone theory. However, the possibility of the effect being caused by the Fermi surface just touching a plane of energy discontinuity inside a prominent Brillouin zone has, in general, been accepted. In fact, Massal-ski13 has interpreted Ellwood&apos;s8 observations as confirmation of Leigh&apos;s14 theoretically predicted zone overlap occurring at approximately 2.67 electrons per atom. Unfortunately, Massalski was apparently unaware that Ellwood9 had revised his earlier results considerably, and the revised data did not confirm Leigh&apos;s analysis. Ellwood&apos;s clata were reexamined by the present authors who noted a possible correlation between the percentage defects as a function of alloy composition and the temperature interval of solidification measured from the respective equilibrium diagrams. This suggested an explanation in terms of shrinkage porosity rather than vacant lattice sites, and pointed to the desirability of reexamining appropriate alloy systems using: both Ellwood&apos;s method of specimen preparation (casting followed by wrought fabrication) and alternativ&apos;e methods, i.e., diffusion, which might be expected to minimize, or even completely obviate, microporosity. ALLOY PREPARATION 1) Cast Allolys and Aluminum Single Crystals. Al(Ag), Al(Mg;l, and Al(Zn) alloys of various compositions up to 20 at. pet silver, 13.5 at. pet mg, and 30 at. pet Zn were prepared by melting under helium and casting into graphite molds. In the first two systems, the maximum alloying addition was quite close to the limit of solid solubility, but the possibility of transformation to a&apos; during quenching somewhat restricted the suitable Al(Zn) composition range. The alloys were prepared from high-purity aluminum, a lot analysis showing 0.002 wt pet Cu, 0.002 wt pet Fe, and 99.996 wt pet A1 by difference. The silver, magnesium, and zinc were of 99.99+, 99.98+, and 99.998 wt pet respectively. Each composition was analyzed chemically. The as-cast ingots measured 7/16 in. diam and 5 in. length. One in. was removed from the top of the ingot, and the bottom 3 in. was machined to 0.275 in. diam; a point was also machined on the smaller diameter end. The remainder of the original ingot served as a top riser during subsequent remelting and controlled solidification. The machined ingots were now remelted using a Bridgman soft-mold technique to ensure directional solidification and, therefore, a minimum of micro-shrinkage. Alumina powder was used as mold material contained in an alundum thimble, and this crucible was placed in a helium-filled Vycor tube. The assembly was lowered through a suitable temperature gradient at approximately 0.5 in. min-l, and the risered portion of the casting was subsequently removed by sawing.

Jan 1, 1962

By R. A. Vandermeer

It is usually assumed that the rate-determining step in the migration of a grain boundary involves the thermally activated transfer of single atoms across the interface. Chemical reaction rate theory then gives a migration rate which is proportional to the driving force when this is small compared to kT.1 In their recrystallization studies on aluminum, Gordon and vandermeer2 obtained data which was capable of providing the first experimental test of this proportionality. They correlated stored energy (driving force) release measurements determined calorimetrically with fraction recrystal-lized kinetic (growth rate) data acquired metallo-graphically at a temperature where a significant amount of recovery takes place concurrently with recrystallization. Within experimental error, the results of Gordon and Vandermeer confirmed experimentally, at least over a limited range, the linear dependence of boundary migration (growth) rate on driving force in accordance with theory. In obtaining these results, however, an incorrect, implicit assumption was made in relating the average instantaneous growth rate of the recrystallized grains to the measured fraction recrystallized kinetic data. The purpose of this present note is to point out and correct this assumption. An alternate approach, whereby a more proper average growth rate can be calculated from the recrystallization kinetic data, is presented. The earlier data, reevaluated in terms of this new approach, show the same general trend as before so that the original conclusion of Gordon and vandermeer2 is still valid. As was shown in a detailed study3 of the geometrical features of recrystallization in aluminum, the colonies of recrystallized grains can be regarded as uniform cylinders embedded in a three-dimensional matrix, the number of such colonies being constant. Thus during the early stages of recrystallization the volume fraction recrystallized, Xv, can be written as Xv=ynvlr2 [l] where y is a shape factor and i and r are defined as the average length and radius of a recrystallized colony and are spatial averages over the specimen. -nv, is the number of such colonies in a unit of volume. The erroneous assumption made in the earlier paper2 was that r in Eq. [I] could be replaced by

Jan 1, 1965

By Dale A. Vaughan, Oliver M. Stewart, Charles M. Schwartz

Solid-solubility limits at 1500°, l000q and 500°C for carbon, nitrogen, and oxygen in high-purity tantalum were determined by X-ray lattice-parameter methods. For carbon, the solubility was found to be 0.17 at. pct at 1500°C, and less than 0.07 at. pct at 1000°C. A nitrogen solubility of 3.70 at. pct at 1500° C decreases linearly with temperature to 2.75 at. pct at 1000°C, and 1.8 at. pct at 500°C. In the case of oxygen, the solubility was found to be 3.65 at. pct at 1500°C, 2.95 at. pct at 1000°C, and 2.5 at. pct at 500°C. The phases Ta2C, the low-temperature modification of Ta205, and Ta,N of unknown composition but which has a superlattice structure based upon the original bcc tantalum lattice have been identified as the initial precipitates in the respective systems. Metallographic methods were employed to verify the X-ray analyses. The etching behavior of Ta is discussed in terms of lattice i?rzperfections and precipitate phases. The excellent fabricability, high melting point, and nuclear properties of tantalum are responsible for interest in this refractory metal. Data on the solid solubility of the interstitial elements (oxygen, nitrogen, and carbon) in tantalum and on the precipitate phases are somewhat limited. The significant contributions are discussed below. Because the purity of electron-beam melted tantalum (only recently available) is considerably higher than that used in previous studies, the present investigation was initiated. Gebhardt et all-3 have investigated the tantalum-oxygen and tantalum-nitrogen systems with particular reference to the changes in physical properties and to the rates of reaction between these gases and the metal. The solubility of oxygen in tantalum was reported2 to be 3.7 at. pet at 1500°, 2.3 at. pet at 100O°C, and 1.4 at. pct at 750°C. Schonberg4 reported that several oxide phases (Ta40, Ta,O, TaO and Ta,05) exist while X-ray studies by Gebhardtl showed only two oxides, Ta,05 and an unidentified phase which was associated with a platelet-type precipitate. La-gergren and Magneli,&apos; however, questioned the existence of compounds other than the two allotropic modifications of Ta,05 for the tantalum-oxygen system. In the case of nitrogen, the solubility was estab- lished by Gebhardt3 to be of the order of 7 at. pct at 1800°c. The solubility was reported to decrease rapidly with temperature, and, although no limits were established, a precipitate phase was observed by Gebhardt except when the high-nitrogen specimens were cooled very rapidly from the reaction temperature of 1800c. He reported the initial precipitate phase to be a tetragonal distortion of the bcc tantalum lattice while Schonberg6 reported the phase lowest in nitrogen Jo be a cubic super-lattice with a cell size of 10.11 A. Two other nitride phases, Ta,N and TaN, were reported; these appear to be isomor-phous with the carbides of tantalum. The tantalum-carbon system was investigated by Ellinger7 and by Lesser and Braurer. Two compounds, Ta,C and TaC, were reported to exist, each with a range of composition. The solubility of carbon in tantalum was found to be practically nil at all temperatures. Thus, of the interstitial elements which are present in small amounts in high-purity tantalum, carbon might be expected to form precipitates. The present investigation was initiated to obtain additional data on the solid-solubility limits of these interstitials at 1500°, 1000°, and 500&apos; with particular emphasis on the distribution and the identification of the precipitate phases. EXPERIMENTAL WORK AND RESULTS In the present investigations of the solid solubility and of the precipitate phases in the systems tantalum-nitrogen, -oxygen, and -carbon, high-purity tantalum was reacted with high-purity gases, homogenized at 1800°c, and annealed at and quenched from 1500°, 1000,

Jan 1, 1962