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By E. J. Ripling, S. I. Liu

IT has been shown in a number of recent publications that much information on the mechanical behavior of metals can be gleaned by first deforming test specimens under one set of conditions, and then evaluating the effect of this deformation by means of a subsequent tensile test. A straining procedure of this type has been applied to study the flow behaviors of a number of metals.1, 2 In these studies the prestraining and testing were both tensile strains, while the straining temperature was varied between the prestraining and testing steps. These data indicate that there is a more or less general flow behavior exhibited by all metals which are pre-stretched at one temperature and then tested in tension at a second temperature. Prestraining a metal at a high temperature produces a lower yield strength during the subsequent low temperature strain than would the same total strain at the lower temperature. On reversing the order of the strains, low temperature prestraining produces a higher yield strength during the subsequent high temperature straining than would a single high temperature strain of the same magnitude. Unlike the flow behaviors, the fracturing characteristics of metals when prestrained under one set of conditions and tested under a second set of conditions is quite material dependent. The fracture behavior of a number of steels2" as well as of a commercially pure zinc,4 have been investigated by these two-step tests and was found to depend upon the position of the transition temperature with respect to the prestraining and testing conditions. Since these fracturing phenomena are complicated by the appearance of the transition temperature, it has been difficult to reliably define the basic effect of a two-step straining procedure in fracturing. Metals crystallizing in the face-centered cubic system do not exhibit transition temperature effects so that the mechanical characteristics obtained on these materials could serve as a base for two-step straining behaviors. Consequently groups of specimens of the aluminum alloy 24s-T4 were prestrained various amounts at room temperature in either tension or compression after which these strained specimens were further strained to failure, or tested in tension, at either room or some lower temperature. Other groups of 24S-T4 specimens were prestretched at various low temperatures after which these were tested in tension at room temperature. These straining techniques then made it possible to compare the behaviors of aluminum with the behaviors previously presented for steels. Material and Procedure The commercial aluminum alloy 24S-T4 in the form of 3/4 in. rods was used in this investigation. The material was subjected to the following treatments before machining: 1—resolution treating at 920" & 10°F for 45 min, 2—quenching in water at room temperature, and 3—aging at room temperature for four days. The re-heat treated material was then machined to either of the specimen shapes shown in Fig. 1. Fig. la shows the threaded-end specimen used for prestraining in compression. Fig. 1b shows the specimen used for both prestrain in tension and final testing. The material subjected to precompression in the form of the specimen shown in Fig. la was re-machined to the specimen shape in Fig. 1b for final testing. Prestraining in tension and final testing were done without any intermediate machining. All straining was performed on a 10,000 1b Riehle tensile testing machine. Tensile strains were conducted in a specially designed concentric fixture which produced an eccentricity of less than 0.001 in." The change in diameter at the minimum section of

Jan 1, 1954

By W. A. Tiller, W. C. Johnston

The solute distribution ahead of an advancing solid-liquid interface is controlled by varying the momentum boundary layer thickness in the liquid adjacent to the interface. Single pass zone-melting experiments on Pb-Sn alloys are described in which the liquid is caused to rotate in the plane of the solid-liquid interface due to the influence of a magnetic .field rotating in this plane. The variation of the diffusion boundary layer thickness with field strength is determined. DURING the freezing of an alloy a partitioning of solute occurs at the solid-liquid interface, the magnitude depending upon the difference in the solid and liquid solubilities at the interface temperature. Because the diffusion coefficient is so small in the liquid relative to normal freezing rates, either a pileup or a depletion of solute occurs at the interface when the partition coefficient, kO, is either less than or greater than unity, respectively. This solute distribution is completely characterized by i) the solute concentration in the liquid far from the interface, C) the ratio of freezing velocityf, to diffusion coefficient, D, iii) the partition coefficient, ko, and iv) the thickness of the diffusion boundary layer, 6,, at the interface (this assumes that an electric field is not applied across the interface). For a particular system, C ko and D are fixed so that the character of the solute distribution can be changed only by a variation of either f or 6c. As is well known, the freezing velocity can be changed by varying the thermal environment of the alloy. Whereas, the thickness of the solute rich layer can be changed by varying the fluid flow conditions in the liquid. It is the purpose of this paper to describe a technique for controlling the fluid flow conditions in the liquid. During most solidification experiments the driving force for fluid flow arises from either mechanical mixing, thermal convection or electromagnetic mixing. The momentum boundary layer thickness, 6m at the solid-liquid interface, within which negligible movement of the liquid occurs, has been calculated for the special case of mechanical mixing where crystals are solidified by the Czochralski technique.l,2 The calculation of 6m for the case of thermal convection has also been made.3 In some calculations it has been assumed that the momentum boundary layer thickness, 6,, may be equated to the thickness of the diffusion boundary layer 6c, at the interface. However, as may be seen from Appendix I this is only true in very special cases and in general where a is a constant of magnitude determined by the particular liquid alloy. Neither calculations nor experimental data exist for the dependence of upon electromagnetic mixing. In this paper experiments are described in which the liquid is caused to rotate in the plane of the interface due to the torque developed on it by a magnetic field, H, rotating in this plane. The variation of is controlled by the variation of H. A magnetic field rotating in a plane perpendicular to the interface has been used for the purification of aluminum. Experimentally, we determined the variation of 5C with H by using the zone-melting technique of pfann5and a theoretical relationship of Burton et a1.2 pfann5 has shown that, after the passage of one molten zone through a long cylindrical charge of uniform concentration, CO, the solute distribution, C,, in the solid is as shown in Fig. 1. The equation describing this distribution is

Jan 1, 1962

By R. I. Jaffee, J. W. Roberts, D. N. Williams

DISPERSION hardening as an alloying process has aroused increasing interest in the past few years. This alloying procedure, in which an insoluble phase is dispersed randomly through a metal or alloy, is believed to be especially suited for the attainment of creep strength at elevated temperatures since the dispersed phase is metallurgically stable. Another advantage is that the physical properties of the matrix phase, such as electrical conductivity, remain relatively unaffected by alloying. These two characteristics resulted in interest in the applicability of dispersion hardening to copper and copper alloys. A study of copper alloys prepared by powder metallurgy methods has shown some strengthening from oxide dispersions.' However, powder metallurgy processing would not be economical for large scale production of dispersion hardened copper-base alloys. Therefore, the research described in this article was initiated to examine methods of forming dispersion alloys which would not require powder metallurgy processing. If powder metallurgy processing is to be avoided, a method must be found by which the dispersion material can be introduced into and dispersed through the melt before casting. When the dispersed phase is an oxide or similar nonmetallic, it is extremely difficult to form a satisfactory liquid: solid dispersion since successful mixing requires that the melt wet the dispersed phase. It is almost impossible to force a nonwetted particle beneath the melt surface. This difficulty can be avoided, however, if the oxide particles are produced in molten copper by reaction within the melt. The problem would then reduce to maintaining randomness until solidification. Four procedures were considered for producing an oxide particle within molten copper by reaction. In all cases, the intent was to react oxygen (0) with a reactive metal (X) to form an oxide (XO) within the copper melt. These reactions were as follows: 1) (Cu-X), + (O)g (Cu)1 + (XO)S [1] 2) (Cu-X)1 + (Cu2O)s (Cu)x + (XO)S [2] 3) (Cu-OK)1 + (Cu-X)1 (Cu)1+(XO)9 [3] 4) (Cu-OK)1 +(X)s (Cu)1 +(XO)s [4] The reactions were carried out in an 8-lb melt of 99.98 pct Cu maintained in the vicinity of 2200oF by induction heating. Where possible the amount of the reactants was controlled to give 1 to 5 vol pct oxide. Mechanical stirring during the reaction period was used to minimize agglomeration of the reaction product. The presence of a reaction product was determined metallographically by study of an ingot cast from the melt at the end of the reaction period. Reaction [I] was studied by dissolving aluminum in the melt followed by forcing oxygen through the melt. The melts became quite sluggish during the reaction period suggesting that A12O3 was formed. However, the reaction product rose out of the melt rapidly, possibly due to the flushing action of the oxygen stream, and little dispersed phase was formed. Reaction [2] was examined by dissolving aluminum, silicon, or nickel i; the melt and then adding Cu20 (melting point 2250F). This procedure was unsuccessful. Although Cu2O was easily stirred into cop-

Jan 1, 1961

By S. L. Couling, D. J-P. Adenis

i2) twinning in poly crystalline magnesium does not usually occur homogeneously but is concentrated in localized regions or bands inclined at about 45 deg to the stress axis. These bands of twinning are in many ways similar to the Luders bands seen in mild steel alzd Al-Mg alloys. Within a hand the percentage of the volume twinned may approach 100 with no twinning outside the band. Bands are not produced in specimens of grain size a3 x 10-= in. or in samples deformed at temperatures 300°F. Annealing of heavily twinned regions leads to re crystallization textures markedly different from those found in the starting material. The exact preferred orientation appears to depend on the starting grain size, the amount of compres-sive strain and the manner in which it is introduced. MAGNESIUM, with its hexagonal crystal structure, deforms plastically at room temperature by a variety of deformation mechanisms, one of the most important of which is (1012) twinning. In single crystals such twinning occurs on compression parallel to the basal plane or tension perpendicular to it. In wrought polycrystalline magnesium, such as rolled sheet, the preferred orientation is such that almost all the grains have their basal planes nearly parallel to the sheet surface. Therefore, if sheet material is deformed by cold rolling or by tension in the plane of the sheet, deformation of the grains by (1012) twinning is not favored. On the other hand, twins form readily on compression parallel to the plane of the sheet as in a compression test, on the compression side of a bent sample, or at the outer rim of a drawn cup. The first part of this paper deals with the morphology of (1012) twinning in polycrystalline magnesium. Some aspects of this subject were covered by Barrett and ~aller.' Of direct bearing on the work to be reported here are the comments of Jetter' in discussion to Ref. 1. He shows that Mg + 1.5 pct Mn alloy sheet when bent about a transverse axis develops a pattern of transverse bands on the surface of compression. A longitudinal section through the sheet shows that the bands are wedge-shaped and inclined to the rolling direction. The bands were identified as "outcrops of regions in which deformation is localized as the result of the reorientation brought about by (1012) twinning". The second part of the paper treats the recrys-tallization texture of the specimens twinned by compression. Magnesium deformed and then annealed generally recrystallizes with no change in orientation.1'3'4 This statement is true provided that the amount of (1012) twinning occurring during deformation is small. In an isolated observation, Anse15 has shown that, when deformation produces much (1072) twinning, annealing causes new maxima to appear in the pole figure. The second part of the paper elaborates on this point. I) MATERIALS AND PROCEDURES All of the experimental work to be reported was done using the commercial sheet and plate alloy AZ31B (nominal composition: 3 pct Al, 1 pct Zn, 0.4 pct Mn, balance magnesium). This alloy is available commercially in two tempers, -0 (fully annealed) and -H24 (partially annealed), and specimens of both tempers were used in various experiments. The average grain. diameter (AGD) for -0 temper 0.125-in. sheet is about 0.5 x 10- in.; where material of larger grain size was desired, anneals at elevated temperature were used to grow the grains. compression tests were made on a screw-driven "hard" machine. The specimens were clamped in a

Jan 1, 1964

By Hsun Hu, R. S. Cline

The formation of annealing textures during the course of recrystallization in 2 pct Al-Fe crystals rolled in the (111) [112], (112) [111], and (112) [Till orientations has hem studied in detail. When the rolling texture is composed of both (111) [121] and (001)[110] components, the annealing texture consists of mainly (110) [001] and (113) [332] components. As the (001) [110] component diminishes from the surface to the interior of the rolled crystal, the relative concentration of the (113) [332] component in the annealing texture decreases accordingly, whereas that of the (110)[001] component increases with the (111)[112] component in the rolling texture. Such dependence of the annealing texture on the composition of the rolling texture is in accmdance with the oriented growth mechanism. Grain-growth characteristics during recrystallization, hence the annealing texture, can he considerablv different in (112) [111]-type crystals depending sensitively on the initial orientation of the crystal. In a previous publication,' the formation of rolling textures in 2 pct A1-Fe single crystals with initial orientations of approximately (1ll)[112], (112)[111], and (112)[111] was studied in detail. The deformation texture of these crystals consisted of either a single (111)[112] or a combination of (111)[112] and (001)[110] components in various concentrations. For the (lll)[112] crystal, the deformation texture was a single (lll)[112] up to 70 pct rolling reduction, but it became (lll)[112] plus (001)[110] after -90 pct reduction. For the (112)[113.]-type crystals, the relative concentration of the (111)[ 112] and (001)[110] components varied with the depth below the surface of the crystal, as well as with the amount of deformation. These series of specimens, having deformation textures with a range of concentration of the (111)[112] and (001)[110] components, could therefore be used for a thorough investigation of the effect of deformation-texture components on the formation of annealing textures. In a study of rolling and annealing textures in Si-Fe crystals, Dunn and Koh3 noted that the addition of a (001)[110] component to the (111)[112]-type deformation texture had practically no effect on the recrystallization texture.* According to the ori- ented growth mechanism for the formation of annealing textures, nuclei related to the deformation texture by approximately 30-deg rotation around a common [110] axis have the highest rate of growth and the resulting annealing textures generally have such an orientation relationship with respect to the deformation textures.314 It was reasoned by Dunn and Koh3 that if the oriented growth mechanism operated the recrystallization texture developed from a deformation texture containing both (111)[112] and (001)[110] components should be strongly centered around (113)[332], because (113)[332] is approximately midway between the (111)[112] and (001)[110], and is related to both of these two orientations by [110] rotations of 25 to 30 deg. Hence, nuclei of (113)[332] orientation should have a high rate of growth in the deformed matrix. However, their results were not in accord with this prediction. It was felt by the writers that a detailed study was needed to clarify the effect of deformation-texture components on annealing-texture formation. For this reason, the present investigation was conducted. EXPERIMENTAL PROCEDURE Specimens used for the present investigation were taken from the crystals rolled previously for deformation-texture studies.' In order to follow the progress of annealing-texture formation during the course of recrystallization, a single specimen was taken from each rolled crystal and its textural changes examined after successive anneals until recrystallization was complete. The specimen was carefully cut from the rolled strip with a jeweler's saw. Prior to annealing, the sawed edges were etched to remove distorted metal, while both faces of the specimen were protected from the etching solution by acid-proof plastic tape. After annealing, the specimen was etched from the "bottom" face only (the reference or "top" face of the specimen was protected by plastic tape) to one half of its original thickness, so that the texture at the surface and at the central section of the strip could be determined by the reflection technique. The

Jan 1, 1965

By D. J. Schmatz

DISCUSSION OF RESULTS The qualitative correlation between low-temperature ductility and prior high-temperature creep strain in nickel obtained in this investigation confirms the result obtained on high-purity brass by Chen and Machlin. However, the quantitative effect is much smaller in nickel. Comparison can be made on the basis of a prior high-temperature strain that is a certain percentage of the total high-temperature elongation to rupture. In the research of Chen and machlin, the prior high-temperature strain of 1/2 pct equaled 8.5 pct of the total high-temperature elongation at rupture. For nickel, in our experiments, 8.5 pct of 21.2 pct equals 1.8 pct. For eh = 1.8 pct, the loss in ductility in percent equals x 100 = b.5 pct. That is, for equivalent bo Formation of Beta Manganese-Type Structure in Iron-Aluminum-Manganese Alloys D. J. Schmatz IRON-aluminum alloys have gained much interest in the past few years for use as a base material for elevated-temperature alloys because of their excel- high-temperature strain the loss in low-temperature ductility is 8.5 pct for nickel as compared to 60 pct for pure a, brass. It is also interesting to note the observation that in nickel the low-temperature fractures, even at the most extreme high-temperature pre-strain, were partly trans crystalline and partly intercrystalline. In the case of a brass, these fractures were completely intercrystalline. According to the data on the percent of the grain boundary area that is cracked, at 22 pct high-temperature elongation, about 12.5 pct of the grain boundary area does not carry load. Thus, the inter-crack areas are carrying a stress that is about 11 pct higher than the nominal stress. A simple model predicts that the overall elongation, which is primarily the elongation in the bulk of the specimen, will correspond to the nominal stress when the stress in the intercrack area equals the tensile strength. Quantitatively this model predicts the equation The form of this equation will agree with that found if the strain-hardening exponent, n, equals unity. Actually this model is too gross an approximation to yield good quantitative results. The question naturally arises as to whether in ordinary hot-working, such as hot-rolling, intercrys-talline cracks are introduced that affect the low-temperature properties. It appears that the answer is that such a possibility cannot be overlooked, if the hot-working induces tensile stresses at temperatures above the equicohesive temperature and if the material tends to be notch sensitive at low temperature. ACKNOWLEDGMENT This research was supported by the Aeronautical Research Laboratory, Directorate of Research, Wright Air Development Center, United States Air Force. REFERENCES lC. Zener: Fracturing of Metals, 1948, Cleveland, ASM. 'H. C. Chang and N. J. Grant: Mechanism of Intercrystalline Fracture. AIME Trans., 1956, voL 8, p. 544; lownal of Metals, May, 1956. 'E. S. Machlin. CreepRupt ure by Vacancy Condensation, AIME Trans., 1956, vol. 8, p. 106; lownd of Metals, February, 1956 'C. Chen and E. S. Machlin: On a Mechanism of High-Temper at ure Inter-crystalline Cracking, lownd of Metals, July. 1957. p. 829. Alloys lent oxidation resistance. Binary alloys of aluminum in iron are ferritic and consequently have poor hot strength. Alloys of iron-aluminum-manganese were made in an attempt to produce an austenitic alloy containing sufficient aluminum to retain the oxidation resistance of binary alloys of iron-alumi-

Jan 1, 1960

By R. Webeler

In order to study the role of work hardening in the fatigue process, use was made of the great sensitivty of the resistivity of AuCu to cold work. A change of the resistivity of AuCu of the order of 1 to 2 pct at the temperature of liquid nitrogen was found to occur as a consequence of severe fatigue. ACCORDING to Orowan's theory,' the process of fatigue In metals 1s associated with the production of a number of small regions which have undergone strain hardening. This phenomenon is supposed to occilr even if the stress applied during fatiguing is always smaller than the yield stress. In an attempt to verity the existence of such regions, Welber and Webeler' undertook to detect the stored energy associated with severe fatigue in copper. Previous experiments" had shown that the energy stored in a sample of copper which has been cold worked by torsion is released in the temperature range between 150" and 250°C when the sample is heated from room temperature and that no more energy is released (or absorbed) between 250" and 450°C. In particular the stored energy amounted to 0.41 cal per g for a case in which the mechanical energy expended in twisting the sample was 11.9 cal per g. In the case of fatigued copper, however, no release of stored energy could be detected between 150" and 250°C, so that the experimental error of &0.02 cal per g represents an upper limit for the amount of energy stored in strain hardening., It seemed desirable to attack the problem in a new fashion. For this purpose, it was decided to make use of the fact that, if an alloy capable of undergoing the order-disorder transition is ordered and then cold worked, the resistivity, p, increases very greatly above the value for the ordered state even if the deformation is very small. Some insight into the nature of the fatigue process may be obtained then by measuring the resistivity of an ordered sample before and after subjecting it to fatigue. For reasons which will become apparent from the following remarks, considerably more can be learned by carrying out the resistivity measurements at two different temperatures. In the case of a material containing impurities, vacancies, dislocations, or other imperfections of essentially atomic dimensions, the resistivity, p, according to Matthiessen's rule, can be represented as a sum of two terms p = p, + p, where p, is the (temperature dependent) resistivity of the pure metal, and p, is the temperature independent contribution of the imperfections. Briefly, the physical basis for this rule is the following: The main contribution of the impurities in question to the resistivity results from the fact that they interrupt the periodicity of the lattice and thus scatter the conduction electrons with a probability which is almost independent of temperature. In order that this be the case, it is necessary that the' extension of the impurities be small enough—roughly less than one electron mean free path—so that their main effect on the resistivity occurs for the foregoing reason. If an alloy like AuCu is partly or completely disordered by quenching from an appropriate temperature, Matthiessen's rule also applies to a very good approximation* with p, representing in this case the resistivity po of the ordered sample and p, the additional (temperature independent) resistivity due to the disorder. In general, the disorder can be represented in terms of atoms which are displaced from their "proper" positions in the superlattice and which thus qualitatively represent the imperfections in the superlattice responsible for the term p,. Since the misplaced atoms are distributed at random throughout the super-lattice, their contribution to the resistivity still can be considered in terms of the scattering of conduction electrons by lattice defects. The situation is somewhat more complex in the case of an alloy disordered by cold work because the process of disordering here does not involve a random redistribution of the atoms; however, Matthiessen's rule also holds in this case. Whenever Matthiessen's rule does apply, the values of the quantity /3 = (p? — /(T, — T,), where p, and p, are the values of the resistivity at two fixed temperatures, T, and T,, respectively, is constant (independent of p,) for a given alloy or metal. In particular, if a sample of AuCu is subjected to ordinary cold work, the value of /3 remains equal to Po, the value for the ordered material. According to Orowan's theory,' as remarked before, a fatigued sample contains a large number of isolated severely cold-worked regions, which make up only a small proportion of the metal. Thus, if a sample of AuCu initially in the ordered state is fatigued, more or less disordered regions will be produced within the ordered material. If these regions are small enough so that Matthiessen's rule applies, then it follows from the previous discussion that /3 again will remain equal to Po. If the effect of fatigue is to produce cold-worked regions which are macroscopic—of the order of at least several electron mean free paths—the effective resistivity, p, has to be computed by use of the ordinary laws of large-scale electrodynamics. For the sake of simplicity, it will be assumed here that the cold-worked regions are completely disordered and have a resistivity, p,. For a given proportion A of disordered regions the effective resistivity, p, for the current in a given direction depends on the geometrical configuration of these regions. In any case, the value of p for such

Jan 1, 1956

By R. W. Hertzberg, R. W. Kraft

A study of the fracture behavior of unidirectwn-ally solidified Cu-Cr eutectic alloy was performed. Fractured whiskers, grain boundaries, and the interface between proeutectic Cr dendrites and the Cu matrix were the predominant failure initiation sites where grain size was larger. Strain induced void formation was restricted at lower solidification rates. This was attributed to a lack of adequate plastic constraint and a probable preferred orientation. A modification of the Crussard et al. model is presented to explain the appearance of "elongated dimples" on the shear fracture surface. A Cu-Cr alloy containing about 1.8 at. pct Cr solidifies by a eutectic reaction forming filamentary crystals of chromium within a continuous copper solid solution matrix.' Webb and Forgeng2 have shown by bend tests that the extracted chromium filaments, which are ordinarily curved and branched (due to random solidification), have the high strengths associated with whiskers. If an ingot of the eutectic alloy is unidirectionally solidified and appropriate control exercised over the thermal gradient, growth rate, and impurity level, the chromium fibers can be forced to solidify as fibers which are substantially parallel to the growth direction, Fig. 1. Uniaxial tensile tests on these straight chromium fibers extracted from controlled ingots3 have confirmed the earlier bend test results on curved fibers. Combining the facts that the strength and modulus of the chromium filaments are higher than the more ductile copper matrix and assuming that a "good bond" exists between the two phases, the Cu-Cr controlled eutectic system fulfills the requirements for effective fiber reinforcement of ductile matrices as established by studies on fiber glass reinforced plastics and other two-phase systems.4 Therefore, it was decided to study the fracture characteristics of morphologically simple specimens of chromium fiber reinforced copper (i.e., specimens of the controlled eutectic with substantially parallel reinforcing fibers) with the objective of establishing the dominant aspects of fracture. PREVIOUS WORK Comparatively little work has been done to understand the manner in which ductile alloys fail be- cause of the limited demand for this kind of information. Ordinarily ductility is specified for safety or similar reasons and when a part deforms plastically its useful life is terminated. In recent years, however, a number of investigators have begun to

Jan 1, 1963

By Robert T. Ault

The nature of fracture in unnotched tensile and notched tensile sheet and round specimens and V -notched and precracked Charpy-type sheet specimens of both wrought stress -relieved and re-crystallized molybdenum was investigated over the temperature range of -78° to 300°C. The sharp rise in fracture stress, for unnotched tensile samples, as the temperature is increased above the brittleness transition temperature (Tb), is found to be a result of an increase in flow stress due to plastic constraint and an increased strain rate which results from the onset of necking at Tb . Quasi-brittle fracture in notched tensile samples is found to occur when the tensile stress at the elastic-plastic interface, beneath the root of the notch, reaches a maximum critical value, which is independent of test temperature over the range from —78° to 25°C, but dependent on microstructure. In the temperature range between 150° and 300°C, unnotched tensile and notched tensile samples alike are found to fracture by a ductile fibrous tearing process which is discontinuous in nature, as a result of the competition between the processes of tearing, through continued plastic flow, and local work hardening. Results from the V-notched and fatigue-cracked Charpy-type impact tests demonstrate that crack initiation is the governing factor in the low-temperature (-78° to 25°C) fracture process for molybdenum. In recent years, there has been considerable interest, and a commensurate number of investigations, concerning the duc tile-to-brittle transition in refractory metals. There has not developed, however, a satisfactory explanation for the uniaxial tensile fracture-stress transition which accompanies the well-known ductility transition. This matter therefore warranted investigation. In a similar manner, the increased importance of notched tensile strength values in evaluating materials and in design criteria requires a better understanding of the factors which control the fracture behavior of notched tensile samples. In a previous investigation1 of the nature of initial yielding and fracture in notched sheet molybdenum at room temperature, it was suggested that plastic constraint was the controlling factor in governing the fracture behavior of notched samples. The final portion of this investigation was concerned with the fracture toughness of molybdenum. Of particular interest was the comparison of effective surface energies for fracture in V-notched samples with fatigue-cracked, Charpy-type samples in order to ascertain the relative importance of the initiation and propagation phases of the fracture process. MATERIALS AND TEST PROCEDURE Sheet tensile, notched tensile, and V-notched Charpy specimens were prepared from 50-mil, stress-relieved molybdenum sheet.* Half of these specimens were vacuum-annealed for 1 hr at 1200°C and 7.5 x l0-5 Torr and furnace-cooled to produce a relatively uniform grain size of 0.30 mm diameter. Round notched and unnotched tensile specimens were prepared from warm-rolled and swaged 5/8-in.-diam bar.* These specimens were vacuum-annealed for 1 hr at 1350°C and 5 x lom5 Torr and furnace-cooled to produce a grain diameter of 0.11 mm. Material analyses in ppm were: C N O H Sheet 290 10 4 1 Bar 50 30 30 2 The unnotched tensile sheet specimens had a 1/4-in. gage width and a 1-in. gage length. The unnotched tensile round specimens had a 9/32-in. gage diameter and a 1-1/4-in. gage length. The sheet and round notch tensile specimens are shown in Fig. 1. All of the notched tensile specimens tested were tandem-notched in order to study the location and mode of fracture initiation. The tandem-notched specimens were carefully machined so that the largest variation in notch depth on a single specimen was 0.001 in. Thus, when fracture occurs, the extent of plastic deformation that exists in the un-fractured notch section is that which exists just prior to fracture. All of the tandem-notched sheet specimens were electrolytic ally polished and chemically etched prior to testing. The V-notched Charpy-type specimens machined from the 50-mil sheet material had the standard dimensions of 2.125 in. long, 0.394 in. deep, and a 0.010-in. root radius. The unnotched tensile and notched tensile tests were conducted over the temperature range of -78° to 300°C, in a 10,000-lb Instron Universal Testing Machine, at a constant crosshead speed of 0.020 in. per min. The V-notched Charpy-type

Jan 1, 1964

By G. Horvay, J. G. Henzel

Nomograms and charts are provided which permit rapid determination of the mold-casting interFace temperature and the speed of solidification when a semiinfinite ingot is cast into a semiinfinite mold. The physical properties of the mold, the frozen metal, and the liquid metal are not assumed to be equal, but they are assumed to be temperature independent. The results are correlated with charts prepared by Paschkis and Hlinka—using Columbia University's Analog Computer—for the freezing of finite ingot slabs when a constant surface temperature is impressed, and with experimental cooling curves obtained by Pellini in sand and iron molds for 7 in.-sq steel castings. x = coordinate directed to right of zero (freezing direction) y = coordinate directed to left of zero (melting direction) e = position of freezing front (in x direction) ? = position of melting front (in y direction) $ = temperature (function of position and time) ? = fixed temperature 2L = width of finite slab Y = a fixed position in the semiinfinite mold, or the width of a finite mold (see Section 7) Properties y = density, lb per cu ft c = specific heat, Btu per lb deg F k = conductivity, Btu per ft hr deg F X = heat of fusion, Btu per lb k = k/Yc = temperature diffusivity, sq ft per hr* b - = = - heat diffusivity, Btu per sq ft deg F Vhr Subscripts 2 = pertaining to the still-liquid metal (case of freezing), or the medium which furnishes the heat (case of melting) 1 = pertaining to solidified metal (case of freezing), or to molten metal (case of melting)* 0 = pertaining to mold (case of freezing), or to the still-solid metal (case of melting) f = pertaining to fusion condition (eg.,?f - fusion temperature) i = pertaining to the location x = 0 (the mold-ingot "interface")

Jan 1, 1960

By R. H. Tien

Temperature distribution as well as position of the solidified front is solved by means of "heat balance integral", for the case of freezing a slab with time-dependent surface temperature. Numerical solutions for the cases of linear variation and exponential decay for surface temperature are given. Application also includes solidification of casting. An increased interest in the heat-transfer problem involving a change of phase has been developed in recent years. Practical problems include solidification of a casting, freezing and thawing of soil, ice formation, and others. Despite the importance of the topic, a literature search reveals relatively few solutions which may be extended to practical problems. Due to mathematical complexity, which comes from the nonlinearity of governing differential equations, exact analytical solutions which have been published are limited to a few cases with simple boundary conditions. Although numerical solutions of these problems have become available after highspeed digital computers were introduced, lack of simple and general methods of programming for computation makes this approach impractical. The case of the semi-infinite slab with constant surface temperature was solved in the 19th century. In honor of Neumann, who first found an analytical solution, this kind of problem is generally referred to as the Neumann solution. As has been shown in Fig. 1, the problem to be analyzed is the freezing of a semi-infinite region (x > 0) which is initially liquid at the melting temperature with the surface (x = 0) maintained at time-dependent temperature. This analysis can be applied to the study of many casting processes where most of the heat removal is essentially unidirectional. "Heat balance integral" which has been used by Goodman1 is employed in this analysis. The concept of "heat balance integral" is to define a quantity, d(t), called the thermal layer. Beyond this thermal layer, for all practical purposes, there is no heat transfer, and the region is at the equilibrium temperature. "Heat balance integral" is obtained by integrating the conduction equation with respect to the space variable over this thermal layer d(t). Choosing some plausible temperature distribution, usually a polynomial or a finite trigonometric series in the space variable, this integral equation becomes an ordinary differential equation, with time as the independent variable, which can be solved by classical methods. The thermal layer and "heat balance integral" are equivalent, respectively, to the boundary-layer thickness and the momentum integral in hydrodynamics. A modern account of Prandtl's concept of the boundary layer and von Karman's momentum integral may be found in Ref. 2. Although the problem considered here has been limited initially to uniform melting temperature, the present method is equally applicable to the case with arbitrary temperature distribution in the liquid. STATEMENT OF THE PROBLEM The physical situation and coordinate system used in the problem to be analyzed are shown in Fig. 1. Notations used are listed in the table of nomenclature. Let us assume a semi-infinite region extending over positive x, initially at the uniform melting temperature. At the surface x = 0, a time-dependent temperature, which has a numerical value

Jan 1, 1965

By J. J. Hauser, H. C. Theuerer

A cathode sputtering technique is described which elin7inates the need for ultrahigh vacuum in preparing thin films of materials sensitive to gaseous impurities. This technique uses a fraction of the atoms sputtering within an anode container to getter actice gases, such as HzO, Oz, and Nz. The gases alzd gettering metal are deposited on the container walls, thus shielding the coating zone of the system from contamination. The use of the method for preparing superconducting-normal metal couples such as Ph-Cu and Ph-Pt is described, and the properties of the individual and composite films are given and discussed. GETTER sputtering is a method which greatly simplifies the preparation of thin films in cases where composition control is critical. A major difficulty with conventional sputtering and other vacuum-deposition techniques is the contamination of the forming film caused by residual gases, such as H20, CO, Oz, and Nz, in the coating equipment. The difficulty arises from the fact that even when the residual pressure in the system is as low as 1 x 10"6 Torr, with a deposition rate of 10A per sec, there are as many contaminating gas collisions with the substrate as there are with film-forming metallic atoms. It is not surprising, therefore, that with reactive metals, such as tantalum and niobium or with semiconductors, such as silicon and germanium, films with properties far different from the starting materials are obtained. In the case of niobium and tantalum, deposited either by sputtering or vacuum evaporation in systems with reactive gases at pressures of the order of 1 x l0-' Torr, the loss of superconductivity is traceable to interstial oxygen or nitrogen. On the other hand, working in vacuum of the order of 1 x l0-" Torr, Marchand and enema' have shown that superconducting films of tantalum with properties approaching those of bulk material are possible. At this level of gaseous impurities -lo6 metallic atoms arrive at the substrate before a contaminating collision occurs again assuming a deposition rate of 10A per sec. It is evident from the above that any successful vacuum technique requires the elimination of reactive gases from the region of the system where coating is occurring. Getter sputtering accomplishes this using conventional vacuum equipment with residual pressures in the 106 Torr range. In fact? vacuum systems with residual pressures of lo-" Torr are adequate for most purposes. With this method, sputtering is confined within an anode can and, by geometric design, sputtering itself is used to purify the argon at the lower and upper parts of the system by the gettering action of the reactive metal. In consequence, the central region of the system where coating occurs is shielded from gaseous contamination. Getter sputtering is particularly useful for the preparation of alloy and compound films. With this method, if a cathode of homogeneous composition is bombarded with high-energy argon ions, transfer of material to the substrate having the same composition as the cathode will occur. This is true after an initial equilibration time, even though the constituents of the cathode may have different sputtering rates. During equilibration, the surface of the cathode changes composition due to differences in sputtering rate, but mass conservation demands a steady-state condition such that the atoms sputtered from the surface have the same composition as the cathode material from which the surface is generated. GETTER-SPUTTERING APPARATUS The original form2 of the getter-sputtering apparatus is shown in Fig. 1. It consists of a closed nickel or stainless-steel can 4 in. tall and 2-3/8 in. in diameter. Mounted symmetrically from each end

Jan 1, 1965

By P. E. Rider, K. A. Gschneidner, O. D. McMasters

The solid solubilities for thirteen rare-earth metals in gold were determined by using the X-ray parametric method. Solubilities ranged from 0.1 at. pct for lanthanum in gold up to 8.8 at. pct for scandium in gold. The solubilities from lanthanum to gadolinium were very small and essentially constant, but a sharp increase occurred from gadolinium to scandium. The large solubilities for the heavy rare-earth metals were not expected because of the large size and electrochemical differences between rare-earth atoms and the gold atom. Contributions from first- and second-order elasticity theory plus an electronic contribution were found to reasonably account for a more favorable size factor. Electron transfer from the rare-earth metal to the gold Is thought to occur such that the resultant rare-earth and gold electronegativities are favorable for solid-solution formation. It was also found that this mutual adjustment of size and electronegutivity does not occur if the pure-metal size factors are greater than a critical value of 25 pet. The eutectic temperatures for ten systems were determined and these remained fairly constant at approximately 809 "C for the lighter lanthanide metal-gold systems until the Er-Au system was reached, at which Point the eutectic temperature successively increased reaching a maximum of 1040°C in the Sc-Au system. This rise was correlated to the size factor becoming more favorable for solid-solution formation at erbium. The valence state of ytterbium was found to change from two in the pure metal to three when ytterbium is dissolved in the gold matrix. RECENT results1 reported concerning the solubility of holmium in copper, silver, and gold, showed that the solubility of holmium in gold was quite large, 4.0 at. pct, compared with 1.6 in silver and 0.02 in copper. The small solubilities of holmium in silver and copper are quite reasonable in view of the large size difference (22.2 and 38.2 pct, respectively), large electronegativity difference (0.59 for both systems), and possible unfavorable valency factor (assuming one for silver and copper and three for holmium). The large solubility in gold, however, is unexpected because these same factors are also unfavorable for holmium and gold (22.5 pct size difference and 0.69 electronegativity difference), and because the light rare-earth metals, lanthanum, cerium, and praseodymium, have negligible solid solubilities in gold.2 In view of this unexpected behavior, it was felt that a study of the solid solubilities of most of the rare-earth metals in gold would be desirable to better understand the factors involved in the formation of solid solutions. Of the rare-earth metals added to gold in this study, only ytterbium is divalent in the pure metallic state (the other rare-earth metals are all trivalent) and many of its physical properties (such as the metallic radius, electronegativity, and so forth) are much different from those of the normal trivalent rare-earth metals.' The properties of ytterbium are such that one would expect solid-solution formation to be less favorable for ytterbium in gold than for any of the normal trivalent rare-earth metals. But chemically ytterbium is known to possess a stable trivalent state, and it is quite possible that ytterbium may alloy as a trivalent metal under certain conditions rather than as a divalent metal. Because of the dual valency nature and because so little is known about the alloying behavior of ytterbium, the gold-rich ytterbium-gold alloys are of special interest. EXPERIMENTAL PROCEDURE Materials. The gold used in this investigation had a purity of 99.99 pct with respect to nongaseous impurities. In general the rare-earth metals were prepared by reduction of the corresponding fluoride by calcium metal.3 The impurity contents of the metals used in this study are given in Table I. Preparation of Alloys. Two- or 3-g alloy samples were prepared by arc melting. The samples, with the exception of some of the Er-Au alloys, had weight losses of 0.5 pct or less. All alloy concentrations noted in this paper are nominal compositions. After arc melting, the alloys were wrapped in tantalum foil, sealed off in quartz tubing under a partial atmosphere of argon, homogenized for approximately 200 hr at 780°C, and then quenched in cold water. X-Ray Methods. The X-ray parametric method was used in determining the solubility of the rare-earth metals in gold. filings were sealed in small tantalum tubes by welding under a helium atmosphere. The tantalum tubes were then sealed in quartz tubing under a partial argon atmosphere, and annealed for times ranging from 1/2 to 3 hr (the length of time was inversely proportional to the an-

Jan 1, 1965

By E. C. W. Perryman

The wide grooves formed at the grain boundaries when high purity aluminum is attacked by hydrochloric acid or sodium hydroxide have been attributed by earlier workers to the high energy of the grain boundary material. The effect has been investigated for high-purity AI-Fe alloys with up to 0.055 pct Fe as a function of iron content and heat treatment. It is shown that the explanation given above is untenable, but that the results can be explained on the assumption that iron segregates to the grain boundary in solid solution. IN 1934, Rohrmann¹ showed that aluminum of 99.95 pct purity suffered intercrystalline corrosion when immersed in 10 to 20 pct hydrochloric acid, and that the susceptibility to intercrystalline corrosion depended upon the heat treatment given. The greatest susceptibility was found for specimens quenched from a high temperature (600°C) and the lowest susceptibility for specimens cooled slowly from that temperature. Lacombe and Yannaquis2 have shown that super-pure aluminum (99.9986 pct) annealed at 600°C suffers intercrystalline attack in 10 pct hydrochloric acid and that this attack is intensified by anodic dissolution in the same solution at a current density of 10 milliamperes per sq dm. No difference in extent of intercrystalline attack was found between the 99.993 and 99.986 pct Al, which led the authors to suggest that impurities played only a secondary role in the mechanism of intercrystalline corrosion. It was found, however, that the attack at the grain boundaries depended upon the relative orientation of the grains, large differences in orientation favoring rapid attack. Boundaries where the two neighboring grains were similarly orientated showed high resistance to attack as did boundaries between grains which were in twin relationship. These observations led Lacombe and Yannaquis to suggest that the intercrystalline attack was due to lattice discontinuities present at grain boundaries. Assuming that the grain boundary is a layer three to five atoms thick and has a crystal structure which is a compromise between the two neighboring grains it is clear that the discontinuities will increase with increasing difference in orientation between the neighboring grains and hence the increasing tendency to intercrystalline attack. Roald and Streicher³ investigated the effect of heat treatment of aluminum alloys ranging in purity from 99.2 to 99.998 pct on the corrosion resistance in 20 pct hydrochloric acid and 0.30N sodium hydroxide. They found that in hydrochloric acid the intercrystalline attack appeared to be determined by the type and quantity of impurities present and by the relative orientation of the grains. No difference in the susceptibility to intercrystalline attack was observed between specimens quenched and those furnace cooled, from 575°C. In 0.30N sodium hydroxide some materials exhibited intercrystalline attack, this taking the form of V-notches. Rohrmann¹ offered no explanation for the greater susceptibility to corrosion of material quenched from 600°C. It seems possible that this difference is connected in some way with a different distribution of impurity elements in the quenched and slowly cooled specimens. The fact that Roald and Streicher8 observed no difference between quenched and slowly cooled specimens may possibly be due to differences in either rate of cooling or silicon content or possibly both. Both these would be expected to have an effect on the distribution of impurity elements. Although the rate of cooling used by Rohrmann was slightly more rapid than that used by Roald and Streicher the position cannot be clarified because Rohrmann does not give the silicon content and Roald and Streicher give the silicon contents of only a few of their alloys. That Lacombe and Yannaquis2 found no difference in corrosion behavior attributable to impurities between the two materials they used may be because both were of high purity compared with the aluminum used by Rohrmann.¹ Although they found no difference in the corrosion behavior of their two materials it is possible that the results obtained by Lacombe and Yannaquis may, nevertheless, have been influenced by impurity distribution, since, on the transition lattice theory of grain boundary structure, it would be expected that sparingly soluble impurities would tend to segregate to boundaries where the orientation difference is such that there is a greater density of atomic sites of suitable size to contain them. It was considered worth while, therefore, to examine the corrosion properties of a series of materials of differing impurity content with the objects of confirming the experimental observations made

Jan 1, 1954

By C. S. Roberts, S. L. Couling

PLASTIC strain in polycrystalline metal as a result of bulk movement of one grain with respect to another along grain boundaries is not new. Rosenhain and Humphrey observed such effects shortly after the turn of the century.' Since then, observations of grain boundary deformation have been made on several metals. In recent years, intensive studies of the deformation at grain boundaries have been performed on polycrystalline metal and bicrystals.14-20 Aluminum or its alloys have been used in these latter studies. The subjects of controversy at present appear to be not whether grain boundary deformation exists, but 1) how quantitatively important it can be in polycrystalline metal, and 2) what its detailed mechanism is. Some investigators have concluded that such de- formation is minor in importance while others have concluded that it is a major consideration. Some have concluded that it involves shear of one grain over another at the interface while others have concluded that it operates by crystallographic deformation within the grains near ,the boundary. A categorical statement for electrolytic magnesium cannot be made on either of -these points. When polycrystalline magnesium is deformed in creep under conditions of high strain rate and low temperature, grain boundary deformation is relatively slight." Under these conditions, much deformation occurs within the grains and boundary contours change to a higher-energy jagged form. The result is shown in Fig. 1, where boundary jaggedness is pronounced upon polishing and etching after a plastic strain of approximately 6 .pct at 300°F and 3000 psi. No migration of the boundaries has been detected in this process. When the same metal is deformed the same amount at 600°F and 300 psi, resulting in a much lower strain rate, the boundaries migrate toward a lower energy configuration, where

Jan 1, 1958

By Che, C. W. Spencer, C. A. Steidel, Yu Li

Grain boundary grooving as it occurs in a 5.5-deg simple-tilt nickel bicrystal immersed in a saturated Ni-S liquid has been studied. A 1/3 (t= time) dependence for the depth of the groove indicates that the rate -controlling meckanism for groove developvnent is volume diffusion in the liquid. The activation energy for the diffusive process is estimated at 15 kcal per mole. Using an extended form of W. W. Mullins&apos; analysis for grooving reactions, a computer is employed to fit the appropriate diffusion equation by a numerical method. From the analysis a possible method of measuring L.S. the solid-liquid interfacial tension is demonstrated. WHEN a polycrystalline solid is heated in equilibrium with a saturated fluid phase, grooves will form at the intersections of the grain boundaries and surface. The equilibrium root angle of these grooves is determined by the balance between the grain boundary and solid-fluid interfacial tensions. The grooves deepen and widen with time due to a difference in chemical potential between the flat interface and the curved interface of the groove. In this investigation solid-liquid interaction at a grain boundary is studied, with the object to determine the mechanism of grain boundary grooving in the presence of a saturated liquid. Extension of Mullin analysis then permits the estimation of the solid-liquid interfacial tension. Herring has demonstrated by dimensional analysis that the quasi-steady state change of the dimensions of a small particle during sintering is proportional flow, evaporation-condensation, volume-diffusion, and surface-diffusion mechanisms, respectively, if geometric similarity of consecutive configurations of the particles holds. Mullins has extended this analysis to grain boundary grooving. In the case of shallow grooves he solves the diffusion equations for evaporation-condensation, volume-diffusion, and surface-diffusion mechanisms, and obtains the same time dependence for any linear dimension of a groove as Herring found for the change in dimension of small particles. In Mullins&apos; analysis2&apos;3 grain boundary grooving of a bicrystal by volume diffusion in the presence of a saturated fluid phase was considered. Several assumptions were made prior to the analysis: 1) the solid-fluid interfacial tension is independent of crystallographic orientation; 2) the Gibbs-Thompson equation relating curvature and chemical potential is applicable at the solid-fluid interface; 3) the relaxation time of the diffusion field is small compared with the time for appreciable changes in the curvature of the groove, so that the diffusion is divergence-less; and 4) the groove has a small slope relative to the initial flat interface. Usually this last condition is fulfilled only for solid-gas systems. The solution of the diffusion equation under the above conditions produces a t1/3 dependence for any linear dimension of the groove in the case where volume diffusion is rate-controlling. The t1/3 dependence is valid because geometric similarity of the grooves exists for all time. EXPERIMENT In the experiment a 5.5-deg nickel bicrystal of <100> simple-tilt orientation was used.4 Grooving was studied in the presence of a saturated Ni-S liquid alloy as a function of time at 750°, 800°, 850°, and 900°C. A low-angle bicrystal was chosen for study to insure that 2L.S. > .b., where l.s.

Jan 1, 1964

By Nicholas J. Grant, A. W. Mullendore

Measurements of grain boundary sliding were made on polycrystal and bicrystal tensile creep specimens of Al-2 pct Mg at 500oand 700oF. Grain and pain boundary orientation factors were studied with respect to their effect on the magnitude and direction of grain boundary sliding. It was concluded that a large part of the observed sliding may be caused by the operation of slip crossing the grain boundaries. Supporting evidence for this model from other investigations is also given. GRAIN boundary sliding in metals during elevated temperature deformation has frequently been thought of as an independent mechanism with its own characteristic stress, temperature, and structure dependence. Further, it is common to regard the grain boundary as the weak link during creep deformation since: 1) the strength of apolycrystallinemetal, as meas-sured by creep rate or rupture life, decreases at\a more rapid rate when sliding comes into action, and 2) grain boundary sliding, as revealed by "boundary darkening" and fold formation is often the first visible deformation. On the other hand, more quantitative observations, in both polycrystals and bicrystals, have shown boundary deformation to be closely related to the over-all deformation of the specimen. The curve of grain boundary contribution to elongation vs time takes a shape similar to that of the total creep curve,&apos;,&apos; and the apparent activation energy for sliding appears in most cases to have the same value as that for total creep.3 In order to reconcile these observations, one is left with these possibilities: 1) The grain boundary and grain deformation rates are both controlled by the same rate limiting processes. 2) The rate of sliding is limited by accommodation deformation in the grains. 3) Sliding is the consequence of grain deformation. 4) Grain deformation is dependent on prior grain boundary deformation. Alternatives 2) and 3) would view grain boundary sliding as occurring in series with another deformation process which could be rate controlling. McLean prefers item 3) as the sliding basis,4 where subgrain rotation results from dislocation accumulation in the substructure at the grain boundary. Crussard and Friedel&apos;s5 treatment of grain boundary migration considers that dislocations are forced into the grain boundary and are dissociated into dislocations with Burgers&apos; vectors nearly parallel to the grain boundary. The movement of these partial grain boundary dislocations then produces the sliding. The results of this investigation have indicated alternative 3) to be the most appropriate and it is this aspect of grain boundary sliding which will be analyzed. EXPERIMENTAL PROCEDURE Three types of tensile creep tests were employed in this study: (I) A constant load test of one very coarsegrained polycrystalline specimen at 500° F, 3600 psi, 1 pct per/hr strain rate to examine the grain and grain boundary orientation factors in grain boundary sliding. (II) Constant strain rate tests of polycrystalline specimens at 510o and 715o F, 2 pct per/hr strain rate to determine the grain boundary contribution to elongation at very low total strains. (m) Constant strain rate tests of bicrystals of various grain and grain boundary orientations at 500°F, 2 pct per/hr strain rate to obtain further information on the orientation effects in grain boundary sliding. The material used in the tests was a high-purity Al-1&apos;.92 mg alloy, kindly furnished by Alcoa. Its composition is given in Table I. The alloy is a solid solution at the test temperatures. The coarse grained polycrystalline specimen for test (I) was prepared by recrystallizingthe machined specimen, straining it about 1pct intension at room temperature and annealing at 900°F for 8hr. The constant strain rate specimens (11), with an 178 in. sq. by 1/2 in. long gage section, were cut from 1/8 in. thick sheet of cold rolled and annealed (8 hr at 1000oF) material. The latter specimens were supported in a special jig during the milling operations to avoid any bending, and the gage section was subsequently heavily electropolished to remove the cold-worked surface layer. The bicrystals (ID) were machined in the same

Jan 1, 1963

By Leonard Bernstein, Harry Bartholomew

MANY of the properties of metals and alloys are structure dependent. Not the least of these is the grain structure. For example, in producing alloy bonds between silicon or germanium and gold-alloy foil at temperatures above their eutectics (which are, respectively, at 370" and 356°C) but below the melting points of the individual constituents, it was found that wetting was more complete with a fine-grain structure than with a coarse-grain structure. In cases where the assemblies were held together for long periods of time at elevated temperatures, wetting was not as critically dependent on the grain structure as was the case for shorter periods of time. When liquid phase forms, it first forms in the grain boundaries due to the fact that most of the impurities are concentrated at the grain boundaries and that most impurities tend to lower the melting point of the gold alloy somewhat. In addition, grain boundaries are at high-surface free-energy levels and are thus in a more favorable condition to initiate good wetting. A fine-grain structure will have more grain boundaries per unit area than coarse-grain structure thereby making wetting somewhat easier. To make the grain structure of an alloy sys- tem visible, a satisfactory method for differentiating between the different grains of which the system is composed must be employed. For the alloy bonding system previously described, the grain structure on the foil surface is of primary interest. Conventionally used etchants for the gold-alloy system will not adequately delineate grain boundaries in their structures. For this reason an alternate method is proposed for those cases where such a determination is necessary. Foil between 0.0005 and 0.005 in. thick has been used in this determination. The equipment used in this investigation was described in a previous publication.&apos; Essentially, it employs a resistance-type filament which can be heated up very rapidly and cooled very rapidly. A thin refractory material is placed on top of the heating element. This refractory material may be molybdenum, tantalum, tungsten, or even ceramic but its thickness should be less than 0.010 in. to minimize the temperature gradient across it. The gold-alloy foil is placed on top of this refractory material. The temperature of the heating filament is raised to 900°C and cooled down to below 100°C in 5 to 10 sec. During this cycle, the foil can be observed to plastically deform due to its own weight. With no further chemical etching, this assembly is then viewed under a standard metallurgical microscope and the grain size measured. Fig. 1 is a Au-1 pct Sb alloy at 400X magnification and Fig. 2 is a Au-1 pct Ga alloy at 130X. This technique has proved to be an adequate means for controlling processing conditions in producing large quantities of gold alloy foil.

Jan 1, 1963

By C. W. Spencer, J. T. Smith

GRAIN-BOUNDARY surfaces are penetrated by a liquid phase when the liquid-solid interfacial tension is less than one-half the tension of the grain-boundary surfaces. Grain growth may occur in the presence of this liquid phase. burke1 reports that grain growth of this nature has been observed in two-phase ceramic systems. He suggests that the presence of a grain-boundary liquid may accelerate or decelerate the

Jan 1, 1963

By R. W. Cahn, C. D. Graham

Two predictions of the oriented growth theory of recrystallization textures have been tested by measuring the orientation dependence of the rate of growth of a single grain into a strained single crystal of aluminum, and determining the orientations of artificially and spontaneously nucleated grains growing preferentially into strained aluminum single crystals. Growth rates are found to be insensitive to orientation, except that new grains with orientations similar to the matrix or to a twin of the matrix have very low mobilities. Similarly, new grains growing preferentially into a strained crystal have random orientations, except that orientations near that of the matrix or its twins are avoided. The predictions of oriented growth theory are thus not confirmed. BASICALLY, the oriented growth theory of re-crystallization textures1 rests on the assumption that the rate of growth of a recrystallizing grain depends strongly on the orientation of the growing grain relative to the strained matrix into which it grows. In particular, the theory holds that in face-centered-cubic metals the orientation which corresponds to maximum growth rate is one in which the growing grain and the matrix are related by a rotation about a common <111> direction. The amount of rotation, as derived from several kinds of experiments,2-1 has been assigned various values, generally in the range between 20" and 40". (A <111> rotation of 60" is a twin relationship.) The conclusion that boundary migration rates depend strongly on orientation is based almost entirely on indirect evidence; there have been very few direct measurements of boundary migration rates as a function of orientation.* " The present investigation was undertaken to provide such measurements, to help make possible a decision between the oriented growth and oriented nilcleation theories of recrystal-lization textures. The basic experimental program consisted of measuring the rate of growth of a single recrystal-lizing grain consuming a strained single crystal, with the orientations of both grains preselected so that the effect of orientation on growth rate could be determined. A prerequisite for such an experiment is a strained single crystal which will support the growth of a new grain but which will not spontaneously nucleate new grains on heating. That is, the crystal must support the growth of a grain nucleated artificially, but contain no recrystalliza-tion nuclei which will become active at the testing temperature. Beck was apparently the first to note that such a condition could exist," and to make use of the condition for am experiment of the type described here.&apos; The present work was actually suggested, however, by a report of Tiedema". " that an aluminum single crystal strip, oriented with a (111) plane in the plane of the strip and a < 112> direction parallel to the tensile axis, would not recrystallize after 20 pet extension even when heated almost to the melting point, provided that the strip was heavily etched before being heated. This result could not be duplicated in the present work. In fact, it was found that any crystal which deformed in multiple slip (<100>, <112> and <111> orientations) underwent spontaneous nucleation after 15 pet extension, even if etched. However, crystals which deformed in single slip, and which did not develop heavy deformation bands, could be extended 15 pet without showing spontaneous nucleation at temperatures up to 600°C. Crystals oriented within about 10o of <110> which developed heavy deformation bands could be extended 10 pet without showing spontaneous nucleation. In all cases a heavy etch was required to prevent nucleation. Etching was necessary because of the presence of an oxide layer on the crystal surface at the time of straining, which leads to preferential nucleation at the surface.&apos;&apos; Grain Growth Rates Experimental Procedure and Results—Aluminum strips of 99.6 pet purity (principal impurities 0.19 pet Fe and 0.12 pet Si), 1 mm by 1 cm in cross section, were grown into single crystals of controlled orientation by the strain-anneal method of Fuji-wara.&apos;"&apos; " A sharp temperature gradient was maintained in the strips during growth by lowering them into a salt bath controlled at 650°C. Crystal orientations were determined by the etch-pit method of Barrett and Levenson" to an accuracy of ±2O. The crystals were extended by 10 or 15 pet in a simple hand operated tensile machine. Crystal orientations were rechecked after extension, and were found to be in agreement with the orientations predicted by the formula of Schmid and Boas." After extension, the grip ends of the single crystal specimen were cut off with a jeweller&apos;s saw, and the crystal heavily etched (at least 20 pet wt loss) in hot 10 pet Na or KOH solution. A region of severe local deformation was then introduced at one corner of the strip, usually by cutting off the corner with shears. Heating this end of the strip caused a large number of new grains to nucleate at the sheared edge. One of these grains grew to occupy the full width of the strip. The appearance of the strip at

Jan 1, 1957