Search Documents

By L. K. Jetter, C. J. McHargue

The use of axis charts for representing the texture of cold-rolled thorium sheet was compared with conventional pole figures. Four texture components were deduced from the axis charts and shown to be consistent with the pole figures. It was shown that consideration of the pole figures alone could lead to an apparent component which is the average of two actually present. It was also shown that the spread about the "ideal" textures and the amount of material associated with each could be readily obtained Fom the axis chart method. BECAUSE of the crystallographic nature of the deformation mechanisms in metals, plastic flow results in the alignment of certain crystallographic directions with the primary flow directions. In the study of the "preferred orientation" thus developed, one wishes to discern the distribution of the crystallographic directions with respect to some reference direction, usually a direction related to the fabrication procedure, such as the rolling direction. The pole-figure method, introduced by ever,' involves the plotting of the distribution of the poles of some family of planes on a stereographic projection which places the reference direction(s) at the north pole and/or in the center. By noting the angles between the reference directions and concentrations of poles on several such pole figures, one can deduce the crystallographic directions which are aligned with the reference directions. If the preferred orientation is relatively simple and well-developed, one to three pole figures may be sufficient for obtaining the desired information; if there are several texture components, more pole figures may be needed. A significant improvement in the method of representing the textures in wires and rods resulted from the introduction of the "inverse pole figure" or axis-distribution chart by Harris.2 Such a chart gives directly the distribution of the reference axis relative to the standard stereographic projection. There has been widespread acceptance of this method for the representation of fiber textures, and methods have been proposed for converting observed diffraction intensities into axis densities.2-6 The suggestion by Mitchell and Rowland3 and Jetter, McHargue, and williams5 that sheet textures could be represented as distributions of rolling, normal, and transverse directions have been criticized on the basis that they offer no significant advantage over a combination of two ordinary pole figures and that it has not been proved that sheet textures can be treated as quasi fiber textures.6 If the purpose of a texture determination is to study some property which is related to the orientation of a particular crystallographic plane or direction, then conventional pole figures certainly are sufficient. For example, the distribution of the slip planes in face-centered cubic metals (the (111) pole figure) serves to indicate the variation in mechanical properties of sheet. On the other hand if the study is directed at an understanding of the factors influencing texture formation, it is desirable to know not only the preferred orientation but the kind and degree of spread from it and the relative amounts of material in each component, if there are more than one. Axis charts give this information as well as the orientation distributions. Consider the procedure for deducing a texture component from a pole figure for the (111) planes

Jan 1, 1961

By C. C. Herrick

The vapor pressure of indium has been measured by the torque-effusion technique, as a function of temperature between 1102o and 1422oK. For liquid indium, the vapor pressure (in atmospheres) can be represented by the equation -R In P = 5.782 x104/T - 25.29from 1000o to 1422oK. Extrapolation yields a calculated normal boiling point of 2329°K and a heat of vaporization at 298 oK of 58.09 kcal per mole by the third-law method and of 58.39 kcal per mole by the second-law method. Calculations indicate that the free-energy functions of Hultgren are to be preferred to those of Guruich. BECAUSE of the potential uses of liquid metals, it is important that convenient experimental methods be developed which will lead to a sufficient body of thermodynamic data so that reasonable estimates of properties of liquid metals can be made. Indium is particularly well-suited to investigation, since it remains liquid over a long temperature interval, it alloys readily, suitable containers for it are easily procured, and relatively few investigations of its thermodynamic properties in the region above 1000°K have been made. PREVIOUS RESEARCH The first determination of the vapor pressure of indium was made by Anderson,' using the Knudsen method and silica-lines stainless-steel cells. Kohlmeyer and spandau2 determined the normal boiling point, and a mass-spectroscopic investigation has been made by Lyubimov and Lyubitov.3 (Unfortunately, only an equation representing the data of the latter investigators has been available to us.) Hultgren et al.4 and Gurvich5 have published discordant tables of the free-energy functions for indium. EXPERIMENTAL METHOD The torsion-effusion principle has been described amply in the literature.8,7 With this method, one observes the angular deflection induced by effusion of vapor from a multihole effusion cell which is suspended from a filament producing a small rotational restoring force. The pressure within the effusion cell can be computed from the relation ziaifiai where k is the torsion constant of the filament, 6 is the observed angular deflection, and ai, fi, and qi are the area, force factor, and moment arm of the ith effusion orifice. The force factor f is analogous to the Clausing factor,' and corrects for the reduction in effusive force attributable to the finite geometry of the effusion orifice. Schultz and Searcy' have tabulated the force factors for various tube geometries. EXPERIMENTAL APPARATUS The physical arrangement employed in this study is shown in Fig. 1. The furnace elements are six Globar heat rods with 15-in. hot zones. Temperature is maintained to * 1°K by a Beck mechanism driving two 26-amp Powerstats in parallel. A Pt (Pt, Rh 10 pct) thermocouple serves as the sensing element. Four inner tubes act as vibration isolators; the air pressure required for maximum isolation was determined empirically, and is maintained by a solenoid valve. The tungsten fiber, 9 by 0.002 in., is joined to an 0.008-in. tungsten wire or graphite rod via a machined lightweight chuck.

Jan 1, 1964

By Gilbert Santoro

In this study tantalum carbide filaments of various compositions in the fcc region were prepared by heating a tantalum wire in a measured amount of hydrocarbon vapor. Such properties as tensile strength, transverse-rupture strength, microhard-ness, lattice parameter, electrical resistivity, and magnetic susceptibility were measured as a function of carbon content. Some of these properties showed a maximum or a minimum between a carbon-to-tantalum molar ratio of 0.80 and 0.85, the composition range at which the color changes from metallic gray to gold. The recent literature has shown that in the large homogeneity range for the fcc phase of the Ta-C system there is a marked variation for such properties as microhardness,' electrical resistivity, ' thermodynamic properties,z'3 lattice parameter and superconductivity. In addition to the technological interest of these variations within a single phase, important theoretical benefits may ensue from a continuous investigation of properties vs stoichiometry in tantalum carbide and other refractory defect compounds, for example the effect of the metal-metal distance and crystal structure upon bond formation and electronic structure. Whether there is a similar variation of the tensile strength is of practical importance. Of theoretical interest would be the knowledge of how the magnetic susceptibility varies with carbon composition. Both of these properties, as well as the transverse-rupture strength, were determined for tantalum carbide filaments in the fcc phase region. The lattice parameter, the electrical resistivity, and the microhardness were also investigated and compared with values appearing in the literature. EXPERIMENTAL PROCEDURE Material Preparation. Tantalum carbide specimens of various carbon content were prepared by statically carburizing high-purity tantalum filaments in measured quantities of pure hydrocarbon gas. The filaments, which were 10 mil in diameter and 20 or 40 cm long, were heated by their own resistance at temperatures from 1800" to 2200°C using alternating current in some cases and direct current in others. Tantalum wire from two sources was used. One had a reported purity of 99.96 wt pct Ta. The ingot from which this wire was drawn had been electron beam-melted as the final step in its purification. The reported purity of the other wire, which was prepared by a powder metallurgical process, was 99.88 wt pct Ta. The impurities of both tantalum sources are listed in Table I. Spec-trographic-grade toluene or research-grade propane was used as the source of carbon. The apparatus for the carburization of the filaments is shown schematically in Fig. 1. The system was evacuated to 1 x l0-' mm of Hg when using the electron beam-melted tantalum and to less than 1 p when using the less-pure tantalum. Neither the difference in the base vacuum, nor in the hydrocarbon gas, nor in the tantalum filaments resulted in any detectable difference in the properties studied in this work. However, only the carbides prepared from the higher-purity tantalum were used in the magnetic-susceptibility determinations. Once the base vacuum had been reached, the system was flushed with the hydrocarbon and re-evacuated. For any desired composition of the carbide, hydrocarbon gas was allowed to leak into a constant-volume flask to a predetermined pressure. These pressures were measured by a Cartesian diver-type mercury gage with a range from 0 to 20 mm and with a scale expanded to nine times. The hydrocarbon gas was allowed into the reaction tube and the filament was quickly raised to the reaction temperature. The slack in the filament due to thermal expansion was taken up by drawing out the movable electrode with a screw mechanism. The filaments were kept at temperature from a few minutes to 200 hr. In the majority of cases the heating time was 6 hr. The reaction tube was cooled by cascading water on its outer surface. By means of an ammeter and a voltmeter the electrical resistance at the reaction

Jan 1, 1963

By P. G. Shewmon, W. M. Robertson

The derivative of the surface tension with orientation, ??/??, for copper has been measured over the entire unit triangle. This derivative or torque term was determined from the variation of the dihedral angles at the intersection of twin boundaries and free surfaces. High-temperature anneals in graphite with a hydrogen atmosphere gave torque terms of 0.097 at (111), 0.066 at (100), and 0.0257 at (110). A variation from -36oto +23oC in the dew Point of the H2 had no effect on these values, nor did a change from 99.98 to 99.999 pct Pure copper. The removal of graphite from the system decreased ??/?? slightly. Considering the surface near a low-index plane to be smooth except for occasional steps, the free-energy increment per cm of step is calculated, and it is shown that the observed variation of ??/?? is consistent with a random distribution of steps and an interaction energy between steps. Integration of ??/?? gave the relative values of y at (100), (110), and (111) as comPared to ymax: (Y111/Ymax) =0.974, (Y110/Ymax) =0.996, (y100/Ymax) = 0.983. The ratio of the surface tension of coherent twin boundaries to the surface tension of the free surface was found to be (yT/ys) = 0.027 * 0.011. In a crystalline solid the surface tension y (surface free energy per unit area) depends on the orientation of the surface relative to the crystallographic axes of the crystal. Measurements of this variation of y with surface orientation have been reported for metals only within the last few years. Consider the grain boundary groove shown in Fig. 1. Here the three surfaces are all normal to the plane of the paper, and each has a different surface tension, y1, y2, and y3. If the system is at equilibrium, the total surface free energy must remain unchanged for a slight vertical displacement of the intersection (points A, B, and C are kept fixed). As shown by Herring,' the following equation is obtained:

Jan 1, 1962

By C. A. Bruch, W. E. McHugh, R. W. Hockenbury

EXPERIMENTAL results of the last decade have shown that both accelerator particles and reactor radiations produce significant changes in the properties of metals. These changes, called radiation damage, are important from both academic and engineering viewpoints. An understanding of the radiation damage produced by reactor radiations is difficult, because many kinds of particles having varying energies are present. Therefore, many fundamental studies are being conducted using accelerators in order to obtain nearly mono-energetic beams of various charged particles. Furthermore, many of these experiments are conducted at low temperatures in order to freeze in the radiation-produced lattice defects, after which the specimens are annealed to study the movement of the defects. It is found that although much of the low temperature radiation damage disappears by annealing at room temperature, a significant amount remains. Because there is no assurance that irradiation followed by annealing at a higher temperature will produce the same effect as irradiation at the higher temperature, and because there is an immediate interest in reactor radiation effects during exposures at and above room temperature, a major program is in progress at this laboratory to investigate some of these effects. This paper, representing a part of the program, compares the radiation damage to a group of metals which were exposed under nearly identical irradiation conditions. The metals, representing the three major crystal systems, include copper, nickel, titanium, zirconium, iron, molybdenum, and type 347 stainless steel. The effects of reactor radiations have been treated from a theoretical viewpoint by Seitz' and Ozeroff.' The problem considered by them has been the atomic displacements produced in an infinite medium by mono-energetic beams of both neutrons and charged particles. For reactor experiments, this treatment is not wide enough in scope, because specimens and reactor components are finite, and there are continuous energy spectra of the various particles. Therefore, the theoretical considerations will be extended in this paper to cover reactor conditions and the findings will be compared with the observed radiation damage. Experimental Materials—The six basic metals for this investigation were of commercial or higher purity, and the type 347 stainless steel was of commercial quality. These materials were supplied in various forms ranging from ingots to finished rods, and were fabricated to rods approximately % in. in diam and annealed for specimen stock. A summary of data pertinent to these materials is shown in Table I. The values for chemical compositions include both actual analytical values and typical values supplied by the manufacturer. More information concerning typical

Jan 1, 1957

By F. H. Buttner, E. R. Funk, H. Udin

A. P. Greenough (University College, swansea, Great Britain)—I have recently made some experiments on the deformation of silver wire at high temperature in an atmosphere of oxygen-free nitrogen. The observa-tions which 1 made confirm the main conclusion of this paper, that the most satisfactory mechanism so far suggested to explain the deformation which takes place

Jan 1, 1953

By Harvey Cline, Donald P. Ferriss

THE violent outgassing of commercial tungsten and other refractory metals when melted in an electron beam zone refining apparatus1"3 is dealt with experimentally by one or both of two approaches. One is to provide a suitable emission current control1,2 the other is to purify the metal in the solid state before melting.4 The first of these is usually sufficient, but the authors chose also to investigate the source of the troublesome gases and to devise means of solid-state purification. Some further insights into the use of tungsten as a structural material at temperatures near its melting point were also revealed in the course of the work. One may speculate on the causes of gas formation in tungsten at high temperature by inferences from the literature and an examination of the impurities in commercial wire. Davenport5 observed microporosity in both tungsten and molybdenum filaments heated to several hundred degrees below their melting points. Studying the function of oxygen in molybdenum welds, Perry, Spacil, and wulff8 attributed similar porosity to the disproportionation of Moo2 to molybdenum metal and Moo3. Tungsten dioxide also disproportionates7 above 2000oC to yield WO3 vapor at considerable pressure. Commercial tungsten contains some 5 to 20 wt ppm O and a similar concentration of carbon depending on the details and precautions of processing. Therefore, evolution of CO is also a strong possibility as a source of gas at high temperatures. Furthermore, even for activities in the order of 0.01, it may be calculated that the pressure of CO at 3000°C would be over 4000 psi, which is in excess of the tensile strength of tungsten at this temperature.9,10 Powder metallurgy tungsten contains some 0.02 pet Fe and 0.002 to 0.005 pet of the elements Ni, Si, Al, Ca, Mn, Mg, and Mo; at temperatures over 2800°c, therefore, these elements will exhibit appreciable vapor pressure, though small compared to that of WO3 and CO. Some of these impurities may react to form high-pressure monoxides such as SiO and A10. Finally, dissolved and occluded nitrogen is an ever-present source of high-pressure gas. Commercial Type 218, General Electric filament wires, 0.025 in. diam, were heated by resistance in 10 -4 mm of Hg and in argon or hydrogen at pressures from 50 µ to atmospheric. For temperature determinations in vacuo, the Jones - Langmuir8 current-temperature relationship was employed. For gaseous atmospheres, the burn-out temperature was assumed to be the same as in vacuo so that a small, constant correction could be made for temperatures below burn-out conditions (i.e., local heating to failure). Several dozen experiments may be summarized by pointing out some structural observations. At 3050oC in 1 atm of A, porosity is very evident after 30 min, as shown in Fig. 1. For the section in Fig. 2, failure occurred 200°C below the melting point and many voids have grown in the grain bound-

Jan 1, 1962

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

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

Jan 1, 1964

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

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

Jan 1, 1961

By D. Geiselman, A. G. Guy

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

Jan 1, 1960

By Joachim J. Hauser

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

Jan 1, 1962

By W. C. Elli, M. E. Fine

YOUNG&apos;S modulus of elasticity in metals ordinarily decreases with rising temperature. The range of the thermoelastic coefficient at room tem- 1/E dE/dT perature (temperature coefficient of modulus, is illustrated1 by the values for tungsten and hard-drawn aluminum, —95 and —1220x10-6 eg C-1. However, a nearly zero thermoelastic coefficient is observed in some ferromagnetic alloys over a limited temperature range. In these alloys, as the temperature is raised, an increase in modulus arising from loss of ferromagnetism compensates the normal decrease. Iron-nickel alloys containing 36 to 52 pct Ni behave in this manner. In the present investiga- tion, the dependence of the modulus and thermo-elastic coefficient on cold working and annealing were studied in iron-nickel alloys in this range of nickel. Although these alloys, when fully annealed, have a coefficient near zero over a very small temperature interval, the temperature range of low coefficient can be extended greatly by straining and then stress-relief annealing. The modulus of face-centered cubic iron-nickel alloys annealed at 1000°C does not vary linearly with composition at room temperature but, as shown by the solid line of fig. 1, from Koster,&apos; is minimum at 40 pct Ni and maximum at 87 pct Ni. The modulus increases with applied magnetic field but retains the minimum near 40 pct Ni. Schematic change of modulus with temperature for three compositions is shown in fig. 2.&apos;. &apos; With increasing temperature, the slope becomes less negative, goes through zero (temperature of minimum modulus for the alloy), becomes positive, and resumes its normal negative value above the Curie

Jan 1, 1951

By E. H. Rennhack

Phase equilibria of the zinc-rich portion of the Zn-Fe-A1 system containing up to 20.0 wt pct Fe and Al have been investigated at 600°C (1112°F), 450°C (842°F), and room temperature by metallographic and X-ray diffraction techniques. The phase relationships were found to involve only those phases present in the three binary systems. THE presence of small quantities of aluminum (approx. 0.2 wt pct*) in zinc galvanizing baths is known to suppress the formation of Zn-Fe alloy layers within the coating.&apos; As part of an extended investigation of this suppression effect and the alloy reactions involved, the zinc-rich corner of the Zn-Fe-A1 equilibrium system containing up to 20.0 pct Fe and Al was determined at 600°C (1112°F), 450° F (842° F), and room temperature. The present paper reports the findings of this study. The constitution of the Zn-Fe system has been reported by Raynor2 based mainly on the work of Schramm3-3 and Truesdale et a1.6 The solid solubility of iron in zinc is extremely small and lies between 0.0009 and 0.0028 pct in the range 150° to 400°C (302°to752°F). Within the temperature and composition range of interest, a eutectic reaction involving nearly pure zinc, liquid = Zn+FeZn13, is observed at about 419°C (786° F) and 0.018 pct Fe along with a peritectic reaction, FeZn7+ liquid e FeZn13, at 530°C (986° F) and 6.2 pct Fe. The latter reaction is sluggish due to the large proportipn of solid phase involved in the transformation. Halla et al.,7 identified the compound FeZn13 as monoclinic with a = 13.68, b = 7.63, c = 5.07, and B = 128°44&apos;. The structure of FeZn7 was reported by Bablik, et al.,8 to be of hexagonal symmetry, belonging to either the C6v = C6/m mc or D46h = C6/mc space group. Divensions of the unit cell are a = 12.81A and c = 57.6a. The Zn-A1 diagram as composed by Raynor9 and later Gebhardt10 is characterized by a eutectic decomposition, liquid 382°C (720°F) and 95.0 pct Zn and a eutectoid decomposition, at 275° (527°F) and 78.0 pct Zn. The eutectoid reaction cannot be suppressed permanently by quenching. Above 275° (527° F), a and a&apos; co-exist in a closed miscibility gap between 31.6 and 78.0 pct Zn. Both phases are fcc and have nearly the same lattice parameter. The maximum solubility of aluminum in zinc (B) is approximately 1.0 pct at the eutectic temperature. PROCEDURE Materials. The experimental alloys were prepared from both massive and powdered material. Cast alloys were composed from three zinc-base master alloys containing 8.0 pct Fe, 16.0 pct Fe, and 50.0 pct Al which were made from C.P. zinc, Armco iron, and

Jan 1, 1962

By E. T. Hayes, A. H. Roberson, M. H. Davies

R. F. Dornagala and D. J. McPherson (Armour Research Foundation, Chicago)—I should like to compliment the authors for a workmanlike job in determining the partial phase diagram of a system comprised of two rnetals which are certainly not easy to work with. We are completing work at Armour Research Foundation on an Atomic Energy Commission-sponsored project for the determination of eight zirconium binary diagrams. Work on the Zr-Cr system has been completed and should be published within the next year. For our work, Westinghouse Grade 3 iodide crystal bar served as the zirconium melting stock. Johnson-Matthey, electrolytic chromium, specially treated for oxygen removal, was employed. The overall constitution of the system determined at Armour Research Foundation is in very good agreement with the present work. We found a eutectic at 18 pct Cr and 1280 °C, somewhat lower than the value reported. This temperature was confirmed by thermal analysis, incipient melting studies, and regular isothermal anneals. The eutectoid was located close to 1 pct Cr and 835°C by metallographic analysis of annealed specimens. Maximum solubility of chromium in /S zirconium was 4.5 pct at the eutectic temperature. Chromium solubility in a zirconium was less than 0.28 pct at all temperatures. We found the compound at 53 pct to melt around 1700°C, with an open maximum, but determined its crystal structure to be hexagonal close-packed (MgZn, type). The lattice parameters were in excellent agreement with those determined by Wallbaum in 1942. The diagrams are in substantial agreement, and .part of the differences are undoubtedly due to the use of different zirconium melting stock. M. K. McQuillan (Birmingham, England)—I read this paper with a great deal of interest, as it covered the same field as some work of my own.&apos; There are a number of points in the present paper on which I would like to comment. First, I should say that I, too, used zirconium prepared by magnesium reduction of the tetrachloride and electrolytically prepared chromium, and melted the alloys in a Kroll-type arc furnace. The purity of my alloys should, therefore, be comparable with the purity of those of the present authors, and any differences in our observations would not be expected to be attributable to this cause. The differences between my observations and theirs concern the presence of the eutectic, the temperature of the eutectoid, and the melting point of the compound. I would be very much interested in any further evidence the authors may have for the occurrence of the eutectic at 1380°C. During the course of my work I noted that a number of my alloys containing 60 to 90 pct Zr melted at about 1400 °C, and for a time assumed that a eutectic occurred at this temperature as described in the paper. On further investigation, however, I found that the structures of the as-melted alloys could not be made to fit in with this interpretation of the system. If a eutectic exists in this region of the system it would be expected that the as-melted alloys would show the usual type of cast structure, i.e., dendrites of the compound plus eutectic. This, however, does not occur, as may be seen from Fig. 9. The compound seen there is not dendritic in form, and the remaining material is by no means certainly eutectic. It may be argued that a compound such as ZrCrl would not form dendrites but would tend to crystallize in geometric shapes. In this case, however, I have evidence to the contrary, as on the chromium side of the compound, where a eutectic occurs at about 1545"C, the compound formed from the liquid takes on a conventional dendritic form, and the eutectic is observed in the interdendritic spaces in the usual way. There is no reason to suppose that the compound would behave differently in an alloy lying on the zirconium side of the compound composition if a eutectic existed there too.

Jan 1, 1953

By D. R. Hay, E. Scala

Electrotransport has been superimposed on the rate-limiling- step in zone refining which is the impurity diffusion through the liquid at the solid/liquid interface. The efficiency of zone refining is increased and relative resistivity ratios (P300°k/P4 2°K) he increased by 50 pel in tungsten for a given number of posses using- the electrotransport field-aided method. The effiect of zotze refining in the presence of an electric field on the relative resistivity ratio is examined as a function of its intensity and polarity. THE effect of electrodiffusion on the effective distribution coefficient of zone refining has been discussed by Pfann and Wagner.&apos; Control of the distribution coefficient in zone refining is of twofold interest. A distribution coefficient of unity can be increased or decreased, making possible the transfer of some previously inseparable solutes. The general efficiency of zone refining can also be increased. In the conventional zone-refining process impurities are removed by their retention in the molten zone and subsequent deposition at the end of the rod after a complete passage of the zone. In higher-melting-point systems a second mechanism may also operate, the volatilization of impurities from the molten zone. It has been suggested by schadler2 that, in refractory metals, vacuum distillation plays the predominant role in purification. In Koo&apos;s results,3 the resistivity ratio decreased beyond a zone-refined length of 6 in. from the starting end, indicating that some purification does in fact occur by true zone-refining action. Hay and scala4 showed that the degree of purity as measured by the relative resistivity ratio method depends on the square root of time in the molten zone (number of passes) and thus appears to be limited by diffusion in the boundary layer at the solidifying interface assuming good mixing in the body of the molten zone where a linear rate would prevail. The final concentration of impurities in electron-beam floating-zone purification depends very much on the operating conditions and results obtained by various investigators2,3,5 are difficult to correlate. The diameter of the starting material, operating vacuum, and rate of traverse are among the factors to be considered. There are, nevertheless, some general observations to be obtained from the literature. Lawley5 reviewed the literature up to 1962 and concluded that the major contaminants generally remaining in tungsten after electron-beam zone refining are molybdenum and carbon. Molybdenum due to its high melting point and distribution coefficient of nearly unity would be expected to be difficult to remove by either volatilization or zone refining. Carbon is not only a common contaminant in vacuum systems, but is also very difficult to remove by conventional vacuum melting. even with vacuums of 10-7 mm Hg. For each of those impurities removed by zone refining the equation of Pfann and Wagner may be applied: It relates the effective distribution coefficient k to a superimposed driving force which accelerates the solute away from the interface with a terminal velocity L" and to the more conventional zone-refining parameters; v = rate of traverse, t = thickness of the diffusion layer at the solidifying interface, D = diffusivity of the solute in the molten zone, and ko = equilibrium distribution coefficient of the impurity.

Jan 1, 1965

Jan 1, 1935

Jan 1, 1942

By Charles S. Barrett

There is a road into the microscopic realm that has remained untraveled through all these years of intense activity with high-power optical and electron microscopy. The road is worthy of careful scouting by metallurgists and other investigators, for it leads into relatively new country and it makes some areas accessible that heretofore could be reached only by very indirect paths or by the use of imagination. And when the road passes through familiar territory it frequently permits a new view of commonplace things that should prove of value from time to time. An accepted way to interest people in new sights such as this is to present an illustrated travelogue. This I propose to do, using many pictures taken in my recent exploration of this road. In the manner of travelogues, I shall touch briefly upon a large number of different subjects in physical metallurgy and shall attempt to give an exhaustive treatment of none, for the objective is to provide a means for further research, to interest others in it, and to indicate what appears at the moment to be profitable directions for it to take. The method I shall present involves X-rays, but does not make use of the usual accompaniments of X-ray research such as reciprocal lattices, Fourier series, or the stereographic projection. The method is so simple in its fundamentals that it could have been developed 2o years ago, or perhaps even 30 years ago. It is well to have a destination for our travels, so that when we are through we shall have explored some region of importance, despite our preoccupation with the novel means of transportation and our interest in the sights to be seen along the way. So let us name the Cold-worked State as our destination, and make side trips into the territories known as Recovery, Recrystallization, and Precipitation-hardening. A great many investigations have been made of the nature of cold-worked metal, and a great variety of methods used, many of which are indirect, such as X-ray line intensities, X-ray line widths, calori-metric measurements, and magnetic measurements. Since comprehensive reviews of these investigations have been published in recent years, they need not be discussed here. The investigations that were the direct forerunners of the present work should be first mentioned. In 1931 I became interested in the structure of individual spots in X-ray diffraction patterns.l When a crystal is placed in the narrow pencil of X-rays in a Laue camera, the spots recorded on the film are not always uniformly black, but may have an internal structure. The meaning of this may be understood from Fig. I, which represents a narrow beam containing X-rays of many wave lengths (&apos;&apos;general radiation") penetrating a crystal in the direction of the arrow and forming a pattern on the vertical film at the right.

Jan 1, 1945

Jan 1, 1941

Jan 1, 1945