Search Documents

By J. R. Cahoon, W. V. Youdelis

In a previous communication by one of us,1 a theory of inverse segregation was presented by which the maximum segregation and segregation distribution throughout a unidirectionally solidified, binary-alloy ingot could be calculated. The theory, which is based on the mechanism of volume contraction and interdendritic flow, quantitatively accounts for the observed maximum segregation in the A1 (rich)-CU' and Al-Zn2 alloy systems, and for the segregation distribution along the ingot lengths for the A1-Cu system.''4 One of the drawbacks to a more extensive use of the segregation equations is their complexity, particularly for the calculation of the segregation distribution throughout the length of the ingot, involving long tedious numerical calculations to obtain the segregation. Computer pro- grams, written in Fortran II for use on an IBM 1620 computer, have been developed by the authors (and are available from them), providing quick and accurate methods for the determination of the theoretical maximum segregation in any binary-alloy system, and also for the segregation distribution in any unidirectionally solidified binary-alloy ingot. The segregation distribution is controlled by the lengths of the various solidification zones'74 which are in turn controlled by the cooling rate, and are determined from temperature-distribution curves obtained during solidification. The theoretical segregation distributions shown in Fig. 1 illustrate the effect of the zone lengths on the distribution Curve 1, indicative of a slowly cooled ingot, represents an ingot having long solidification zones, while Curve 2, indicative of a rapidly cooled ingot, represents an ingot having relatively short zones. Although these distributions are calculated for an A1-10 pct Cu ingot, the shape of the distribution would be similar for any binary-alloy ingot. These curves show clearly why early workers obtained results which indicated that the maximum (chill-face) segregation approached zero at very fast cooling rates.3 Actually, the maximum segregation is independent of cooling rate,' but even at short distances from the chill face the amount of segregation drops considerably, particularly in a rapidly cooled ingot, making it very difficult to establish the amount of segregation occurring at the chill-face. The authors would like to thank Dr. J. A. Goldak for his assistance in the preparation of the programs. The financial assistance of the Steel Co. of Canada and of the National Research Council of Canada in the form of Scholarships to one of us (J. R. Cahoon) is gratefully acknowledged.

Jan 1, 1964

By J. H. Brophy, S. J. Michalik

A constitution diagram for the system Mo-Ir has been determined. The maximum solubility of iridium in molybdenum is 16 at. pct at 2110ºC and decreases to less than 5 at. pct at 1500°C. The solubility of molybdenum in iridium is 22 at. pct. Three intermediate phases appear in the system: 8 MoJr, having the p-tungsten structure; a phase, a cornplex tetragonal structure; and the hcp ? phase. Metallography, melting point determinations, X-ray diffraction and fluorescence, and electron micro-probe unalyses were employed in establishing the diagram. PREVIOUS to the present investigation, the intermediate phases in the Mo-Ir system were identified, but no detailed account of the phase diagram has been reported in the literature. Raub1 investigated alloys of Mo-Ir over an extensive range of composition between the temperatures of 800º and 1600°C. The in-termetallic compound MosIr was found to exist with nearly pure molybdenum, as the solubility of iridium in molybdenum was not detectable parametrically in this temperature range. MO3Ir was found to be iso-morphic with a ß-tungsten type structure, having a parameter of 4.959Å. An intermediate hcp phase, designated as the ? phase, ranged in composition from 52 to 78.5 at. pct at 800ºC, and from 41 to 78.5 at. pct Ir at 1200°C. Parameters noted for the ? phase were as follows: at 42.7 at. pct Ir, a = 2.771i0, c = 4.4366, c/a = 1.601; at 78.5 at. pct Ir, a = 2.736A, c = 4.378A, c/a = 1.600. Molybdenum was found to be soluble in iridium up to 16.5 at. pct Mo (83.5 at. pct Irj, with the parameter of iridium increasing to 3.845A at the solubility limit. Knapton,2 who investigated alloys between 15 and 85 at. pct Ir, essentially agreed with Raub's data, but, in addition, found a a phase in as-melted alloys near 25 at. pcto Ir. The oaphase lattice parameters were a = 9.64Å, c = 4.96Å, c/a = 0.515. The a phase was replaced by the 8 -tungsten phase on annealing at 1600°C. Knapton concluded that the a was stable only at elevated temperatures, and placed the composition of the a phase at approximately 30 at. pct Ir. The intermetallic compound Mo3Ir, with a lattice parameter of 4.965A, was included among the 8-tungsten structures reported by ~eller.' Matthias and Corenzwit,4 and Bucke15 studied the superconducting nature of MosIr, and reported a superconducting transition temperature of 8.$K. The present investigation describes the phase relationships in the Mo-Ir alloy system determined by melting point measurements, X-ray diffraction and fluorescence, and metallography. EXPERIMENTAL PROCEDURES Alloys for the determination of the phase diagram were prepared from powders. Commercial 99.9 pct Mo from Fansteel Metallurgical Corp. and 99.9 pct Ir powder from J. Bishop and Co. Platinum Works were used. The powders were weighed to nominal compositions, mixed, and then pressed, without binder, into compacts weighing 4 to 6 g. These were presintered in uacuo between 1200' and 1400°C for 1 hr, to reduce the degree of spattering during subsequent arc-melting. The compacts were arc-melted in a nonconsumable tungsten electrode furnace six times on alternate sides on a water-cooled copper hearth in an atmosphere of zirconium-getter ed argon at 500 mm of mercury pressure. In almost all cases, this procedure yielded buttons of satisfactory homogeneity. The composition of all melted buttons were confirmed by X-ray fluorescent analysis using the experimentally determined ratio of the iridium La1 line intensity to that of the molybdenum Ka1 line as a function of composition. In this determination four alloys analyzed by wet chemical methods were used as standards. An uncertainty range of ±1 at. pct has been attributed to all indicated compositions. All heat treatments and solidus measurements were carried out in tantalum resistance heating elements in vacuum conditions of 10-4 to 10-5 mm of mercury. A detailed account of this procedure has been reported by Schwarzkopf and Brophy.8 In the heat treatment and solidus measurements of iridium-rich alloys (50 at. pct Ir or greater), a tungsten lining was inserted into the tantalum resistance heating element because of a eutectic reaction which occurs between iridium and tantalum at 1948ºc.7 Heat treatments and solidus measurements carried out at compositions less than 40 at. pct Ir both with and without tungsten linings within the resistance

Jan 1, 1963

By N. Pessall, A. D. McQuillan

The phase relalionsllips in an isothernzal section of the Ti-Zr-H system at 750°Chave been investigated by measurement of hydrogen equilibrium pressures. The resulting diagram indicates that the hydride phase has an anomalously wide range of homogencity extending from 66.6 to 30 at. pct H in alloys containing about 15 al. pet Zr. Measurement of the heat of solution of hydrogen as a function of alloy composition in ß-phase alloys indicates no anomalous behavior in the region of 15 at. pet Zr, and suggests that the extensive range of homogeneity in the hydride phase at about this composition must he attributed to an enhanced stability of the, hydride phase. THE manner in which titanium and zirconium react with hydrogen and the constitutional diagrams of the two metal-hydrogen systems are qualitatively very similar,'-6 as can be seen from Fig. 1 which shows the constitutional diagrams of the two systems. Quantitatively, however, there are some differences. For example, the exothermic heat of solution of hydrogen in ß titanium is smaller than that in ß zirconium, and consequently the equilibrium hydrogen pressure of a Ti-H alloy is higher than a Zr-H alloy at the same temperature and hydrogen concentration. Other differences manifest themselves in the hydride phases which exist at high hydrogen concentrations. In the Ti-H system, above room temperature, there exists only a single hydride phase in which the metal atoms are arranged on a fee lattice, but in the zirconium system there are two hydrides, and whereas the hydride of lower hydrogen concentration has a fee structure, the higher hydride has a face-centered tetragonal structure. The tetragonal hydride retains its stability up to temperatures in excess of 450oC.7 From the foregoing, it would be expected that the constitutional diagram of the ternary Ti-Zr-H system would have a very simple form, especially as titanium and zirconium are completely miscible in both the a and ß forms.8 The present work, which consists of a study of an isothermal section of the ternary system, was carried out in order to check the assumption frequently made that the electronic structure of the two metals and the mechanism by which hydrogen is held in solution in the metals is the same for each. Although this proved largely to be true, certain inter esting and unexpected features of the ternary system emerged which must be explained before we can really say that the reactions of titanium and zirconium with hydrogen are fully understood. EXPERIMENTAL PROCEDURE The most convenient method of studying hydrogen-metal systems is by the measurement of the hydrogen pressure in equilibrium with the hydrogen dissolved in the metal as a function of hydrogen concentration and temperature. In binary systems, the results are easily interpreted in terms of alloy constitution, since two-phase regions can be recognized by the fact that the hydrogen pressure at constant temperature does not vary with the hydrogen concentration in the alloy when it is in the two-phase condition. This criterion does not apply in ternary systems, but there is usually a marked change of slope in the isothermal pressure-composition curves when a phase boundary is crossed, and with care, and a knowledge of the limiting binary systems, the phase structure of the alloys can usually be deduced. In the

Jan 1, 1962

By Horace Pops, L. L. Isaacs

SOLID-STATE transformations at low temperatures are frequently studied by optical metallography. Greninger and ooradian' and Hull and Gar-wood2 have examined the martensitic-type transformations in 0-phase Cu-Zn alloys during continuous cooling below room temperature. The lowest range of temperatures in the apparatus described by these investigators is limited to approximately 110°K. Present studies of reversible first-order phase transitions near liquid-helium temperatures have necessitated the design of a new cold-stage cryo-stat for optical metallography. The features of interest of this instrument are as follows: a) temperatures down to 4.Z°K are obtainable; b) the specimen is always under vacuum, thereby avoiding the condensation of moisture; c) specimens can be rapidly cooled or heated at varying rates, thus permitting studies of transformation hysteresis. Fig. 1 shows the details of the cryostat. All major parts are made of type 304 stainless steel. Both helium and nitrogen cans are Heliarc-welded to the helium filling tube, permitting the use of a common shielding can. Hence, the over-all weight and the area of the evacuated surface are mini- mized. The copper sample holder is screwed into the bottom of the helium can. To assure good thermal contact between the sample holder and the refrigerant, an indium ribbon is placed on the threads

Jan 1, 1964

By P. Pietrokowsky

lntermediate phases in the binary metal alloy systems Ti-Zn, Ti-Hg, Zr-Zn, Zr-Cd, and Zr-Hg have been investigated by X-ray powder diffraction methods. Gamma-TiBHg and Zr3Hg have a beta tungsten structure; TiHg and ZrHg are analogous to ordered AuCu (L l0 type); delta-TixHg and ZrHg, are isomorphous with ordered AuCu,, (L l2 type); ZrZnz is face-centered cubic (C 15 type); TiZna crystallizes in a C 14 type structure; and Zrll-, occurs in cubic and tetragonal modifications in which a random distribution of atoms exists. Additional information for the intermediate phase TiZn, is presented. THE physical metallurgy of titanium and zir-conium when alloyed with elements in subgroup 11-B of the periodic table has received comparatively little attention in the literature. Laves and Wallbaum' reported the existence of several intermediate phases in the system Ti-Zn. They identified TiZn as a CsCl (B 2) structure and described TiZn, as an ordered Cu,Au (L 1, type) crystal structure. Gebhardt' investigated very limited zinc-rich regions in the systems Ti-Zn and Zr-Zn. Phase relationships in these partial constitution diagrams were deduced from the results of thermal analysis and metallography, X-ray results being inconclusive. The first zinc-rich intermediate phase in either system was not identified. More recently, Anderson, Boyle, and Ramsey" have had occasion to refer to a partial Ti-Zn phase diagram (unpublished data) covering the region 0 to 10 atomic pct Ti, wherein two intermediate phases corresponding approximately to TiZn,, and TiZn,, were indicated. The metals used in this investigation and typical analyses as determined by the suppliers are given in Table I. The iodide-process zirconium which was used was not hafnium free. Experimental Methods Alloy Preparation: The relative ease with which titanium and zirconium combine with other elements places extensive restrictions on the methods by which alloying can be achieved. The direct current electric arc melting procedure was found to be unsatisfactory for preparing these binary alloys and for this reason solid state diffusion methods were utilized. The iodide process titanium and zirconium rods were filed by hand. Fines were subjected to a magnetic separation and classified as to size as either finer than 200 mesh or coarser than 200 but finer than 80 mesh. Powder mixtures of various binary combinations of titanium and zirconium with zinc and cadmium were compacted in a 12 mm diameter die and then placed in Vycor or quartz vials which were evacuated and sealed. The mercury alloys were prepared in a similar manner; the proper weight of liquid mercury being placed in a vial with minus 200 mesh titanium or zirconium. These ampoules were then heat treated at various temperatures and times depending on the characteristics of the particular alloy system. Upon completion of the heat treatment the ampoules were cooled rapidly and the specimens weighed. The loss in weight varied from 1 to 3 pct (except as noted in the text) and for this reason the calculated compositions were accepted as a fair measure of the actual alloy compositions. X-Ray Dif raction Techniques: Powder diffraction experiments were conducted at room temperature with a 143.2 mm Debye-Scherrer X-ray camera in which the film was placed in the Straumanis arrangement. When copper radiation was used, a nickel filter was employed, and for the cobalt target a filter of iron oxide was used. In both cases, the /i? filter was placed between the X-ray target and the powder specimen which was mounted on a glass fiber. The lack of information based on optical metallography placed reliance on the results obtained from the X-ray experiments for determination of

Jan 1, 1955

By P. Duwez, H. Martens

Dimensional changes generally occur during the sintering of metal powder compacts. These changes may have several causes and their magnitude depends upon the numerous variables involved in the process, such as the nature of the powder, size and shape of the grains, compacting pressure, rate of heating, maximum temperature, length of time at temperature, and furnace atmosphere. Among all the variables, time, temperature, and compacting pressure are probably the most important ones, and the effect of each one of the other variables can be studied separately once the effect of these is well understood. The most precise method of studying the phenomenon of dimensional changes in a compact consists of heat treating the compacts at various temperatures for different lengths of time. In this method, only very small specimens can be used, in order to achieve rapid rates of heating and cooling. The technique involved in these measurements is very simple, but is time consuming. Another experimental approach to the problem consists of measuring the change in length of a compact as it is being heated at a constant rate. Although the two variables, time and temperature, are combined into a single one (rate of heating), the results obtained by this technique may be of great interest from both practical and theoretical points of view. The purpose of this paper is to describe a systematic investigation of the change in length during sintering of compacts made of one or several metal powders. Experimental Procedure The change in lenght of compacts during sintering was measured with an automatic recording dilatometer. In this instrument the change in length and the temperature are recorded as functions of time on two separate charts and the rates of heating and cooling may be varied from 1 to 20°F per min. The temperature may be kept constant at any value up to 2200°F during any predetermined length of time and the change in length recorded as a function of time. Provision is made for atmosphere control inside the fused silica tube containing the specimen. Three different magnifications are provided, so that 1 in. on the chart corresponds to 0.002, 0.005, or 0.010 in. change in length. The mechanism following the change

Jan 1, 1950

By J. W. Downey, R. A. Morris, M. V. Nevitt

An experimental survey has determined the occurrence of Ti2 Ni-type phases in binary and ternary alloys of Ti, Zr, or Hf with first, second, or third long-period transition metals and also in ternary systems in which 0 is the third component. The existence of eleven previously unreported isomorphs is cited and some approximate phase boundaries are given. Lattice parameters are reported for the new phases. The periodic table relationships involved in the occurrence of the phase are discussed. A previous paper' reported the occurrence of a group of Ti2Ni-type phases (structure-type E93) containing Zr in combination with Rh, Ir, and Pt, and Hf in combination with Rh, Pd, Ir, and Pt, and cited evidence to show that all of the Zr phases and the Hf-Pd phase are not binary phases but occur only when 0 is present. More recently one of the present authors found that in the ternary systems of Ti and 0 with Cr, Mn, Fe, Co, and Ni the occurrence of the Ti2Ni-type phase could be correlated qualitatively with valency electron concentration, and that the role of 0 appeared to be that of an electron acceptor.' This paper describes the results of a broader investigation of the occurrence of Ti2Ni-type phases in binary and ternary systems containing Ti, Zr, or Hf. EXPERIMENTAL PROCEDURE Alloys were prepared by arc melting. The purity of the metals Zr, Rh, Hf, Ir, Pd, and Pt was given in the previous paper.' The additional materials used for this work were metals with a minimum purity of 99.9 pct and reagent grade ZrO2, TiO2, Cr2O3, and NiO. Chemical analysis of several alloys in each system indicated good agreement between intended compositions and cast-button compositions. For the heat treatment precautions were taken to avoid oxygen contamination. The specimens were wrapped in Mo foil and sealed in fused quartz tubes at a room temperature pressure of 1 x mm of Hg. These capsules were then annealed in a vacuum furnace at an external pressure of 5 X mm of Hg. Since the major constituent in most of the alloys studied was the brittle Ti2Ni-type phase, Debye-Scherrer patterns with sharp lines could be obtained with powder crushed from the annealed solid samples without being reannealed. Metallographic, X-ray diffraction, and density determination techniques previously described1, 2 were used. RESULTS AND DISCUSSION Zr-Rh-O, Zr-Ir-Oand Zr-Pt-O Systems-Figs. 1 through 3 show the approximate boundaries of the Ti2Ni-type phase fields at the temperatures indicated in the ternary systems Zr-Rh-O, Zr-Ir-O and Zr-Pt-0. In each isothermal section the Ti2Ni-type phase field is labeled E and the unidentified binary phase found in the previous work' is labeled ?. The dotted lines, which are not phase boundaries, correspond to the composition (Zr2 B)1-xOx. In each system the Ti2Ni-type phase field is displaced to the high-Zr side of this composition line. However, the departures from Zr2B stoichiometry for the metal components are not as high as Zr3B, as was inferred from the previous work. Lattice parameters of the Ti2Ni-type phases in the alloys shown as triangular data points in Figs. 1 through 3 are given in Table IA. The probable compositions of the Ti2Ni-type phases have been estimated from the isothermal sections. Although there are a few exceptions that probably result from uncertainties in phase boundary location and from the effect of variation of oxygen content, the generalization can be

Jan 1, 1961

By G. D. Oxx, L. F. Coffin

The concept of using a phase that is liquid at service temperatures as a component of coatings for refractory metals has been described. The liquid, an alloy of gold and silicon, is retained on a molybdemum surface by a capillary system made of molybdenum disilicide. The coating has the advantage of good thermal shock and has a self-henling chracteristic. In order for highly stressed structures to exceed a service temperature of 2000°F, it has become apparent that a development that does not depend on the traditional iron, cobalt, or nickel-base alloy is needed. Alloys of the refractory metals, i.e., molybdenum, tungsten, tantalum. niobium (colum-bium), and rhenium are potentially useful at extremely high temperatures that more conventional alloys would never be expected to achieve. A new alloy of molybdenum has become available that has a 100-hr rupture strength of 35,000 psi at 2200°F.1 As a result of this work, it may be assumed that a material with adequate mechanical properties at 2200?F is now available. Unfortunately, this alloy and all other known alloys of the refractory metals suffer from not being; serviceable in an oxidizing atmosphere for a very long time. In order to permit general use of refractory metals at high temperatures, it is necessary to prevent destructive oxidation by appropriate alloying or by protective coatings. The liquid phase coating reported here is representative of a concept for the protection of metals that permits higher service temperatures and introduces a new group of materials for selection as coatings. Coating Requirements—Service conditions that represent potential applications for refractory metals vary considerably: however, it is possible to consider two conditions that are usually present. The refractory metal1 component must be heated to the service temperature at least once and usually frequently. When a solid coating is used, usually the coating and basis metal do not have the same coefficient of expansion. This difference causes thermal stress in the coating that is aggravated by rapid heating and cooling and eventually causes coating failure. The second consideration is the probability that there will be damage to the coating by some environmental condition. In jet engines, for example, it is expected that large particles, stones, metal parts, and so forth, will strike a bucket at high speed and cut a hole in the coating. In addition to the above considerations, the coating must also have other fundamental properties. Obviously, it must be oxidation resistant. In addi- tion, it must prevent permeation of oxygen and subsequent oxidation of the basis metal at the interface. Also, diffusion of the basis metal to the outside surface and subsequent oxidation there must be prevented. Finally, the coating must not react with the basis metal to form a weak bond at the interface. It should be noted that the coating need not support a load: it must only remain intact. Liquid Phase Coating Design Factors—In the use of a liquid as a principal coating constituent, it would be expected that the two service conditions mentioned above would be satisfied. A liquid would flow under the influence of the thermal strain developed by coating-basis metal expansion mismatch such that failure from this source would not be expected to occur. It is also probable that the ability of a liquid to flow would provide a self-healing effect. Thus, damage caused by particles in the atmosphere would be repaired. A third advantage is evident in that vapor pressure rather than melting point limits the service temperature. This latter advantage permits use of low melting but oxidation resistant metals such as gold or copper that would be quite useless if the solid state was required. A low viscosity liquid alone. however, is a totally unsuitable coating because it will simply flow off a component, particularly under the influence of a high acceleration field. A method of preventing liquid loss must be devised. In this case, it is desired that the liquid have a low viscosity so that it may easily flow into flaws; thus, raising the viscosity is not a satisfactory solution. One other inherent difficulty is caused by the high mobility of atoms in the liquid state as compared to the solid state. Because of this mobility, it would be expected that gases would diffuse more rapidly through a liquid. It is also probable that the solubility of oxygen in the liquid would be comparatively high. These factors would tend toward rapid permeation of oxygen and oxidation of the substrate. It is most reasonable that this problem could be solved by incorporating a solid phase, which is impermeable to gases, as a component of the coating. To overcome the tendency of a liquid to flow easily, it is possible to use surface tension to advantage. If the surface were made up of a large number of capillary tubes of sufficiently small diameter, then surface tension would hold the liquid even against the acceleration of a centrifugal field.

Jan 1, 1961

By E. Hornbogen, R. C. Glenn

Copper precipitates from a iron as fcc E phase without formation of intermediate compounds. In the first stage of the precipitation, spherical particles with diameters < 100A are formed at a high rate. During the second stage, the particles grow at a rate given by Zener&apos;s equation for growth of a spherical precipitate. In the third stage, growth is slower. Rod-shaped particles form after long aging times at 700°C. Maximum strengthenzng was observed at the beginning of the second step of precipitation. During plastic deformation of the aggregate, particles appear to deform initially by twinning. THE work discussed herein was part of a study of precipitation of substitutional elements from a iron. Copper was chosen as one of these substitutional elements because it has about the same atomic size as a iron, and does not form an intermetallic compound with iron. The data on the iron-copper system then available were summarized by Daniloff1 several years ago. The solubility of copper in a iron has been determined by electrical conductivity measurements,2 lattice parameter measurements,3 and by saturating thin iron foils with copper and determining the copper content.4 The results of the three investigations do not agree very well, but the value of 2.4 wt pct for the maximum solubility at 840°C seems to be the most reliable,4 Fig. 1. An alloy containing 1.23 wt pct Cu was used in our work to assure starting with a completely homogeneous material. On the copper-rich side of the diagram, there is a maximum solubility of about 4 wt pct Fe in copper at 1094°C ( phase). The precipitation of

Jan 1, 1961

By J. Intrater, E. S. Machlin

In a study of grain boundary sliding in superpure Copper (99.999 pct),&apos; bicrystals of a specific shape were used, Fig. 1. That shape was adopted in order to minimize the deformation of grains on both sides of the boundary due to clamping. Another requirement was to obtain bicrystals with a rnicroscopically straight boundary, Fig. 2. Single crystals of predetermined orientation (growth axis parallel to <310>) were grown in a graphite mold from seed crystals. The apparatus for growing single crystals consisted of a vacuum system, argon purification train, vycor tube (in which a graphite mold was placed), a carriage for the induction coi1,and a Lepel (7-1/2 KW) high-frequency converter. The graphite mold was heated by induction and the charge in turn was heated by conduction. The induction coil was moved by means of a motor at a speed of 1 1/2 in. per hr. Single crystals of two different orientations were grown from the melt in one-half of a split graphite mold, Fig. 3(a). Two such crystals were then placed in contact with each other in another split mold, Fig. 3(b) using tapered inserts. The pair of crystals was then remelted starting 2 in. from the top to insure that the whole top portion of the crystals was maintained molten. By moving the induction coil

Jan 1, 1960

By R. D. Carnahan, J. E. White

A study of dispersion strengthening in TD-Nickel (nickel plus 2 vol pct Tho2) was conducted employing microstrain techniques at ambient room temperature. It was found that optimum strength was due primarily to the incorporation of stored energy developed by a variety of thermal-mechanical treatments. The relatively low strength of the recrys-tallized condition implies that the dispersed particles themselves offer only token resistance to deformation. The development of resistance to large-scale recovery or recrystallization at temperatures near the melting point requires a more extensive sequence of strain-anneal cycles than does the development of optimum strength. A micro-Bauschinger effect was observed which appears to be related to the lattice resistance to the movement of free dislocations. The effect was nearly identical to that in pure nickel indicating that the presence of the dispersed phase and considerably increased dislocation density (stored energy) only alters the number or effectiveness of barriers. THE early stages of deformation of engineering materials can be conveniently studied by utilizing strain-gage techniques which permit resolution of strains less than 5 X 10-7 in. per in. for testing in four-point bending (Carnahan and white1). The present investigation, part of a continuing study on the very early stages of deformation, was designed to reveal the true role of a dispersed phase in promoting high strength in a commercially available dispersion-strengthened alloy. Although this technique has been used for some time to study microdeformation in pure metals and alloys, it has just recently received attention as a means of investigating dispersion strengthening. Studying the very early stages of deformation in alloys which depend upon a finely dispersed inert phase for strength may prove to be a very important method for a better understanding of these materials. It is essential to obtain considerable clarification of actual dislocation movement and the kinds of deformation barriers which exist before optimum properties can be designed into this type of material with any degree of confidence. Considerable research on a variety of dispersion-strengthened materials has resulted in two different schools of thought regarding the strengthening mechanism. One faction2-4 favors the idea that the particles themselves resist the motion of dislocations. The criterion for yielding is the fracture of the dispersed second-phase particles due to an array of piled-up dislocations. Other invesfigators5-a have shown that particles are effective primarily by allowing a greater buildup of stored energy or dislocation density through thermal-mechanical treatments in the composite than the pure matrix material. The particles themselves, then, are not exclusive obstacles, but the complex network of particles, dislocation tangles, subboundaries, and grain boundaries are strength determining. The development of such a complex dislocation network in SAP has been studied recently in some detail by Goodrich and Ansell. The ability of dispersion-strengthened alloys to resist softening or recrystallization is also of considerable importance; however, the criteria for maximum stability may not necessarily be those for maximum strength. In this study, in addition to the evaluation of the microstrain properties of TD-Nickel, it is felt that considerable clarification of the true dependence of strength and stability on the dispersed phase is shown. I) MATERIAL AND PROCEDURE TD-Nickel is a dispersion-strengthened alloy developed by the E. I. DuPont de Nemours Co., which contains 2 vol pct thoria (Tho2) in a pure-nickel matrix. The average ThO2 particle size is approximately 0.1 p and the interparticle spacing is less than 1 u. The material was supplied by DuPont in two conditions: hot-extruded bar stock, and stress-relieved cold-rolled sheet 0.025 in. in thickness. The bar was extruded at 2200°F from a cold-pressed and sintered billet. The sheet stock was prepared from the extruded material by a process involving ten or more 50-pct cold reductions by rolling with intermediate anneals at 1800° to 2000°F. Test specimens used in this study were prepared in the form of rectangular parallelepipeds measuring 0.375 by 1.375 in. in thicknesses ranging from 0.025 to 0.040 in. Samples prepared from sheet and extruded stock were mechanically polished before heat treatment and were handled with extreme

Jan 1, 1964

By E. T. Peters, L. E. Tanner

In the course of a study concerned with the rnechanical behavior of the intermetallic compound CO3V, both structural observations and anomalous electrical-resistivity behavior indicated the presence of a new high-temperature phase in an alloy with the stoichiometric composition, Co-22.4 wt pet V. The evidence, which is given below, suggests that the new phase is situated between the low-temperature ordered hexagonal phase, k,1, 2and the high-temperature disordered fee solid solution, a,3 within a small range of temperature in the vicinity of 1070°C. Structural studies included X-ray diffraction analysis* and electron-transmission microscopy examination* of stoichiometric composition speci- mens homogenized for 1 hr at 1200oC and either air-cooled or water-quenched. The air-cooled specimens yielded X-ray diffraction evidence of the k phase, while electron microscopy revealed a microstructure of both heavily and moderately faulted regions as shown in Fig. 1. The high density of stacking faults (or fine twins) in region A is reminiscent of hexagonal cobalt following its allotropic transformation.4 Selected-area diffraction from this region revealed distinct superlattice reflections of the ordered hexagonal phase, as well as continuous rel-streaks which were normal to the fault planes in the micrograph. The latter is indicative of extremely small spacings between the faults.&apos; Regions such as ß were found to be only partially transformed to the k phase. Attempts to study the antiphase domain structure by either bright- or dark-field techniques were unsuccessful in these initial studies. This was due to the low intensity of the superlattice reflections arising from the closeness of the cobalt and vanadium scattering factors. Quenching Co3V from above Tc appears to suppress the formation of the k phase. Both X-ray and electron-diffraction results indicated that the disordered phase, a, was partially ordered during severe cooling and that the structure of the ordered phase was of the L12 (Cu3Au) type,6 designated here as a&apos;. As in the case of the hexagonal phase, examination of the domain structure was unsuccessful; however, significant information concerning the morphology of this condition was revealed by the appearance of dislocation arrays. In particular, it

Jan 1, 1965

By Abdul-Fattah K. Kaddou, P. C. Rosenthal

THE authors have studied the problem of temper brittleness in steel1 employing an internal friction method. The specimens are in the form of wire, 14 B and S gage (0.064 in diam), 6 in. long. It was very desirable to have an apparatus to test the wire specimens for temper brittleness without making standard notched-bar Izod or Charpy impact tests. Such a device would have two favorable advantages: the first is that no standard impact specimen would be necessary, thus saving time and labor; the second is that there would be a direct correlation with internal friction results, thus eliminating the size factor if standard impact specimens had to be used. A search was made without result to find a commercial apparatus for this purpose. The literature was surveyed to investigate if such a test had been utilized. No such work has been reported in the literature; however, zapffe2 has described an apparatus used for testing for hydrogen embrittlement in

Jan 1, 1961

By W. M. Lehrer

RECENT development of high-temperature brazing alloys has required information regarding the eutec-tic temperature and composition of the Pd-rich section of the Pd-B system.. Literature on this subject was found to be scanty with no complete system yet determined. Buddery and welch1 report an inter-metallic compound occurring in the Pd-B system at 6.33 wt pct B (PdsBz). Another source, Sieverts and Bruning,2 indicates that after annealing at 700°C, a 1.6 and a 2.0 wt pct B alloy were two phase whereas a 0.75 pct B alloy was single phase. Recent work3 using a hot-stage microscope has proposed a eutectic temperature of 743OC. This method utilized the observation of the onset of incipient melting at grain boundaries. The eutectic composition, however, was not determined. METHODS AND PR0CEDURES Five alloys were prepared by triple inert arc-melting high-purity palladium (95.98 pct) with additions of 2 to 6 pct purified amorphous boron. The alloys were crushed within a hardened steel mortar with a steel pestle. The 2 pct alloy, however, was too tough to be crushed in the above manner so was crushed by successive reductions through a rolling mill. Approximately 17 to 18 g of the crushed alloy was used in the thermal analysis. The alloys were melted in pure quartz crucibles. The thermocouple protection tubes were also of quartz and fused along the inside wall of crucibles to prevent floating of the thermocouple. This was an expediency as centering of the thermocouple in the melt would have been preferable. Melting was done in a tube furnace with a slow flow of tank helium maintained as a protective atmosphere. Heating and cooling rates were maintained at 3.5OC per min through the critical temperature ranges by means of a synchronous motor hook-up to a furnace controller. All specimens were heated to 100°C over the indicated liquidus on heating prior to reversing to the cooling cycle. Specimens emerged from the furnace with mirrorlike brightness attesting to the protective quality of the helium atmosphere. Thermal arrests were detected by the differential thermocouple technique using chrome l-alumel couples and nickel as the reference specimen. Arrests were recorded on a Leeds-Northrup automatic X-Y recorder. The specimen temperature and temperature difference were read to + 7.5OC and ± 1.5OC, respectively. These readings were well within the sensitivity of the instrument amplifier. Chromel-alumel couples were used in lieu of Pt-Rh as very few arrests were contemplated in excess of 1200" to 1300°C, the approach of instability. No standardization was performed on these thermocouples subsequent to their use. RESULTS The thermal arrest temperatures obtained are plotted in Fig. 1 as a function of wt pct B. The composition function was obtained by chemical analysis of portions of the specimens after the thermal analysis was completed. The 2 to 6 pct nominal alloys were found to have 1.80, 2.35, 3.65, 4.18 and 5.90

Jan 1, 1960

By E. R. Buchanan, R. E. Reed-Hill, F. W. Caldwell

Poly crystalline zirconium tensile specimens containing a sizable fraction of grains unfavorably oriented for slip were deformed at 77°K to strains as high as 9 pct. The contributions of the various twinning modes to the observed strain were deter~nlned quantitatively using measured twin volume fractions and Schrnid orientation factors. The results indicate that at very small strains twinning can account for almost all of the observed strain. At higher strains slip becomes the dominant means of deformation. The most significant form of twinning was {1121}. PLASTIC deformation in polycrystalline aggregates is poorly understood even today. This is primarily because slip cannot be easily observed or studied in the interior of a metal. On the other hand, twinning can be discerned inside a specimen after deformation. Twinning studies can therefore often yield quantitative information about polycrystalline deformation not otherwise obtainable. This investigation uses the above aspect of twinning in determining the contributions of twinning to the strain during tensile deformation at a cryogenic temperature (77°K). Polycrystalline zirconium was used as the object of study. There are several reasons why this information should be of value. In contrast to many metals, both the strength and ductility of zirconium increase with a corresponding decrease in temperature. This may be related to the fact that twinning becomes more profuse and complex with decreasing temperature. Secondly, it has been discovered that certain room-temperature properties of zirconium can be greatly improved by about 1 pct prestrain at 77°K. These include an increase in tensile elongation in critical directions by over 50 pctl and a large mechanical hysteresis effect.2 Both effects are believed to be related to twins formed by prestraining: plastic twin-boundary movements accounting for the increased ductility, and anelastic twin-boundary movements for the internal friction. Thirdly, hexagonal metals which twin primarily on only the (1012) mode (such as beryllium, zinc, and magnesium), unlike zirconium, are very limited in ductility at cryogenic temperatures. Therefore, the significance of the various types of twinning in zirconium at cryogenic temperatures is of more than academic interest. Three twinning mechanism-s have beenobserved in quantity at WOK, {1012), {1121), and {1122). Each must be considered as a unique deformation mechanism because of their markedly different twinning shears and basically different angles between twinning and basal planes, as shown in Table I. It is therefore necessary to separately consider the role of each of these twins during plastic deformation at 77°K. Fortunately, each twin possesses unique morphological features which makes its identification possible on a properly prepared metallographic section. The use of the polarized microscope3 can also greatly aid in identification of the various forms of twins. EXPERIMENTAL PROCEDURE Arc-melted sponge zirconium plate, previously describedY4 was machined into 1/8 by 1 1/4 in. threaded-end, round tensile test specimens. These specimens were deformed to the desired strains in a liquid-nitrogen cryostat mounted in an Instron testing machine. The tensile axis was the transverse plate direction. This specimen direction resulted in large numbers of grains in orientations unfavorable for deformation by prism or basal slip. Deformed specimens were sectioned, mounted in epoxy cold-mount resin, ground on metallographic papers, electropolished, and anodized to provide surfaces sensitive to polarized light. Standard quantitative metallographic procedures5

Jan 1, 1965

By R. E. Ogilvie, J. I. Goldstein

The a and y solubility limits in the Fe-Ni phase diagram have been redetermined at temperatures above 500°C. Both a diffusion-couple and a quench and anneal technique were used. The solubility limits were measured with an electron-probe micro-analyzer. The nickel concentration at the phase boundary is increased below 700°C and the a solid-solubility range is much larger than had been previously measured. The solubility limits are also extrapolated to 300°C. It is suggested that the solubility of nickel in a FeNi reaches a maximum in the temperature interval 400o to 500°C. THE equilibrium diagram has been of great use in the field of meteoritics, where the phase relations between kamacite (a) and taenite (?) in metallic meteorites can be described by means of the Fe-Ni diagram. The study of metallic meteorites by electron-probe microanalysis has cast some doubt on the accuracy of the presently available Fe-Ni diagrams.1, 2 Recent thermodynamic studies of the Fe-Ni system also suggest that the diagram may be in error.3 For these reasons the high-temperature (800o to 500°C) part of the diagram was redetermined. INTRODUCTION The currently accepted Fe-Ni diagram is that of Owen and Liu.4 Above 910°C, there is a region of complete solid solubility, ? (fee). Below 910°C, the a (bee) phase is stable in pure iron. The effect of increasing amounts of nickel is to stabilize the y phase. The phases that form when Fe-Ni alloys are heated or cooled bear little relation to the equilibrium diagram. If an alloy is cooled from the y state and held at a temperature within the a + y field, no evidence has been found for the occurrence of the y - a transformation.5 If the alloy is cooled to low enough temperatures the y phase breaks down into a supersaturated bee phase called a2. In fact, in alloys over 27 pet Ni the y phase is retained at room temperature.6 The a, phase has the same composition as the original y. The temperature at which a2 forms, the M, temperature, has been determined experimentally.&apos; A state of equilibrium can be approached by cooling below M, to form a2 and then reheating the alloy into the two-phase region of the diagram. The y phase will then begin to precipitate out of the a2 phase and grow. The growth of the phase, however, is quite slow. Using the interdiffusion coefficients -Da of Goldstein et al.,8 it is estimated that it takes about 1 year to grow a 10-µ-wide region of ? at 700°C in a 5 pet Ni alloy. Owen and Liu4 used the technique just described to form the equilibrium phases. The phases present were determined by means of X-ray analysis. The accuracy of their diagram depends on the number of alloys available near the phase boundary at a given temperature. In this study two different techniques were used to determine the a/a + ? and ?/a + ? solubility limits. The inherent accuracy of both techniques was greatly improved over that used by previous investigators because the phase-boundary compositions were measured with an electron-probe microanalyzer. PROCEDURE The two methods used to determine the Fe-Ni diagram are the diffusion couple (D.C.) and the quench-and-anneal (Q.+A.) techniques. In the first method, diffusion couples whose diffusion path goes through a two-phase region of the phase diagram were used. A description of the technique used for making the diffusion couples has been described in a previous paper.&apos; After the diffusion treatment a discontinuity in the resultant concentration vs distance profile was measured. The nickel concentrations in the a and ? phases at the interface of the discontinuity are the solubility limits of the a and ? phases in the phase diagram at the diffusion temperature. If the interface com-

Jan 1, 1965

By Stanley L. Lopata, Eric B. Kula

SEVERAL methods are available for determining pole figures by X-ray means.&apos; The earlier film methods have been replaced by techniques in which the intensities are measured by Geiger counters on an X-ray diffractometerZm7. These methods utilize either flat transmission or reflection samples,214°8 cylindrical specimens,3 or spherical specimens.7 A single transmission or reflection sample will not yield information over the complete pole figure. The cylindrical specimens suggested by Nortod and the spherical specimen of Jetter and Borie7 have the advantage of allowing the whole pole figure to be obtained without any corrections to the intensity for absorption, There is a lower limit to the size of sheet which can be conveniently studied, however, and sample preparation can be rather tedious. Probably the most common method today for determining the complete pole figure is that developed by Schulz. A flat reflection sample is used for determining the pole figure from the center out to about 70". Because of the geometry of the system used, little or no correction for absorption or irradiated volume is necessary.4&apos;6 A separate transmission sample is used for the region near the edge of the pole figure. This procedure requires two separate samples, one of which must be a thin carefully-prepared transmission sample. Furthermore, since the reflection and transmission data are in different arbitrary intensity units, a region of overlap must be obtained, and the intensity data from one set of measurements converted to units of the other. These are serious disadvantages of this method, and they point out the need for a simplified procedure. Since the reflection technique can be used for planes whose normals lie up to about 70° from the sample surface normal, it is apparent that a complete pole figure can be obtained by reflection alone if sample surfaces are cut at oblique angles to the rolling plane Specifically, if a rolled sample is cut so that the normal to the surface formed lies equidistant (54" 44&apos;) from the rolling plane normal, rolling direction, and transverse direction, then complete information for one quadrant of the pole figure can be obtained by reflection from the surface. Fig. 1 shows this oblique surface, as well as the position of the pole of this surface in the pole figure. When a surface has been cut oblique to the rolling plane, the standard polar stereographic net is inconvenient to use, and it would be more desirable to have the center of the net coincide with the pole of the oblique plane. Fig. 2 shows such a net, where the center has been offset 54&apos; 44&apos; to correspond to a specimen cut as in Fig. 1. This net was in effect obtained by rotating a standard polar stereographic net 54" 44&apos; with the help of a Wulff net. With the experimental setup used. a sample can be cut from plate of 1/2-in. thickness or br Gen- erally thinner sheet is under investigation, and a composite specimen must be used. A convenient procedure has been to bond together, using epoxy resin, sufficient sheets to form a cube. These are clamped in a vise, and when dry, the whole vise is rotated and a flat surface ground at the required angle. The sample is then mounted inside a larger steel ring using Koldmount, the backside ground flat and parallel to the approximate desired thickness. The sample is then polished and etched to remove any effects of cold working during grinding. With this method only one quadrant of the pole figure is obtained. Often pole figures show symmetry around the rolling and transverse directions, and any slight asymmetry is due to scatter. Should the pole figure not be symmetrical, four oblique surfaces, corresponding to the four quadrants of the pole figure, would have to be examined. In most cases there is symmetry at least around the rolling direction, which reduces to two the number of quadrants to be investigated. For many purposes all that is required is an average polefigure for the four quadrants. This canreadilybe obtained with composite specimens of sheet material, where sheets Corresponding to each of the four quadrants can be intermixed. The four quadrants can be obtained by considering sheet in the normal position, and by rotatiolls of 180" around the sheet normal, the rolling direction, and the transverse direction. If desired, the whole thickness of the sheet can be used, yielding an average of the surface and interior textures; or the surface material can be removed from each sheet, resulting in a pole figure for the center alone. Eugene S. Meieran of the Massachusetts Institute of Technology has independently developed the same method. His results, adapted to a pole figure goniometer with a specimen spiraler, will be described in another publication.

Jan 1, 1962

By Paul A. Farrar, Harold Margolin

The system Ti-Cr has been re investigated From 40 to 100 pct Cr. The high-temperature modification of TiCr, was found to exist in the temperature range from 1365 where it terminates in the eutectoid reaction TiCr,(TI)* — HE chromium-rich region of the Ti-Cr system was investigated by Vogel and Wenderott,&apos; Mc Quillan,&apos; Van Thyne et dl.,&apos; and Cuff Duwez and Taylor determined the crystal structure of the low-temeperature modification of TiCr, to be fcc a = 6.943A and Levinger&apos; discovered the existence of a second (high-temperature) modification of TiCr, and determited its crystal structure to be hexagonal a = 4.932A, c/a = 1.617i. No information was obtained as to the temperature range over which each modification of TiCr? existed; therefore the present investigation was initiated. I) Experimental Techniques Alloys employed for the delination of this system were prepared from iodide titanium and high-purity chromium. The purity of these materials is as follows: Iodide titanium: purity 99.99 pct; major impurities—carbon 0.0001 pct; oxygen 0 to 0.002 pct; nitrogen 0 to 0.002 pct; silicon 0 to 0.005 pct; manganese 0.001 pct; copper 0.001 pct (Foote Mineral Co., Lot 609-29). Chromium #1: metallic purity 99.997 min.; interstitial content—oxygen 0.27 to 0.46 pct; hydrogen 0.028 to 0.038 pct; nitrogen 0.0002 pct (Ave-quipo Inc.). Chromium #2: purity 99.9 pct; major impurities—carbon 0.01 pct; oxygen 0.013 pct; nitrogen 0.02 pct; silicon 0.01 pct; sulfur 0.03 pct; iron 0.01 pct (Fulmer Research Institute Ltd.). A total of sixteen alloys of thirteen different compositions was prepared in the range from 40 to 95&apos; *All percentages are given in weight percent. pct Cr. The compositions of the alloys prepared were as follows: Ti-40, 45, 50, 60, 62, 64, 66, 68, 70, 80, 85, 90, and 95 pct Cr. Two buttons were prepared of the 66, 90, and 95 pct Cr alloys. The 40 pct Cr and one of the 66 pct Cr alloys were prepared from the chromium # 2. All the other alloys were prepared from chromium #1. The alloys were arc-melted as 25-g buttons in a copper-hearth glass-walled furnace7 under an inert atmosphere of high-purity helium. The alloys were sintered at 250 amp and melted twice at 350 amp for 30 sec with the buttons being turned over between melts. Weight losses during melting were determined and in the range 45 to 68 pct Cr they were found, in all cases, to be less than 1.25 pct of the total alloy weight. A number of the high-chromium alloys shattered during cooling from either the first or second melt, which made the weight loss considerably larger than usual. The 70 and 80 pct alloys lost approximately 5.7 pct of their total weight, the 85 pct alloys 1.5 pct, the 90 pct alloy 2 pct, and the 95 pct alloy 3 pct. However, it is felt that the actual composition of the alloys in this region is probably within approximately 1 pct of the intended composition, as a large portion of the material lost was that due to shattering after melting. Nominal compositions were therefore used in plotting data and referring to the alloys. The alloys were cut into specimens, wrapped in molybdenum sheet, and encapsuled in argon-filled quartz or Vycor tubes for heat treatment. The heat-treatment times and temperatures are given in Table I. The specimens were quenched in iced brine (I.B.Q.) following heat treatment. The standard techniques of grinding, polishing., and etching were used in preparing the specimens for metallo-graphic examination. For alloys below 68 pct Cr

Jan 1, 1963

By Paul A. Farrar, Felix Ermains, Harold Margolin

The systems Ti-Crand Ti-Vhave been reinvesti-gated in the region up to 40 wt pct alloying addition using both conventional and rapid quenching techniques. The Ti-Cr eutectoid temperature was determined to be at 667° & 10° C and 14.5 wt pct Cr. The solubility of the Cr in a Ti was found to be less than 1 pctat 700"C. The P transus of the Ti-V system was found to be depressed to 510°C at 40 wt pct V and the solubility of V in a Ti was found to be less than 2 wt pct at 700°C. Investigation by a. d. McQuillan1-3and m. k. McQuillan4 on the systems Ti-Co, Ti-Cr, Ti-Cu, Ti-Fe, Ti-Mn, Ti-Ni, and Ti-V has cast doubt as to the position of the ß/a + ß boundaries in many of these systems. Their investigations were carried out using hydrogen pressure and/or rapid quenching experiments, as opposed to the conventional quartz capsule techniques employed by most other investigator.&apos;" By these methods, the ß/a + ß boundary was found to be lower than that obtained by conventional techniques in all except the Ti-Fe system. In the latter, the ß/a + ß boundary was essentially the same as the boundary obtained by conventional technique.7&apos; On the basis of rapid quenching results in the Ti-Cr system, M. K. McQuillan4 placed the eutectoid temperature below 550°C whereas other investigations using conventional techniques had placed the eutectoid variously as between 650&apos; and 700°C,5 between 675&apos; and 700°C,6 between 650" and 675°C,7 at 670°C,8 and above 625"C.la9l3 In order to check these results, a reinvestigation of four of the systems was undertaken using both conventional and rapid-quenching techniques. The Ti-Fe and Ti-Mn systems will be dealt with in anoth er paper, with only the Ti-Cr and Ti-V systems being discussed here. EXPERIMENTAL TECHNIQUES Alloys employed for the delineation of the systems under investigation were prepared from iodide titanium sheet capsules containing the alloying materials,

Jan 1, 1962

By Wilhelm in der Schmitten

A necessary condition for a uniaxial stress distribution in compression testing is that the specimen end surfaces make full contact with the apparatus compression plates. In addition all compression surfaces must be machined perpendicularly to the loading axis. In general this condition is not sufficiently fulfilled in a simple apparatus. Therefore on application of the load the compression plate may first touch the specimen at one point only. This may cause crumbling of the specimen if the material under investigation is brittle (e.g., ionic crystals). It also precludes a precise study of the beginning of deformation as the effective cross sectional area is unknown. In addition a complex stress state is set up which renders quantitative work impossible, e.g., on dislocation density and arrangement as a function of stress. To overcome these difficulties a "self-adjusting" upper compression plate is required. A simple and reliable method of achieving this is shown in Fig. 1: A steel hemisphere is placed on the specimen. As soon as the compression plate (which no longer needs precise machining) makes contact with this hemisphere the load is uniformly distributed over the whole specimen surface, and a homogeneous uniaxial state of stress results. An advantage of the method is that the loading is always central, even when the specimen surface is not parallel to the compression plate (Fig. 1, dashed line). Therefore to a first approximation a uniaxial state of stress is maintained if the misorientation of the specimen end surface is small. Two typical stress strain curves of identically prepared sodium chloride crystals are shown in Fig. 2; curve 1 was taken without and curve II with the hemisphere under otherwise identical conditions. The improvement in the accuracy of defining the beginning of elastic and plastic deformation is clearly indicated. The writer wishes to thank the Deutsche Forschungsgemeinschaft for financial support, and Professor P. Haasen for providing facilities for this work.

Jan 1, 1962