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By F. G. Tahmoush, N. J. Grant, E. P. Abrahamson

The effect of grain size on the brittle -ductile transition temperature of pure iron and three dilute Fe-W alloys has been investigated by slow bend tests. The brittle-ductile transition temperature for pure iron increased with increasing grain sizes from 8000 to 500 grains per sq mm where the transition temperature then decreased with further increase in grain size. The dilute additions of tungsten lowered the transition temperature for fine grain sizes, suppressed a reversal of the curve in the coarse grained portion, and raised the transition temperature for this region. The frequency of twin occurrence increased with increasing grain size and decreasing temperature. The object of the present investigation was to re-examine the effect of grain size on the brittle -ductile transition of pure iron and several dilute Fe-W alloys. Current literature normally presents a simple relationship between grain size and the brittle-ductile transition temperature, namely, that the transition temperature increases with increasing grain size. Heslop and etch' have studied the transition temperature of mild steel by V-notch Charpy impact tests for the grain size range between 200 and 6000 grains per sq mm. The result was a linear plot of In 1-1/2 vs brittle-ductile transition temperature, where 1 is the grain diameter. Recent experiments by sipos2 revealed the possibility of a reversal in the slope of the grain size vs transition temperature plot for pure iron; however, his investigation was limited in scope, and the data obtained were insufficient to permit a definitive curve. The present investigation was undertaken in an effort to confirm or extend the grain size effect observed in iron by Sipos. PROCEDURE All alloys were vacuum induction melted, using 99.95 pct Fe containing 0.03 pct 0 and 0.004 pct C. Four ingots were made, ranging from pure iron to iron with 0.035 pct W. The chemical composition of each alloy, after processing, is given in Table I. The four alloys were prepared as 45 lb heats and cast into 4 in. diam by 16 in. molds. They were then extruded into 3/4 in. rods at 1800oF. Specimens for chemical analysis, taken from various positions along the rods, revealed no variation in tungsten content along the length. The extruded rods were reduced to 0.156 in. diam stock by a series of cold swaging operations involving intermediate vacuum annealing treatments. This procedure yielded a final cold reduction in area ranging from 10 to 90 pct. The swaged rods were chemically cleaned, cold pressed to a cross section of 0.10 by 0.18 by 1.0 in. long (2.54 by 4.73 by 25 mm). The specimens were wrapped in iron foil and vacuum sealed (10-4 mm Hg) in quartz. Various heat treatments at temperatures from 700" to 1300oC were utilized to produce grain sizes from 8000 to 1 grain per sq mm. Grain sizes were determined by measuring the average area of grains in a polished section. In specimens with grain size greater than 20 grains per sq mm, the total number of grains in the cross section was counted and then divided by the area to yield grains per sq mm. Grain size was measured both for longitudinal and transverse cross sections. The average of the two measurements was plotted vs transition temperature. An Instron Table Model testing machine was used to determine the transition temperature of specimens tested in three point horizontal bending. The specimen was supported by two 1/4 in. dowels one in. apart. Bending was accomplished with a push rod, the end of which had an 1/8 in. radius. The head speed was 50 in. per min. Temperatures were established through the use

Jan 1, 1963

By G. W. Tuffnell, S. Floreen

Three Fe-18 pet Ni-base ternary alloys cortaining carbon, molybdenum, or cobalt were aged to pgroduce hardening by carbides, Ni3Mo, or ordering, respectively. Each alloy was tested in rotating-beam fatigue tests after hardening to 195 ksi ultim.ate tensile strength. The fatigue properties of three alloys soere essentially identical. The results suggest that tlze fatigae strength of an igron-base alloy should depend primarily upon the tensile strength, and not iipon the hardening mecaanisrn. THE fatigue strengths of many steels have been found to be directly related to their ultimate tensile strengths. For ultimate strengths below 200 ksi, the fatigue endurance limit at 107 to 10' cycles is approximately half the ultimate strength. Essen- tially all of the steels that have been tested, however, have been hardened by carbon. Thus it is not certain whether the relationship between fatigue and ultimate strengths is a general one that applies for other types of hardening in steels, or whether it applies only for the particular method of hardening by carbon. The recent developments of the martensitic precipitation-hardened stainless steels and the marag-ing steels have shown that it is possible to achieve high strengths in iron-base alloys by other hardening mechanisms than that due to carbon. Therefore, it is now possible to compare the fatigue properties of several iron alloys having the same ultimate strengths but hardened by different mechanisms. For the present study a binary Fe-18 pct Ni martensite was selected as a base material. This particular matrix composition has been found to have deformation characteristics very similar to pure iron.' Three ternary alloys were prepared by adding either 0.23 wt pct C, 5 wt pct Mo, or 20 wt pct Co to this base composition. After suitable heat

Jan 1, 1965

By J. F. Butler

The degree and type of carbide dispersion resulting from changes in the cooling rate from austenite determine the amount of carbon remaining in solution after slow cooling- from a subsequent subcritical annealing treatment. A difjusion model has been proposecl to explain the effect of carbide dispersion on the amount of carbon retained in solution and the amount of carbon in solution has been related to the degree of carbon strain aging. COTTRELL and Leak' have shown that the rate of strain aging in low-carbon steels is dependent upon the amount of carbon and nitrogen in solution. Carbon can be effectively removed from solution as Fe , C by quench aging at temperatures of 200" C or lower; however, the relatively higher solubility of nitrogen at these temperatures prevents sufficient removal of nitrogen as iron nitrides. For this reason, nitrogen in solution has been considered the major cause of strain aging in rimming grades of commercial low-carbon steels. Nitrogen can be effectively removed from solution and nonaging steel produced through the addition of aluminum to form the stable nitride, AlN; however, the aluminum also causes deoxidation resulting in a killed steel. III an attempt to produce a rimmed steel which was also nonaging, Morgan and Shyne 2 investigated tile strain-aging properties of low-carban steels containing boron and found that strain aging was suplx-essed in steels containing as little as 0.007 pet B. The original purpose of this investigation was to determine the mechanism of strain-aging suppression by boron. Early in the study, the function of boron was discovered to be much like that of aluminum in that the formation of a nitride, BN, removed the nitrogen from solution.' However, during the course of the investigation, an effect of heat treatment upon the strain-aging properties and the amount of carbon in solution was found which could be related to the microstructure of the steel. The purpose of this paper is to examine these relationships among heat treatment, microstructure, carbon in solution, and strain aging in steels where nondetectable amounts of nitrogen are present in solution. EXPERIMENTAL PROCEDURE The investigation was carried out using 0.030 in. by 12. in wire specimens which had been cold swaged and drawn to the final diameter. Table I lists the compositions of the low-carbon steels used. Those with 'V' designations were vacuum melted and cast; the alloys designated 'AISI' were prepared from high-purity iron obtained from the American

Jan 1, 1962

By K. M. Rolls, R. M. Rose, H. B. Shukovsky

Studies of the phase structure, critical current density, and resistive critical magnetic field of a 45 pct Nb-55 pct Zr superconducting alloy after final-size heat treatments are reported in this paper. A combination of optical metallography, X-ray diffraction, and electrical-resistivity measurements were used to determine the phase structure. Superconductivity measurements, made with heat-treated wires, are correlated with microstructure. Although no quantitative relationship between microstructure and critical current density is found, it is shown that SINCE Kunzler1 as well as Berlincourt, Hake, and Leslie2 first described the high-field, high-current-density superconductivity of Nb-Zr alloys, it has be- the critical current density is highest when the microstructure is finely divided by fibering, coring, precipitation, or fine-scale phase dispersions. The resistive critical field is very sensitive to the compositions of the phases present. Since the alloy investigated here is near the maximum resistive critical field for the Nb-Zr system, any phase decomposition results in a lower H,. Elimination of the effects of cold work lowers H, also. A possible interpretation of the latter in terms of internal surface superconductivity is suggested. come apparent that the resistive critical field and the current-carrying capacity of such alloys are, in large measure, dependent on composition and processing. The resistive critical magnetic field (Hr) for low current densities has been found to increase progressively with zirconium content until a flat maximum is reached between 50 and 65 pet Zr.3 For any single composition, a characteristic maximum value of H, is attained by heavily cold-drawn wire.4 critical current density (J,) depends not only upon cold work but also, apparently, upon microstructure. Heat treatments of cold-worked wires generally

Jan 1, 1965

By H. E. Biber

DURING the production of tin plate a thin layer of FeSn2, is formed at the interface between the steel sheet and the protective tin coating. Because excessive amounts of this alloy layer are undesirable, the kinetics of its formation is a subject of interest in the tin-plate industry. A recent study of this subject at our laboratory uncovered a relationship which should be of general interest to anyone studying kinetics of reactions in metallic systems. It had been previously concluded that, at any given temperature in the range 175" to 330°C, the Fe-Sn alloy layer would have a parabolic growth rate.1,2 However, our studies showed that this rule apparently holds only when the tin plate is heated very slowly to the "reaction" temperature; when the tin plate is rapidly heated, considerably different growth rates occur. An example of this effect of heating rate on growth behavior is contained in the accompanying results of alloy-layer growth measurements at 240°C in oil baths stirred at 10,500, 1800, and 0 rpm. The heating curves for these three conditions are given in Fig. 1, and the growth data are presented in Fig. 2. With the rapid heating rate, provided by the stirring at 10,500 rpm, the alloy layer had three distinct stages of growth. In the initial stage, which persisted well beyond the time required to heat the tin plate to bath temperature, the alloy layer formed very rapidly. The growth followed a rate law of the form w = ktn where n > 1. This initial stage was followed by a growth-retardation stage of about 50-sec duration in which little additional alloy was formed. In the third stage the growth again followed a rate law of the form w = ktn, but here « =0.3. With the intermediate heating rate provided by stirring at 1800 rpm, the three-stage nature was less pronounced and the slope of the third stage increased (i.e., n > 0.3). With the slow heating rate provided by the unstirred oil bath, the alloy layer grew in two stages. The initial rapid-growth stage persisted only until the specimen was heated to bath temperature, no growth retardation was observed, and the slope of the main portion of the plotted data was greater than in the stirred baths, having a value of almost 0.5. Similar results were obtained for other bath temperatures in the range 200" to 300°C. This effect of heating rate on growth behavior may be due to changes in the rate of nucleation of FeSn, crystallites. The iron and tin are in contact from the onset of heating. Thus the initial formation of FeSn, occurs not at the "reaction" temperature but rather while the tin plate is being heated to that temperature. Because nucleation is in general temperature-dependent, different heating rates could cause different over-all nucleation rates, which in turn could cause different growth behaviors. A more detailed discussion of the growth of Fe-Sn alloy layer and the effect of heating rate will be published shortly.

Jan 1, 1965

By R. A. Nadler and

Specimens of Ti-155A (Ti-5Al-1.3Fe-1.3Cr-1.2Mo), Ti-6Al-4V and Ti-4Al-3Mo-1V were hydrogenated, aged to high strength levels, and subjected to notched stress-rupture tests and tensile tests at two strain rates. Both Ti-6Al-4V and Ti-155A were relatively unaffected by hydrogen in amounts exceeding those found in commercially -produced material. Inconsistencies in the data and a relatively low initial level of ductility prevented an accurate determination of the hydrogen tolerance for aged Ti-4Al-3Mo-1V, but there was no evidence that this alloy was any more susceptible to hydrogen embrittlement than Ti-155A and Ti-6A1-4V. THE metallurgical literature has been considerably enriched in the past five years by the publication of the results of many investigations which were concerned with the effects of hydrogen on titanium and its alloys. Although it is not the authors' intention to provide a complete literature survey of this vast field, it is worthwhile to summarize briefly some of the important factors which influence the embrittling phenomenon in a - B alloys. Some of the influencing factors are those of strain rate, temperature, and composition. Hydrogen embrittlement in a - B titanium alloys is now believed to be a strain-induced phenomenon, and whether or not embrittlement occurs at high hydrogen levels depends largely upon whether sufficient time is available for hydride precipitation. This condition is fulfilled by tensile testing at very slow strain rates or by rupture testing smooth or, preferably, notched specimens over relatively long periods. Conveniently, maximum embrittlement occurs at or near room temperature. The presence B - stabilizing elements, in amounts sufficiently small to prevent an all -B or nearly all -P condition, promotes hydrogen embrittlement and this tendency is believed to be related to the amount of a - B interfacial area present. Aluminum, by increasing the solubility of hydrogen in A titanium, greatly reduces the danger of hydrogen embrittlement, while oxygen has been shown to have detrimental effects.' The preceding discussion is based on experimental work performed on annealed a - P alloys. This early work has shown that annealed Ti-6A1-4V and Ti-155A are relatively insensitive to the embrittling effects of hydrogen.' Although no work has been reported on annealed Ti-4A1-3Mo-lV, the alloy would be expected to exhibit somewhat the same insensitiv-ity as Ti-155A. In sharp contrast to the voluminous literature on annealed titanium alloys is the paucity of reported investigations on materials receiving commercial heat-treatment cycles. To date, the most notable contributions in this field have arisen from two separate investigations on Ti-3Mn-1Fe-1Cr-1V-lMo, the so-called 3Mn comple~. These investigations

Jan 1, 1961

By Charles Wurms, Robert Steinitz

DURING an investigation to determine the compatibility of several metals with tungsten, the degree of reaction between tungsten and lead was determined. A literature survey showed considerable disagreement between the results of various earlier investigators. Information presented by M. Hansen1 states that, according to S. Inouye,2 tungsten has very poor resistance against attack by molten lead, even at the low temperature near the melting point of lead. A phase diagram in the same reference indicates a solubility of 30 wt pct W in molten lead at 1300°C. Contrary evidence was shown by Parkman and shepard3 in their investigation of materials for use in heat transfer systems containing liquid lead alloys; they performed experiments at 980°C for times up to 50 hr without noticing any appreciable attack on the tungsten. Tungsten sheet was immersed in molten lead contained in Vycor tubes evacuated to at least 10-4 mm Hg. R. Bernard4 and R. I. Jaffee5 also indicate that no reaction occurs between molten lead and tungsten. However, no experimental data were included in these reports. In order to settle the question of the solubility of tungsten in molten lead, tungsten powder with an average Fisher subsieve particle size of 6µ was pressed in a double-acting die at 6 tsi to small compacts. They were then sintered in an atmosphere of hydrogen for 2 hr at 1700°C, resulting in a sintered density of 64 pct of theoretical with final dimensions of 0.260 in. in height and 0.245 in. in diameter. For all tests, the tungsten pellets were immersed in molten lead. Table I is a summary of the experimental procedures showing atmospheres, temperatures, and times. The first experiments were performed at 650°C; at this temperature, the liquid lead should wet the porous tungsten better than at its melting point, and penetrate into the pores. The lead was heated in a graphite crucible with a graphite cover. No protective atmosphere was used, as it was expected that the formation of CO would be sufficient to prevent oxidation. This, however, proved to be wrong, and all tungsten samples showed a slight oxide film after treatment. The tungsten samples were immersed in the molten lead for times of 5 min, 10 min, 1/2 hr, 1 hr, and 2 hr. After this time, the melt was poured into a form and the

Jan 1, 1962

By C. E. Ells, A. Sawatzky

The effect of neutron irradiation on tensile properties of the Zr-2.5 wt pet Nb-0.5 wt pet Cu alloy has been evaluated for integrated neutron fluxes up to 3 x 1020 n per sq cm (E > 1 Mev). Specimen temperature during irradiation was normally 300°C. The material was studied both in annealed and in quenched and aged conditions. When the alloy (fab-ricatedfrom sponge zirconium) is quenched from a temperature =40°C below the a + ß/ß transformation and aged 6 hr at 535oC, neutron irradiation up to the maximum studied has little effect 071 reduction in area, although there is a drop in uniform elongation and the yield strength is increased by = 25 pct. Conversely, irradiation of the alloy in an annealed condition can result in much greater changes in properties, with yield-strength increases of up to 200 pet. The dose dependence of irradiation hardening obeys the saturation equntion proposed by Makin and Minter to explain hardening in copper and nickel: Act = C[1 - exp(-Døt)/1/2 A rnodel is proposed to explain the effect of niobium content and metallurgical condition on irradiatiotz behavior. THE Zr-Nb alloys form a class of material susceptible to marked strengthening by quench and age heat treatment. With niobium concentrations as low as 2.5 wt pet, strengths can be developed which are double those of annealed zircaloy-2.1 Since the neutron-capture cross section of the Zr-2.5 wt pet Nb alloy is nearly identical to that of Zircaloy-2, significant gains in power-reactor neutron economy could be obtained by replacing stressed in-reactor components of Zircaloy-2 with the heat-treated Zr-Nb alloy. When the solution heat-treatment temperature is in the high (a + ß) phase, then the tensile properties of the quenched (and aged at 500°C) material have been shown to be relatively insensitive to neutron irradiation.1-3 Addition of small quantities of copper to the binary Zr-2.5 wt pet Nb alloy gives a useful reduction to the corrosion rate in air and carbon di- oxide,&apos; and a ternary alloy of composition Zr-2.5 wt pet Nb-0.5 wt pet Cu was chosen for one component in the Douglas Point Reactor. This application utilizes both the corrosion resistance to a moist air-carbon dioxide environment and the strength developed by a quench and age heat treatment. By suitable choice of solution heat treatment and aging temperatures, tensile properties of the ternary alloy can be made nearly identical to those considered as optimum for the binary alloy. One effect of the copper addition, however, is to give marked changes in the aging kinetics of the alloy.&apos; For this reason, it appeared that neutron irradiation might promote overaging in the ternary alloy, particularly at the elevated service temperature (=300°C). This paper describes the effect of neutron irradiation on the tensile behavior of the Zr-2.5 wt pet Nb-0.5 wt pet Cu alloy in several metallurgical conditions pertinent to its use as a reactor material. The metallurgical conditions included those for which aging occurs in the unirradiated material, and fully annealed conditions for which a higher degree of thermal stability could be expected. 1) EXPERIMENTAL Two batches of alloy were used, both made from sponge zirconium. The fabricator&apos;s analysis of principle constituents showed no significant difference between the two batches, Table I. The rod material was rolled to 1.5 in. diam, and then swaged to final sizes of 0.5 to 0.375 in. diam at nominal temperatures of 785" and 625°C for the AM and AS batches, respectively. Subsequent hydrogen analyses at CRNL confirmed that the hydrogen concentration of the as-received rod was indeed <20 ppm. However, it was found that the (a + ß)/ß transus for the AM material was approximately 25°C lower than that of the AS material, indicating rather more difference in oxygen concentration than given in Table I. Except for a small difference in yield-point behavior, the tensile prop-

Jan 1, 1965

By J. B. Clark, A. J. McEvily, R. L. Snyder

The nonuniform distribution of precipitate particles has been recognized as a leading factor contributing to the relatively low fatigue resistance of aluminum alloys. The structure of many of these alloys is characterized by narrow precipitate-free zones adjacent to the grain boundaries. Alloys with such zones exhibit a tendency for brittle inter crystalline fracture. The interrelation between this type of structure and mechanical properties was investigated in an Al-10 wt pct Mg alloy. It was found that deformation during fatigue occurs preferentially along these zones and cracks initiate there. In Al-10wt pct Mg, the zones were found to be supersaturated even after extensive general precipitation and are due to the absence of proper precipitate nuclei in the region near the grain boundaries. Cold working the alloy prior to aging improves the mechanical properties by inducing precipitation within the zones and also by jogging of grain boundaries. The mode of fracture is changed from brittle inter crystalline to more ductile trans granular fracture. THE process of fatigue is highly structure sensitive, with the strength of the whole often dependent upon some localized discontinuity, either geometrical or metallurgical in nature. Much has been learned about the role of geometrical discontinuities, e.g., notches, in fatigue, but with the exception of the effects of inclusions or the shapes of carbides, relatively little is known about the specific effects of discontinuities in metallurgical structure such as nonuniform precipitation. In most age-hardening aluminum alloys, metallo-graphic studies have shown that the extent of precipitation adjacent to grain boundaries is much less than that which occurs in the interior of the grains. The width of these almost precipitate-free regions, which are sometimes called denuded zones, and the extent of solute depletion within them, are dependent upon the particular alloy and its aging treatment. It has been observed1 that these zones are relatively soft with the result that plastic deformation takes place preferentially within them. It has also been shown 2-4 that there exists a tendency for intercrys- talline cracking in fatigue when such zones are present. It is of interest to note that Broom et al.2,3 were able to reduce the incidence of this type of failure in an A1-4 wt pct Cu alloy by stretching the material 10 pct prior to aging. In the present study, the effects of precipitate-free regions on the fatigue properties of an A1-10 wt pct Mg alloy were studied in detail, and the effects of deformation prior to aging on the nature of the precipitation process as well as on fatigue properties were also investigated. MATERIAL AND PROCESSING An A1-10 wt pct Mg alloy was selected for this study, because it was known that well-defined precipitate-free regions along the grain boundaries are readily obtained in this alloy after aging at 200oC.5 The starting materials were 99.998 pct A1 and singly sublimed magnesium of about 99.9 pct purity. The aluminum was induction melted in a graphite crucible, and then the magnesium addition was immersed until dissolved. Chlorine gas was then bubbled through the molten alloy for 4 min to degas the melt, after which the melt was cast at a pouring temperature of 730" to 760°C into a cold, graphite-coated, tapered steel mold. Since A1-Mg alloys are difficult to homogenize,5 special care was taken to obtain a uniform composition. Two-in. cubes were cut from the ingot and heated at 446°C for 30 min. These cubes were then hot forged approximately 35 pct in each of the three cube directions and homogenized for 16 hr at 446°C. Sheet specimens were then obtained by pressing 40 pct and rolling 35 pct per pass with reheating between reduction steps to a final thickness of approximately 0.10 in. The sheet was then solution treated for 16 hr at 446°C and water quenched. The age hardening behavior of this material at 200°C was then determined, and the results are shown in Fig. 1. The age hardening of this alloy when subjected to cold work prior to aging is also shown in this figure. Preliminary work indicated that extensive deformation after quenching was required to affect drastically the precipitate-free regions in this alloy, and a rolling reduction of 50 pct was chosen. For purposes of comparison the following three conditions were studied: a) Solution treated, quenched, and aged 20 hr at 200°C

Jan 1, 1963

By C. H. Li, S. H. Bendel, J. A. Sartell

Small additions of Mg to a 62 Cu-38 Ni alloy reduce the oxidation yates drastically between 500° and 850°C. Metallographic examination of the oxide scale disclosed a continuous network, identified by X-ray diffraction as (Ni, Mg)O solid solutions, located along the former alloy grain boundaries. This network acts as a barrier to diffusion. It is thought to result from the segregation of mg to the alloy grain boundaries. Oxidation occurs preferentially in these regions because of the presence of this more active element. To substantiate these ideas, homogenized alloys ulere oxidized. No oxide network was produced and oxidation rates were the same as for the parent 62 Cu-38 Ni alloy. An interesting aspect of the oxidation of the 62 Cu-38 Ni alloy previously described by the present authors, is the relationship between oxidation kinetics and changes in the microstructure of the oxide.&apos; The oxide scale on these alloys consists of two layers: a thin layer of CuO outside a much thicker layer of Cu20 in which particles of NiO are dispersed. In addition, immediately beneath the oxide-metal interface there is an internally oxidized zone in which NiO particles are dispersed in a copper-rich alloy matrix. Experimental observations on the growth of the individual layers under isothermal conditions have led to the conclusion that the rate-determining step in the oxidation of this alloy is the diffusion of anions through the Cu20 layer. It has been found that this diffusion rate is increased by the recrystallization of the outer CuO layer. Willardson and Gorton have reported that the addition of magnesium to the 62 Cu-38 Ni alloy causes a decrease in the oxidation rate.2 The present investigation was undertaken in order to determine the mechanism by which magnesium additions improve the oxidation resistance of the 62 Cu-38 Ni alloy. EXPERIMENTAL PROCEDURE Fifty-gram ingots of Cu-Ni alloys were prepared by vacuum melting materials of 99.999+ pct purity. These ingots were then remelted in a He atmos- phere and magnesium added in the form of a previously prepared and analyzed Cu-Mg master alloy. This procedure was necessitated by the high reactivity of pure magnesium at high temperatures. The proportion of the alloying elements was adjusted so as to obtain alloys with the desired magnesium content while maintaining a Cu-Ni ratio of 62 :38 by weight. (All alloy compositions will be given in weight percent.) Since it was considered desirable to study the oxidation of only single-phase, solid-solution alloys, it was necessary first to determine the approximate limit of solid solubility of magnesium in the 62 Cu-38 Ni alloy. A series of melts with various magnesium contents was made, homogenized by annealing for 48 hr at 975OC, then cooled in the furnace. Metallographic samples were prepared, etched in a potassium dichromate solution and examined at XI500 for the presence of a second phase. The alloys were then chemically analyzed and it was found that the approximate limit of solid solubility of magnesium in the 62 Cu-38 Ni alloy was 1 pct Mg. The ingots containing less than 1 pct Mg (0.19, 0.29, 0.58, and 0.87 pct Mg) were cold-rolled down to thicknesses suitable for oxidation experiments and specimens for gravimetric studies were cut to dimensions of 3.0 by 1.5 by 0.05 cm, specimens for inert marker studies, 0.6 by 0.6 by 0.17 cm. These were heat-treated in a protective atmosphere at a temperature (975" C) well above the oxidation temperatures and furnace-cooled to insure structural stability of the alloy during oxidation. Immediately prior to oxidation, the specimens were chemically cleaned by immersion for 1 min in a solution of 2 parts nitric acid, 1 part acetic

Jan 1, 1961

By N. A. D. Parlee, I. D. Shah, W. C. Phelps

THIS note reports on a continuation of a program on the thermodynamics of Fe-S-X systems in the "steel-burning" temperature range begun by Bock, Barloga, and parlee.&apos; Small coils of 0.039-in.-diameter pure iron (Ferrovac-E) wire were equilibrated with Fe-S-0 melts in ingot iron crucibles under argon at 1324°C in the assembly shown in Fig. 1, the lower part of which was heated in a large Globar furnace. Fig. 1 shows (R) the coiled iron wire sample, (M) the Fe-S-0 melt prepared from desired proportions of ferrous sulfide and ferric oxide, (K) the iron crucible, (I) a mullite guide tube, (J) an alumina crucible, (L) alundum sand, (N) crushed mullite, (Q) hollow cylinders of K30 brick, (C) a steel rod, (B), (El, (F), (G), (P), and (O), details of brass water-cooled head, and (H) a mullite tube 2-3/4 in. ID and 26 in. long. The rod (C) bearing the sample could be removed at will and be replaced by a tube for sampling the melt, or by a thermocouple for comparing the melt temperature with a control thermocouple not far from the 2-3/4-in. mullite tube. After equilibration the iron coils were treated with acid to remove the outer layer of metal and then they were analyzed for sulfur by a standard combustion method. The melt samples were analyzed for oxygen by a variation of Lander&apos;s2 hydrogen-reduction method for mattes, and for sulfur by the ASTM combustion-iodometric method NO. E 30-47. When the results of some forty-two runs were examined it was found that the sulfur and oxygen contents of the equilibrated melts showed good consistency, in that the plotted compositions fell along the smooth curve shown in Fig. 2. The points on this curve represent the experimental compositions of melts in equilibrium with ?-iron (Fe-S-0) solid solutions. These solid solutions are saturated with sulfur and oxygen with respect to the melt and therefore have the same sulfur and oxygen activities as the melt. The curve drawn through the points therefore delineates the ? liquidus. It falls in such a position as to roughly confirm the liquidus curves of Hilty and crafts3 at 1200" and 1300°C which are

Jan 1, 1965

By Irving B. Cadoff, Ernest Levine

The fracture path in a Cu-4 pct Ag alloy wet with mercury was found to he dependent on the heat treatment used prior to tensile testing. Both quenched and slow-cooled alloys were embrittled by the mercury.. For quenched alloys, which were single -phase, the crack path was intergranular. Slowly cooled alloys, which contained precipitate platelets, exhibited transgranular fracture. By comparing stress-strain data for these alloys with similar data on mercury -embyittled solid-solution alloys, it was found that the role of the precipitate and that of the grain boundary in the fracture process were equivalent . THE fracture path which results when metals are strained in a liquid environment appears to be dependent upon the nature of the specific system. Mixed transgranular and intergranular cracking has been observed in the 2024 T4 aluminum alloy when wet with a Hg-Zn amalgam.&apos; Transgranular fracture was induced in an A1-4 pct Cu alloy by masking off the grain boundaries from the liquid Hg-Zn amalgam.&apos; The embrittlement of solid-solution alloys of copper in mercury results in intergranular fracture.&apos; The effect of a precipitated phase on the fracture path in copper alloys is the subject of the present investigation. Cu-4 pct Ag was chosen so that its behavior could be compared with previous work on embrittlement of copper alloys. PROCEDURE High-purity copper (99.999 pct) was used as a base metal, along with 99.999 pct purity silver. Melting was carried out in graphite crucibles with manual agitation to get adequate mixing. The ingots were homogenized by means of vacuum annealing, chemically cleaned, and cold-rolled with intermediate vacuum anneals, to the desired thickness of 0.025 in. The rolled sheets were sheared to the final specimen size of 1 by 0.025 by 0.1 in. The specimens were then electropolished in phosphoric acid (concentrated) and heat-treated in an evacuated capsule at the solution temperature of 770°C. One batch was slow-cooled and the other quenched in water. The thermal etching which occurred during heat treatment was sufficient to permit grain boundary and precipitate delineation. Tensile tests were carried out in air and in mercury on a Table-Model Instron at a pulling speed of 0.2 in. per min. Wetting was accomplished by electro-polishing in phosphoric acid, rinsing in alcohol, and immersing in a pool of mercury. Once wet the coating was stable throughout the mechanical tests. In our studies it was found that wetting the surface or total immersion in mercury produced identical results. For convenience, the wetting technique was used for the experiments described. The crack pattern was observed directly on the surface by removing the mercury after testing. De-wetting was accomplished by flame heating the samples in a vacuum after testing and before observation of the surface. No etchant or polishing was used so as not to obscure the crack pattern on the surface. The mercury removal, however, resulted in a pitted surface but otherwise left the pertinent features visible. Photomicrographs were taken in this condition so as not to disturb the structure associated with the crack pattern. The average precipitate spacing was measured previous to coating the sample with mercury by use of an optical eyepiece micrometer. RESULTS The microstructure of the quenched specimens was single-phase while that of the slow-cooled specimens contained thin platelets of a second

Jan 1, 1964

By John W. Cahn, John E. Hilliard

Single crystals of copper and silicon-iron were cold rolled in orientations chosen to produce individually the major components of the poly crystalline deformation texture. The orientation dependence of the recrystallization kinetics was studied relative to the primary recrystallization textures of these specimens. It is not possible to rationalize the poly crystalline re crystallized textures on this basis. The results suggest an important role of the interaction of adjacent crystals during the deformation of aggregates. BRICK and Williamson1 first noted evidence that the recrystallization temperature was different for straight-rolled and cross-rolled copper given comparable reductions. Michalak and Hibbard2 investigated quantitatively the effect of rolling procedure on the kinetics of recrystallization of cold-rolled copper and found that material cold-rolled the same amount by straight-pass, cross-pass, and compression-pass techniques developed different deformation and recrystallization textures, different 1-hr recrystallization temperatures, and different recrystallization kinetics. However, the temperature dependence of the rate of recrystallization was essentially the same for all techniques. Similar results were obtained on iron. Dunn and Koh3 in studying the recrystallization textures of cold-rolled silicon-iron single crystals reported large differences in the annealing temperatures and times required to recrystallize specimens of different orientations cold-rolled the same amount. Liu4 and Liu and Hibbard5 utilized the concept of different recrystallization temperatures for different orientations of cold-rolled crystals to rationalize the difference in recrystallization textures found in various face-centered-cubic metals. Their explanation predicted a significant difference in the recrystallization kinetics of deformed (110) [112] crystals as compared to (358) [352] crystals, and, in fact, Liu4 reported evidence that this difference existed at least qualitatively. Verbraak6 who rolled and recrystallized a series of copper single crystals found that the double (112) [111] rolled orientation is related to recrystallized cube texture formation. The effect of rolling intensity on the relative amount of cube component suggests an important role of recrystallization kinetics. Walter and Hibbard7 while trying to relate the behavior of rolled and recrystallized single crystals of silicon-iron to the behavior of polycrystal-line silicon-iron again noted that differences in recrystallization kinetics were necessary to rationalize their results. The purpose of the present investigation was to obtain quantitative kinetic data on the recrystallization of single crystals of both copper and silicon-iron rolled to initial isolated individual orientations corresponding to those found in the polycrystalline deformation textures. These data might indicate the importance of the deformation orientation, i.e. the range of available nuclei, the deformed matrix orientation into which these nuclei grow, and the orientation dependence of their growth rate during primary recrystallization on this texture. I. COPPER Experimental Procedure—A single crystal of 99.98 pet purity copper, grown by the Bridgman technique, was purchased in the form of a bar 1 1/2

Jan 1, 1962

By R. D. Barer, M. B. Bever

Age hardening alloys are quenched from the solution treatment to room temperature in order to retain a supersaturated solid solution. Some alloys age "naturally" in this condition but in most alloys aging is induced "artificially" by heating to intermediate temperatures. Cold working of the supersaturated solid solution accelerates the aging process and quenching strains have the same effect. The investigation reported here is a study of the progress of aging in specimens quenched directly from the solution treatment to various aging temperatures. This procedure reduces the temperature interval of quenching and the resulting quenching stresses. It also eliminates any changes which would take place in the undercooled sample at room temperature prior to aging at an elevated temperature. Isothermal aging is thus approached and its kinetics may be studied. An aluminum-copper and an aluminum-silicon alloy were chosen for this investigation. The aging mechanism of aluminum-copper alloys is complex while the aging of aluminum-silicon alloys is nearly ideal. As standards of comparison for the samples directly quenched to the aging temperature, specimens were also age hardened by the usual procedure in which solution treated samples are first quenched to room temperature and then reheated to the aging temperature. Review of Previous Work The mechanism of age hardening has been the subject of a controversy which has ranged from the theory of outright precipitation of an equilibrium phase to theories based on subtle changes occurring in the matrix prior to precipitation. A detailed critical review of the literature up to 1939 is available1 and contributions to the general theory of age hardening continue to be made.2,3 Age hardening, whatever its mechanism, involves the nucleation of a second phase within a supersaturated solid solution. Theoretical considerations4,5 indicate that the rate of nucleation reaches a maximum at an intermediate temperature below the temperature at which supersaturation sets in. Studies of precipitation at various subcritical temperatures have demonstrated that the largest property changes in a given time occur at such intermediate temperatures.6,7,8 The precipitation of a phase from supersaturated solid solution is accelerated by strains which may result from quenching or cold work. Phillips and Brick9 established that quenching strains are an essential condition for the age hardening of aluminum-copper alloys at room temperature, at least for aging periods of less than 30 days. They also found that on aging at 300°C the hardness increased faster and reached a higher maximum after quenching into water than after quenching directly to the aging temperatures. Fink and Smith10 observed preferential precipitation on slip bands and grain boundaries in aluminum-

Jan 1, 1950

By G. Sachs, E. J. Riping

All ferrous alloys can be made brittle by straining at sufficiently low temperatures. However, the changes in mechanical properties for different ferrous materials with decreasing testing temperature do not appear to follow any universal law. In particular, complex effects of testing temperature have been observed if cold worked steels were subjected to tensile tests at low temperatures. EFFECTS OF PRESTRAINING AT A TEMPERATURE ABOVE THE TESTING TEMPERATURE ON THE FRACTURE CHARACTERISTICS‡ A considerable amount of data has been presented by a number of investigators on the fracture characteristics of various cold worked steels.&apos; These data usually relate to a two-step procedure first used by Davidenkov,² consisting of stretching by tension to a certain strain or " prestraining" at room temperature and then completing the tensile test, or "testing" at the temperature of liquid air. On the basis of data of this type made available to date, ferrous alloys can be classified into two groups with respect to their fracture characteristics observed on testing at a low temperature after prestraining at room temperature. Very complex phenomena have been observed for all annealed steels. On the other hand, some observations indicate that steels in certain other conditions represent a fundamentally simpler relation. In considering the effect of prestraining at one temperature on the properties obtained at some lower temperature, it should be expected that any cold work reduces the ductility retained in proportion to the magnitude of the cold work. However, the test data presented to date indicate that only heat treated (quenched and tempered) steels appear to conform to this expectation, according to the very limited test data in Fig 1, presented by McAdam, Geil and Mebs. This series of tests, Fig 1, shows that the retained ductility became smaller the larger the prestrain. However, this decrease is less than the amount of prestrain or, in other words, less than the decrease in ductility at the prestraining temperature. These effects of prestraining are fundamentally identical with those observed by Bridgman3 when a steel was prestrained (in tension) under hydrostatic pressure and then subjected to a regular tension test. It appears, therefore, that the basic effect of prestraining under conditions which yield a higher ductility than the (subsequent) testing procedure, consists of gradually increasing the total ductility of the metal from the initial low value of testing to the higher value of prestraining. On the other hand, all annealed steels, if cold worked by tension at room temperature and then tested at a lower temperature, provided that some ductility is retained, showed a far more complex behavior than that discussed above. This relationship is exemplified by Fig 2, for three pearlitic steels.4,5 These particular steels were selected because of the various shapes of their ductility-prestrain curves. All three steels, and any other investigated so far, suffered a rapid decrease in retained (and consequently also in total) ductility when subjected to small pre-strains. Then, after exceeding a certain prestrain it was generally observed that the ductility recovered.* This rather complex behavior of annealed steels may be tentatively correlated with the presence of stretcher strains at small restrains. Heat treated steels do not exhibit stretcher strains. This fact might possibly explain their simpler prestrain-retained ductility relationship. The destructive effect of these stretcher strains may possibly be associated with the presence of triaxiality, which may occur in any highly non-uniform stress and strain state (and which is retained as residual stress after unloading). Even a small degree of triaxiality may then cause a reduction in ductility, or even embrittlement at a sufficiently low testing temperature. The discussion presented above deals with the effects of cold working at a high temperature on the fracturing

Jan 1, 1950

By J. O. Nelson, C. J. Altstetter

Single crystals of hcp cobalt, 3 mm in diameter and up to 35 cm long, were grown using an electron-beam, zone-melting technique. The martensitic-phase transformation was studied in single-crystalline and polycrystalline specimens by making length-change measurements as a function of temperature under various elastic compressive stresses. Upon thermal cycling, single-crystalline or polycrystalline specimens repeatedly transformed almost entirely on the same variant of close-packed plane provided the maximum temperature did not exceed 600°C. Cycling to 1000°C resulted in transformation on more than one {111} variant. This behavior is termed multivariance. The multivariant transformation occurred very rapidly at an M, temperature 2° to 6°C lower than the M, of a transformation which would result in a single-crystal product. Elastic compressive stresses (up to 253 g per sq mm) tended to lower the A, and raise the M, temperatures, decreasing the width of the temperature vs dilatation hysteresis loop. The transformation habit plane and transformation shear direction of an as-grown single crystal were not grossly affected by elastic compressi?ie stress. This was evidenced by similar dilatations on the temperature us dilatation loops joy specimens with and without compressive stress. A dislocation mechanism is proposed to explain the observed results. IT has been shown that, on heating, cobalt transforms martensitically from the hcp to the fcc phase.&apos; The transformation habit plane is (0001)hcp || (lll)fcc and the transformation shear direction is (1010)hcp || (112)fcc. The transformation involves a shear of 1g°28&apos;, which may be achieved by a shearing of a/6(112) of every two planes with respect to the plane beneath, thus changing the ABABAB stacking of hcp to the ABCABC stacking of fcc. Associated with the phase change is a 0.3 x 10"3 contraction in the habit plane and a 4.2 X 10"3 expansion perpendicular to the habit plane resulting in a 3.6 x X volume increase on heating.&apos; On cooling, an identical volume decrease takes place. The temperature at which the fcc phase begins to form on heating (A,) is reported as 430°C, and the temperature at which the hcp phase begins to form on cooling from an elevated temperature (A&) is reported as 390oC1,3 Consequently, temperature vs dilatation plots have the form of a hysteresis loop. If heating or cooling is reversed during a transformation, a smaller hysteresis loop results. Upon heating, the transformation is always complete; whereas, fcc is often retained at room temperature as a metastable phase entrapped in the polycrystal-line hexagonal matrix.1,4,5 Two obstacles in the theory of the allotropic-phase transformation of cobalt have been: 1) a detailed knowledge of the product nucleus, and 2) a plausible method of propagation of the transformation. Bilby,8 christian, 7 and seeger 8,9 have suggested a "pole mechanism" as a means of propagation of partiai dislocations from plane to plane. A pole dislocation and a Shockley partial come together at a node. The a/6(112) Shockley partial rotates about the pole dislocation effecting the transformation shear. The pole dislocation must have a 2a/3(111) screw component which causes extension of the transformed region by two atomic planes with each full rotation of the Shockley partial. Bollmannl0 suggested, on the other hand, that transformation propagation occurs due to the stress fields of intersecting (111)-type stacking faults. As faults intersect, a stress distribution is set up about their intersection which is in turn reduced by the emergence of another fault on the second nearest plane. This process continues with the final result of a complete phase transformation. In view of the similarities between deformation and transformation in cobalt, the effect of stress on the transformation would, hopefully, yield valuable information concerning nucleation and propagation. In the present work single-crystalline and polycrystalline specimen length changes were measured as a function of temperature at various compressive loads. PROCEDURE Several orientations of single crystals of hcp cobalt in lengths up to 25 cm were grown by electron-beam floating zone melting from 99.95 and 99.999 pct, 3-mm-diam cobalt rod as supplied by Johnson

Jan 1, 1964

By A. Rosen, P. Wynblatt, J. E. Dorn

The temperature, strain rate, and structure dependence of the flow stress in a poly crystalline Fe-2 pct Mn alloy was investigated between 77" and 370°K. It was possible to identify the low-temperature data from 77° to 160°K with Dorn and Rajnak&apos;s theory of the Peierls mechanism of plastic deformation. Above 160°K one or more thermally activated mechanisms must he operative; however, these were not identified in this investigation. The mechanistic basis for the rapid decrease in the flow stress of bcc metals with an increase in temperature over the low-temperature range is yet being debated. Various dislocation mechanisms have been suggested in the past but the agreement between the various proposed theories and the experimental results have not been definitive. In the present paper, the authors will demonstrate that the plastic behavior of polycrystalline iron containing 2 wt pct Mn plus interstitials agrees excellently with predictions based on the Peierls mechanism from 77" to 160°K whereas from 160" to about 370°K other as yet unidentified thermally activated mechanisms take over. Undoubtedly, the overlap of these mechanisms with the Peierls mechanism contributed to the difficulties of rationalizing the low-temperature behavior of iron and its alloys. I) EXPERIMENTAL TECHNIQUES AND RESULTS Although extensive data are now available on the effect of temperature and strain rate on the flow stress of various bcc metals and alloys, it was, nevertheless, deemed necessary for the objectives of the present study to obtain highly accurate data of the type most pertinent for checking the theories on a series of well-documented work-hardened states. Iron containing 2 wt pct Mn was used in this investigation in order to obtain a lower ductile to brittle transition temperature than that for iron.&apos; The additional elements present were 0.004 pct C, 0.05 pct 0, 0.004 pct S, 0.003 pct P, 0.006 pct N, and 0.001 pct Si. The as-received 3/8 by 3/4 in. bars were cold-rolled to 0.100-in. thickness, recrystallized under argon for 30 min at 1073"~, further cold-rolled to 0.063-in. thickness, and finally recrystallized under argon for 30 min at 1000°K. This treatment gave a stable reproducible equiaxed grain structure having an average grain diameter of about 90 p. Prior to the final recrystallization treatment, the sheet was machined into tensile specimens 1/4 in. wide having a 1.625-in.-long gage section. All specimens were tested in controlled-temperature baths on an Instron Testing Machine. For convenience in the theoretical analyses the data will be given in terms of the shear stress for flow, 7, the shear strain rate, f, and the shear strain, y. A series of three standard strain-hardened states were obtained by prestraining specimens at 300°K and at a shear strain rate of 7.68 x lo-&apos; per sec to three stress levels of 6.89 X l08, 10.3 X lo8, and 14.5 x 10&apos; dynes per sq cm, respectively. Immediately following this prestrain the temperature bath was changed and each specimen was pulled in tension at either f = 7.68 X lo-&apos; or f = 3.06 X 10"3 per sec. In terms of the accuracy that was achieved, the values obtained did not deviate more than *0.1 X 10&apos; dynes per sq cm and * 1°K from the reported values of stress and temperature and not more than *5 pct in the reported values of the strain rate. The tensile stresses were converted to shear stresses using a factor of 1/2. The shear stress for the initiation of flow at the test temperature was determined by taking a y = 6.16 x 10&apos;3 offset. from the modulus line at which point good accuracy could be achieved in determining y and the associated flow stress 7, with only a negligible increase in the pre-

Jan 1, 1965

By E. C. Rudolphy, M. E. Potter, J. R. Mitchell

The effects of 0.006 to 0.20 pet Sn ml the hot workability and the annealed mechanical properties were investigated for Types 302, 410, and 430 stainless steel. The hot workability of these steels was not significantly affected by their tin content within the range studied, although some effects on mechanical properties were noted. Apart from the effect of tin, optimum hot-working temperatures and V-notch Charpy impact transition temperatures for these grades were determined. HIGH tin residuals in some heats of stainless steel have been blamed for the poor hot workability, particularly during secondary mill rolling. However, very little quantitative information has been available. Previous work1"6 with carbon steels indicates that tin increases tensile strength and hardness but de- creases tensile and impact ductility. Halley,7 in reviewing the sources and effects of residual elements in carbon and alloy steels, concluded that much of the surface checking (hot shortness) encountered in rolling was caused by copper, and that tin, arsenic, and antimony combined with copper to form low-melting constituents which further increase the steel&apos;s sensitivity to hot shortness. These elements had little effect in the absence of copper. A more recent paper by Langenberg and Johnson8 concluded that tin reduces hot workability but that researchers disagree concerning the amounts which will cause trouble. They state that laboratory investigations with small ingots seem to indicate a higher tolerable level of tin than do statistical studies of mill data, and also that statistical analysis of mill data indicate that small amounts of residual tin are detrimental to the surface quality of stainless sheet. The accumulative increase in the general level of tin and other tramp elements in steelmaking materials will present greater problems to steelmakers in the future. The purpose of the present study was to obtain quantitative information on the specific effects of tin on the hot workability and mechanical properties of such common stainless steels as Types 302, 410, and 430.

Jan 1, 1962

By J. Szekely

The paper discusses simultaneous heat conduction and diffusion. These problems may arise in slag-metal kinetics and in connection with rapid heating or cooling of specimens. A mathematical formulation is given and it is shown that the transients due to either the variability of the diffusion coefficient with temperature, or thermal diffusion, are unlikely to be important for molten or solid metals and slags. The negligibility of these effects is due to the large values of the ratio thermal diffu-sivity/molecular diffusivity. In many problems relating to transport-controlled metallurgical kinetics the diffusion process is accompanied by the transfer of heat; large-scale metal refining or metal reduction may be quoted as examples. It has been shown that due to turbulent mixing in these systems the relevant transport phe- nomena are best described in terms of "surface renewal models" which require the solution of the unsteady-state diffusion equation.1-1 Problems involving simultaneous diffusion and heat conduction are also encountered in the laboratory in connection with rapid heating or cooling of specimens. The effect of variable temperature on diffusion may be twofold: a) in the absence of "cross effects" the problem, due to variable temperature, is that of diffusion with a variable diffusion coefficient; b) if the Soret Effect is nonzero, thermal diffusion must also be taken into account in the formulation. Although information is available on thermal-diffusion transients in a steady-temperature gradient,4&apos;5 little work has been done on the effect of unsteady temperatures on either the diffusion coefficient or on thermal diffusion.&apos; In the following a formulation is given and solutions presented with a view of examining the areas where these effects may be important.

Jan 1, 1965

By B. Ramaswami, Y. Nakada, R. Schaefer

EARLY investigations1 of the tensile properties of fcc single crystals did not reveal the easy glide region of crystals with axial orientations inside the standard stereographic triangle. With the production of high-purity metal, a region of easy glide became known1 Consequently, modern work of fcc single crystals ordinarily uses high-purity metal. In order to determine whether further purification of aluminum beyond 99.992 pct purity would result in significant alteration of the tensile properties of single-crystal specimens, metal was zone-refined and crystals grown from the purified material were compared to crystals grown from the original material. Some similar studies were made of gold and silver crystals. Aluminum. The material to be zone-refined was cast into bars 1/4 by 1/2 by 8 in. A zone, approximately 1-1/2 in. in length, was passed over each bar eighteen times at a rate of 6 in. per hr. Melting and stirring were carried out by an induction heater under a vacuum of approximately 10"5 mm Hg, the metal being held in a graphite container. he last 3 in. of each processed bar were then cut off and discarded. No quantitative determination of purity was made, but the effectiveness of the zone refining was tested by a method first suggested by Walton, Tiller, Rutter, and winegard3 depending on the relation between cell structure and impurity content. Rutter and Chalmers4 have shown that a cellular substructure is associated with the presence of impurities during solidificatibn, and have shown how solute rejection at the freezing interface can lead to such an association. Thus the observation of cells gives evidence of impurities being present. To look for cells, the last quarter of a zone-refined bar was cut off, remelted, and grown rapidly into a single crystal. It was then heavily electropolished and thermally etched.~ Cells were revealed by the presence of many parallel rows of etch pits. The same process was carried out with material from the first half of the bar, but no cells were detected. These observations give evidence that a significant amount of impurity material was moved to the "dirty" end of the zone-refined bars. Further indication of purification was obtained from recrystallization experiments. It was found that, after cold rolling to a 97 pct reduction in thickness, the material from the pure end of the bar re-crystallized at room temperature, but the material from the "dirty" end did not. Other investigators6 have previously reported that zone-refined aluminum recrystallized at room temperature. The purified material was cast into 1/4 by 1/4 in. bars, and seeded crystals were grown in a (100) orientation and in a single slip orientation where the Schmid factor is m =2. The crystals were then cut to the desired length, annealed for 24 hr at 610°C, furnace-cooled, and etched in Tucker&apos;s etch. The crystals were tested in a floor-model Instron machine, using a gage length of 4 in. and a strain rate of 1/2 pct per min. The resulting curves are shown in Fig. 1. It is seen that the differences between the curves for zone-refined and original-purity materials are small. These differences are within the scatter observed for crystals of the original purity. In particular, the zone refining does not significantly affect the onset of the different "stages" of the curves.

Jan 1, 1964