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By H. S. Cannon, F. N. Rhines

The application of a static load to a copper powder compact during sintering at an elevated temperature accelerates the rate of sintering in such a way that a given load induces the same proportional increase in rate for all times of sintering. It is shown that sintering under a load is like creep under a fixed load in that the stress required to accomplish a given degree of densification is proportional to the logarithm of the sintering time. VIRTUALLY all of the theories of sintering that have been put forward within recent years have contained the assumption that the chief driving force of the process is the surface tension resident in the exposed surfaces and internal pores of the compact, or powder mass. An externally applied load might be expected to provide a somewhat equivalent driving force for sintering. It is known that the application of a compressive load, during sintering, hastens densification, but it is by no means clear whether sintering under the influence of surface tension alone and sintering under an applied load are fundamentally similar processes. The present study was undertaken in an effort to obtain an answer to this question and with the hope that the answer may contribute to an understanding of the mechanism of sintering. It has been found that there is a close relationship between sintering and creep processes. Copper powder compacts were sintered in hydrogen at 1000 °C under dead loads of 0 to 165 psi and the progress of sintering was observed by means of density measurements. Using a commercial reduced oxide copper powder, see Table I, cylindrical compacts Yz in. x x in. high were made at a pressure of 12,500 psi. For sintering, these were placed in a cylindrical graphite container into which they fitted snugly. A compressive axial load was applied to the compact through a graphite rod of similar diameter, which rested upon the upper end face of the compact; iron weights, in suitable amount, were placed upon the graphite rod to provide the load. This assembly was encased in a vertical silica tube within a resistance-type furnace capable of maintaining a substantially constant temperature within the working zone. After various predetermined times at temperature, the samples were removed from the furnace and their density was measured by conventional means. The heating-up and cooling-down times have been included in the computed sintering time, using the assumption that the sintering rate doubles for each increase of 10 °C in temperature. The experimental results are presented in Table 11. Upon metallographic examination of the specimens, it was found that there was no apparent change in the shape of the pores as a result of loading, i.e, no flattening, Fig. 1. Substantial contraction away from the container walls was observed in all samples sintered with loads of 10.5 psi and less.

Jan 1, 1952

By Elmars Ence, Harold Margolin

The Ti-Fe and Ti-Fe-0 systems were re-examined because of the controversy regarding the existence of Ti2Fe, and to consider all available data points to the existence of Ti,Fe. The Ti-Fe-0 system contains two ternary compounds: E, corresponding to Ti2Fe; and y. SEVERAL authors have investigated the constitution of titanium-rich alloys of the Ti-Fe system. The most extensive study of titanium-rich portions of the Ti-Fe system was by Van Thyne, Kessler, and Hansen,' who investigated this system up to 50 pet Fe and used the highest purity materials available for their alloy preparation (iodide titanium was used for alloys up to 20 pet Fe). According to Van Thyne et al., phase relationships in the region of investigation are governed by phases a,ß, and TiFe. No evidence of an intermetallic compound Ti,Fe was found. although earlier. works by Laves and Wallbaum,' and Duwez and Taylor' reported its existence. Rostoker's study on the occurrence of TilX phases" confirmed the findings of Van Thyne et al. Rostoker proposed that the compound Ti Fe found by Duwez does not exist but is actually a ternary compound, Ti1Fe3O, originated by inadvertent oxygen contamination. The partial isothermal section of the ternary Ti-Fe-0 system as reported by Rostoker' seems to confirm this explanation. In the course of phase diagram work conducted at New York University, however, certain irregularities were observed to be associated with ternary systems of the type Ti-Fe-X. The ternary phase 6, observed in the systems Ti-Fe-Mo' and Ti-Fe-V." was found to be structurally identical to the com-pound Ti2Fe as reported by Duwez and Taylor, and to Rostoker's compound Ti1,Fe2O. Since the amount of oxygen possibly present in the Ti-Fe-Mo and Ti-Fe-V systems could not account for the observed amounts of the compound, it appears that the d phase in these systems is not Ti,Fe,O. On the other hand, considering the amounts of the 6 phase, particularly in the Ti-Fe-Mo system, the location of the phase was uncertain. It was felt that the introduction of the Ti2Fe phase would alleviate some of the inconsistencies of the two systems. Because of the uncertainties relating to the phase Ti2Fe, or Ti1Fe2O, it appeared worthwhile to re-examine the Ti-Fe and Ti-Fe-O systems in the vicinity of these compounds with highly sensitive metallographic techniques and with X-ray methods. Experimental Procedure Alloy Preparation—For the study of the binary system four alloys were prepared, containing 26.9 (30 wt pct), 34.0 (37.5 wt pet), 41.2 (45 wt pet), and 56.3 (60 wt pet) atomic pet Fe, and for the ternary Ti-Fe-O system 18 alloys were prepared in the composition range of 1.6 to 16.9 atomic pet 0 and 24.3 to 55.7 atomic pet Fe. The materials used for the Ti-Fe alloys were iodide titanium (99.98 pet Ti, 0.002 pet 0) and Ferro-vac-E iron (99.95 pet Fe, 0.0052 to 0.0072 pet 0). For the Ti-Fe-O study the materials used were sponge titanium containing less than 0.06 pet 0, Ferrovnc-E iron, and Baker's analyzed TiO2. The nominal weight and atomic percentages of the ternary alloys prepared are shown in Table I. Melting—Charges of 10 to 15 g were melted in a nonconsumable arc furnace in argon atmosphere according to the technique described elsewhere.'" Since there was practically no weight loss through the various stages of melting and oxygen losses have not been observed previously, it appeared justifiable to use nominal composition for interpretation of data. Iodide titanium control buttons, of the same mass as the Ti-Fe charges, and melted under the same conditions, were used to check hardness pickup during melting. A hardness increase of 2 to 3 Vhn was found. Heat Treatment—The specimens were annealed in quartz capsules under argon. To avoid contact between the specimen and capsule material all specimens were wrapped in titanium sheet. The annealing times are given in Table 11. The attain-

Jan 1, 1957

By B. L. Averbach

Recovery and primary recrystalliza-tion in cold worked metals are usually considered as two competing processes. Some of the effects which usually accompany recovery are: alleviation of stress corrosion tendencies, changes in thermal emf,1 damping capacity,2 electrical resistivity,2 and magnetic properties,3 and only minor changes in hardness or the related strength properties. During primary recrystalliza-tion new unstrained grains are formed at the expense of the strained matrix. These new grains eventually become visible metallographically, and nucle-ation and growth kinetics have been indicated for this process.4,5 Frequent attempts have been made to study the cold-working phenomenon by observations on the line broadening by X ray diffraction patterns. Relatively few measurements of line intensities have been made, although Brind-ley and his collaborators, 6,7,8 by means of film techniques, compared the intensities of cold worked Cu, Ni, and Rh patterns with those from chemically precipitated powders. These precipitated powders were presumed to be strain free, and it was found that the intensities for the cold-worked materials progressively decreased as the Bragg angle increased except for the first line, where there was an increase due to reduction in extinction. This was interpreted as a randomness in atomic position induced by cold work. Such randomness is similar to that caused by thermal agitation and has been described as "frozen heat" displacement of 0.08-0.10 A from the mean atomic position. In a recent study9 on the effect of cold work in metals on their powder pattern intensities, the changes in integrated intensity for heavily cold worked alpha brass were observed as a function of the annealing temperature. These measurements were made with a manually operated Geiger-counter spectrometer using CuKa radiation monochromated with a rock salt crystal. Intensity measurements were made with a scaling meter over small intervals of angle, and the equipment was so arranged that the diffracted and incident beams made equal angles with the specimen. Intensities could be compared directly by simply interchanging specimens, and comparisons from day to day were made with a standard whose line intensities did not change on aging. It was shown that a cold worked alpha brass standard was stable for at least a year. Table 1 indicates the results of the integrated intensity measurements on a 70 Cu-30 Zn brass. In the sample preparation, a brass plate was first cold rolled 50 pct and then filed, screened to —325 mesh, compacted into briquettes at a pressure of 60,000 psi and finally annealed for one hour at various temperatures up to 400°C. The briquetting pressure did not seem to influence the integrated intensities, and most of the cold work was introduced by the filing. Although this method of cold work is not quantitative, it was used to obtain random orientation (and thus uniform diffraction lines) in order to make accurate measurements of integrated intensity. Back reflection patterns were taken in each case to check the uniformity of the lines, and from the observed line broadening it was apparent that this type of plastic deformation was quite severe. Care was taken to traverse the entire background of the pattern and to assign to each peak the total intensity above this background. The bases of the diffraction lines were quite broad and spread out over several degrees, even for the narrow peaks. The theoretical intensities were calculated to include a temperature correction, a dispersion correction, and a Lorenz- polarization factor corrected for the crystal monochromated beam. In Table 1 it was necessary to match the calculated and observed values at only one point, and the rest of the experimental values were converted directly to this arbitrary scale. The integrated intensities in Table 1 are listed in arbitrary units, and the accuracy was sufficient to reproduce any of the measured line intensities to within + 1.5 units. It is evident that the percentage error on the strongest line (111) was quite low. The calculated values and the observed intensities for the cold worked material matched reasonably well. As the annealing temperature was raised, however, the intensity of the strongest reflections, particularly the (lll), decreased measurably. Since the background intensities of all of these patterns were identical, such behavior could be interpreted as a primary

Jan 1, 1950

By J. Washburn, R. Drouard, E. R. Parker

Temperature dependence of the rate of recovery in zinc single crystals after a simple shear deformation at low temperature was investigated. Some tentative suggestions regarding the annealed and strain-hardened states of a crystal are discussed. RECOVERY may be defined as the gradual return of the mechanical and physical properties of strain-hardened metal to those characteristic of the annealed material; an increase in temperature increases the rate of recovery. The annealing process in strain-hardened polycrystalline metals is complicated by the inhomogeneity of strain which always exists in aggregates. Polygonization in bent regions of the crystals and growth of new almost strain-free grains starting at points of severe local distortion1-:' make it almost impossible to isolate and study the recovery process. Homogeneously strained single crystals, however, do not polygonize or re-crystallize and hence they can be used advantageously to study recovery. In such crystals strain hardening is completely removed by recovery alone. Since recovery is a process whereby certain lattice disturbances introduced by plastic flow are gradually reduced, a knowledge of the rate and temperature dependence of this process for various conditions of prestrain might be helpful in formulating a model of the strain-hardened state. For simplicity it seemed desirable to limit the type of prestrain to the simplest obtainable, i.e., simple shear strain. In the experiments to be described, recovery was studied by observing changes in the stress-strain curve of prestrained zinc single crystals held for various times at temperatures above that employed for straining. Single crystals were grown from the melt by a modified Bridgeman technique from Horse Head Special zinc 99.99 pct pure, and from spectrographically pure zinc 99.999 pct pure. They were grown as 1 in. diameter spheres and acid-machined' to the final specimen contour. The test section was a cylinder about 1/8 in. high and 3/4 in. in diameter. The conical sections adjacent to the test section were cemented into the grips so the load could be transmitted to the crystal as uniformly as possible. The specimens were oriented so that in testing the maximum shear stress was applied along one of the slip directions, [2110], in the (0001) plane. Details of the production and testing of such specimens have been presented.' Each test was carried out according to the following schedule: 1—The crystal was strained at — 50°C until it reached a maximum shear stress, ,,,. The strain rate was approximately 5 pct per min in all cases. 2—After straining, the crystal was unloaded before the temperature was changed. Unloading required about 3 min. 3—The temperature of the specimen was then increased from — 50°C to the temperature, T, of recovery. This change in temperature was completed in a time of less than 2 min. The specimen remained at temperature, T, for a time, t, which differed for the various specimens. 4—Thereafter the temperature was again reduced to — 50 °C in approximately 3 min. 5—While at —50°C, the stress-strain curve after recovery was obtained. 6—The specimen was then unloaded and annealed for 1 hr at 375 °C in a helium atmosphere to bring about complete recovery. Cooling to room temperature after anneal required 90 min. 7—The same crystal could be re-used for another test because the plastic properties after annealing closely duplicated those of the original crystal. The specimen was immersed during the test in a bath of methyl alcohol which, through a system of tubes, could be pumped through either of two heat exchangers to regulate the temperature; this was accomplished by circulating the liquid through coils immersed in a bath of acetone and dry ice for cooling or in a bath of warm water for heating. Test temperatures were thus maintained constant within ±1°C. The — 50°C temperature was low enough so that no measurable recovery occurred during unloading and reloading. The stress-strain curve continued after recovery along a path below, but approximately parallel to, the path of a curve obtained in an uninterrupted test. Fig. 1 shows some of the results from a specimen of 99.999 pct Zn. The amount of downward displacement of the curve due to recovery was a

Jan 1, 1954

By Louis Raymond, John E. Dorn

The object of this investigation was to analyze the recovery that arises when the stress on a specimen undertaking creep is reduced. For this purpose annealed specimens of high-purity aluminum were precrept under a stress of 1000 bsi to a strain of 0.08 following which the stress was reduced for various periods of time to 10, 250, 500, or 700 psi. When the original stress was reapplied the subsequent creep curve lay above that for the unre-covered state and below that for the original annealed state. Analyses on the kinetics of this recovery as a function of the temperature gave a stress-sensitive activation energy that decreased as the reduced stress was increased from a value of 64,000 cal per mole at 10 psi to 37,000 cal per mole at 750 psi. Recovery was also detected and measured during creep under the reduced stress. Following a short initial period, the creep rate under the reduced stress increased monotonically until it reached the secondary-creep rate for the reduced stress. The temperature dependence of this phenomenon was also shown to be correlatable in terms of the previously deduced activation energy for recovery. The activation energies for creep of most pure metals at high temperatures have been shown to agree well with those for self-diffusion.'j2 Since the true secondary stage of creep is usually due to the steady-state balance between the rate of strain hardening and the rate of recovery, it is generally thought that the activation energy for recovery of the creep-induced substructure equals that for creep itself. A shoft time ago, however, Ludemann, Shepard, and Dorn~ found that the activation energy for recovery of the creep-induced substructure in high-purity aluminum under zero stress was almost twice that for self-diffusion, namely about 65,000 cal per mole; obviously recovery under reduced stresses differs in some significant way from the recovery that accompanies the secondary stage of creep. The major purpose of this investigation is to study the effect of stress on the re- covery of the creep-induced substructure in order to provide a better understanding of the recovery mechanism itself. EXPERIMENTAL TECHNIQUE High purity aluminum, containing 0.004 pct Cu, 0.002 pct Fe, and 0.001 pct Si, used in this investigation, was in the form of 0.100-in.-thick sheet which has been cold-rolled to the H-18 temper. Creep specimens were milled from the sheet with their tensile axes in the rolling direction. All specimens were then heated at 686°K for 1 hr followed by air cooling in order to produce an annealed structure which exhibited a uniform equiaxed grain size of about 4 grains per mm. Tests were run in creep machines fitted with Andrade-Chalmers type of lever arms so contoured as to maintain the stress constant to within 0.05 pct of the reported values. Constant temperatures to *O.l°K were obtained by complete immersion of each specimen in a temperature-controlled and agitated bath of molten KN02-KNOs mixture. Where changes in temperature were involved, the change was effected in less than 2 min by manually replacing one bath by another controlled at the second temperature. Displacements over the gage section were sensed by linear differential transformers, the output of which was autographically recorded. The calculated strain measurements were sensitive to 5x EXPERIMENTAL PROCEDURE The following analyses are based on extensions of the previously announced effect of the temperature on the creep strain,2 namely for a = constant, where e = the total true tensile creep strain for a given applied true tensile stress, t = the duration of the test, R = the gas constant, T = the absolute temperature, Q, = the activation energy per mole for creep which is independent of the stress, / = a function of 8, = and of the stress, and a = the stress. The validity of this correlation for high-purity aluminum is demonstrated in Fig. 1 for temperatures in the near vicinity of 600°K; the activation energy for creep, Q,, which is approximately that for self-diffusion, is insensitive to the applied stress

Jan 1, 1964

By H. L. Couch, J. D. Lubahn

In decarburized mild steel, the strain hardening arising from 1/2 pct strain can he partly recovered by subsequent heating, even though re crystallization or grain growth does not occur. This recovery varies from 5 pct in an hour at room temperature to 70 pct at 800°C. The variation with temperature was qualitatively similar to that reported for copper, but occurred at lower temperatures. Except for the initial portion (Bazdschinger effect), the stress-strain curve following recovery can be superimposed on the original curve by shifting it to the left. In other words, the tensile behavior is essentially the same after straining and heating as if there had been less strain and no heating. The importance of this observation in understanding simultaneous deformation and recouery is explained. AN earlier investigation1 on copper showed that strengthening due to strain hardening was augmented by heating at moderate temperatures, but was diminished by heating at higher temperatures, Fig. 1. Auxiliary experiments1 indicated that recovery and strain aging are independent processes, which may proceed simultaneously, and whose effects are additive as indicated in Fig. 1. In order to study recovery by itself, similar tests were made on decarburized mild steel, where strain-aging effects are known2 to be absent. MATERIAL, TESTING PROCEDURE The specimens were made from rimmed, hot-rolled SAE 1020 steel 0.040 in. thick, by stamping out rectangular blanks and end holes, Fig. 2, and pack milling the reduced section. These were wet-hydrogen treated2 for 16 hr at 720°C to remove carbon and nitrogen completely and then heated 1 hr at 850°C in vacuum to stabilize the grain size. Auxiliary ex- periments showed that heating up to 800°C will not cause grain growth. They were prestrained 5 to 7.5 mils per in. using the special grips shown in Fig. 2. Such small strains are less than the "critical" strain for recrystallization and, therefore, will not cause recrystallization, even at high temperature. The recovery treatment after prestraining and before the retesting consisted of heating for 1 hr in wet hydrogen at the desired temperature. In one test, Huggenberger gages were used to define more accurately the loading and unloading curves. Fig. 3 illustrates the creep during the early stages of unloading, the hysteresis due to cold stretching, and removal of hysteresis by heating.3 RESULTS The load-deflection curves had ratner widely differing shapes for different specimens, both before and after the recovery treatment. Some specimens showed perfectly smooth curves, Fig. 4, while others exhibited an inflection more or less suggestive of a yield point (Fig. 4 shows all extreme case). Some curves were much steeper than others; Fig. 5 shows two extremes. Some additional ex-

Jan 1, 1960

By R. L. Rickett, S. H. Kalin, J. T. Mackenzie

Aluminum killed low carbon steel, § which is now used extensively for severe deep drawing or other difficult forming operations, is unusual in that its grain structure, after cold reduction and box annealing in accordance with conventional continuous sheet or strip mill practice, often is elongated, although at times it is equiaxed. Since this unusual structure has been found superior for many, but not all, severe forming operations, recrystallization of the steel, both at constant temperature and on continuous heating, was investigated and compared with that of rimmed steel in the hope that something might be learned about the mechanism of, and the factors controlling, the formation of such elongated grains. In this structure, the grains are elongated both in the lengthwise direction of the strip and transverse to this direction, even though nearly all of the extension in both hot and cold rolling is in the lengthwise direction. The grains are thus roughly pancake-shaped, being longer and wider than they are thick, as observed also by Burns and McCabe,1 and as illustrated by the typical structures shown in Fig 1. Fig la, representing a conventional longitudinal section, shows the length and thickness of the grains, whereas Fig Ib shows their length and width as seen by examining a section parallel to the sheet surface. Both illustrate the very irregular grain boundaries usually associated with the elongated grain shape. A finer equiaxed grain structure in this same grade is shown in Fig Ic. Either the elongated or the equiaxed structure may be present in the annealed product, and in rare instances the two types may coexist in a single specimen, as shown in Fig 1 d. Isothermal Recrystalliza-tion of Rimmed and Alamimum Killed Steel An aluminum killed steel known to have an elongated grain structure after conventional processing (Steel B, Table l), was selected for the initial recrystallization studies; for comparison, a rimmed steel, A in Table 1, was used. Samples of each in the form of hot rolled strip 0.075 and 0.095 in. thick, respectively, were cold rolled on a small laboratory mill in steps of about 0.010 in. per pass to obtain total reductions of 40 and 60 pct. Small pieces of the cold reduced strip were heated in lead at selected constant temperatures for one of several periods of time, then cooled in air. Rate of heating in the lead was, of course, very fast. Hardness of the cooled specimen was measured and a longitudinal section examined metallographically. Isothermal recrystallization curves for these two steels at 1050°F, based on hardness of the air cooled specimens, are shown in Fig 2 in which the amount of recrystallization corresponding to each plotted point is indicated. The marked difference in the behavior of these two types of steel is evident. After a corresponding amount of cold reduction, the rimmed steel recrys-tallizes in a much shorter time than the killed steel and the shape of its recrystallization curve, (plotted on a logarithmic time scale), is very different. The curve for rimmed steel indicates that recrystallization is analogous to isothermal transformation of aus-i.enite in that it proceeds at a progressively faster rate up to some 50 pct recrystallization, then at an increasingly slower rate. For the aluminum killed steel, however, the start of

Jan 1, 1950

By H. P. Leighly, J. W. Marx, H. L. Walker

A relationship between recrystallized grain size and prior deformation is predicted from elementary statistical considerations, and reasonable agreement with experiment is obtained. RECRYSTALLIZATION phenomena have received much theoretical and experimental attention, and very adequate discussions of the various mechanisms suggested have been given by Anderson and Mehl,' Cook and Richards,' and Burgers," and others. It suffices to note here that the initial concepts fitted one of two general hypotheses: I—The new crystals are nucleated within microscopic regions at which there is a concentration of internal stress, i.e., volume elements of maximum strain energy. 2—The new crystals have their inception in volume elements of minimum strain energy. In a comprehensive early review of the subject, van Arkel' considered both possibilities and came to the conclusion that hypothesis 2 was inconsistent with the experimental fact that the number of nu-cleations increased with increasing deformation. He suggested that, if allowance was made for a preliminary atomic rearrangement at the points of large internal strain, hypothesfs 1 provided the more reasonable concept. Following the initial observations of Collins and Mathewsonb nd Crussard,Y he systematic X-ray investigations of Cahn' and Guinier and Tennevin" established the existence of a polygonized structure in metals that had been cold-worked, and subsequently annealed, under conditions such that re-crystallization did not occur. This new experimental evidence by no means disproved the first nucleation hypothesis, a fact recognized by both Beck" and Cahn,10 who independently suggested nucleation mechanisms based on the idea that regions of large strain might polygonize before the bulk of the less deformed material. These mechanisms, together with others recently proposed," are dependent upon the prior existence of some degree of polygonization in the deformed material. On the other hand, a critical examination of the published data leads to the supposition that polygonization may not be the necessary precursor of recrystallization, but merely its favored energetic competitor. In regions where the lattice distortion is not too severe, the limited adjustment afforded by polygonization may permit the lattice to drop to a relatively stable low energy state in which the nucleation of a new crystal becomes improbable, even at elevated temperatures. Such structures, of course, might provide a fertile field for the growth of nuclei, if these could be introduced. In regions of concentrated lattice distortion, polygonization alone may not be able to accomplish an adequate strain reduction, and in these volume elements sufficient thermal activity permits the more drastic atomic rearrangement involved in nucleation. Completely polygonized structures are known to withstand extended heating close to their melting points," with no other effect than a slow enlargement of some of the subgrains at the expense of others. Once started, macroscopic recrystallization might be expected to go to completion in a matter of minutes under similar heat treatment. Crussard12 and his coworkers have found that recrystallization may occur in single crystals of impure (about 99.7 pct) aluminum without any detectable prior polygonization. The indication here is that large Cottrell impurity atmospheres inhibit dislocation movement, thus suppressing polygonization to such an extent that the alternative process, recrystallization, dominates the lattice restoration. Experimental studies relating recrystallization directly to stored energy have not, at the present time,

Jan 1, 1954

By S. F. Reiter

The paper presents isothermal recrystallization curves for 0.08 and 0.15 pct C steel at subcritical temperatures following small amounts of plastic deformation. The effects of deformation, temperature, and aging on nucleation and growth rates ore described. The free energy of activation for grain boundary migration in steel is given. SEVERAL excellent reviews of the literature have appeared concerning the recrystallization of metals.'-' The present investigation follows the approach advanced by Mehl, Stanley, and Anderson,6-7 in which the rate of recrystallization was analyzed in terms of N, the rate of nucleation, and G, the rate of growth of recrystallization nuclei. Two lots of low carbon, capped steel of the analysis given in Table I were studied. Each lot consisted of a 150 lb coil which had been hot rolled to 0.083 in. and then cold rolled to 0.042 in. at the mill. Strips 0.930 in. wide were sheared perpendicular to the rolling direction. Both steels were normalized before studying their recrystallization characteristics. The strips were cleaned, painted with a magnesia-acetone paste, and made into packs of equal weight, wrapped in 0.002 in. copper foil. The packs were placed in a salt bath at 900°C for 30 min and air cooled. A relief anneal followed in a second salt bath for 15 min at 650°C. The relief anneal was found necessary from early tests in which a longer incubation period and slower rate of recrystallization were observed in relief-annealed lot A steel than in similar material which was strained and recrystallized directly after being normalized. This effect, which indicates the presence of transformation and/or cooling stresses in steel air cooled from above the A, temperature, has also been observed by Samuels8 and Masing.9 Figs. 1 and 2 show the microstructure of lot A and B materials and illustrate the rather uniform No. 8 ASTM grain size produced by this heat treatment. Winlock and Leiter10 observed that strip specimens which had their sharp edges removed elongated more uniformly than those which were not polished. Similarly, when the sheared edges were removed on a belt grinder, it was found in the present investigation that such samples recrystallized more uniformly than did unpolished strips. Therefore, all strips were carefully rounded prior to their extension. The approximate strain limits for the production of large recrystallized grains are from 6 to 12 pct extension." It was found that for the purpose of this investigation, 8 and 9 pct elongation were suitable deformations. The strain rate employed was 0.01 in. per in. per min and produced a yield point elongation of 4 pct. Winlock and Leiter found that mild steel of No. 8 ASTM grain size gave the same yield point elongation when extended at 0.012 in. per in. per min. All of the lot A and B strips extended in tension developed a straight, stretcher strain line at each grip when the upper yield point was reached. The lines were parallel and made an angle of 55" with the edge of the strip. They approached each other with increasing strain and met near the center of the sample at the end of the yield point elongation. Immediately thereafter, a small drop in load was observed and then the load increased in a regular manner with increasing extension. The grips were initially 8 in. apart. After extension, the 6 in. gage length was carefully cut into 1 in. samples. The remainder of the strip was discarded. After a flash pickle in hot 50-50 hydrochloric acid, six samples, each of which had been taken from a different strip, were placed in a basket and submerged in a lead pot for isothermal recrystallization. Although no recovery effect was observed, strain aging did occur after extension. Therefore, samples were always recrystallized within 24 hr after their cold deformation. After recrystallization, the samples were etched with a solution comprised of one part by volume of nitric acid with three parts of water. Bromide printing paper was exposed directly at low magnifications and later used with a mask to measure the desired quantities. First, the average diameter of the largest grain visible in each sample was determined using dividers. Next, the number of recrystallized grains per unit area was counted and recorded as n. Then, for each sample, the combined area of the recrystallized grains was measured by transcribing the grain outlines to standard graph paper. Many determinations of the area of the recrystallized grains were repeated five times and indicated a standard error that was not greater than 25 pct. The average area for six samples was divided by the area of the mask to yield the percentage recrystallized. Recrystallization of 0.08 Pct C Steel The progress of recrystallization at 670°C after 8 pct elongation of lot A steel is shown in Fig. 3, a through f. The shapes of the growing crystals are approximately equiaxed, as is assumed in the

Jan 1, 1953

By F. V. Lene, E. J. Westerman

The recrystallization behaviors of two extruded and cold-drawn experimental sintered aluminum powder alloys, containing 1.75 and 3.0 pct Al2O3 by weight, were compared with that of extruded and cold-drawn commercially pure alumirzum. The kinetics of recrystallization of the alloys are described semiquantitatively. For the alloy containing 1.75 pct A l203 the rates of nucleation and of growth were also semiquantitatively determined. THE most striking property of aluminum alloys strengthened by a dispersion of Al2O3, the so-called SAP alloys, is their stability at elevated temperatures. One of the manifestations of this stability is their resistance to recrystallization after they have been cold worked. Most of the commercial grades of either the Swiss SAP or of Alcoa's Aluminum Powder Metallurgy Products have not been recrys-tallized after cold working, even when they are heated for a long time at a temperature near the aluminum melting point. Lenel, however, observed that the dispersion strengthened aluminum alloys with a larger spacing between the oxide particles than that of most commercial grades would recrys-tallize.1 It appeared to be of interest to further investigate the mode and kinetics of recrystallization of these alloys, and to compare their recrystallization behavior with that of commercially pure aluminum. Because homogeneous deformation of these SAP alloys in tension did not provide sufficient cold work to induce recrystallization, they were cold worked by wire drawing; the nonuniformity of this deformation unavoidably complicated the interpretation of the recrystallization studies. EXPERIMENTAL DETAILS Extrusions—Two types of sintered aluminum powder extrusions were used in this study. One type, designated AT-400, was produced from Reynolds atomized aluminum powder consisting of spherical particles averaging 3µ in diam and containing 1.75 wt pct of Al2O3. This powder was very similar to the R3M powder from which extrusions were previously prepared with an average spacing of 0.9µ between oxide particles.2 The second type, designated MD 2100, was produced from Metals Disintegrating Co. flake powder containing 3.0 wt pct of Al2O3, with an average flake thickness of 0.8µ. The average spacing between oxide platelets in MD 2100 extru- sions was 0.45µ.2 Powder compacts of 3/4-in. diam were extruded at 1000°F into 0.097-in. diam (AT-400) and 0.093-in. diam (MD 2100) wires by methods previously described.3 In order to compare the recrystallization behavior of sintered aluminum powder extrusions with that of wrought commercially pure aluminum 3/4 in. rod stock of 1100 F aluminum was extruded at 1000°F into 0.102-in. diam wire. Wire Drawing—Tungsten carbide dies were used for the AT-400 and 1100 F alloys. They had an included angle of about 15 deg and reduced the wire area approximately 7 pct per pass. Steel dies with an included angle of 11 to 13 deg and an average reduction per pass of 10 pct were used for drawing the MD 2100 alloy, because drawing this alloy through the carbide dies produced overdrawing defects. Heat Treatment—The cold-drawn wires were cut into small samples, and the deformed ends were etched off. The samples were each wrapped tightly in a single layer of aluminum foil, and individually isothermally annealed in a lead bath. Metallography—The modes and kinetics of recrystallization were determined by metallography. Mounted and polished specimens were anodized in a solution of 1.8 pct HBF4;4 examination under polarized light clearly revealed their grain structures. The recrystallized grains were generally much larger than those of the unrecrystallized matrix, and could clearly be distinguished because they alternated between maximum and minimum light reflection when the microscope stage was rotated, while the unrecrystallized matrix had a comparatively homogeneous "salt and pepper" structure. The fractional recrystallized volumes of the dispersion hardened alloy wires were determined by cutting and weighing of recrystallized and total transverse areas on photomicrographs. The recrystallized grains in the 1100 F alloy were too small to be cut out individually; therefore a combination of cutting and lineal analysis was used in this case. RESULTS AND DISCUSSION Modes of Recrystallization—The modes of recrystallization of the three alloys varied widely. In the 1100 F alloy nucleation and growth started in the region midway between the center and the surface;

Jan 1, 1961

By M. S. Burton, G. V. Smith, A. Rosen

The kinetics of re crystallization and the effect of recovery on recrystallization of pure iron were investigated within the temperature range of 517" to 632 OC. Grain growth and activation energies were also studied. Two stages can be distinguished during recrystallization; the first is gvowth-controlled and the second is nucleation-controlled. The extent to which the first stage succeeds before the second stage begins depends on both temperature of recrystallization and temperature of recovery. The softening of cold-worked metals and alloys due to transformation of the deformed crystals to strain-free equiaxed grains during annealing is well-known, and early inestiators established that recrystallization kinetics is strongly influenced by minute quantities of impurities. Generally, it is believed that impurities decrease the rate of recrystallization and the rate of grain growth. To understand the basic phenomena of recrystallization, investigations should be on pure materials. Most of the research on high-purity materials has been on metals having the fee Bcc materials, and especially high-purity iron, have been studied only in recent years. It is known that recovery may influence recrystalliation;" however, no general description of the influence, applicable to all materials, has been presented. This paper presents results of a study of the recrystallization kinetics of high-purity iron, after 60 pct cold deformation by drawing, with particular reference to the influence of recovery on the rates of recrystallization and grain growth. From observations of these rates, conclusions are drawn concerning nucleation. MATERIAL AND EXPERIMENTAL PROCEDURE Preparation of Material. High-purity iron, prepared by zone refining of vacuum-melted electroiytic iron at Battelle Memorial Institute under sponsorship of the American Iron and Steel Institute, was used in this study. Table I gives the reported chemical analysis of the material, taken at a point near the last molten zone and thereby rep- resenting the maximum impurity level for the entire bar. Prismatic specimens, approximately 10 x 10 X 50 mm, were sawed from the 50-mm-diam bar, perpendicular to the zone-refining direction, and turned to cylindrical shape. These specimens were sealed in quartz capsules under vacuum, approximately 10"e mm Hg, austenitized at 930° C for 15 min, slowly cooled, removed from the capsules, and cold-worked in air by swaging to approximately 20-pct reduction of area. The encapsulating, austenitizing, and swaging operations were repeated two additional times, after which the samples were encapsulated, austenitized, and cold-drawn to 60-pct reduction of area. A further vacuum anneal at 630°C for 120 min and cold drawing to 60-pct reduction of area produced wire 2.8 mm in diameter. The drawn wire was electropolished to remove deformed material on the surface, after which it was sawed into 4-mm-long specimens for the recrystallization study. Microscopical examination before the final cold reduction revealed equiaxed grain structure with very fine grains in a thin layer near the surfaces of the specimen and nearly uniform ASTM 3-4 grain size in the center. Recrystallization Heat Treatment. a) Direct Recrystallization of Cold-Worked The 60 pct cold drawn iron specimens were recrystallized at five temperatures, 517, 556, 590°, 612, and 632C, in a lead bath covered with graphite (the temperature was controlled to 1°C). Specimens were treated for twelve different times at each temperature, and all were water-quenched after heat &eatment. b) Recrystallization Following Preliminary Recovery Heat Treatment. After cold working, specimens were sealed into quartz capsules under vacuum, 105 mm Hg, and recovery-annealed at 362", 400", and 440°C for 20 hr prior to recrystallization. No evidence of recrystallization was found

Jan 1, 1964

By D. Harker, W. E. Seymour

CERTAIN alloys of iron and nickel, when rolled and annealed, possess a preferred crystal orientation: (001) in the rolling plane and [loo] in the rolling direction, when recrystallized at 850" to 1050°C after approximately 98 pct cold reduction. Since the preferred orientation makes a direction of easiest magnetization coincide with the rolling direction, these alloys, especially a 50 pct iron in nickel alloy, have found wide application in the electrical industry' for choke coils and special types of transformers. The rate of the recrystallization reaction was studied at temperatures ranging from 500° to 600°C. The heat of activation for the reaction was calculated from the observed rates, and crystal orientation determinations were made before and after re-crystallization. A vacuum melted iron-nickel alloy* analyzing 49.6 pct nickel, 0.018 pct carbon, and 0.30 pct manganese was used for the experiments. The alloy was cold-rolled 98 pct into strips 1/2 in. wide by 0.002 in. thick. Specimens 1 in. long were sealed under a vacuum (approximately 10-8 mm Hg) in 1/2 in. ID pyrex glass tubes. For heat treatment these tubes were fastened to Nicrohm wires and submerged in a molten salt bath controlled to ±2°C. (The maximum measurement error was within 3°C.) The time at temperature was varied logarithmically from one sample to another, and runs were made at 500°, 525", 550" and 575°C. A molten lead bath was used for a run at 600°C which was controlled to the same accuracy. To determine the extent of recrystallization after a particular time at a given temperature, a method was used suggested by the work of Decker, Asp, and Harker.3,4 This method employs an X-ray spectrometer whereby X rays are diffracted from crystallites whose diffracting atom planes are parallel to the rolling plane of the specimen. The intensities of the diffracted rays are measured by a Geiger counter. The counter can be rotated through a range of angle, and can be motor driven through this range at a speed of 2" per min. The measured intensities are plotted vs. angle by a potentiometer recorder. In a 50 pct iron-nickel alloy it was found that only (200) reflections were obtained from the rolling plane with recrystallized material, and that only (220) reflections were obtained from the rolling plane with unrecrystallized material. No other reflections were obtained under these conditions over a range of Bragg angle of 0 to 45" using either type of specimen. As a consequence, the intensity of the (200) reflections from the rolling plane was taken to indicate the amount of recrystallized ma-terial present in a specimen, and the corresponding intensity of the (220) reflections was taken to indicate the amount of unrecrystallized material present. To insure flatness and proper alignment of the reflecting specimen in the spectrometer, the sample was laid in a slot 1/2 in. wide x 0.001 in. deep which was machined in a 3/4x2x1/2 in. steel carrier. The specimen then was taped down with cellophane tape. This steel cradle was mounted vertically in the specimen holder of the spectrometer so that the bottom edge of the carrier rested against a horizontal shoulder. Intensity data used in plotting the percent of recrystallized material vs. time at temperature were obtained by directly counting the diffracted beam of nickel filtered copper Ka radiation used throughout the work. The X-ray spectrometer was employed also in obtaining pole figure data to be used for orientation determinations. At the beginning of this investigation a transmission pole figure holder was used." As a thickness of 0.002 in. of this alloy was found to be opaque to the copper Ka radiation, it was necessary to reduce the thickness of the pole figure specimen. A cold-worked sample was etched in a 50 pct HCl solution for 5 min and was found to transmit a

Jan 1, 1951

By Y. C. Liu, W. R. Hibbard

An aluminum single crystal cold-rolled from (110) [1121 essentially retains its initial orientation after 99.6 pct reduction in thickness. The orientation of the recrys-tallized grains of this material can be described in terms of crystallographic rotations about principal poles of deformation texture. DURING the study of the recrystallization of a copper single crystal cold-rolled from a (110) [112] initial orientation, the orientation of the re-crystallized grains could be derived by a 30" rotation of the orientation of the cold-rolled matrix about its <111> poles.&apos; The present investigation was undertaken to extend the work done on copper&apos; to an aluminum crystal also cold-rolled from a (110) [112] initial orientation. Experimental Procedure The procedure of this experiment was similar to that reported for copper.&apos; An aluminum (99.998 pct) single crystal rod* 1 % in. in diameter was grown in back-reflection technique.&apos; The specimen (1.20x 1.004x0.6787 in. thick) was then rolled along the [112] direction. The final thickness was 0.0028 in., giving a reduction in thickness of about 99.6 pet. Specimens were cut from the rolled strip with scissors, and approximately in. of disturbed metal was removed with Tucker&apos;s reagent. The rolling edge remained intact. The specimens were sandwiched between two graphite plates and annealed in a lead or lead alloy bath which was electrically heated. Pole figures were constructed using the techniques previously described.&apos; Specimens were electrolytically polished4 and etched with 47 pct HNO8, 50 pct HC1, and 3 pct of 48 pct HF. The electrolytic polishing method and etching reagent employed for aluminum specimens were not entirely satisfactory and the microstruc-tures could not be studied in any detail. Results and Discussion The octahedral pole figure of cold-rolled aluminum strip is plotted in Fig. 1. The <111> poles spread in the transverse direction approximately 8" for the highest intensity areas. The spread in the transverse direction can be related to a rotation about two <110> directions lying in a plane containing the rolling direction and rolling plane normal. The two <110> directions and a scale of rotation for the <111> poles are shown in Fig. 2. The amount of rotation is consistent for three of the four <111> poles, about 35" to 40". The discrepancy for the fourth pole is believed to be due to limitations of the film technique. Alternate inter-

Jan 1, 1956

By C. J. Bechtoldt, H. C. Vacher

Quenched alloys, prepared by powder metallurgical techniques, were examined by microscopic and X-ray diffraction methods. The compositions and heat treatments were chosen so that the chromium and nickel solvuses could be determined and a range of composition and temperature, in which a eutectoid had been reported, could be explored in small intervals. The results showed no evidence of eutectoid reactions having taken place. ALLOYS containing iron, chromium, molybdenum, and nickel are extensively used in high-temperature applications. In order to provide basic information on the solid-state reactions that occur in such alloys, the National Bureau of Standards is engaged in an extensive study of the equilibrium phases in the binary, ternary, and quaternary systems involving these four metals. Attention was directed to the chromium-nickel system because a review of the literature showed conflicting data. A recent compendium1 of the constitution of binary alloys gives two diagrams for the chromium-nickel system, one a simple eutectic and the second a diagram showing a eutectoid and a eutectic. The eutectoid was the result of an allotropic transformation in a high-temperature solid-solution form of a chromium-rich phase called 0. The approximate temperature and composition of the eutectoid was 1200°C and 30 at. pct Ni. In the preliminary study, at the Bureau, no transformation was indicated in the chromium-rich phase of ternary and quaternary alloys in which chromium and nickel were major components. Similar results have been reported from time to time in the literature,2-8 In consequence of this situation, a systematic study was made of the constitution of heat-treated chromium-nickel alloys using metallographic and X-ray diffraction methods. The compositions of the alloys were selected so as to determine the boundaries of the chromium-rich and the nickel-rich phases and to explore in small intervals the ranges in composition and temperature in which the eutectoid had been reported. The results of this study are reported and discussed in the present paper. EXPERIMENTAL PROCEDURES Materials, Alloys, and Heat Treatments—The alloys were prepared by a powder metallurgy technique similar to that used in earlier work.9 Analyses of the materials used are given in Table I. Powders were mixed using a vibrator in 30-g batches of predetermined composition; 2-g pellets were made from the mixture by compacting at room temperature in a 1/2-in. diam mold under 60,000 lb per sq in. pressure. The pellets were sintered in dry hydrogen for 10 days at 1300°C. At the end of the sintering treatment the specimens were quenched in water, which caused a pale green film to form on the chromium-rich alloys and thin black scale to form on the nickel-rich alloys. The pellets after sintering were approximately 1/2 in. diam by 3/32 in. thick. The purification train9 was modified by inserting a tube of titanium turnings, heated at 700°C to increase the efficiency of the removal of oxgen and nitrogen. It was found in the earlier work that the sintering treatment lowered the carbon, oxygen, and nitrogen contents of chromium-rich alloys to 0.01, 0.01, and 0.004 wt pct, respectively, and that there was a loss of chromium. In order to ascertain the extent of this loss, the chromium contents of certain alloys were determined chemically. They included those alloys used to determine the parameter-composition curves and those of critical composition, used to determine the chromium-solvus microscopically; these analyses were made on samples after the final heat treatments. The mixed powder values for the chromium content of those alloys that were not analyzed were adjusted to conform to a smooth curve based on the chemically analyzed values for

Jan 1, 1962

By A. H. Daane, W. J. Wunderlin, B. J. Beaudry

In an earlier study at this laboratory,&apos; the authors investigated the solid solubility of holmium in copper, silver, and gold, and also the melting point of the first eutectic on the noble-metal-rich side in these systems. In a more recent study of the solubility of rare-earth metals in gold at this laboratory. Rider, Gschneidner, and McMasters2 noted that the reported eutectic temperature in the Ho-Au system was lower than the corresponding eutectics in systems of dysprosium and erbium with gold. A redetermination of the eutectic temperature in the Ho-Au system with the same alloy used in the original study showed the eutectic temperature to be 810°C instead of 778°C as originally reported. (The eutectic temperatures in the Ho-Ag and Ho-Cu systems were also redetermined and were found to be 795" and 864°C compared to 787° and 868°C, respectively, which were reported originally.) Since this large change in eutectic temperature made the solubility data appear questionable, new alloys were prepared, heat-treated, and examined metallographically. The procedure of sample preparation and heat treatment used in the original work&apos; was followed except longer heat treatments were used ranging from 7 days at 600°C to 6 hr at 900°C. The results obtained are shown in Fig. 1. There is good agreement between the two studies in the maximum solubility of holmium in gold. Since the slope of the solvus is less pronounced in the present study, the extrapolation to 550°C shows a solubility of 1.6 wt pct Ho in gold compared with 1.0 wt pct in the original work. Since additional data were obtained and longer heat treatments were used in the present study, the larger value is believed to be more accurate. The authors wish to express their appreciation to P. Rider and K. A. Gschneidner. Jr., for bringing this discrepancy to their attention, and also to D. Thompson for assisting in the present study.

Jan 1, 1965

By S. J. Hruska

Rate expressions for the formation of two-and three-dimensional nuclei on foreign substrates are developed, taking into account previously neglected contributions to the standard Gibbs free energy of formation of critical nuclei. The temperature dependence of critical super saturation data predicted using these expressions is in accord with data for cadmium on copper and sodium on CsCl. EXPERIMENTAL data on the heterogeneous nuclea-tion of metal crystals from the vapor phase1&apos;2 exhibit the temperature dependence predicted by a nucleation rate equation derived by Pound et al.3 In their treatment, the critical nuclei are visualized according to the Volmer4 model as cap-shaped (three-dimensional). Accordingly, it seems desirable to compare these data with a nucleation rate equation which is derived on the assumption of disk-shaped (two dimensional) nuclei. Further, Lothe and Pound5 have recently shown that the standard Gibbs free energy of formation of these critical nuclei contains a contribution which has heretofore been neglected. Thus it is necessary to re-examine these nucleation data using a rate equation which contains this contribution. The van&apos;t Hoff isotherm relates n(i), the concentration of nuclei of critical size i (i = number of atoms), to nil), the concentration of adsorbed single atoms: where standard Gibbs free energy of formation of critical nuclei given by is temperature insensitive and is the bulk free energy change/volume of transformed material], T = substrate temperature and k = Boltzmann&apos;s constant. Previously,3 was determined by considering only the contributions of bulk and surface free energies in transforming i atoms from the population nil) to a cluster of i atoms. It has been shown5 that this procedure does not take into account the free energy contribution arising from the multiplicity of sites, q, where the clusters can be situated. If this contribution, -kT In q/n(l),is added to iG3 [Note that this increases n(i) by a factor q/n(l).] Since the above does not affect the remaining terms in the rate expression of Pound et al., the details are referred to their paper. The resulting nucleation rate is If the experimental AGV and T values at some common value of are employed, a plot of vs T(ln C3/l + In p&apos;) should yield a straight line of slope k/B<p and intercept . The corresponding plots for / = 1 nucleus per sq cm sec and C3 = 1018 are shown in Figs. 1 and 2 for cadmium on copper1 and sodium on CsCl2 and the values of obtained therefrom are entered in Table I. It is apparent that the data yield reasonable straight lines with about the same scatter as found using the equation of Pound et al. When the configuration of minimum free energy for a nucleus is a circular monatomic layer, the standard free energy of formation is

Jan 1, 1963

By A. J. Griest, A. P. Young, P. D. Frost

A study was made of the effect of ß grain size on the tensile ductility of a-ß titanium alloys haet treated to strengths in the range 165,000 to 180,000 psi. It was concluded that the primary cause of $ embrittlement is the large grain size which is obtained so rapidly in many a-ß titanium alloys when heated into the ß field. It was also found that grain-boundary a and acicular intragranular a in the microstructure are not necessarily detrimental to the tensile ductility if the prior ß grain size is sufficientlv fine. BETA embrittlement occurs in a-ß alloys when the finish hot-working or stages of the subsequent heat treatment have been done at temperatures in the ß field. In order to avoid this embrittlement, for-gings must be finished at temperatures under the ß transus. For better workability, it would be desirable to forge at temperatures in the ß field. For this reason, research has been conducted to determine the cause of ß embrittlement. Although ß grain size has been considered as a possible contributing factor to ß embrittlement, only limited research has been done to evaluate its effect. The effect of addition elements on ß grain growth in unalloyed titanium has been studied by Liu.&apos; Complete mechanical property data, however, were not obtained for correlation with grain size. Ogden and coworkers2 have investigated the effect of both a and ß grain size and grain shape in Ti-Cr-Mo alloys. Their data indicated that tensile ductility was relatively insensitive to ß grain size at annealed strength levels (140,000 psi ultimate). No study has apparently been made to determine the relationship between ß grain size and ß embrittlement in a-ß alloys heat treated to high strength (180,000 psi ultimate). The high-strength condition is that in which ß embrittlement is particularly severe. Beta grain size is not easily varied through the use of a range of annealing times and temperatures in the ß field, because of the rapidity with which ß grain growth occurs. Short-time heating techniques are needed to obtain the smallest ß grains. EXPERIMENTAL PROCEDURE In this research, the experimental procedure was as follows: 1) Tensile and microimpact specimen blanks were resistance heated to produce a range of ß grain sizes. 2) The tensile and microimpact blanks were then solution-treated in the a-ß field and aged to produce predetermined ultimate tensile strengths in the range 165,000 to 180,000 psi. Tensile and impact ductility were then correlated with a grain size for constant strength levels. Materials—The alloys Ti-6A1-4V, Ti-4A1-4Mn, and Ti-16V-2.5Al are representative of the heat-treatable a-ß types in which ß embrittlement can be severe. The compositions and ß transi of the heats studied are given in Table I. The Ti-16V-2.5Al heat was melted and fabricated to 1/4 in. round at Battelle; the other alloys were obtained as 1/4 in. round rolled from commercial heats. The micro-structures of the as-rolled alloys were fine a-ß mixtures. This structure is typical of titanium alloys hot-worked extensively in the a-ß field. Resistance-Heating Treatments to Establish ß Grain Size—For direit resistance heating, a 1/4-in.-diam s~ecimen was heated with a 3000-watt transformer rated for 1000 amp with adjustable secondary voltage. The apparatus included a spray quench fixture. Both heating and quenching periods could be automatically controlled. For temperature measurements, 28-gage Chromel-Alumel wires were tack-welded to the specimen at its midpoint. A high-speed recorder-controller was used to control the heating cycle.

Jan 1, 1960

By K. T. Aust

The relative interfacial energies of symmetrical tilt boundaries in silver of greater than 99.999 pct purity were measured as a function of orientation difference 0 between 9° and 36° about <001>. The results are in good agreement with the dislocation model of the grain boundary. The energy vs H curve may be represented by the Shockley and Read equation in the form Eoe (0.55—In 8). READ&apos; has indicated that an ideal experimental method of testing the predictions of the dislocation theory of the grain boundary would be to measure the interfacial energies of symmetrical tilt boundaries between face-centered-cubic grains that have a common <001> axis, as a function of orientation difference 0. The misfit H should be defined by a rotation of each grain through an angle of H/2 away from the boundary. Such boundaries might be expected, from geometrical considerations, to be made up of a series of edge dislocations, at least for small values of 0. Energy vs H relationships for tin&apos; and lead:&apos; were previously obtained for an asymmetrical tilt boundary separating two grains in which generally only one grain was rotated about a <001> specimen axis through an angle of H away from the boundary, the other grain remaining fixed. It is possible, however, that the boundary atoms in tin and lead may have attained a symmetrical position, in relation to the orientations of the grains on either side of the boundary, during equilibrium annealing. The two sets of measurements on silicon ferrite&apos; were somewhat better suited for comparison with theory, since the boundaries were symmetrical tilt boundaries in which the axis of relative rotation was <110> in the first series and <l00> in the second; but this alloy has a body-centered-cubic structure. Although the grain boundaries in silver" were symmetrically tilted, the axis of relative rotation was not a simple crystallographic direction, and it varied from boundary to boundary. Although the above measurements were in good agreement with the Shockley and Read equation,"&apos;: it appeared desirable to carry out experiments under the ideal conditions specified by Read.&apos; Consequently, the relative energies of symmetrical tilt boundaries in silver between grains that have a common <001> axis were measured. The technique of equilibrating grain boundaries in oriented tricrystals was used rather than the less satisfactory thermal groove method previously employed for silver bicrystals." Experimental Details and Observations The solidification and seeding techniques, described previouslyh for growing tricrystals of controlled orientations, were used to prepare tricrystal specimens from silver of greater than 99.999 pct purity. The silver was obtained from American Platinum Works, Newark, N. J., in the form of poly crystalline rods 10 cm long and 7 mm in diam. These rods were then cold worked by rolling or drawing them into suitably shaped blanks. Single crystal seeds and tricrystals were grown in a high purity graphite boat by means of a movable furnace with globar heating elements. The graphite boat was enclosed in a Vycor tube, which was first evacuated to about l00/u Hg and then filled with a static argon atmosphere. The maximum temperature outside the Vycor tube was 1250°C. A typical tricrystal specimen of silver is shown in Fig. 1. Grains B and C were grown from seed crystals with a <001> specimen axis or longitudinal direction parallel to the direction of growth and with another <001> direction perpendicular to the surface. Each of the two seed crystals was rotated 18" about the <001> specimen axis but in opposite directions away from the boundary. A symmetrical tilt boundary, therefore, separated grains B and C with an orientation difference 8 of 36" about <001>. Grain A in Fig. 1 was grown from the middle seed with a <110> direction parallel to the specimen axis and with a <001> direction inclined at 45&apos; to the surface of the specimen. The interfaces sepa-

Jan 1, 1957

By K. R. Van Horn

RESIDUAL stresses in metals operate under a cloak of mystery, as they have neither been seen in the laboratory nor detected by means of the microscope. In spite of their phantom-like nature, they frequently exert metallurgical effects that cannot be ignored. In some cases the results have been detrimental, causing rejections or premature failures, but frequently the effects have been highly beneficial to the producer or consumer of metal products. First, however, what is a residual stress? When a metal is plastically deformed by bending, rolling, pressing, or by a phase transformation or precipitation from solid solution, or by a sharp temperature gradient resulting from nonuniform cooling, quenching, or welding, it remains in a state of strain. The strains or strain gradients produced by such operations and retained after all external forces are released are known as residual strains, and the accompanying stresses as internal or residual stresses. Many defects or failures in metal products have been ascribed to residual stresses, sometimes erroneously, because there was no other apparent explanation after the usual metallurgical tools of diagnosis had been applied. For example, during World War 11, the forged aluminum alloy aircraft cylinder head in the reciprocating engine began to replace the cast head with the familiar cooling fins. The fins were machined in the solid forged head by an ingenious milling operation. One plant reported an epidemic of excessive distortion during the delicate high-speed milling. A thorough examination revealed that the composition, heat treatment, mechanical properties, and metallurgical quality of these heads were comparable to those of forgings that machined satisfactorily. It was then claimed that the cause of the machining difficulties was connected with residual stresses resulting from the quenching during the solution heat treatment. An elaborate stress analysis actually demonstrated, however, that the magnitude of residual cooling stresses was lower in the cylinder heads which machined poorly than in those which were satisfactory in this respect. Subsequent tests proved that the machining problems in this case originated from variations in the tools and tool design. Sources of Residual Stresses in Metals Residual stresses are of two origins—mechanical and thermal. Thus, stresses may be produced in a metal by any cold-working process. The distribution and magnitude of these mechanically produced stresses can be calculated in a satisfactory, although approximate, manner for such simple cases as bending, torsion, and expanding of tubes. However, most manufacturing processes are too complex, and the original stress-strain relations in the products are not sufficiently known to permit calculation of the resulting residual stresses. Also, a specific process, such as wire drawing, may vary in complexity or uniformity of working, and large or small residual stresses may result, depending on the conformation of the dies and other features of the working process. Neither substantially unidirectional deformation, such as can be imparted by stretching a metal product having essentially the same mechanical properties throughout the cross section, nor deformation

Jan 1, 1954

By R. C. Nelson, T. L. Weaver, A. I. Michals

This paper describes the design and performance of an apparatus for making continuous nondestructive resistance measurements throughout a spool of fine wire. Highly reproducible results on clean and graphite coated tungsten and rnolybdenum wires from 1 to 9.5 mil are presented. A linear relation between resistance and wire weight (per standard length) was obtained on clean wires, but only on those coated wires with very uniform coatings. Results indicating a correlation between tensile strength, hardness, and resistivity are reported. THE increasing demand for greater uniformity in fine tungsten and molybdenum wires destined for use as mandrels, grids, and coils in radio tubes and as filaments in light bulbs has rendered inadequate the standard (sampling) approach to the control of wire diameter and other physical properties. This ap-

Jan 1, 1961