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By C. S. Smith, L. H. Beck

KNOWLEDGE of the Cu-Zn constitution diagram was critically examined in 1944 by G. V. Ray-nor,1 who suggested the diagram reproduced in Fig. 1 as the best evaluation of available data. No pertinent work on the constitution has been published since that time, although a number of authors have discussed transformation kinetics and theory. Despite the large amount of work that has been done on the constitution of these industrially important and scientifically interesting alloys, minor uncertainties still exist. For example, it is still not possible to say definitely whether a two-phase region exists between the ordered and disordered forms of the 8 phase. A careful re-examination of the phase boundaries in this part of the diagram was therefore undertaken. Two methods were selected for the new investigation—quantitative metallography for the higher temperatures and precision lattice parameter measurement for lower temperatures. Because of the relatively narrow two-phase regions flanking the ß phase in these alloys, quantitative metallography is particularly suited for their examination, since the relative amounts of the two phases are very sensitive to their compositions. The method, however, is useless below about 350°C because of the inadequate resolution of the two constituents. Below 400°, however, the X-ray diffraction method is applicable, although it is of somewhat lower sensitivity in this system. The changes of composition that occur during quenching from above about 500°C entirely vitiate X-ray measurements at room temperature though they do not affect metallographic area measurements. The two methods overlap and supplement each other admirably. Both methods depend on the attainment of equilibrium composition of the two phases in a more or less intimate mixture and thus avoid the difficult problems of nucleation and long range diffusion involved in the conventional metallographic bracketing method. The alloys were melted from a master alloy made from re-electrolyzed cathode copper and Horsehead 99.99 pct Zn. Melting was done under a cover of either borax or charcoal and the alloys cast into a 7/8 in. sq graphite mold for the a-ß alloys or a 3/8 in. diam cylindrical graphite mold for the ß-? alloys. The a-ß alloys were rolled at 750°C to 5/8 in. sq; annealed for 24 hr at 800°C and quenched; then rolled and swaged at 200°C to 3/8 in. diam rods, annealed 24 hr at 200°C, quenched and cold rolled 2 pct reduction. This treatment was intended to obtain a small grain size and to produce many nuclei of the minor phase for growth on subsequent heat treatment. The unworkable ß-? alloys were given preliminary treatment by sealing in Vycor tubes in vacuum and annealing for 4 hr at 800°C followed by cooling in air. Samples of homogenized alloys were checked spectrographically for impurities, but the principal components were determined on samples subsequent to heat treatment. The impurities analyzed averaged approximately as follows: Ag, 0.0002 pct; Fe, 0.004; Si, 0.0008; Cd, 0.005; Mg, 0.0002; and Pb, 0.002. For metallography, samples of appropriate composition were cut into rods 5/8 in. long, sealed in pyrex tubes in vacuum and annealed for eight weeks at temperatures of 470°C and below, two weeks at 480°, 500°, and 600°C, and 4 hr at 700°C, followed by quenching in cold water. Temperatures were accurate to ±2°C. The cylinders were then machined to 8.7 mm diam and a slice weighing 1.5 g cut with a thin saw transversely from the center of each. This

Jan 1, 1953

By C. Dean Starr

The physical basis of the equation correlating electrical conductizlity and temperature coefficient of resistance of solid solution alloys has been inzlestzgated and the nature of the constants evaluated. It is shaun that the same form of correlation is valid irrespective of the magnitude of the temperature coefficient. However, the effect of therma1 expansion and change in resistivity with temberature nust be considered when the magnitude of the temperature coefficient of resistance is near zero. In a comprehensive literature survey conducted at the Armour Research Foundation in 1950, it was found that a linear relationship exists between the electrical conductivity, K, and the temperature coefficient of resistance, a, for solid solution alloys. This was expressed by the equation where B, a constant, depends on the solvent metal but not the solute. A continuing investigation by Hansen, Johnston, and Parks showed this equation was generally appropriate for Cu, Ag, Au, Pd, Pt, and Co base binary solid solution alloys as well as for many ternary alloys of copper over a range of conductivities and temperature coefficient of resistances from 0.02 to 0.60 reciprocal pohm cm and-0.00015to0.004Q per 0 per "C respectively. Eq. [I] was not always valid for alloys that exhibited a change in state (magnetic to nonmagnetic) or for alloys that had a temperature coefficient of resistance near or below zero. For example, in nickel alloys, a simple linear curve as predicted by Eq. [l] was not obtained when the conductivity was plotted against the temperature coefficient of resistance. Hansen suggested that deviations observed were caused by transitions from a ferromagnetic to a nonmagnetic state. Subsequent and more extensive data by ronin on Ni-Mn alloys confirmed Hansen's postulate. While both states independently showed a linear relationship between K and a, the value of B was different for the two states. In some copper and gold base alloys, as well as the platinum and palladium alloys investigated by Hansen, the conductivity did not extrapolate to zero at zero a as demanded by Eq. [I]. This deviation can be readily corrected by simply adding a constant to Eq. [I.] whence Eq. [2] shows the K decreases as a decreases but that K has a positive value when a = 0 which is observed for commercial solid solution alloys as well as the experimental alloys tested by Hansen. While other methods of correlation of electrical properties have been made such as the one by Starr and Wang3 who found a linear relationship between resistivity and temperature coefficient of resistance for Ni-Cr-Al-Cu alloys, the data, in general, can also be correlated by a form of Eq. [2]. Thus, Hansen's empirical equation has considerable merit. The objective of this paper is to determine the physical basis for this equation and to examine the region near zero a in more detail. ELECTRICAL CONDUCTIVITY VS TEMPERATURE COEFFICIENT OF FU3SISTANCE The resistance of a metal or alloy is defined as

Jan 1, 1963

By E. J. Ripling, M. W. Toaz

Tensile tests were conducted on pure magnesium and on four commercial alloys over a variety of temperatures and strain rates. The high positive slope of the ductility vs testing temperature curves that is found over a short range of testing temperatures for these materaturerials was shown to result from the fact that the microstructure was not stable at these testing temperatures. Pure magnesium did not display a transition temperature, although its sub-room temperature ductility was low. This poor ductility resulted from a grain boundary weakness. The aluminum-bearing commercial magnesium alloys had a higher ductility than the pure magnesium. ness.Thealuminum-bearingcommercialThese alloys did exhibit a transition temperature and grain boundaries that were stronger than the grain material. Both pure magnesium and the commercial alloys began initiating cracks at strains equal to one half of their fracture strain. MAGNESIUM base alloys' enormous potential as structural materials lies in their high strength to weight ratios. At present, the high strength magnesium base alloys such as AZ-80, which will be discussed later, have about as high a tensile strength to specific gravity ratio as the highest strength wrought aluminum alloy, 75s-T6, and, of course, a much higher strength to weight ratio than structural steel. Further, since the magnesium base alloys develop their high strength to weight ratios with moderate strengths and extremely light weights, the ratio of load carrying capacity to the weight of many structures is relatively higher for the magnesium base alloys than their strength to weight ratios would indicate. This results because judicious increases in section size, such as increasing the depth of bending members or adding reinforcing ribs, can frequently increase the weight of a structure linearly while the strength and stiffness increase as the second or third power of the added weight. Strength and rigidity must be designed into lightweight structures by those techniques which establish multiaxial stress states. Consequently, strong, lightweight structures frequently also possess a greater propensity toward brittle failures. In order to insure against these catastrophic failures, an extra premium must be placed on ductility and toughness in light alloys. Current knowledge of the ductility and toughness behaviors—notched behaviors—of magnesium base alloys is limited.* Most of the magnesium base alloys * The state of present knowledge regarding the effect of testing temperature on mechanical properties has recently been summar-ized by Pritchard.' crystallize in the hexagonal system, so that they are expected to exhibit a tough and ductile to brittle transition temperature. Actually, a transition temperature behavior has been reported for commercially pure magnesium in the literature, but the characteristics of this transition temperatureh uggest that it may not be a transition in the usual meaning, but simply the onset of some thermal softening, a performance much like that which face-centered-cubic lead might exhibit slightly below room temperature. If transition temperatures do exist, such important questions as the manner in which they are affected by internal variables such as chemical composition and grain size, or the effect of external variables such as rate of straining or notch severity have never been investigated. The investigation reported upon herein was undertaken in order to define some of the mechanical behaviors of the magnesium base alloys better, to gain a better understanding of the influence of some of the above listed variables, and particularly to understand their effect on ductility and toughness better. Material and Procedure Material-—Pure magnesium and four commercial alloys were used in this investigation. The alloys were selected so that chemically they made up a series with approximately the same minor alloying

Jan 1, 1957

By A. J. Griest, P. D. Frost, J. R. Doig

During the past 5 years, research directed toward the development of titanium alloys having improved strength-ductility relationships and heat treatability has been carried out at Battelle for the U. S. Air Force.1"3 In the course of this work, a method of heat treating ß-stabilized titanium alloys was developed which produced a wide range of useful properties.4 The heat treatment consisted of two steps: a) solution treating at temperatures in the a-ß phase region, and b) overaging at a lower temperature in the range 800°to 1100°F. Corollary to the alloy development work, research was conducted on the mechanism of the heat-treatment reaction. The investigations of Frost and co-workers on isothermal transformation in Ti-Cr5 and Ti-Mn8 alloys disclosed the existence of the transition phase, w, during the course of the decomposition of metastable ß phase. Subsequent work at Battelle7,8 'and at Case Institute by Brotzen and co-workerss further clarified the nature of the decomposition process. Beta decomposition was found to proceed by the following series of reactions: 1 2 3 4 a + Ti, My (in eutectoid systems). ßo, ßr, and ßU refer to ß phase of original, enriched, and ultimate alloy contents, respectively. Omega is a transition phase having a complex structure. 10-13 Step 4, of course, occurs only in ß-eutectoid systems. This paper presents data correlating transformation behavior with mechanical properties for the following alloys: Ti-8Mn, Ti-8Mn-2A1, Ti-4Mn-4A1, Ti-6Al-4V, and Ti-4Fe. The isothermal decomposition of ß in titanium-manganese alloys of similar composition has been investigated by Frost and coworkers8 and the effect of various annealing treatments on alloys in this system has been studied by Holden, Ogden, and Jaffee.14 The compositions Ti-8Mn-2Al, Ti-4Mn-4A1, and Ti-6A1-4V, were studied in the present work in an effort to define more clearly the effect of aluminum on the response to solution and aging treatments. Ogden, Holden, and Jaffee15 have invesitgated the effect of aluminum on the response of a similar alloy (Ti-8.8Mn-2.46A1) to annealing treatments, and Luini and Lee16 have made an exploratory investigation of the heat-treatability of the Ti-4Mn-4Al alloy. The Ti-4Fe alloy was studied as an example of a moderate1y active eutectoid system. Holden, Ogden, and Jaffee 17 have studied Ti-Fe alloys and have presented some hardness data for aging at 400°C for alloys of Ti-2.56, 5.01, and 7.35 iron after quenching from the a-ß field (750°C). EXPERIMENTAL PROCEDURES The experimental procedures generally used in the precipitation-hardening study are outlined in the following sections. Departures from these techniques are noted in the discussions of the individual alloys. Table I presents the nominal and actual compositions of the alloys studied, together with the swaging and rolling temperatures. In all cases, these temperatures were in the a-ß field and the microstructures consisted of an equiaxed a-ß mixture. Melting and Fabrication—Except for the commer-

Jan 1, 1960

By R. J. Sherman, M. R. Achter

Creep rates have been measured for nickel at 1200°F in air and in vacuum, and related to the depth of surface cracks in the specimens tested in the two environments. The surface cracks were observed to grow faster in air than in vacuum in both short-time and long-time tests. Crack depths, however, could be correlated with creep rates only in the short-time tests. Although no cracks were observed in a relatively brittle Ni-Cr-A1 alloy creep tested at 1300°F, the appearance of alloy specimens fractured after interruption in creep indicated that there was a decrease of intergranular cohesion resulting from the diffusion of atmospheric gases into grain boundaries. PREVIOUS investigations1-3 have demonstrated that the effect of atmosphere on the high-temperature strength of nickel and nickel-base alloys may be reversed by changes in the stress or temperature of the test. At high stress and low temperature the creep-rupture life is longer in vacuum than in air, while at high temperature and low stress the relative strengths are reversed. A mechanism to explain this behavior was proposed based on two competing processes. Oxidation hardens and strengthens a metal, but adsorption of gas, by lowering surface energy, reduces the work required to propagate an intergranular crack. The controlling process is determined by temperature and stress. Basic to this mechanism is the concept that environment determines the ease of propagation of intergranular cracks and thus affects creep rate and rupture life. To explore the mechanism in greater detail, this investigation was undertaken to determine the effect of atmosphere on crack initiation and propagation rates in nickel1 and a relatively brittle Ni-Cr-A1 alloy.3 EXPERIMENTAL PROCEDURE The materials were the same as used previously. Nickel of 99.8 pct purity had the following impurity content: 0.02 pct Co, 0.03 pct Fe, 0.02 pct Mg, 0.03 pct Si, and 0.008 pct C. Rods were cold swaged from 1/2 in. to 3/8 in. in diam and machined into speci- mens with gage sections 1/4 in. in diam by 1-1/4 in. long. They were annealed in vacuum at 1600" F for 1 hr to achieve a grain size of 0.07 mm. The alloy was composed of 19.1 pct Cr, 3.6 pct Al, 1.7 pct Si, 0.57 pct Fe, 0.10 pct Mg, 0.027 pct C, 0.004 pct S, and the balance Ni. Sheet specimens of 0.500-in. width and 1.25-in. gage length were machined from 0.033-in.-thick strip and annealed in vacuum at 2000° F for 2 hr, resulting in a grain size of 0.036 mm. Large amounts of an intergranular phase were introduced as a result of the anneal. Creep tests on both materials, using equipment previously described by Shahinian; were conducted in air and in a vacuum of 1 x 10-5 mm Hg. They were continued to rupture and interrupted at various stages of the test. Although extensions were measured from dial gage readings of movement of the lever arm, it is considered that valid comparisons of creep rate may be made in this manner.l Two parameters were measured metallograph-ically* on longitudinal sections of nickel specimens interrupted during creep—the mean depth of surface cracks 2, and the density n as the number of cracks per unit length of surface. They were combined into one parameter by the relation p = n-d [1] As used here, p is equal to the total of crack depths per unit length of surface. RESULTS Nickel. It is well known that the incidence of intergranular cracking is increased with increasing rupture life. Indeed, it is evident in Tables I and I1

Jan 1, 1962

By A. R. Troiano, W. J. Barnett

IN recent years the demands of space limitations and increased loads, particularly in the aircraft industry, have accelerated the trend toward utilization of ultra-high strength steels. The increased application of such steels has focused attention on the phenomenon of delayed failure or static fatigue. Parts subjected to a static load, after successfully sustaining the load for an extended period of time, may fail in a brittle manner. Subsequent examination of such failed parts by conventional laboratory tests in many cases reveals no apparent signs of embrittle-ment. That is, the material exhibits good ductility and impact resistance. Furthermore, consideration of the service conditions (environment and temperature) under which this brittle failure occurred eliminates its classification as a stress-corrosion or creep type of failure. Recently this unique time dependent fracture process has been the subject of numerous investigations. The most significant result of these studies was the recognition of hydrogen as the source of embrittlement. While the effect of numerous variables on the occurrence of static fatigue failure has been defined, an adequate explanation of these behaviors is lacking. The occurrence of this phenomenon in steels generally has been limited to strength levels in excess of 180,000 lb per sq in. Although steels at high hardness levels have exhibited delayed failure in the absence of hydrogen introduction after heat treat-ment,'.' this behavior was most prevalent when the material in processing had been subjected to an environment conducive to the absorption of hydrogen. Delayed failures have been produced in high strength steels by the introduction of hydrogen

Jan 1, 1958

By R. J. Sherman, M. R. Achter

IT has often been reported that coatings may strengthen single crystals and polycrystalline specimens of coarse grain size. This note reports the effect of a surface layer of fine grains on the creep-rupture properties of coarse grained nickel 99.8 pct pure. Sheet specimens were machined from cold-rolled material, finished by surface grinding and annealed at 1230°C in vacuum for 4 hr. Half of them were re-ground on faces and sides and annealed at 925"C for 1 1/4 hr. The double grind-anneal treatment produced a structure consisting of a surface layer of fine grains of 0.02 mm diam on a coarse-grained substrate of grains of 0.40 mm diam. Comparison with specimens which received only the single grind showed that the second grind-anneal did not alter the structure of the substrate. Several modifications were made in specimen design to eliminate erratic rupture behavior outside of the gage length. In the final design the gage section, oriented parallel to the rolling direction, was 1.00 in. long, 0.4 in. wide, and 0.0625 in. thick. End tabs were pinned in place. Although other configurations (welded end tabs, transverse orientation, and wider gage section) showed similar effects of a layer of fine grains, because of the erratic rupture behavior, only the data from the final design are reported here. Creep tests were performed at 650°C in air and in a vacuum of 10~5 mm Hg. Creep rates were measured from the movements of the lever arm. Since the broken sheet specimens could not be fitted together, elongations at fracture measured by means of gage marks, do not include the necked portions adjacent to the fracture. Results of the creep tests with and without the fine grained surface are given in Table I. An explanation for the lower strength in air than in vacuum has been proposed previously in terms of the reduction of crack propagation energy by gas adsorption.l In both environments the fine-grained layer produced a small decrease in minimum creep rate and, except for the shortest test in air, a substantial increase in rupture life. The elongation values at rupture, as they are measured here, do not demonstrate an appreciable effect of the grain structure but do show much smaller ductilities in air than in vacuum. Greater elongations maybe associated with the finegrained layer, however, especially in vacuum, in creep curves such as those in Fig. 1. Duplicate tests were not run to determine the re-producibility of the data. It is felt, however, that, in view of the consistent behavior, the prolongation of rupture life may be attributed to the effect of the fine-grained surface. In the data not reported be-

Jan 1, 1962

By W. F. Domis, F. von Gemmingen, R. W. Whitmore, F. Garofalo

Constant-load creep-rupture tests at 1100°, 1300° and 1500°F were made on a Type-316, 18 Cr-8 Ni-ZMo, austenitic stainless steel to determine the relationship between ruptzire life and other aspects of creep behavior, The test program was designed on a statistical basis to check the variability of various creep properties and to determine emprically the dependence of minimutn creep rate and ruptzire life on initial stress, The dependence of the rupture life, tn, on the initial stress, a,, is found to be related to the stress dependence of the wrinimum creep rate, i,, and secondary creep strain, The instabilities or breaks found in the conventionual log - logt, plots can be traced to either a change in the linear dependence of log i, on log a, or to a change in secondary creep strain. In the alloy tested, rupture is found to be predowmanantly of the inter crystalline type, For this material, the secondary creep strain is -found to depend on the nature of the grain boundary precipitate, which affects grain boundary migration. It has been shown for a variety of metals and al tested at elevated temperatures under creep conditions that the empirical relationship exists between rupture life, tr, and minimum creep rate, i,. This relationship, in which C and a are in some cases independent of stress or temperature, shows in a general way that creep rupture depends on creep behavior prior to tertiary creep stage. To determine more fully the factors which control creep rupture requires, therefore, more knowledge of the relationship between rupture and creep behavior. To obtain such information, constant-load creep-rupture tests have been made on a Type-316, 18 Cr-8 Ni-2 Mo, austenitic stainless steel at 11000, 1300°, and 1500°F. These tests were designed on a statistical basis to determine the variability of the various creep properties measured and to determine empirically the stress dependence of minimum creep rate and rupture life. As a result of this work, various empirical relations have been established defining more closely the factor, C, in the relation between rupture life and minimum creep rate. This factor is found to be proportional to the amount of strain during secondary creep. The variation of secondary creep strain with rupture life and temperature is determined and its effect on rupture behavior discussed. The variability in minimum creep rate and rupture life is also dis- cussed and the dependence of these quantities on initial stress is interpreted. TEST MATERIAL AND TEST PROCEDURES The material tested is an austenitic stainless steel, AISI Type 316, of the following composition: C, 0.07 pct; Mn, 1.94 pct; P, 0.01 pct; S, 0.021 pct; Si, 0.38 pct; Cr, 18 pct; Ni, 11.4 pct; Mo, 2.15 pct; All 0.003 pct and N, 0.043 pct. The material was received as a hot-rolled 0.5-in. diam bar which was sectioned into 3.25 in. long blanks. Each blank was heat treated by holding 1/2 hr at 2000° F followed by water quenching. A 3/8-in. coupon was removed from each heat-treated blank and the microstructure was examined, the grain size determined, and the hardness measured. The microstructure was found to be uniform from blank to blank and the grain size was found to range from 4 to 6 ASTM numbers. Hardness, measured using a 20-kg load, varied between 127 and 148 Vpn. Tensile creep-rupture specimens having a 0.25 in. diam within a 1.5-in. reduced section were machined from the heat-treated blanks. Constant-load tests were made on these specimens at 1100°, 1300°, and 1500 F. Six specimens were tested at each stress level. Three creep-rupture machines were employed for tests at each temperature, two specimens being tested in each machine for each stress level. To minimize any effect due to local inhomogeneities along the length of the as-received bar the specimens were randomized before test. Each specimen was tested to rupture and in most cases an autographic extension-time curve was obtained. For very low stress levels at 1500°F no auto-

Jan 1, 1962

By N. J. Grant, A. W. Mullendore, Y. Ishida

Creep tests were performed at 500°F on polished specimens of A1-3 pct Cu at stresses of 2000, 4000, and 6000 psi. The effects of the size and distnbution of the second phase were studied in connection with the mechanisms of deformation, especially grain boundary sliding. Although the amount of grain boundary sliding varied considerably for the different heat treatments, yestriction of grain boundary sliding is not due primarily to precipitate on the grain boundary. NUMEROUS prior investigations of grain boundary sliding, notably those of McLean, 1 Rachinger, 2 Rhines, Bond, and Kissel, 3 and Brunner and Grant,4 have established the importance of this phenomenon in the deformation of pure aluminum and its solid-solution alloys at elevated temperatures. An extension of this kind of study to the case of a simple two-phase structure is an important step towards understanding the deformation behavior of more complex alloys. A two-phase A1-3 pct Cu alloy was selected for this study. The creep behavior of alloys in this system has been studied by Sully and Hardy,5 by Underwood, Marsh, and Manning,' and by Pelloux, Chaudhuri, and Grant.7 In these studies, the prior heat treatments were such that some precipitation took place during the tests in most cases. Pelloux, Chaudhuri, and Grant7 studied the creep of A1-2 and 3 pct Cu alloys in the overaged condition. Their results indicated that the structure most effective in promoting high-temperature strength consisted of a fine, closely spaced grain precipitate and large, widely spaced particles on the grain boundary. The present work consists of quantitative meas- urements of grain boundary sliding during creep of an A1-3 pct CU alloy with four different precipitate distributions. The aims were to quantitatively define the role of the second phase on grain boundary sliding, and to obtain information regarding the mechanism of grain boundary sliding. MATERIALS AND PROCEDURE A high-purity A1-3 pct Cu alloy, kindly supplied by Alcoa, was used in this investigation. The composition of the alloy in weight percent was as shown in Table I. This composition is such that A12Cu exists as a second phase at temperatures below 850°F. A homogeneous grain size of 0.6 to 0.8 mm was obtained by annealing the machined test bars for 5 min at 1000°F, furnace cooling to 930°F, and homogenizing for 5 hr. Following the recrystalli-zation and homogenizing anneal, four different heat treatments shown in Fig. 1 were utilized. The F7 and F5 treatments utilize a furnace cool to the aging temperature while Q7 and Q5 have a water quench from the homogenization temperature before aging. Figs. 2 to 5, and Table 11, show the size and shape of precipitate dispersions obtained with the above heat treatments. The heat treatments produce variations in the dispersion both in the grains and along the grain boundaries. Precipitate particles along the grain boundaries are rounded and large (about 1.5 p diameter) in the F5 and F7 structures (Figs. 3 and 5). The grain boundary precipitate was somewhat smaller (0.9 p diameter) in the Q7 structure and no grain boundary precipitate was detected in the Q5 structure using light microscopy. The pre-

Jan 1, 1964

By Nicholas J. Grant, Italo S. Servi

Extensive data of minimum creep rates and rupture times for high purity and commercial aluminum confirm the existence of a transition range from the low temperature-type to the high temperature-type behavior. The data are analyzed in line with the suggested theories of deformation of metals. CONSIDERABLY more work has been done on the rupture and creep behavior of commercial alloys than on the less complex, high purity metals. As a result, certain fundamental behaviors are overlooked. One of the lesser known variables affecting the high temperature behavior of metals is the impurity content (or alloy content). Impurities are known to affect strongly the recrystallization temperature, electrical resistivity, and other properties of metals, but the effect on creep and other high temperature mechanical properties has been determined for very few materials. In view of these facts aluminum appears to be a fairly ideal metal, since it is available in a wide range of purity contents from 99.995+ down through the 2s (99.0 + Al) and 3s (1.2 Mn) grades in small steps. It is highly resistant to oxidation and other surface instabilities, leaving recrystallization and grain growth as virtually the only instabilities. Control of grain size is also well standardized. Limited data on the creep of aluminum have been obtained by Dushman et a1.l for high purity aluminum; by Sherby2 on 2s aluminum of variable grain size; and by Dorn and Tietz³ on cold-worked 3s aluminum. Experimental Procedure The apparatus consisted of a constant stress, creep testing unit similar to the type described by Hop-kin.' The specimens were held at temperature for 30 min before loading. The loading time was less than 2 min. Factors affecting the accuracy of the data were: 1-—the temperature gradient and control, ± 3°F; 2-the stress determinations, ± 1.5 pct; and 3—elongation measurements (1 in. gage), ? 0.001 in. Three grades of aluminum were tested: 1— high purity (99.995 pct Al), 2—2s (99.3 pct Al), and 3—3s (98.2 pct Al). The spectrographic analyses of these materials are reported in Table I. The specimens were annealed then electropolished in a perchloric-acetic mixture before testing. Data on heat treatments and grain size obtained appear in Table 11. The entire creep curve was determined for almost all of the tests. A few tests were interrupted after the beginning of the third stage of creep, and in these cases the rupture time was estimated. Experimental Results Constant stress creep-rupture testing gives a much longer, more accurately measurable second stage of creep than constant load testing. This behavior is in agreement with the results obtained by Andrade for lead (see Fig. 1). If the test is run to completion, the third stage of creep appears as soon as stress intensification occurs. In the case of specimens which fail in a ductile manner, the stress intensification begins when the sample starts "necking". This differs from the "high temperature brittle" specimens in which the stress intensification is caused by intercrystalline cracking. These specimens

Jan 1, 1952

By C. S. Roberts

Four binary alloys in this system were creep tested at 300°' to 600°F. A photographic study of microstructural changes showed that the outstanding creep resistance results primarily from a potent precipitation hardening locally at grain boundaries. Twinning was correlated with the primary stage and nonbasal slip with the tertiary stage of creep. THE utility of the rare earth metals as ingredients of magnesium alloys destined for elevated temperature application has been recognized for about 15 years. A review of the early development of these alloys has been given by Leontis. 1,2 It has been only recently that a desire has arisen to understand basically their remarkable creep resistance. The present research had that object. The work of Leontis showed that the differences between the behavior of the individual magnesium-rare earth element binaries was of commercial significance. However, the variations were small compared to the overall difference in creep resistance between the group as a whole and the magnesium alloys of the Al-Zn type. It was decided to conduct this investigation with one binary system which would be representative of the magnesium-rare earth element alloy group. Cerium was chosen as the solute because of its near-middle position in the series and because of its availability in the commercially pure form. A previously published description of the creep behavior of electrolytic magnesium" serves as the background to this research. The experimental approach used in that investigation has been partially repeated here. A series of binary alloys was planned to include the following: 1—A dilute alloy which would contain the cerium almost entirely in solid solution. This would assess the solid solution effect. 2—An alloy which is nearly saturated at the selected solution heat treatment temperature, 1070°F. Here the effect of nearly maximum precip- itation would be obtained without the influence of undissolved Mg-Ce intermetallic. 3—An alloy containing slightly more cerium than is soluble at 1070°F. This would allow the investigation of the effect of a small amount of excess intermetallic. 4—A high cerium alloy in which the influence of a large volume of undissolved intermetallic may be examined. Experimental Details In order to specify compositions of the binary alloy series a knowledge of the solubility of commercially pure cerium in solid electrolytic magnesium and also of the composition of the terminal intermetallic phase was necessary. The latter has been proven to be approximately Mg,Ce by Voge14 and Haughton and Schofield.5 A series of both cast and extruded alloys were solution heat treated 24 hr at 1070°F for a solubility determination. Lineal analyses of the polished and etched microstructures were accomplished with the aid of a Hurlbut

Jan 1, 1955

By Milton R. Pickus, Earl R. Parker

THE modern theories of creep¹-4 in general have been based upon the concept of generation and migration of dislocations, with the generation process normally assumed to be rate controlling. The theories are generally deficient in that they fail to take into account many factors that are known to influence creep. The influence of the state of the surface of the test specimen has been almost completely overlooked; yet the present report shows that the nature of the surface may, in certain cases, govern the creep characteristics of a specimen. In the period since Taylor" applied the concept of dislocations to a study of metals, a school of thought has developed that closely relates the plastic deformation of metals to the generation and migration of dislocations through the crystal lattice. It might be expected that the thermal energy required for the generation of a dislocation would be different from that for migration of the dislocation through the lattice. Furthermore, the activation energy for generation would be expected to vary for different parts of the solid metal. It has been predicted that dislocations would be generated most easily at external surfaces, but could also be activated at certain internal surfaces such as grain or phase boundaries. Within the body of the metal a range of values for the activation energy might be expected because of different degrees of disorder at such regions as grain boundaries, impurities, and second-phase particles. The particular value of the activation energy that was rate determining could then depend on the specific conditions of a test. If, for example, the surface atoms were by some means constrained, the generation of dislocations in the body of the metal might become the important factor. On the other hand, other conditions may favor generation at the surface. It is possible then that the creep behavior may not be completely determined by the inherent properties of the metal. Even the environment in which a test is carried out could have a significant effect. In fact it is conceivable that in order to obtain the maximum creep resistance from a given alloy, the surface atoms must be so constrained that the activation energy for generating dislocations on the surface is at least equal to that required for generation in the body of the metal. On the basis of such considerations, and in view of the limited number of publications discussing this subject, it seemed that an investigation of the influence of the state of the surface on creep might yield information of both theoretical and engineering interest. Experiments on single crystals, demonstrating a variation in the mechanical properties due to alterations in the surface layer, have been reported by several investigators.6-13 he results of these experiments have been briefly summarized;14 consequently, the earlier work will not be reviewed here. As an example of these findings the observations of Cottrell and Gibbons may be cited. They reported the critical shear stress of a lightly oxidized cadmium single crystal is greater by a factor of 2½ than a specimen with a clean surface. Materials and Methods Single crystals M in. in diam and 8 in. long were prepared from Horse Head Special zinc, melted under an atmosphere of helium in a large pyrex test tube, and drawn up into a long ½ in. diam pyrex tube by means of a vacuum pump. The cast zinc rods thus produced were cut into convenient lengths and sealed in evacuated pyrex tubes. Single crystals were grown by gradual solidification of the remelted rods. Cleaving the ends of the single crystal specimens chilled by liquid nitrogen proved a simple method for determining orientations from the exposed basal plane from the markings left on the cleaved surface that gave the slip directions with sufficient accuracy for the experimental work. The specimens chosen for the experiments were those having the angle between the basal plane and the specimen axis within the range of 15" to 65". Since zinc single crystals are quite delicate, it was necessary to devise an appropriate method of gripping the specimens in order to suspend them in the furnace and apply the load. Stainless steel collars were prepared having an inside taper, the smaller end of the taper being of such a size that the specimen could just pass through freely. The tapered hole did not extend the full length of the collar; a sufficient thickness of metal remained so that a hook could be attached to provide a means of applying the load and suspending the specimen. One of the collars was slipped over the upper end of a specimen which was supported vertically in a steel jig. The collar was then heated electrically until the end of the crystal melted and filled the collar with molten zinc. At this point the application of heat was discontinued, whereupon the molten zinc quickly solidified, due to the chilling effect of the jig. The specimen was then inverted and the second collar applied in a similar manner. The jig served several purposes: limiting the length of specimen that was melted, providing excellent alignment of the collars with respect to the specimen axis, and protecting the specimen from mechanical damage. Once the specimen was suspended in the furnace and loaded, it was desired to accomplish the surface treatment with a minimum of disturbance of the specimen. Around the specimen was a long pyrex tube, the upper portion of which was approximately 1 in. in diam, and in it was a copper coil of such a diameter to fit snugly against the tube. A specimen, approximately ½ in. in diam and 4 in. long, was suspended by means of a stainless steel rod so that it hung within the copper coil. The lower portion of the glass tube was approximately ¼ in. in diarn, and passing through it was a 5/32 in. diam stainless steel rod which hung from the lower specimen collar. This portion of the glass tube and the stainless steel rod extended through the bottom of the furnace. A T-connector, with suitable packing, was attached to the lower end of the stainless rod to provide a water-

Jan 1, 1952

By ED. E. Furman, R. H. Atkinson

HITHERTO the practical creep testing of precious metals has received little or no attention. The only previous creep tests of precious metals have been made with wires under conditions such as to yield much more rapid rates of creep than in engineering tests.', ' Up to the present time the value of creep bars of adequate size, in the absence of real need for engineering data, has deterred investigators. However, the increasing use of platinum at high temperatures has demonstrated the need for reliable creep data for the guidance of engineers, especially those engaged in designing certain specialized chemical plant equipment. In order to supply this need, creep tests were conducted at 1382°F (750°C) on 0.290 in. diam specimens of platinum, 90 pct Pt, 10 pct Rh and palladium. The platinum was high purity, nominally 99.95 pct Pt. The 90 pct Pt, 10 pct Rh was of the same high quality as is used for making gauzes for the catalytic oxidation of ammonia. The palladium was also of high purity; two batches of palladium bars were tested, one deoxidized with calcium boride and the other with aluminum. Spectrographic examination of the palladium confirmed its good quality; the only significant impurities apart from the residual deoxidizers were traces of silicon and lead. Procedure The creep bars, which were furnished by Baker and Co. to our specification, were 6 ¾ in. in overall length with a 4½ in. (4 in. gage length) reduced section 0.290 in. in diam and had the ends threaded (?-NC16). It may be of interest that the bars were valued at up to $600 each. The specimens were supplied in a 50 pct cold-worked condition to facilitate attachment of the creep extensometer, which was of the push rod type. Because of the softness of the platinum and palladium, the extensometer rings were secured to the test section by means of circular knife edges instead of the usual pointed set screws. The extensometer rods extended through the bottom of the furnace and readings were taken with a 0.0001 in. "Last Word" dial gage fastened to the rods for the duration of the test. The bars were directly loaded by hanging weights from the lower specimen grip. All tests were conducted at 1382°F ± 2°F, and an effort was made to maintain the temperature gradient over the test section within 2°F. The ends of the furnace tube were packed with asbestos wool, which allowed a very slow circulation of air through the tube. Annealing was accomplished in the creep furnace before the load was applied. The platinum and palladium specimens were annealed at the test tem- perature for about 17 and 24 hr respectively; in the case of the rhodioplatinum it was found expedient to anneal for 1 hr at 1922°F (1050°C). Pilot samples cut from the same stock as the bars were used to check annealing procedures. Pertinent measurements of grain size and hardness were recorded. Results and Discussion The creep data obtained are given in Table I and the creep curves are plotted in Figs. 1, 2, and 3. Two platinum specimens, tested under a stress of 250 psi, had almost identical creep rates at 2000 hr, namely 0.000008 and 0.000009 pct per hr. A third platinum specimen, stressed at 400 psi, had a creep rate at 2000 hr of 0.000026 pct per hr; the reason for a rather sharp decrease in creep rate during the period from 1200 to 1600 hr is unknown. As it was thought that 90 pct Pt, 10 pct Rh would have a lower creep rate than platinum, the first sample was tested at 400 psi; however, the creep rate was approximately 50 pct greater. Microex-amination revealed that differences in grain size might be responsible for the unexpected result, as annealing at 1382°F developed an average grain diameter of 0.0021 in. in the rhodioplatinum specimen compared with 0.004 in. in the platinum bar. Annealing the alloy for 1 hr at 1922°F (1050°C) increased the average grain diameter to 0.0032 in. and materially improved the creep resistance, making it much better than platinum. A second specimen annealed at 1922°F (1050°C) and tested under a stress of 550 psi had a creep rate of 0.000022 pct per hr at 2000 hr, which was still substantially lower than that shown by the specimen annealed at 1382°F (750°C) and stressed at only 400 psi. In contrast to the creep behavior of the platinum and rhodioplatinum specimens, the palladium bars, whether deoxidized with calcium boride or aluminum, were characterized by high first stages of creep. However, after about 1200 hr of test, the creep

Jan 1, 1952

By O. D. Sherby, J. E. Dorn

SEVERAL years ago Zener and Hollomon1 suggested that the flow stress of metals might be related to the temperature and strain rate in accord with the functional equation: s=s(eeh/rt) [1] at the same state. The Zener-Hollomon relation also contains the significant tacit implication that the energy for activation, AH, is substantially independent of the state of the material. The utility of this method for correlating creep data with tensile data was illustrated in a preliminary reportL on the effect of alloying additions on the secondary creep rates of binary a solid solutions in aluminum as shown for Al-Mg alloys in Fig. 1. Not only do the secondary creep and ultimate tensile properties for each alloy correlate well on this plot but in addition the activation energy, AH = 17,900 R cal per mol. is identical for the various compositions. Similar types of curves correlating the secondary creep rates at 422°K (300°F) with ultimate tensile data were also obtained for a series of dilute a solid solutions of copper, germanium, zinc, and silver in aluminum. In all cases the activation energy for creep, AH, was found to be equal to about 17,900 R cal per mol independent of the type of alloying element or its concentration. The coincidence of the activation energies for these alloys is probably due to the fact that the activation energies for creep are rather insensitive to small composition changes. Alloying additions, as shown in Fig. 1, however, increased the stress necessary to obtain equivalent values of ee?H/RT. Thus the stress level in curves of the type represented by Fig. 1 gives the relative creep strengths of the various alloys. Inasmuch as these correlations between creep and tensile data were obtained for creep tests at 422°K, it appeared advisable to ascertain the range of secondary creep rates and temperatures over which correlations between creep and tensile data could be made on the basis of the Zener-Hollomon relationship. If, for example, the activation energy changes with different ranges of creep temperatures, the utility of the proposed analysis would be severely weakened. But if AH is constant not only for all dilute alloys, but also over wide ranges of temperature and secondary creep rates, confidence will be developed not only in the broad utility of the Zener- Table I. Chemical Analysis':' and Grain Size of Alloys Mean Grain Residual Impurities. Wt Pct Diam- Alloying Atomic-eter, Element Pct Si Fe Cu Mg Mn mm Aluminum 99.987 0.003 0.003 0.006 0.001 0.25 Magnesium 1.617 0.003 0.004 0.006 0.26 Copper 0.101 0.003 0.003 0.0006 0.001 0.29 Zinc 1.616 0.003 0.005 0.007 0.001 '0.26 * The authors express their appreciation to the Aluminum Company of America for the preparation and chemical analyses of these alloys. Hollomon relationship, but also in its theoretical justification. The following investigation was instituted in order to ascertain the range of validity of the Zener-Hollomon relationship when it is applied to creep and tension data. Materials, Equipment, Technique In view of rather extensive correlatable data now available on the plastic properties of a series of binary a solid solutions of magnesium, copper, germanium, zinc, and silver in aluminum, these alloys were again selected for the present investigation. Previous reports have already covered the tensile properties of these alloys at subatmospheric temperatures," and at elevated temperature," as well as their fatigue properties at atmospheric temperatures, nd their creep properties at 422°K.' Resistivity measurementsa as well as precision lattice constant determinations? evealed that these alloys are a solid solutions. After homogenization. 0.100 in. thick sheets were rolled to 0.070 in. in thickness and recrystallized to about the same grain size. Since the details of these treatments were reported previously," they will not be repeated here. In order to appropriately reduce the scope of creep tests in this investigation only the typical alloys shown in Table I were investigated. All creep specimens were machined such that their tensile axes were in the rolling direction of the 0.070 in. sheet stock. The gage section was 2 in. long and 0.500 in. wide with a reduced section of 3.50 in. Creep strains were measured by means of rack and pinion type extensometers with a sensitivity of 0.005 in. per division. Readings were estimated to 1/10 of

Jan 1, 1953

By R. M. N. Pelloux

This study of aluminum-copper alloys had two aims: 1) To determine the effect of the amount and distribution of a second phase, CuAl2, on the creep-rupture strength, ductility, and fracture characteristics of the alloys. The work of Gemmell and grant' on single-phase aluminum-copper alloys provided a basis for the present study. 2) To attempt to provide a relation between the microstructure and strength of two-phase alloys deformed at comparatively high temperatures (greater than 0.45 T,). The creep behavior of the two-phase magnesium alloys Mg;Ce and Mg-A1, has been treated by Roberts. 9 In work reported by Sully and Hardy4 and by Underwood, Marsh, and Manning~ on A1-Cu two-phase alloys, and also in a portion of the work of Gemmell and grant,' aging took place during the creep tests. 'In the present work, overaged aluminum-copper alloys were subjected to creep deformation at two temperatures, 500 and 700OF. The overaging treatments to produce the precipitate dispersions were performed prior to the test, at temperatures which were the same as the ultimate respective test temperatures. Hence, the present study is concerned with the creep behavior of stable (in contrast to "underaged") two-phase A1-Cu alloys, i.e., alloys in which no depletion of the solid-solution matrix occurred during: creep. MATERIALS AND PROCEDURE A 2 and a 3 pct Cu alloy, supplied by Alcoa, were studied; Table I shows the compositions. The grain size of the specimens, 0.9 to 1.0 mm, was achieved by annealing the machined test bars for 2 hr at 1000°F, followed by furnace-cooling to 900°F, and homogenizing for 4 hr. Both compositions are in the single-phase condition at 900°F. Two types of overaged dispersions, termed "over-aged I" and "overaged 11" were prepared after the grain size and the homogenization anneals. The overaged I alloys were prepared by quenching to room temperature after homogenization, aging at either 500' or 700°F for 72 hr, and air-cooling to room temperature. The overaged I1 alloys were prepared by furnace-cooling after homogenization, to either 500' or 700°F, and holding at the necessary temperature for 72 hr. The times for furnace-cooling from 900°F to 700° and 500°F were, respectively, about 2 and 3.5 hr. The structures of the A1-2 pct Cu alloys are shown in Fig. 1 (overaged I) and in Fig. 2 (overaged 11). A comparison of Figs. 1 and 2 shows that in the overaged I alloys the precipitate particles along the grain boundaries are much more closely spaced and the grain boundaries are straighter than they are in the overaged I1 alloys. Further, the particle size and spacing in the grains are smaller than in the overaged I1 alloys. Microstructures of the A1-3 pct Cu alloys have not been shown; the structures of these alloys differed from those of the A1-2 pct Cu alloys only in that the distribution density of the particles was greater. The creep specimens had a gage section 1 in. long with a diameter of 0.155 to 0.195 in. Before testing, specimens were electropolished in a solution of 100 cc glacial acetic acid, and 30 cc of 60 pct perchloric acid, at 40' to 50°F, at 24 v. The specimens were kept refrigerated prior to testing to avoid precipitation at room temperature. Constant stress creep tests were conducted; the load was applied 75 min after heating of the specimens to test temperature had begun. EXPERIMENTAL RESULTS Creep-Rupture—Fig. 3 shows the log stress-log rupture life plotfor the overaged alloys studied, and also for the underaged A1-2 pct Cu alloy.' At 700°F, the stress-rupture life relationship is nearly independent of both the amount of precipitate (i.e., composition) and of the type of overaging treatment (i.e., precipitate dispersion). At 500°F it is apparent that the increase in rupture life that was ex-

Jan 1, 1960

By B. A. Wilcox, A. H. Clauer

DURING the course of an investigation on the high-temperature creep behavior of TD Nickel* (Ni + 2) vol pct ThO2), it was observed that the creep fractures were similar in appearance to low-temperature ductile fibrous fractures and creep ruptures by cavitation. Microfractographs of fibrous ruptures are typically characterized by a dimpled appearance, with second-phase particles frequently found near the bottom of the dimples.'-4 These somewhat resemble creep ruptures by cavitation, in that fracture occurs by void formation, with the subsequent growth and final merging of the voids to form a complete fracture.' It is the purpose of this communication to describe the creep fracture of TD nickel and suggest a mechanism for the rupturing process. The discussion is relevant to material crept to fracture in vacuo at a constant stress of 18,000 psi, over the temperature range 900" to ll00°C. The material used in this investigation was 1/2-in.-diam bar stock supplied by Du Pont, contain- ing 2.3 vol pct Tho2. The final fabrication treatment consisted of -95 pct reduction by swaging followed by a 1-hr anneal at 1000°C. Transmission and replica electron microscopy revealed that the material had a fibered structure with a transverse grain size of -1 µ and a longitudinal grain size of 10 to 15 µ. Selected-area diffraction indicated that the fiber axis was parallel to (00l), in agreement with the results of Inman et a1.6 The thoria particle size varied from 80 to 1000Å, with an average size of 400Å, and the mean particle spacing was about 1200Å. The remarkable structural stability7 was confirmed by annealing for 6 hr at 1300°C (about ' 0.9 the absolute melting point). Transmission electron microscopy revealed that the only structural change was a slight decrease in dislocation density. Furthermore, recrystallization or grain growth during creep has not been observed. All specimens were annealed in vacuo at 1300°C for 3 hr prior to creep testing. The following times to rupture were obtained for vacuum creep tests at a constant stress of 18,000 psi: 900°C, 854 hr; 930°C,

Jan 1, 1965

By G. S. Ansell, J. Weertman

The creep behavior of an aluminum alloy hardened with a finely dispersed phase of aluminum oxide was investigated. The as-extruded alloy shows an approximate steady-state creep in which the creed rate depends exponentially on the applied stress. The activation energy of creeb is abbroximately 150,000 cal per mole. The recrystallized alloy shows no steady-state creep. ONE method of improving the creep resistance of a metal is to introduce a finely dispersed second phase into the metal matrix. The improvement of the creep resistance has been qualitatively explained by assuming that the dispersed second-phase particles act as obstacles to dislocation motion. If the main effect of second-phase particles is simply to hinder dislocation motion then it is possible to derive a high-temperature creep equation for a dispersion-hardened alloy in a straightforward manner. In the Appendix of this paper such an equation is derived from a creep model which works very well for pure metals. Recently, F. V. Lenel has fabricated, for the first time, powder extrusions of aluminum-aluminum oxide in a large-grained recrystallized form. This alloy, designated as MD 2100, consists of a fine dispersion of aluminum oxide plates in a matrix of commercial purity aluminum. A considerable amount of investigation has been carried out concerning the microstructure and physical properties of this alloy.&apos; ) The aluminum oxide is present in the form of flakes 130A units thick and 0.3 u on edge. They are dispersed in the aluminum matrix with an average spacing of approximately 0.5 jx. The spacing varies in the range of 0.05 to 1.5 µ. The alloy structure is extremely stable at high temperatures. For this reason the alloy offers a unique opportunity for a fundamental study of creep of a very finely dispersed two-phase alloy. Lenel supplied specimens in both the unrecrystallized and recrystallized condition. This paper reports high-temperature creep experiments carried out on these specimens. The results obtained were rather unexpected. No steady-state creep was observed in the recrys-tallized material. In fact, after some transient creep which takes place upon loading, the creep rate is essentially zero ( < 10-8per min). If the second-phase particles acted solely as obstacles to the motion of dislocations, measurable steady-state creep would be expected. Since none is observed it appears that the main effect of the fine dispersion in the recrystallized material is to inactivate the dislocation sources themselves, rather than hinder the motion of dislocation loops created at these sources. EXPERIMENTAL DETAILS Specimens were tested in wire form, 0.087 in. in diam for the as-extruded alloy, and 0.035 in. in diam for the recrystallized alloy. These samples were held in friction-type wire grips; a gage length of 2.5 cm was used for all the creep tests. The specimens were held at 600°C in the test apparatus for at least 15 hr prior to each test. The tests were run under the condition of constant loading and, since the creep strains were small, can be considered as constant stress tests. The temperature of testing was held constant within 3°C. Elongations were measured with an optical cathetometer which was capable of measuring strains as smaIl as 0.00012. This allowed the measurement of strain rates as low as l0-8&apos;per rnin. In addition to the creep tests optical micrographs were made in order to determine both the grain size and microstructure of these materials. RESULTS Fig. 1 shows a few typical creep curves obtained from the as-extruded material. The elongations were somewhat erratic, but each curve shows a region of quasi-steady-state creep from which an approximate steady-state creep rate can be obtained. In general the higher the stress at a given temperature, the greater the total elongation before fracture. The lower the applied stress, the longer is the region where the creep rate is almost constant. Summary data from the creep tests of the as-extruded material are listed in Table I. The steady-state creep data of the as-extruded material for a range of stresses at a constant temperature follow a creep equation of the type creep rate = K&apos; = A exp (&) [11 where A and B are constants, k is Boltzmann&apos;s constant, T is the absolute temperature, and a the stress. The standard error of estimate of the data received is less than one order of magnitude. As shown in Fig. 2, if one compensates the creep-rate data for the effect of temperature over the range of test temperature, the steady-state creep data roughly follow a creep equation of the type Temperature compensated creep rate = K* = A exp

Jan 1, 1960

By Ervin E. Underwood

IT has been recognized for many years that dis-persed particles have great value in raising the creep resistance of metallic alloys. In fact, some of the most successful high-temperature alloys owe their superiority to this factor above all others. A recent observation by Glen1," indicates that even better high-temperature resistance to deformation results in alloys capable of two successive precipitation reactions. The ramifications of this finding are of great interest. Unfortunately, our understanding of the reasons for such notable improvements has not kept pace with technical developments. In an effort to uncover some of the basic facts governing strengthening by particles, a program was initiated at the Battelle Memorial Institute with the primary goal of comparing creep strengths in single-phase and two-phase (precipitating) alloys. The effects of precipitation from solid solution on the creep properties of alloys are generally such that the resistance to creep is increased. However, if alloys are heat treated to different degrees of hardness before creep testing, it is often found that those possessing the maximum hardness initially do not necessarily have the maximum creep resistance. Depending on the stresses and temperatures involved other structures may prove more desirable. Considerations of the above nature indicate the importance of defining the initial state of the alloy. Here, it was decided to start with quenched single- phase alloys in which precipitation and creep deformation proceed concurrently. Equipment and Experimental Procedures Preparation of the Specimens—Four 25 lb ingots were prepared from 99.999 pct Cu and 99.996 pct Al to compositions of 1, 2, 3, and 4 wt pct Cu. Spec-trographic and chemical analyses are listed in Table I. After heat treatments and intermediate reductions, the alloys were cold rolled to 1/8 in. thick sheet. The final cold reductions amounted to 50, 40, 20, and 10 pct for the 1, 2, 3, and 4 pct Cu alloys, respectively. The specimens for creep testing were machined into tensile flats 7 in. long, 3/4 in. wide (at the shoulders), and 1/8 in. thick. The reduced sections were 1/4 in. wide and 21/2 in. long. After heat treatments at 540°C to an ASTM grain size of 1 1, the specimens were quenched into water at room temperature, then electropolished in a glacial acetic acid and perchloric acid solution. The gage marks were Knoop impressions placed 2 in. apart on the reduced sections. Blanks of 1 x 1 in, were cut from the same sheets for the age hardening runs and were given the same grain size heat treatments. The specimens and blanks were stored in a refrigerator at —40°C until needed for testing. Creep Measurements—Creep tests were conducted in a constant temperature room which was maintained at 26° ±1°C. A split-type, hinged, vertical-tube furnace was mounted on a horizontal track so that the specimen could be enclosed suddenly. Thus, it took about 15 min for the specimen to come within 5°C of the test temperature. The temperature variation along the specimen was controlled to about

Jan 1, 1958

By O. D. Sherby, J. E. Dorn, C. D. Wiseman

MCLEAN&apos; has shown that the total strain obtained during creep of aluminum polycrystals arises exclusively from the mechanisms of 1) microscopically observable slip, 2) subgrain tilting, and 3) grain boundary shearing. Extensive analyses, however, suggest that the high temperature creep of metal polycrystals is controlled by a single thermal activation process."" These somewhat contradictory observations might be reconciled if it could be shown that the activation energies are identical for each of the mechanisms isolated by McLean. Such identity of the activation energies, of course, would demand that the same unit process controls the functioning of each individual mechanism. Under these conditions the activation energies for creep of single metal crystals and polycrystalline aggregates and for grain boundary shearing should be identical. This paper is primarily concerned with the possible identity between the activation energies for high temperature creep of single crystal and polycrystalline metals. In addition, comparisons will also be made between the activation energies for creep of single crystals and polycrystals with previously reported activation energies for grain boundary shearing.0"8 Materials and Techniques The same high purity aluminum, lead, and tin were used in the creep tests for single crystals and polycrystalline aggregates. Single crystals of aluminum and tin were prepared by the strain-anneal technique, whereas lead single crystals were prepared by growth from the melt. The tensile creep stress was maintained constant by Chalmers-Andrade parabolic-type lever arms. Strains were measured to &0.0002 in. per in. with rack and pinion type extensometers, and temperatures were maintained to within & 0.2"C of the reported values by mercury-thermoregulated resistance-heated silicone oil baths. The previously reported unambiguous technique for determination of the activation energy for creep was employed throughout this investigation.&apos; ." It involves periodic abrupt small changes in temperature during the course of creep, accomplished by rapidly replacing one creep bath at temperature TI by a second bath at T,. The abrupt change in creep rate from i, to & attending the abrupt change in temperature is due exclusively to the change in temperature, since both the stress and the substructure are identical the instant before and the instant after a change of temperature. Therefore, all other factors being identical where AH is the activation energy for creep and R is the gas constant. Results Typical examples of the creep rate vs creep strain data during temperature cycled creep tests of single

Jan 1, 1958

By M. J. Sinnott, W. R. Kiessel

The creep characteristics of commercially pure titanium sheet in the annealed state, cold-worked state, and cold-worked and recovered state in the temperature range from 75&apos; to 750°F have been determined. Titanium has been found to exhibit strain aging characteristics. The effect of strain aging on creep has been determined. A possible explanation for the poor creep properties of titanium is proposed. THE metal titanium exhibits many desirable properties but results on its creep properties have been somewhat disappointing. The creep strength is low even though the material has a very high melting point.&apos; The present work was undertaken to determine the creep strength of titanium in various conditions; annealed, cold-worked, and cold-worked and recovered and to determine why titanium shows such relatively poor creep properties. The general procedure followed in this research consisted in obtaining the usual mechanical prop- erties such as creep strength, short time tensile strengths, and hardness on materials treated to a controlled degree of internal strain, as determined by X-ray diffraction measurements, and their subsequent interpretation in terms of this internal strain. The material used in this work was sheet stock taken from one heat of commercially pure titanium. As-received, this sheet was 0.060 in. thick. The analysis was given as 0.037 pet C, 0.023 pet Si, 0.50 pct W, 0.063 pct Ni, 0.08 pct Fe, and the remainder titanium. The oxygen and nitrogen were unreported but generally are about 0.2 pct in commercial heats. In order to put the material in a state of minimum internal strain all the sheet was given an anneal in a static argon atmosphere for 1 hr at 1600°F prior to processing and testing. The microstructure of the material after this treatment was essentially a single-phase solid solution of uniform equiaxed grains. For the studies on the cold-worked sheet, the material was reduced by rolling in a two high, 5 in. mill. Rolling was done at room temperature in passes

Jan 1, 1954