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By I. R. Kramer

I. R. Kramer (Martin Co.)—In a recent paper Nakada and Chalmers24 reported some observations of effects of surface conditions on the stress-strain curves of aluminum and gold single crystals. It is of interest to compare these observations with the results published previously in this journal and to comment on their general conclusions. In brief, Nakada and Chalmers concluded that the removal of the surface layer of a prestrained specimen lowered the stress-strain curve for aluminum but not that for gold. Further, they concluded that the surface work hardening of aluminum is confined to a depth not more than l0-3 cm. In our results25 published previously, it was pointed out that when prestrained specimens of aluminum and gold were polished to reduce the thickness upon reloading the initial flow stress decreased markedly. Further if a sufficient amount of metal was removed, the yield point failed to appear. With continued application of the load the stress-strain curve became coincident with that of the virgin crystal. We have found this behavior in some 100 determinations to hold consistently for gold, aluminum, and copper in both single and poly-crystalline specimens. The amount of strain required before the curves coincided depends upon the amount of metal removed but it is usually less than 0.01. This type of behavior is the same as that reported for metarecovery by other investigators.29 For aluminum specimens which have been prestrained and then heated to temperatures above 50°C we have consistently found that the stress-strain curve was typical of the orthorecovery28 type. In this case the stress-strain curve always lies below that of the virgin specimen. With respect to Ref. 24 the curves for aluminum are always below that of the virgin curves, while those for gold become coincident. This observation indicates at least for aluminum that the specimens must have been heated to a temperature high enough to cause recovery by an alteration of the internal dislocations. In addition, a recovery would be expected because of the removal of the surface work-hardened layer. Nakada27 had reported that, with his particular apparatus in which a perchloric acid polishing solution was used, the temperature of the specimen increased 65°C. The curves presented in Ref. 24 for gold do not permit one to detect the initial flow stress upon reloading after the surface-removal treatment. In fact, contrary to the method used by Nakada and Chalmers, the change in the stress-strain curve produced by a surface-removal treatment cannot be described in terms of a decrease in stress at strains much higher than that at the initial flow stress because of the coincidence of the curves at the higher strain values. With regard to the depth of the work-hardened surface layer, our data show for aluminum single crystals (7.5 by 0.3 by 0.3 cm) that the initial flow stress remained constant after 12 x 10-3 cm had been removed from the thickness. This depth was independent of the prior strain. For gold crystals this depth is somewhere between 10 x 10-3 and 20 x 10-3 cm. Y. Nakada (author's reply)— Kramer states,28 "for aluminum specimens which have been prestrained and then heated to temperatures above 50°C, we have consistently found that the stress-strain curve was typical of the orthorecovery28 type. In this case the stress-strain curve always lies below that of the virgin specimen." However, Cherian et a1.26 discovered that aluminum polycrystals annealed at 32" and 100°C showed the metarecovery behavior. They showed that the orthorecovery behavior did not appear until the crystals were annealed at 150°C. Kramer suggests28 that the drop in the flow stress of aluminum crystals after the surface removal by electropolishing24 may be due to the recovery caused by the temperature rise which may occur during the electropolishing.27 However, as indirectly stated in Ref. 24, the current density used in these electro -polishing experiments was 0.15 amp per sq cm. According to ref. 27, this current density should cause a temperature rise of only 40°C. This may cause the metarecovery but not the orthorecovery. Furthermore, as stated explicitly in Ref. 24, the surface removal was accomplished by chemical etching as well as by electropolishing. The results were the same for both electropolishing and etching. During the etching, the specimen temperature did not rise above 35°C. Some aluminum crystals were placed in water at 35° C for 30 min. These crystals did not show the decrease in flow stress. Therefore, it is quite clear that the flow-stress drop after the surface removal is not caused by a high-temperature recovery. However, as Kramer points out,28 it is quite possible that the internal dislocation structure may have been altered because of the removal of the highly work-hardened surface layer. However, how much this rearrangement contributes toward the flow-stress decrease is not known at present.

Jan 1, 1965

By R. J. Stokes

S. Floreen (international Nickel Co.)— One fairly simple way to differentiate between em brittle me nt due to surface microcracks or due to a dislocation barrier effect might be to load a brittle rock salt crystal in tension to some stress just below the fracture stress and then immerse the loaded crystal in water. If a surface film is retarding plastic flow then one should observe some plastic deformation of the rock salt as

Jan 1, 1962

By J. Richter, D. Schulze

J. Richter and D. Schulze (Deutschen Akademie der Wissenschafte zu Berlin)—Introduction. In a recent paper R. G. Garlick and H. B. Probst reported on experimental results of investigations of room-temperature slip in zone-melted tungsten single crystals.17 In the paper it was pointed out that slip lines could be detected with an optical microscope only after about 10 pet plastic strain of the crystal. In our investigations we could observe slip lines in tungsten single crystals of defined orientations already with an elongation of 0.02 to 0.03 pet.18"9 Experimental Technique and Results. The tungsten single crystals were produced from 4 to 5 mm sintered rods* as starting material by electron- beam zone melting. With single-zone-pass melting a speed of 0.5 mm per min was used, while three-pass melting could be handled at a speed of 3 mm per min. Crystal axis orientations were located in the shaded area of the stereographic triangle, see Fig. 6. Orientation 1 is located at about 18 deg and orientation 2 at about 5 deg on the great circle from [011] to [ill]. This corresponds approximately to the orientations P and M referred to by Garlick and Probst. Our single crystals had a length of about 70 mm and were profiled solely by electrolytic means, leaving grip ends at both ends of the crystals. Between the latter, a cylindrical crystal of 45 to 50 mm length and about 2.4 mm diam was obtained. The crystals were deformed at room temperature in a commercial tensile-testing machine to obtain a strain of 0.02 to 5 pet. The average strain rate e = eP/t for all tensile tests amounted to approximately 10 -6 to 10-5 per sec, with ep representing plastic strain and t the duration of applied stress. In Fig. 7 a crystal is shown elongated by 0.03 pet. The picture was obtained by means of an optical microscope. Figs. 8 and 9 give electron-microscopic pictures of slip lines of crystals elongated by 0.07 and 1.1 pet, respectively. For crystals with the orientation 1, see Fig. 6, only the two main slip systems (101)[111] and (110)[111] were found. With the crystals of group 2 the two main slip systems are again evident, with

Jan 1, 1965

By Elmars Ence, Harold Margolin

A. J. Goldak and J. Gordon Parr (University of Alberta) —While we appreciate the difficulties involved in any investigation of this system, and we wish to congratulate the authors on their comprehensive efforts, there are several aspects of their paper that are not clear to us. 1) If the 6 phase is, in fact, isomorphous with Ti3Sn, it should not be designated Ti,Al. An 4B structure cannot be isomorphous with an ordered structure of the DO type. Anderko et al.' suggested that the structure be called Ti3A1, and we believe this to be a more reasonable designation. The confusion is compounded when the authors designate the phase Ti3Al—yet the composition limits of this phase (according to their diagram) are approximately Ti,A1 and Ti,Al. Further, while Pietro-kowsky is said to have pointed out that the structure of the 6 phase is isomorphous with Ti3Sn, we understand that this was only a suggestion that was not confirmed. Margolin and Ence do not appear to have presented any evidence to support the suggested isomorphism. 2) In referring to the precipitation observed microscopically during the initial breakdown of high A1 a during quenching, the authors state that "such precipitation is not likely to be detected by Debye-Scherrer techniques". We suspect that if the precipitate was visible by optical microscopy, it must have at least one dimension of the order of 1 or greater, and would therefore be readily detected by diffraction techniques. 3) The authors state: "The basis for this suggestion (that 6 forms peritectically P + L—6) is the observation that the ,'3 + 6 and 6 phase fields were

Jan 1, 1962

By J. Suiter, H. F. Ryan

H. F. Ryan and J. Suiter (CSIRO)—In this paper the authors have presented "a physical model which has as its central hypothesis the solution strengthening of regions along grain boundaries in the order of tens of angstroms thick", and their calculations have used 40Å as the zhalf-width of this boundary region. Selection of this value by the authors suggests that they were unaware of a number of recent field-ion microscope observations of grain boundary structures (e.g., Refs. 29 and 30). The accompanying figure, Fig. 9, shows a portion of an ion micrograph of a tungsten specimen containing a grain boundary, and the regular arrangement of atoms in various crystal planes in each grain can be seen, except in the boundary zone which is not more than two atom diameters in width. Since it is expected that solute atoms will segregate only to the region where the lattice is disturbed, it would seem that a value of 4Å for the half-width of the boundary region would be more appropriate than the value of 40Å assumed by the authors. If the former value is used in Eq. [8] of their paper to obtain curves showing solute concentration in the grain boundary as a function of temperature, the resulting curves differ significantly from those obtained by the authors. Although there are only relatively slight changes in the regions corresponding to higher temperatures (i.e., grain boundary concentrations of approximately 1 at. pet), at lower temperatures the curves are no longer realistic. For example, the curve corresponding to u = 7000 cal per mole gives a solute grain boundary concentration in excess of 100 pet at a temperature of approximately 360°K, and "flattens out" at a grain boundary concentration of about 300 pet! Similar results are obtained with each of the other curves. Ion microscopy of dilute solid-solution alloys has shown that solute atoms give rise to image points which in most cases are of higher intensity than those of the solvent atoms.31 If the same behavior occurs when the solute atoms are present in much lower concentrations then ion microscopy should provide a sensitive tool for studying the segregation of impurities to the grain boundary regions. Although many grain boundaries in tungsten have been examined after different thermal and mechanical treatments, there has not been, as yet, any systematic study of such segregation. In general the micrographs show no clear indications of marked grain boundary segregation, but occasionally areas are found where the grain boundary contains an appreciable number of image points of high intensity in a very narrow zone, see Fig. 9. If it is assumed that these correspond to impurity atoms then it is possible to estimate the impurity concentration both in the grain boundary and within the body of the grains. Application of this method (to a larger area

Jan 1, 1965

By Joachim J. Hauser

William F. Hosford, Jr. (Massachusetts Institute of Technology)—Dr. Hauser has used a very interesting method to study the interaction of dislocations on different slip systems, but it should be pointed out that the analysis of the experiments is subject to a serious criticism. He states that "the effect of the compression can be adequately described by one slip system." The effect of frictional constraint during the compression makes this quite unlikely. When a block of metal is compressed its lateral expansion requires a sliding of the metal over the compression platens. The role of friction in the interface between the deforming metal and the platens is to increase the normal force required for the compression. Analyses1213 have shown that, in general, the additional force, p, required for the compression is a function of l/h where is the coefficient of friction, I is the length of the speci- men in contact with the platens. For a constant COefficient of friction, isho' shows that P should increase exponentially with pl/h for both plane strain and axially symmetric compression. For a compression specimen, Fig. 7, whose cross section perpendicular to the compression axis is a rectangle whith one dimension L, much larger than the other W, a much larger force would be required for appreciable flow parallel to L than for flow parallel to U7. Therefore lateral strain in the W direction, EW, should be much greater than the lateral strain in the L direction EL. Since L/H = 14.5 for Dr. Hauser's crystals, and since no lubrication was used, it seems questionable that appreciable lengthening of the crystals could occur. Because the theories of frictional constraint have been derived for isotropic polycrystalline materials, it was decided to make experimental measurements on a single crystal. A section 3.590 in. long was sawed from an aluminum single crystal with a square section of 0.249 in., so that L/W= 14.4. This crystal was tested in compression between dry ground steel platens. Fig. 8 shows the orientation of the crystal and the axis of compression. The face for compression was chosen so that the operation of the single-slip system which would be predicted in the absence of friction would lead to a larger strain in the length direction than in the width direction. The dimensional changes of the width and length as well as the height were measured frequently during the compression with micrometers. Width strains were calculated from the average of readings near each end and at the center. A plot of the length strain, EL, against the width strain E w is given in Fig. 9. The slope indicates that the EL amounted to only 2.5 pct of cw. Other compression tests on similar crystals with shorter lengths also showed severely limited elongation. Even for a crystal with L/W = A.0, EL was only about 26 pct of cw. Because of the frequent interruptions of the tests for dimensional measurements should have decreased the frictional constraint by allowing a reseating of the platens, even smaller elongations under continuous testing seem probable. These tests on long narrow crystals show that essentially plane strain conditions prevailed. We may assume that Dr. Hauser's crystals deformed similarly. That the compression can be described by the

Jan 1, 1962

By I. L. Dillamore

I. L. Dillamore (University of Birmingham)—The different textures developed in various fcc metals have long awaited satisfactory explanation and it has now become clear that these differences are related to parallel differences in the deformation characteristics of the metals. Liu is correct, therefore, in seeking to account for the observed textures in terms of the flow mechanisms but I believe, for the reasons outlined below, that the particular interpretation of flow mechanisms proposed by Liu is open to substantial objections. By considering the forty-eight possible designations of the twelve octahedral slip systems found in fcc metals as distinct and separate deformation modes, Liu has fallen into the error of assuming that only positive glide dislocations associated with each system are present. In fact both positive and negative dislocations will be present and the only difference between for instance the systems B4 and B4' (in Liu's notation) is that under a stress of given sign the direction of motion of a dislocation is reversed on changing from B4 to B4'. For both orientations positive and negative dislocations will be present. In considering possible dislocation interactions it is, therefore, inadmissible to differentiate between R4 and R4' as Liu does. Liu considers those dislocation interactions which give the biggest reduction in energy to be the most favorable and neglects, on the grounds that they will form strong barriers to slip, interactions between dislocations with perpendicular Burgers vectors. Setting aside interactions between positive and negative dislocations of the same slip system, which must occur regardless of the combination of slip systems chosen, the biggest reduction in energy occurs for the Lomer-Cottrell interaction and it is Lomer-Cottrell barriers which are thought to provide the stronger dislocation obstacles. On the other hand the intersection of dislocations with perpendicular Burgers vectors is thought to be a low-energy process which contributes only a fairly small temperature-dependent part of the total work hardening. On this basis it seems doubtful whether the reduction in energy through possible dislocation interactions provides a reasonable criterion for choosing the operative slip systems. From the point of view of texture development it is unsatisfactory to ignore the slip rotations leading to an end position and to neglect to consider the stability of the chosen end point. It is also unsatisfactory to treat the two stress axes as interchangeable since, if the stress system is idealized as biaxial, one stress is compressive and the other is tensile. For the same reason the rotations of the two stress axes are not made compatible simply by assuming that the same slip directions are responsible for the rotations of the two stress axes. It is, in short, essential to treat the two stress axes as acting together on the same slip systems. Turning to the question of the difference between the copper-type and the brass-type texture, there now remains little doubt that the difference is attributable to differences in stacking-fault energy (y), as noted by Liu, but it is doubtful whether the temperature dependence of the texture in copper and in silver is due to increasing stacking-fault energy with increasing temperature. The results of Swann and Nutting42 cited by Liu were obtained in Cu-A1 alloys and the apparent increase in stacking-fault energy on raising the temperature may be influenced by short-range ordering. In pure metals such effects are absent and the only data available on the variation of y with temperature are those of Buhler et a1.43 for silver. They report a minimum at 200°C which does not fit the hypothesis put forward by Liu. It is much more likely that thermal activation of cross slip is important in determining which texture develops, as proposed by Dillamore and tors. These workers have proposed an explanation for the differences in observed texture among the fcc metals and the pole figures predicted consist of an orientation spread which is in better agreement with observation than the limited number of discrete orientations suggested by Liu. The theory of Dillamore and Roberts is also able to account for the differences between aluminum and copper which Liu still leaves unexplained. Y. C. Liu (author's veply)—The writer appreciates the interest of Dr. Dillamore, but must discuss some of his comments in order to avoid cross purposes. The phrase, "forty-eight slip systems," which appeared twice in the text—in the caption of Fig. 1 and the first paragraph in the Discussion—might unfortunately have led Dr. Dillamore to disagree

Jan 1, 1965

By I. R. Kramer

A delay time for yielding in cold-worked face-centered-cubic metals was found. Slip on (123) planes was observed. Glide on these planes occurred during the delay-time period before slip starts on the (111) planes. AN important approach to the study of the anchoring and blocking of dislocations is available through the delayed-yield phenomenon which has been observed in body-centered and hexagonal close-packed metal by several investigators. Clark and his associate1-5 showed that a delay time for yielding is present in mild steels and fine-grain molybdenum. Type 302 stainless, SAE 4130 normalized, SAE 4130 quenched and tempered, and 24s-T aluminum aid not have a delay time. Kramer and Maddin6 studied the delay-yield effect. in metal single crystals. While they found a delay time in body-centered-cubic metals none could be found in the face-centered-cubic metals. Later7 a delay time was found in hexagonal close-packed metals. cottrell8 has proposed an explanation for the difference in the yield phenomena of b.c.c. and f.c.c. metals based upon the anchoring of edge dislocations by the proper types of impurity atoms (C and N). In the body-centered-cubic lattice the interstitial atoms are near a cube edge and can interact with an edge dislocation, while in a face-centered-cubic lattice the distortion around an interstitial atom is of spherical symmetry and cannot anchor a screw dislocation which has practically no hydrostatic component. Cottrell's theory seems to account rather well for the behavior of body-centered-cubic . metals. EXPERIMENTAL PROCEDURE The apparatus used in these experiments is essentially of the same design as described previously.' Single crystals 1 in. long and having a diameter of % in. were placed in a pendulum which consisted of a bar 8 ft long designed with a crystal holder to accommodate the specimen at low temperatures. This portion of the apparatus was supported on fine molybdenum wires. A bar of the same diameter and length comprised the other portion of the apparatus. This bar was supported on a set of roller bearings arranged around the periphery of the bar to allow accurate alignment. This bar was propelled by means of a spring-loaded gun and allowed to strike the lead bar in front of the single-crystal specimen. SR-4 type A-8 resistance strain gages were cemented to the specimen and the strain measurements were obtained by amplifying the strain-gage output by means of a high-gain preamplifier. A tektronix 545 oscilloscope was used together with a polaroid camera to record the strain and time sweep. An Ellis Associate Bridge was used to calibrate the strain gages and calibration readings were obtained before each test. The sweep of the time signal was initiated by means of a miniature thyraton which was fired when the two bars came into contact. The single-crystal specimens were cut from single-crystal bars about 12 in. long, grown by a modified Bridgman technique. The aluminum crystals were made with material of 99.99 pct purity while the purity of the copper was 99.999 pct. A cut-off wheel was used to prepare the specimens which were then machined to the desired length. The two opposite faces of the specimen were parallel to each other and perpendicular to the axis of the specimen. The specimens were compressed 1 pct. No machining followed thereafter. In some cases prestraining was carried out in liquid nitrogen by impacting the specimens directly in the apparatus so that subsequent observations could be made without allowing the specimen to warm up to room temperature. The single crystals were compressed 1 pct at room temperature in a hand press without much control of the rate of deformation. In some cases specimens were recompressed to obtain the desired length change. As far as could be determined in these experiments this factor did not seem to influence the results. The SR-4 strain gages were glued with a cellulose type cement onto the specimen surface and baked at 45°C for 12 hr. As a check on the baking treatment gages were allowed to dry at room temperature. All delay time tests in this paper were conducted in a liquid nitrogen bath at -195°C. A schematic delay time oscilloscope trace is shown in Fig. 1. At point B the elastic stress wave caused by the impact reaches the strain gage on the specimen. The portion BC is the elastic strain. In this investigation the strain at point C was used to calculate the critical resolved shear stress by multiplying by the proper modulus depending upon the orientation of the single-crystal specimen. The time between C and D is the delay time portion of the curve. This portion of the curve is fairly flat but does have a definite microstrain associated with it. After the point D is reached the specimen deforms rapidly and the strain reaches a maximum at E. Following this, depending upon the length of the bar behind the specimen, the strain remains constant for a period and then decreases when the reflected elastic wave returns from the end of the pendulum bar. A permanent plastic strain is recorded on the oscilloscope trace and also measured by a strain-measuring bridge. The strain, E p,

Jan 1, 1960

By J. Weertman

It is shown that conditions suitable for the conversion of straight dislocations into helices are common in crystals hardened either through long-range dislocation interaction or by jog formation on dislocation lines. For dislocations other than screw dislocations or dislocations nearly screw in orientation, helices can be formed with the aid of core difhsion at temperatures low relative to the melting point of the material. It is assumed that, once formed, helices will degenerate into dislocation tangles. THE dislocation tangle is one major dislocation arrangement observed by the transmission electron microscope which had not been predicted previously from dislocation theory. Since first being observed, the tangle itself has become important in applied dislocation theory. The Cambridge school (P. Hirsch) bases part of its theory of work hardening upon this phenomenon.' In spite of the fact that the tangle obviously is a structure of prime importance to a cold-worked crystal, until recently relatively little attention has been paid to the question of exactly why or how tangles arise. It was generally assumed at first that cross slip and perhaps jog formation will lead to tangles. However Wilsdorf and schmitz2 concluded that cross slip cannot markedly contribute to the tangles. The Wilsdorfs and Maddin3'* have proposed that tangles arise by means of prismatic dislocation loops and superjogs which are produced by a precipitation of point defects. Dislocations with superjogs or which have joined with prismatic loops are themselves dislocation sources and they can produce new dislocations, a process they call "mushrooming", which then tangle with each other. There is no question that the Wilsdorfs et al. mechanism as well as the cross slip one can pro- duce tangles. However these may not be the only paths leading to tangle formation. In this paper we wish to consider another way tangles can form. Our work will be based on the theory of dislocation screw We wish to show that whenever a crystal is cold-worked there always is present a "driving force" leading to helix formation and thus to tangle formation. We do not expect to observe well-developed, regular helices in cold-worked metals. Rather we would expect that after a helix is formed random interactions with nearby dislocations will cause a well-developed helical dislocation to go over into an irregular form. A dislocation tangle is, of course, a grouping of dislocations with irregular forms. Therefore we feel that, in accounting for the formation of dislocation tangles, it is sufficient to show that many dislocations in a cold-worked crystal will take on helical form. The crucial step is helix formation. In order to have a straight dislocation assume a helical form, diffusion of vacancies, or interstitials, must occur. Our discussion of tangle formation therefore will be limited to crystals which have been deformed at temperatures ranging from about one fifth to half their absolute melting point. In this tem per a ture range appreciable core diffusion is possible. (There is no problem in explaining tangle formation at temperatures greater than half the melting point. At such temperatures dislocation climb through a bulk diffusion of point defects gives an extra degree of freedom to dislocation motion. This extra freedom of motion makes tangle formation easy.) At temperatures much below one fifth the absolute melting temperature diffusion processes are sufficiently slow that helix formation does not occur. Of course helix or tangle formation could occur in material deformed at very low tempera-tures which was subsequently warmed in order to make the thin specimen necessary for electron-microscope examination. Since within the temperature range of approximately one fifth to half the melting temperature the diffusion of point defects in the core of the dislocation is rapid, we can reasonably assume that within

Jan 1, 1963

By J. D. Meakin, H. G. F. Wilsdorf

Using a combined decoration and etching technique the dislocation structure of annealed and deformed a brass has been studied. Annealed crystals revealed a low density forest and well-developed subboundaries; lightly deformed crystals contained discrete groups of dislocations. The dislocation density and the number of dislocations in a group were obtained from the micrographs. Using slip-line data, the mean path of a dislocation and the configuration of groups along an active slip plane have been deduced. Observations on secondary and cross-slip are reported. It has been the aim of many investigations to obtain detailed knowledge of the dislocation patterns which are present in metals before and after their deformation. The "decoration" of dislocations with impurity atoms has been considered as one of the promising experimental approaches, and much work has been done to develop this technique for revealing dislocation sites in metals. Following the early work by Castaing,' Castaing and Guinier,' and Lacombe and Berghezan~ on aluminum-rich aluminum-copper alloys, dislocations in this material have been studied extensively by others.+' In these alloys the dislocation sites act as nuclei for the precipitation of the second phase. The main results of the investigations on aluminum with copper are: i) the confirmation of the earlier contention that subboundaries consist of dislocation walls, ii) that many more dislocations are found in slip bands than in regions where less glide had taken place, iii) the observation of individual dislocations, lying nearly parallel to the surface investigated, and iv) that parts of dislocation loops, apparently emitted from a dislocation source, could be made visible. Recently, Jacquet, Weill, and Calvert have succeeded in revealing nearly concentric dislocation loops in quenched A1-4 pct Cu and thus indicated directly the existence of dislocation sources in a fcc metal specimen of normal dimensions. Another decoration method developed by Dash10'11 and applied to silicon crystals makes use of diffusing copper to the dislocations from a surface deposition. The dislocation pattern can then be observed by an infrared technique. His results include evidence for symmetrical and spiral Frank-Read sources, and for arrays of dislocation loops which follow simple crys-tallographic directions. Recently Low and Guard" have studied the dislocation structure of silicon-iron using carbon for the

Jan 1, 1961

By K. R. Janowski, H. Conrad

As part of a program to establish the effect of crystal imperfections on laser output, a detailed study was made of the dislocation structure of ruby crystals obtained from varioius sources. Using KHSO4 as an etchant, a detailed mapping of the dislocation structure on the (0001) and the (1150) planes was carried out. A less extensive study was made of the rhombohedral planes. The average dislocation density on the basal plane was 1.5 to 3 x 106 cm&apos;2 and on the (1120) planes -5 x 10&apos; cm-2. Howe7!er, considerable variation existed between areas on a given plane. The subboundaries in the basal plane tended to lie along [1100] type directions while those on the (1120) plane tended to lie: a) parallel to the basal plane, b) along truces of the (1101) plane, and c) along normals to the traces of the (0001) planes. The orientations suggest that mang of the dislocations lie on the (0001), (1701), and (1150) planes A Laue back-rellection nnalysis Of c-axis wander in one crystal revealed a gradual increase in misorientation from me end of the crystal to the other, with a maximum variation of 1°35&apos;. Slight etching of a mechanically polished crystal revealed mumerous polishing scratches, suggesting the existence of a plastic flow layer. It is recognized that chromium concentration, lineage, and other crystalline imperfections play a role in the efficiency of ruby lasers.&apos; Consequently, it is desirable to establish in detail the imperfection structure of ruby crystals to be used as lasers. Some exploratory work along this line had already been done by Barnes&apos; and Dils and Martin.&apos;" How- referred to as the morphological system, as described by Kronberg.4 The Miller indices given in the present paper will be based on this morphological system. In this system, the three common growth planes are the (0001), the {1120}, and the {1101}.5 Since these planes are of high stability, it is expected that they are most suitable for study by the etch-pit technique. In the present investigation, a detailed mapping of the dislocation structure was carried out for the (0001) and the (1130) planes. A less extensive study was made of the etch-pit structure on rhombohedra1 planes. An analysis of dislocations in sapphire (the ruby host) was first made by kronberg,4 who postulated that slip on the (0001) plane occurred by motion of dislocations with Burgers vector 1/3 <1150> and that these dislocations might dissociate into quarter partials. An etch-pit technique using boiling phosphoric acid was developed by Scheuplein and Gibbs6, 7 for identifying dislocations intersecting the (0001) planes and the planes near (2021) in sapphire. Al-ford and Stephens8 were able to reveal dislocations on the (0001) and {1120} planes in sapphire and ruby by etching in fused potassium bisulfate (KHS04) at 675°C. The termini of basal dislocations [(000l), <1120>] were revealed by Palmour and Kriegel9 on {1120} and {1010} by thermally etching sapphire. Bond and Harvey10 were able to decorate dislocations in sapphire by adding 1 pet by weight of ZrO2 to the Al2O3 powder used in the growth of the crystals by the Verneuil technique and then heating the grown crystals for 4 hr at 1500°C. They found, using optical transmission microscopy, that many dislocations had straight segments which were parallel to one of the six [1120] directions in the basal plane. Single dislocation lines curved smoothly from one alignment to the other, turning through angles of 60 to 120 deg. Also observed were isolated hexagonal loops, approximately 10 µ in diameter, the sides of which lay along the same directions as did the longer dislocations. MATERIAL AND ETCHING PROCEDURE The ruby specimens used in this study (all containing approximately 0.04 pet Cr) had been obtained from four different sources: Linde Co., Meller Co., Valpey Crystal Corp., and those grown at Aerospace Corp.* For the initial phase of this study, several specimens were cut from the slab shown schematically in Fig. 1 which had previously been cut from a disk boule obtained from the Linde

Jan 1, 1964

By Nicholas J. Grant, Oliver Preston

PUBLICATION of data by Irmann&apos; indicating outstanding thermal stability and elevated-temperature strength properties in a sintered aluminum powder product (SAP) stimulated interest in the strengthening of metals by means of a highly dispersed oxide phase. This material was produced by compacting, sintering and extruding a fine flake aluminum powder, resulting in a dense product containing 10 to 16 volume pct alumina, which arises from the thin oxide film on the starting powder, highly dispersed in a matrix of pure aluminum. The method of producing SAP, and the stable high-temperature properties obtained from it, introduced the possibility of developing superior materials for high-temperature service by powder metallurgy methods. The composition of the materials of this type which are presently under consideration is predominantly metallic, containing from less than 1 pct up to about 20 volume pct of the oxide. As a result, other properties of these materials, such as electrical and thermal conductivity, thermal shock resistance, and to a certain extent ductility, notch sensitivity, machinability and hot working properties, are also predominantly metallic. These alloys do not constitute, therefore, a completely new class of materials as do the cermets, but rather present a new means of modifying the properties of a metallic matrix. In this sense, SAP type alloys are more closely analogous to the alloy aging systems. While the strength properties realized in the oxide-pure metal systems at the lower temperatures are substantially less than the best attainable in the aging systems, the thermal instabilities in the latter make them of less value for use at temperature much above their optimum aging temperatures, as indicated in Fig. 1. While the means of obtaining an oxide dispersion are more difficult and costly than conventional aging processes, in the light of the as yet limited understanding of such systems there is considerable promise of improved high temperature properties arising from the thermal stability of these structures. Since the development of SAP in 1946, its properties and the properties of a series of similarAl,O,-A1 products containing from about 1 to 20 pct aluminum oxide have been fairly extensively studied and reported.&apos;- "articular attention has been given to

Jan 1, 1958

By Nicholas J. Grant, Oliver Preston

A series of dilute solid solutions of a1uminum and silicon in copper, in powder -form, were internally oxidized, compacted, and extruded, to produce Cu-A12O3 and Cu-SiO2 alloys with 0.1 to 12 vol pct of oxide. Room-temperature tensile tests, creep-rupture tests from 450oto 850°C. conductivity measurements, and recrys-tallzzation studies were made. Oxide particle size and interparticle spacings were determined in an effort to relate the structure to measured strength values by means of known dispersion strengthening theories. A new dispersion strengthening theory, based on the effect of the dispersed phase on the retention of strain energy from the deformation step, zs proposed for this type of alloy, THE study of dispersion strengthening is of partitular interest in high-temperature materials technology in view of the excellent creep-rupture Properties and thermal stability achieved with SAP.1-5 Considerable effort has been devoted to this study in recent years, and encouraging results have been obtained in a number of systems.6 In general, the most

Jan 1, 1962

By W. A. Backofen, G. Y. Chin, W. F. Hosford

The ductile fracturing process was studied in single-crystal and poly cvystalline aluminum deformed in tension over a temperature range from 295° to 4.2°K. At temperatures as low as 77°K, the fracture of "inclusion-free" material, including zone-refined aluminum, was by rupture (-100 pct RA). At 4.2 OK, fracture was brought on by adia-batic shear. Metallographic examination did not disclose any voids or slip-band microcracks, thus negating for inherently ductile metals any mechanism of void nucleation by vacancy condensation or of cracking due to dislocation pile-ups. In Izigh-purity aluminum not treated to be inclusion-free, fracture at temperatures as low as 45°K was of the double-cup type and a result of void formation. The reduction-of-area decreased as temperature was lowered, corresponding to the earlier appearance of voids. Such behavior was rationalized in terms of a larger increase, with decreasing temperature, in the .flow stress relative to the strength of the inclusion-matrix interface. Evidence for low-temperature adiabatic shear was found in discontinuous flow at 4.2"K, in the transition to a localized shear fracture at low temperatures, and in the suppression of shear fracture with an elastically hard pulling device. A simple analysis for the initiation of adiabatic shew permitted a general correlation of the various contributing factors. It has been pointed out that the duration of shear depends upon effective mass and elastic stiffness of the deformation system. IT has long been recognized that fracture* may Throughout this paper, the term "fracture" is taken to mean any process that results in the separation of a material into two (or more) parts. Thus rupture as it may be encountered in a tension test leading to 100 pct reduction-of-area is included in this category. occur in a ductile mode, and that the process can be of great practical as well as general interest. Much information about ductile fracture has also been accumulated over this period, but only recently has an understanding of mechanism begun to appear. Ludwik,&apos; in 1926, first reported fracture in a tensile specimen starting with a central crack in the necked section. Since then, other studies have disclosed that such cracks may form by the coalescence of voids nucleated in this region where hydrostatic tension is highest.2-4 Rogers and Crussard et al.&apos; have emphasized void formation and reori-entation along localized shear bands as a mode of crack propagation. pines6 has considered the tensile rod as a bundle of fibers joined by weak interfaces, which subsequently separate to allow individual fiber contraction. The notion of cavity growth and coalescence by purely plastic processes was discussed by Cottrell: who added that the tensile reduction-of-area ought not to be sensitive to temperature. On the other hand, it has been observed that the reduction-of-area is greatly increased if tests are carried out at high temperaturesa or under high hydrostatic pressure.&apos; Fracturing anisotropy in wrought products lends support to the idea of void formation from preexisting flaws strongly aligned by earlier processing.&apos;&apos;-l2 There is evidence that many voids result from the fracturing of inclusions or separation at the inclusion-matrix interface Another possibility is that voids grow out of pore volume produced in the initial solidification and never fully removed in later working. In general, a structure 3f particles, pores, and weak interfaces can be expected, at least in materials of engineering interest. Vacancy condensation has been suggested as an alternative mechanism of void formation for materials considered to be inclusion-free.13 Yet experience has shown that tensile reduction-of-area increases with purity, to the extreme of rupture as so often observed in single crystals. Adiabatic shear has an important bearing on ductile fracture. It occurs when the decrease of flow stress, as a result of local temperature rise from heat generated during straining, becomes larger than the increase due to strain and strain-rate hardening. As demonstrated by experiments on punching of plates,14 a large temperature rise may be brought about by rapid straining. Adiabatic flow as a result of the high strain rate reached in an ordinary tensile specimen just prior to separation may account for the cone formation in cup-and-cone fracture;14 evidence of such local heating has been presented.15 For geometrical reasons, however, pure sliding along the conical surfaces is unlikely, and separation under tensile forces is probably an important accompanying feature of the shear.7 In deformation processing operations, a high shear-strain rate may exist at boundaries between plas-

Jan 1, 1964

By J. Greenspan

The anisotropy of fracture and slip, that is, the brittleness and ductility of the beryllium single crystal, is characteristic also of po1ycrystalline beryllium in which the grains are oriented in a preferred manner. Beryllium with grain orientations resulting from hot working either unidirectionally or bidirectionally is ductile or brittle in directions given by the anisotropy and orientation of the grains. Textures developed from various hot-working sequences are given, and tensile results are correlated with textures. Not only texture, but fine grain size is necessary for obtaining high tensile elongation. Ultimate tensile strength and elongation are both correlated with grain diameter. Of particular interest is the case in which unusually high tensile elongations of 30 to 40 pct are obtained when basal planes are oriented to carry THE beryllium crystal (of nominal purity) is probably unique among metals with respect to its unusually acute anisotropy of slip and fracture. While extensive slip can occur on the system (1010) [ll20] starting at about 19,000 psi, the (0001) plane is particularly vulnerable to fracture at 4500 psi or less. Fracture occurs also on the (11zo) plane at about 26,000 psi.1"3 Further, there seems to be no other slip System which contributes significantly to

Jan 1, 1960

By Erhard Hornbogen

Twins were propagated into large, well-annealed crystals of a, iron-phosphorous and a, iron-molybdenum solid solutions. Strain fields caused by interaction of these twins were made visible by precipitation. These strain fields can be explained by assuming that transmitted and reflected plastic waves are created when a twin strikes an obstacle with high velocity. The twin front itself can be regarded as a shear wave that may be able to develop a one-dimensional shock front. The occurrence of {WO} fracture by the reflected stress is also discussed. The described effects were not found when twins propagated at lout velocity into disturbed crystals, for example, into crystals previously deformed by slip. DEFORMATION twinning leads to shearing of a crystal lattice under external load. The shear appears to be homogeneous over a large number of crystal layers. In a iron, shear occurs on the (112) planes and in the <1ll> directions. The formation of a twin proceeds by the movement of partial dislocations that change the stacking at the twinning plane.l, In the bcc lattice, this partial dislocation can be created by dissociation of a sessile a/2[111] dislocation that lies in the (112) plane: Cottrell and Bilby&apos;s spiral mechanism can explain the homogeneous shear, but has not been proven experimentally. Nevertheless, this mechanism can explain the possible high velocity of formation of a twin. In Cottrell and Bilby&apos;s model, as in other models of twinning or phase transformation, a much higher energy is required to spread the first stacking fault than to add new layers by further movement of the partial dislocations. The dislocations will therefore become accelerated proportional to the difference between the stress, tN, to nucleate and tp to propagate the twin. It has been assumed3,4 that tn is the stress required to make two partial dislocations of apposite sign pass for the first time. After the first layer of new stacking has been formed, the maximum stress is TN=Gb/4pd where G is the shear modulus, b is the Burgers vector of the partial dislocation, and d is their perpendicular spacing so that the amount of shear is S = b/d. From this formula, a value of 25 kg per mm2 has been estimated for twinning in Zn3. The measured values are smaller, but local internal stresses may help to provide the necessary stress. For a iron, a higher value can be expected, mainly due to the higher value of G. That agrees with the observation that "burst" twinning occurs if the yield strength is in-

Jan 1, 1962

By N. K. Chen, R. B. Pond

IN the study of slip band* formation, there have been many examples to show that they do not always appear as lines traversing the entire crystal, but as segments whose ends seem to vanish in their path through the crystal. This characteristic appearance of slip bands has been witnessed under the optical microscope at various magnifications&apos;-&apos; and also under the electron microscope.&apos; A typical example of this behavior seen with the optical microscope is shown in Fig. 1. However, the slip band studies were generally conducted on polished surfaces of single or poly-crystalline metals which had been previously deformed; i.e., the load was generally released so that the observation could be made. Any picture of slip bands so obtained can represent the surface phenomenon only in a static state of the strained material. The conditions prior to their formation cannot be definitely and clearly assigned. Thus, while a segmented slip band may suggest that slip is a growth process as supposed by the theory of the nucleation of slip,V he usual appearance of suddenly and fully developed slip bands around the crystal has generally been considered as a consequence of uniform shear of the entire slip plane akin to a cataclysmic process. Little clear-cut information is available with regard to the speed at which a slip band forms, its direction of motion, the geometry of its position with regard to its neighbors, and its dependence on orientation. A description is given in this paper of experimental apparatus by which the progressive formation of slip bands can be recorded while the specimen is undergoing deformation. Qualitative and quantitative data on the dynamic formation of slip bands will be presented with special interest concerning the propagation of slip bands, the spacing of slip bands, and their relations to strain hardening. Views on the formation of slip bands are discussed and a mechanism of the unit process involved in the formation of a slip band is proposed. Preparation of Specimens Single-crystal specimens of high purity aluminum (99.997 pct), 1/8 in. square in cross-section and 1% in. long in gage length, were made by the method of gradual solidification from the liquid state. Since no machining work could be introduced in preparation of crystals of such small size, a special mold was designed for casting them to final shape. The mold consisted of two, separate, high purity graphite blocks. Generally, 20 molds were packed together in one container so that 20 specimens could be obtained by one casting operation. This was desirable since it was possible by this method to obtain groups of crystals with similar orientations. The as-cast crystals were carefully clipped from the gate, etched, and homogenized for 24 hr at 600°C. They were then very gently polished using a 4/0 paper, re-etched, and finally electrolytically polished after the method previously described by Chen and Mathewson.6 The crystallographic orientations were determined using a back-reflection, Laue method. Tensile Testing and Photographic Method The tensile testing equipment for these tests was composed of a specially designed microtensile machine, microload cell and microclip gage with necessary appurtenances. The members of the microtensile machine consisted of three parts, as shown in Fig. 2. The chassis is equipped with an oil cylinder, A, and piston, the piston being part of the movable cross-head, B. Pressure in the oil cylinder is controlled and regulated by an external pneumatic-hydraulic cell, C, which is connected to the cylinder by a Vs in. high pressure copper tube. This cell is half filled with hydraulic oil and has a needle valve, D, on the oil exit side as well as a needle valve, E, on the gas inlet side. A quick-acting valve, F, as well as a pressure gage is provided for the gas side. The oil exits into the load piston on the microtensile machine. By connecting a tank of inert gas to the gas inlet, regulated pressures were provided over the oil so that the oil would leave the cell at a rate determined by the setting of the exit needle valve, the gas pressure, and the pressure of the oil in the load piston of the microtensile machine. With this pneumatic-hydraulic appurtenance it was possible to

Jan 1, 1953

By R. L. Fleischer, W. F. Hosford

Tensile data for coarse grained aluminum Polycrystals suggest that the "grain size" effect is not due to dislocations piled up at grain boundaries but rather is primarily a relative size effect due to surface crystals being weaker and less confined. STUDIES directed at interpreting hardening of poly-crystalline metals normally identify their strain hardening properties with those in some particular type of single crystal.1"4 The recent recognition in face centered-cubic metals of a nearly linear stage with rapid hardening occuring at comparable rates for both polycrystals and single crystals, suggested that the same process or processes determine both cases and hence that there exists some justification for the use of single crystals to understand polycrystals. Further evidence for the above view may be found by an approach initiated by Chalmers:5 By using bicrystals of controlled orientation it is possible to begin to assemble a polycrystal and also to study grain boundary effects in detail. In this way it has been found that a single grain boundary affects easy glide but not the subsequent stage II hardening.6 This result suggests that a sensitive way to observe grain boundary effects in polycrystals would be to vary grain size and measure easy glide. As will be seen, easy glide is only possible for coarse-grained samples, and hence the results will serve to fill in the gap in measurements between single crystals and bicrystals on one hand and fine-grained polycrystals on the other. One problem inherent in comparing single crystals with polycrystals is the uncertainty as to what slip systems are acting in a polycrystal. To compare the two types of samples, rates of shear hardeninn---L. on the acting -planes are needed. and these may be computed only if it is known what particular systems are active. The acting systems were examined for a coarse-grained polycrystal and it will be shown that the systems supplying the preponderance of slip can be determined with little ambiguity. EXPERIMENTAL PROCEDURE Twelve samples of aluminum were prepared by chill casting into a heated graphite mold, followed by annealing at 635° ± 5°C for 24 hr with an 8-hr fur- nace cool, and finally either etching7 or electropol-ishing.&apos; The samples, with a 7 to 10 cm length between grips and 4.4 by 6.6 mm in cross section, were deformed at a strain rate of about 3 10 -3 . per min in a tensile device which has been described elsewhere.5 The composition was reported by Alcoa as 99.992 pct Al, 0.004 pct Zn, 0.002 pct Cu, 0.001 pct Fe, and 0.001 pct Si; nine samples were deformed while immersed in liquid helium and three in air at room temperature. The stress-strain curve for one of the samples (P-1) deformed at 4.2 "K has been reported previ~usl~.~ This sample was selected for determination of active slip systems. Eighteen of the crystals were examined by optical microscopy to determine the angles of slip line traces and by X-ray back reflection to determine orientation. By this means the slip planes were determined and the resolved shear stress factors for possible slip systems could be computed. Finally each sample was sectioned so that after etching, the number of crystals could be counted for each of ten newly exposed surfaces. The average of these ten values will be termed n, the number of crystals per cross section. Values of 11, varied from 1.9 (nearly bamboo structure) to 12.7. Sketches of typical cross sections appear in Fig. 1. RESULTS AND DISCUSSION: SLIP SYSTEMS 1) Determination of Acting Slip Planes—The stress axis orientation and operative slip planes in eighteen crystals of sample P-1, as determined by slip line traces and crystal orientation, are summarized in Fig. 2. For one of the crystals two planes had a common trace. so that the traces alone did not distinguish which plane or planes were slipping. However it was found that the stress resolving factor for the primary system was 0.386, .while that for the most stressed system in the other plane (indicated bv the dotted arrow) is 0.138. It will be assumed tgerefore that only the primary plane acted. Since the orientations were determined after extending the samples 4 pct, the stress axes may be rotated from their original value by as much as 2 deg in some cases. It is interesting to note that in five crystals only one slip plane acted, in eight two acted, and in five three planes were observed—an average of two slip

Jan 1, 1962

By M. J. Marcinkowski, A. Szirmae, R. M. Fisher

Room -temperature hardness measurements obtained from single and polycrystalline samples of a 47.8 at, pet Cr-Fe alloy which were aged for various times al 500°C show a two-fold increase over that of the unaged alloy after annealing for 1000 hr. A detailed examination of the deformation markings in the neighborhood of the hardness imbressions reveals that twinning becomes an increasingly more important mode of deformation as aging proceeds. this observation is shown to be inconsistent with the Proposals that the transformation is eve of order-disorder On the other hand, the results are in agreement with previous observations of Fisher et al. of a coherent chromium-rich precipitate which forms in an iron-rich matrix as a result of a miscibility gap in this alloy system as proposed by Williams . Using the coherent precipitate hypotlzesis as a model, a detailed analysis of the various possible strengthening contributions to both the slip mid twinning stresses is made. In the case of&apos; slip, lattice friction within the chromium-rich phase and the chemical energy associated with the interface between the two phases contribute about 60pet to the total strength. The contributions from coherency strains and modulus differences are thought to contribute the remaining 40 pet of the strength but are difficult to evaluate because of uncertainties regarding the flexibility of the dislocation line. All of the factors have nearly the same or else a smaller effect on the twinning stress in the aged alloy. Twinning is never observed in the unaged alloy because the twinning stress is much higher- than that for slip. With increased aging times, the various contributions to the total stress for both twinning and slip increase, but most of those for slip increase much more rapidly, so that, in the fully aged alloy, it surpasses the stress for twin propagation. When a twin is nucleated by the chance occurrence of an internal stress concentration during a test, the subsequent twin burst results in a low hardness reading. FeRNTIC Fe-Cr alloys from about 15 to 80 at. pet Cr content show considerable change in properties such as hardness, electrical resistivity, saturation magnetization, and so forth, after aging in the vicinity of 500°C.* The most marked change is a large increase in hardness accompanied by a sharp decrease in ductility, so the phenomenon has often been referred to as the 475°C (885°F) em-brittlement problem. Changes in microstructure are rather subtle and most investigators have not been able to observe any X-ray diffraction or metal-lographic changes during aging. There is little doubt that the phenomenon is inherent to the Fe-Cr binary system and is not directly related to the formation of a phase. Two distinct schools of thought have developed during the past decade concerning this problem. Masumoto, Saito, and sugiharal have concluded, from their own specific-heat measurements, that atomic ordering occurs in this temperature range. Pomey and Bastien2 have also attributed the changes in physical properties with aging in the neighborhood of 500°C to atomic ordering. In addition, Takeda and Nagai3 claimed to have found X-ray verification for superlattices corresponding to the compositions FesCr, FeCr, and FeCr3. However, all known attempts to observe superlattices in Fe-Cr alloys using neutron diffraction, which should be much more sensitive, have been unsuccessful. These have been reported by Shull et al.4 for 25 at. pet Cr, williams5 for 75 at. pet Cr, and Tisinai and samans6 for a 28.5 at. pet Cr. steel. The second and more prevalent opinion ascribes the 475°C embrittlement phenomenon to the formation of a coherent precipitate due to the occurrence of a miscibility gap in the Fe-Cr system below about 550°C. This latter concept was first indicated by the results of Fisher, Dulis, and Carroll,7 who were able to extract fine particles about 200Å in diameter from samples of 28.5 at. pet Cr steels aged from 1 to 3 years at 475°C. The extracted material was found to be nonmagnetic, to have a bee structure with a lattice parameter between that of iron and chromium, and to contain about 80 at. pet Cr. Williams and paxton8 and williams5 confirmed these results and first explicitly proposed the existence of a miscibility gap below the a region in the equilibrium diagram. Alloys aged within this gap

Jan 1, 1964

By H. T. Green, R. M. Brick

True stress-strain data on alloys of pure iron with up to 2.4 pct Al were obtained in the temperature range +100° to —185°C. Alumi-num was found to reduce yield and flow stresses of iron at low temperatures but to have little or no effect on ductility. The effects of temperature and composition on strain hardening are discussed. SEVERAL independent studies of the behavior of high purity iron binary alloys at low temperatures are now in progress in attempts to evaluate systematically the variables affecting the low temperature brittleness of ferritic steels. This paper reports the results of one such investigation in which the tensile properties of aluminum and aluminum plus silicon ferrites were measured from 100" to —192°C. True stress-natural strain data have been obtained in order to evaluate as many as possible of the parameters which describe the behavior of the materials involved. In comparable studies at the National Physical Laboratory in England, iron and iron alloys of high purity have been produced&apos; and tested at subat-mospheric temperatures.&apos; True stress-natural strain curves were obtained there also. The purest iron contained 0.0025 pct C and 0.001 pct O and N. Even this, as normalized at 950°C following hot rolling, showed little ductility at -196°C. The grain size was ASTM No. 3, and the room-temperature yield strength was 17,800 psi (which seems too high for pure iron). Some of the NPL irons contained considerably more oxygen and demonstrated intergran-ular fracture at —196°C. The authors2 carefully differentiated between intergranular fractures associated with excessive oxygen content and transcrys-talline cleavage with little ductility encountered at —196°C in the purer material. The cleavage stress was half again as great as that associated with inter-granular fracture. Test Material, Preparation, and Procedures Of a number of Fe-A1 alloys produced, eight were considered to be sufficiently pure for testing. Partial chemical analyses (Table I), low observed yield points, and high ductilities indicate these alloys to be comparatively pure for vacuum-melted irons of sizable ingots, 5 Ib or more. To produce the binary Fe-A1 alloys, electrolytic iron was melted in air, cast into slabs, and rolled to strips 0.010 in. thick. These strips, joined into a continuous ribbon and wound into 2 1/2 in. diameter spools, were subjected for four weeks to a moving atmosphere of purified dry hydrogen in a stainless-steel tube at 1050" to 1150°C. Charges of these spools were melted in beryllia crucibles under good vacuums (1 micron), and aluminum (99.97 pct Al) was added to the melts. Compositions of these alloys are recorded in Table I. The ingots were hot forged and then cold rolled at least 65 pct to 3/8 in. rods which were vacuum annealed to the desired grain size, approximately ASTM No. 4, prior to machining into tensile test bars. All tensile specimens had gage sections 1 in. long, with a fillet of 1.5 in. radius to the shoulder. Gage diameters were 0.250 in, except for a few rods where additional cold work required use of a 0.200 in. gage section. After machining, 0.002 in. was removed from the gage diameter using 240, 400, and 600-grit metallo-graphic papers. The final polish with 600 grit left the fine scratches running in the longitudinal direction. By this means, surface metal strained during machining was removed. A few specimens heat treated after machining were similarly reduced 0.004 in. to remove any material affected chemically by the atmosphere during heat treatments, as is discussed in a later section. Tensile tests of the eight alloys at constant temperatures from +100° to —185°C were performed in apparatus which has been described." The essentials include a double-walled insulated metal vessel which contained the liquid heat-transfer medium surrounding the test specimen. A constant temperature was maintained by means of a pyrometer which regulated the pressure of dry air driving liquid air through a copper coil. Temperature variation was less than ±2°C during a specific test. For axial straining, two lengths of case-hardened chain, terminating in simple shackles, loaded the specimen through threaded grips. The lower grip bar passed through a hole in the bottom of the test vessel to which it was joined by a thin-walled

Jan 1, 1955