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By P. Breidt, E. S. Greiner

THIS note reports a determination of the melting point of germanium, and the liquidus of the Ge-Ga alloys; lattice constants of the a phase are given. The alloys were prepared by melting germanium (>20 ohm-cm resistivity) and gallium (99.6 pct) in evacuated silica tubes. The materials (50 to 70 g) were heated at 1000°C, held in the liquid state for about ¾ hr, and then cooled rapidly in the tubes. Points on the liquidus were obtained by thermal analysis which consisted of obtaining time-temperature data during heating and cooling the materials in high purity graphite crucibles and a helium at- mosphere. Temperatures were determined with a Pt—Pt-Rh thermocouple protected by a silica sheath. The couple was calibrated against a National Bureau of Standards calibrated couple and also against the freezing points of copper, silver, aluminum, and the 28.1 wt pct Cu, 71.9 wt pct Ag alloy eutectic. The samples for X-ray analysis were prepared by heating small pieces of the ingots in evacuated glass or quartz tubes at temperatures between 600" and 900°C for periods ranging from 2 hr to 22 days, periods deemed sufficient for equilibrium to be attained, followed by quenching in water. The heat-treated samples were ground to powder for X-ray analysis. The lattice constants of the germanium-rich phase (a) were determined with a baok-reflection focusing camera. The X-ray reflections (331 and 422 Cr Ka, 422 and 333 Cr KB) were corrected

Jan 1, 1956

By L. D. Jaffe

IN previous metallographic work on titanium and its alloys, difficulty has been encountered in distinguishing spheroidal particles of titanium hydride, dispersed in a-titanium, from other phases that may be present, such as p-titanium. This problem is common in examination of commercial unalloyed titanium.' In the course of an investigation of the Ti-H phase diagram, it was noted that titanium hydride, dispersed in a matrix of a-titanium, showed strong optical anisotropy when examined under polarized light. With sensitive tint illumination, particles of the hydride, when the stage is rotated, changed from bright yellow to bright blue in color. Since P-titanium is cubic, it showed no color change on rotation, remaining dark gray or blue-gray. Although a-titanium is hexagonal, it showed only a minor color change, going from pale pinkish-blue to pale purplish-blue. These colors could be modified somewhat by adjustment of the illumination. They were observed in specimens mechanically polished, both without etching and after etching with hydrofluoric acid-nitric acid mixtures in either water or glycerine. The strong color change of the hydride seems to offer a simple method for its metallographic identification. Optical anisotropy of titanium hydride is inconsistent with its accepted face-centered-cubic structure.' Samples of iodide titanium containing 6 to 40 atomic pct deuterium were prepared for diffraction studies. After deuterating and slow cooling' the samples were held 21 % hr at 400 °C, water quenched, held 61 hr at 100°C and quenched, then held 64% hr at 255 C and quenched. Debye ex-posures with MoKa X-rays and 1.111A neutrons were made at room temperature of samples as-deuterated and after the 100" and 255°C treatments. Table I shows the lines observed, in addition to those attributable to a-titanium. These data show that the hydride phase was not cubic, but probably tetragonal. The titanium atoms appeared to form a body-centered-tetragonal lattice complex, two titanium atoms per cell, with approximate dimensions: a = 3.12A, c = 4.18A, and c/a =1.34A. This is equivalent to a face-centered-tetragonal complex, four titanium atoms per cell, with approximate dimensions: a = 4.42A, c = 4.18A, and c/a - 0.946A. The presence of the 2.98 and 1.81A neutron lines indicates that the true Bravais lattice is not identical with this lattice complex, but may be primitive tetragonal with dimensions some multiple of those of the complex. The relative intensities of the hydride and a-titanium X-ray lines as functions of overall composition indicated that the hydride, presumably in equilibrium with the a at 100" to 255"C, contained more than 62 atomic pct H. Acknowledgments The experimental work covered in this report was done at Brookhaven National Laboratory, through the courtesy of D. Gurinsky. The cooperation of J. Sadofsky, 0. Kammerer, A. McReynolds, and A. Cendrowski is gratefully acknowledged.

Jan 1, 1957

By Edward A. Loria

A SERIES of papers on the study of austenite grain A size in cast steels has been published recently.'" These studies show that in the as-cast state, the austenite grains are quite large, for they form as the steel freezes at a very high temperature, but a simple reheating above the critical range produces a new set of austenite grains which, in many instances, is finer than ASTM grain sire No. 8. Furthermore, there is no apparent relationship between as-cast austenite grain size and subsequent grain size produced by heat treatment. The as-cast austenite grain size can be determined easily in plain carbon and low alloy steels which produce a continuous grain boundary f errite envelope in the as-cast structure. In the case of cast steels whose alloy content produces greater hardenability and suppresses the proeutectoid ferrite transforma-

Jan 1, 1952

By R. Bakish, W. D. Robertson

IN the course of a study of stress corrosion cracking of AuCu,, it was necessary to develop new electropolishing and metallographic etching methods. The techniques are generally useful for Cu-Au alloys, including the AuCu composition in which transformation markings are well delineated. For electropolishing, the only satisfactory electrolyte and procedure that has been found1 has the composition given in Table I. The solution must be vigorously stirred while polishing and the temperature maintained in the range of 55" to 62°C. The electrolyte is very unstable and can be used only for 10 to 15 min after which its color changes and a dark-brown precipitate forms. The polishing time is between 1 and 4 min depending on the initial surface preparation. The use of a hood is recommended to avoid the danger of cyanide gas which may form at one of the electrodes even though the solution is alkaline. The optimum current and voltage conditions for vertical anode and platinum cathode are on the plateau shown in Fig. 1, in which voltage is measured across the cell terminals. At voltages below the plateau, etching of grain boundaries occurs and under some conditions, which have not been clearly defined, octahedral etch figures are observed. For general purpose grain-size determination in polycrystalline alloys, a 3 pct solution of iodine in methyl alcohol is used with excellent results. However, when it is necessary to reveal small orientation differences or concentration gradients in an alloy, the iodine etch is not satisfactory. For this purpose, a highly satisfactory etching procedure was developed during this investigation. It involves the use of the vapor given off by freshly prepared aqua regia. The solution employed is 3HC1 to lHNO, which decomposes in accordance with the reaction HNO, + 3HC1 = NOCl + 2H,O + Cl,. The polished specimen surface is held about 1 to 2 cm above an aqua regia solution for 2 to 10 sec depending on the intensity of the contrast required and the surface is not subsequently washed. The results obtained with a coarse grained cast structure are shown in Fig. 2. Subgrain boundaries in a single crystal and concentration gradients within the boundaries are developed by the same treatment with the results shown in Fig. 3. Obviously, any conclusions regarding structure-dependent properties will be modified by the pronounced heterogeneity, which is not clearly evident when more conventional methods are used. Interesting structural details are also revealed by treatment for 4 hr at 850°C in unpurified tank argon. Fig. 4 shows a pattern characteristic of orientation-dependent oxidation.

Jan 1, 1956

By Nicholas J. Grant, Italo S. Servi

SPECIAL polishing and etching techniques were developed during an investigation of the high temperature mechanical properties of high purity aluminum (99.995 pct Al).* Electrolytic polishing was done successfully in the following electrolyte: 5 ml perchloric acid (72 pct), and 95 ml glacial acetic acid. No special precautions need be taken during the preparation of the electrolyte since no appreciable heat of mixing is evolved. Although the electrolyte is not an explosive, it is recommended that Jacquet's safety rules' be followed during the polishing operation. A voltage of 25 to 60 v gives a good polish in about 2 min at room temperature after preparation on 3/0 metallographic paper. Most of the grain boundaries are visible under the microscope after polishing. Since the current is controlled essentially by the resistance of the bath, it is necessary to keep the anode-to-cathode distance as constant as possible. Accordingly, polishing of irregularly shaped pieces will be difficult. A cooling bath and a stirring system are advisable in order to keep the temperature of the bath uniform and constant. Coarse-grained samples can be macroetched in a few seconds by lowering the voltage below 10 v. This is done after electrolytic polishing, without removing the sample from the bath, Fig. 1. The specimen can be repolished in less than 1 min by raising the voltage above 25 v. The "galvanic etching" technique, which has been described elsewhere,' was found to be helpful not only for macroetching, but also for microetching coarse-grained specimens. In fact, the different orientations of adjacent grains provide good contrast at the grain boundaries, when the sample is observed under polarized light. If the specimen is only partially etched, Fig. 2a, the grain boundaries can be located without completely destroying the appearance of the surface of the specimen. The unetched surface appears black under polarized light. Excellent color contrast is obtained by using a "sensitive tint" plate in the optical system of the microscope. In this case, the unetched surface has a magenta color, while the etched part of the sample assumes different colors varying from green to brown, according to the orientation of the grains. Etch pits were produced on high purity aluminum by using the technique suggested by Lacombe and Beaujard." Good results also were obtained by substituting 70 pct nitric acid for the fuming nitric acid recommended. This gave an etching reagent of the following composition: 70 ml nitric acid (70 pct), 50 ml hydrochloric acid (37.5 pct), and 3 ml hydrofluoric acid (48 pct). An example of the results is shown in Fig- 2b. The outline of the etch pits is revealed sharply if the specimen is observed under polarized light, as shown in Fig. 2c. These metallographic techniques are not suitable for the examination of commercially pure (2s) aluminum. References 'P. A. Jacquet: Metal Finishing (Nov. 1949) 47, p. 62. 21. S. Servi: Metal Progress (1950) 58, p. 732. 3 P. Lacombe and L. Beaujard: Journal Inst. of Metals (1947) 74, p. 1._________________________

Jan 1, 1952

By A. A. Burr, D. Caplan

IN carrying out experiments in metal-gas systems, it is often difficult to estimate how long a reaction period must be allowed for equilibration. This is especially true in systems for which the diffusion coefficient is not known. In an investigation of the Cr-O system, the necessary information was obtained in the way described subsequently. Two pieces of chromium sheet of different thicknesses were packed in mixed powders of chromium and Cr2O3 and sealed into an evacuated metal capsule by welding. Austenitic stainless steel proved suitable as a capsule material up to 1350°C and molybdenum at higher temperatures. The capsule then was heated at a specific temperature for a time sufficient to saturate with oxygen the thinner but not the thicker specimen. The time is readily estimated from a preliminary experiment if a sufficient thickness differential is chosen. Under these experimental conditions, the metal sheet is exposed to a partial pressure of oxygen equal to that of the dissociation pressure of the oxide and hence can become saturated with oxygen without developing any second phase. After cooling, both samples were analyzed for oxygen by the vacuum fusion technique. Assuming that the surface of the specimens is kept saturated with oxygen throughout the experiment, the diffusivity can be calculated by application of the appropriate solution to Fick's second law. This is most conveniently accomplished by use of a plot of mean fractional saturation (Cm-Co) / (Cs-Co) vs (Dt) ½/L as given by Darken,' where t is time, L the half-thickness of the sheet, and D the diffusion coefficient. Cm, the mean concentration at time t, is given by the oxygen percentage in the thicker specimen; Cs, the constant surface concentration, is the oxygen percentage in the thinner specimen; Co is the oxygen content of the original chromium sheet. (Cm-Co) / (Cs-Co) is calculated and the corresponding (Dt) ½/L is read from the graph and D thereby calculated. By performing the experiment at two temperatures and plotting log D vs 1/T, the D for any temperature is established. (The activation energy for diffusion may be obtained from the slope of the line.) Once D is known as a function of temperature, it is a simple matter to estimate the correct reaction time for experiments with single specimens at other temperatures by equating (Dt) ½/L to its value for effective saturation. Darken' points out that this is approximately unity. The solubility of oxygen in chromium, as determined from the thin samples at each temperature, proved to be approximately 0.03 pct at 1350°C and less at lower temperatures. Due to low solubility and to the known difficulties of the vacuum fusion method in this low range, the values obtained for D (5x10-0 sq cm per sec at 1350°C) are estimated to be correct only within an order of magnitude. Nevertheless, the method has proved useful in estimating reaction times. Its usefulness will be greater in metal-gas systems where the solubility is appreciable. A second function of the method is to permit the determination of diffusion coefficients in systems for which the conventional techniques are experimentally difficult or impossible.

Jan 1, 1956

By I. Sheinhartz, H. M. McCullough

DURING the course of a lubrication study in relation to the compacting of metal powders, it became desirable to measure the thickness of sprayed graphite coatings on steel dies for hot pressing. The thickness of these lubricant coatings ranged between 0.0001 and 0.002 in. In their particular case, the authors were interested in a method for measuring the lubricant thickness on tapered die inserts having curved surfaces. The lubricant was sprayed on the inserts at an elevated temperature and it was desirable to measure the thickness as soon as possible after application. Various standard types of commercial equipment were tried. Most of the available devices operated on either a mechanical or magnetic principle. The mechanical devices, such as micrometers, dial indi-

Jan 1, 1956

By L. D. Jaffe

IT is now well established that quenched and tempered titanium alloys have much better ductility when the quenching is from a two phase a-B structure, rather than from an all B structure. The corresponding microstructural differences, however, have not been shown in previous publications. Accordingly, specimens were cut from a % in. rod of commercial RC-130A, containing 7.9 pct Mn and 0.12 pct C, which had been previously hot rolled, heated 1 hr at 1100°F, and air cooled. (The same heat has been studied by others." 7 Samples about 1/4 in. cube were heated in helium 1/2 hr at 1450' or 1700°F, quenched in brine, tempered in helium 1 hr at various temperatures up to 1250°F, and quenched in brine. They were then sectioned and metallo-graphically examined, using an etchant of HF-HNO, in glycerine. As quenched from 1700°F, the microstructure observed was clear /3. (Probably also present was U, as the hardness was 400 Vhn, but w is not yet reliably revealed by any metallographic technique.) When the /3 quenched alloy was tempered at a high temperature, a precipitated as a grain boundary film

Jan 1, 1957

By P. Dayal, L. S. Darken

THE migration of carbon in austenite under the influence of an electric current has been observed qualitatively several times.14 Lebedev and Guterman5 recently have reported quantitative measurements; their method consisted of welding a low-carbon to a high-carbon wire, passing current, and later estimating the carbon distribution metal-lographically. We believe the method reported in this paper is superior in principle since electrolytic migration and ordinary diffusion are not necessarily coupled as in the weld method; also for the first time the extent of migration is determined by combustion analysis for carbon. A uniform tubular specimen (S.A.E. 1045 or 1095) was mounted as illustrated in the figures. the whole assembly being in an atmosphere of purified nitrogen. Direct current (129 to 226 amp at 0.65 to 1.0 v) served as source both of heat and of potential gradient for carbon migration. The duration of experiment was 7.5 to 12 hr, during which time the temperature was controlled (±10°C) manually. The experimental conditions are indicated in the first five columns of table I. With this experimental arrangement, the temperature initially has a maximum value at the central plane. Also, in this vicinity (by virtue of the symmetry), the carbon entering any volume element is equal in quantity to that leaving; the loss or accumulation of carbon occurs near the electrodes since the carbon moves uniformly near the center and is "frozen" at the cold ends. Hence, providing the time of experiment is not sufficiently long to seriously influence the conditions at the central plane, carbon crosses this plane only under the influence of the electrical potential gradient and not under the influence of temperature or concentration gradient. The amount of carbon which has crossed this plane was determined by combustion analysis of the two halves of the specimen. The results of these analyses are shown in the sixth and seventh columns of table I. It will be noted that substantial amounts of carbon migrated from the anode portion to the cathode portion (except at 920°C, which temperature was too low to exhibit the effect in the allotted time). In spite of precau-tions taken, considerable decarburization occurred as may be seen by comparing cols. 8 and 5. In three cases (indicated by asterisks in table I) the specimen was ground on one side, polished, and examined metallographically before analysis. One specimen was normalized and re-examined. Micrographs of selected areas in specimens 4 and 6 are shown in figs. 1 and 2, respectively. Evidence of carbon migration from the anode toward the cathode is quite apparent. Fig. 2 shows abundant graphite as well as cementite in a region near the cathode. The temperature of this zone is estimated at about 800°C. In fig. 1, particularly in the micrograph on the extreme right (the right side of which is of unaltered carbon content), there is evidence of slight depletion of carbon in the immediate vicinity of the cathode as contrasted to the general increase in carbon of the cathode half of the specimen. Although this may be attributed in part to decarbur-ization, it is believed that it is occasioned also by thermal diffusion—migration (of carbon) from a cool to a hot zone4—a phenomenon superimposed upon the electrical migration. Evidence of carbon migration was visible particu-larly during the course of the high-temperature,

Jan 1, 1951

By R. C. Troxell, S. C. Sun

EFFORTS to obtain definite quantitative data when employing the currently used bubble pick-up method1,2 as a pre-flotation investigation tool led to the adoption of the magnifying mirror method and the microscopic method modifications. Quantitative data obtained by these two methods were converted into bubble pick-up indices and bubble pick-up coefficients. Rough correlations were established between the calculated indices and the results of contact angle testing as well as actual flotation under the same conditions. The basic steps of the magnifying mirror method are as follows: 1—mixing 200 ml distilled water, sized and cleaned mineral particles of approximately 0.5 g, pH regulator, and flotation reagents in a glass beaker; 2—swirling the mineral particles to the center of the beaker to leave a clear circumference; 3—pressing an air bubble against the mineral particles for about 1 sec, and then moving the mineralized air bubble to the clear part of the beaker; and 4—dropping all the attached mineral particles of the air bubble by tapping the bubble holder, and counting the number of the dropped particles by looking at the magnified image in the mirror positioned beneath the beaker. This method is impractical for mineral particles which are transparent in water or finer than 200 mesh. The microscopic method is essentially similar to the above described magnifying mirror method, with the exception that the mineralized air bubble was drawn up into the bubble holder and subsequently discharged onto an externally placed watch glass, where the number of pick-up particles was counted with the aid of a microscope or hand lens. Drying was necessary when the discharged liquid interfered with the counting. The results of the bubble pick-up tests can be simply expressed in the form of the actual count. However, this can be misleading because the number of pick-up particles varies not only with the size of bubble but also with the size of particles. This short-coming is largely remedied by the use of the bubble pick-up index. as calculated from the following equation: PI = (pn/p) 100 [1] in which PI and pn are respectively the pick-up index and the number of pick-up particles under any test conditions, and p is the maximum number of pick-up particles of the same mineral under optimum flotation conditions, with the same size holder and particle. The bubble pick-up coefficient is a term coined to denote the difference between the bubble pick-up index of mineral particles in a liquid and that of the same mineral-liquid mixture plus a chemical reagent at the same pH value. For example, the difference between the pick-up index of a naturally floatable bituminous coal in a solution of water and kerosene and that of the same coal in water alone is a bubble pick-up coefficient. Compared with the contact angle method, the quantitative bubble pick-up method is inferior in accuracy but superior in sensitivity. Other advantages of the bubble pick-up method are that the apparatus can be easily assembled, the mineral sample is conventionally prepared, and the test procedure is relatively simple. References S. R. B. Cooke: The Flotation of Quartz Using Calcium Ion As Activator, Trans. AIME (1949) 184, p. 306. 'G. A. Last and M. A. Cook: Theory of Collector-Depressant Equilibrium at Mineral Surfaces. Paper presented at St. Louis Meeting, AIME (February, 1951).

Jan 1, 1954

By G. Vaux, M. L. Fuller

AN apparatus and procedure for the determination by X-ray reflection of preferred orientation of crystals in rolled metal with the Geiger counter X-ray spectrometer was described by Schulz.' This is an excellent procedure and we have used it continually for several years. In our use of the procedure, two modifications have been made and used during most of this period. One of these provides for automatic scanning and recording of the reflections, and the other makes possible the application of the procedure to coarse-grained specimens and permits measurement of almost all orientations without resort to the transmission technique. The automatic scanning and recording are accomplished by a motor drive of the inner ring of the Schulz apparatus (see R, in Fig. 2 of his paper and R2 in Fig. 1 of this note) in synchronism with the chart recorder of the North American Philips 90" X-ray spectrometer. A rate of 10" per min is used. A scan of 180" is obtained corresponding to poles on the stereographic projection whose locus is a great circle. The modification for coarse-grained material is accomplished by allowing a larger area of the specimen to contribute to the X-ray diffraction. In the Schulz apparatus the incident X-ray beam is confined by a slit system to rays in the plane of the spectrometer. Schulz demonstrated that this restriction of the X-ray beam permits a survey of the X-ray reflections without correction up to about 80" on either side of that specimen position in which the specimen is perpendicular to the plane of the spectrometer. This is the angle + of rotation of the inner ring R2. One of these slits is horizontal and extends across the X-ray source side of the specimen. In the modification this slit is removed, thus permitting greater divergence in the X-ray beam and the irradiation of a larger area of the specimen surface. Fig. 1 shows the apparatus with the motor drive and with the slit removed. Discontinuities in the recorded X-ray intensity plot due to the few participating crystals in coarse-grained metal are much lessened. The increased divergence does not cause reflections from other crystal planes to enter the Geiger counter slit. An important advantage of the original Schulz scheme is thus lost and a system for correction is required. To do this, a compact of atomized copper powder was prepared and tested by the original Schulz method for the absence of preferred orientation. The horizontal slit was then removed and a curve recorded showing the variation of intensity with angle +. In our arrangement the intensity was uniform within the range + equals ±30°. Beyond this the intensity fell off rapidly reaching zero at ±90°. The curve thus produced is then used to correct measurements made on preferred orientation specimens. In practice this is accomplished by constructing from this calibration curve a family of curves which, as a transparency, can be superimposed on the recorder chart to read corrected intensity directly. Not only does this method permit the handling of coarse-grained material but it also makes possible the plotting of intensities almost to the circumference of the stereographic pole figure projection. Thus, nearly the entire pole figure can be plotted without the necessity of using the transmission technique. Moreover, intensities are much greater, an advantage when surveying crystal planes of poor reflecting power.

Jan 1, 1954

By Kehsin Kuo

DIE steel with 1.47 pct C, 0.42 pct Mn, and 8.22 pct W contains Fe,C and WC in the annealed state and WC embedded in a martensitic matrix in the hardened state (quenched from 800°C). The presence of a large amount of undissolved angular WC carbide particles makes this steel extremely wear-resistant. However, the WC carbide begins to dissolve in the austenite when the heating temperature is raised above 1000°C, but this solution process is still not complete at 1250°C although partial melting has already taken place at the austenite grain boundaries. At 1325 C, this steel contains austenite and liquid metal but no WC carbide, Fig. 1. On quenching into brine, the liquid metal solidifies into a constituent which etches differently from the austenite-martensite matrix. This constituent appears lighter than the matrix at the 1250°C stage when etched with 2 pct nital but darker in Fig. 1 when etched with Murakami's reagent. Such a constituent has also been found in burnt tungsten high speed steels. This constituent has been isolated from the matrix by anodic dissolution in a 5 pct HC1 electrolyte and was found by the X-ray powder method to be iso-morphous with &manganese, Table I. The agreement in line intensity between these two phases indicates that there is no ordering in this new phase. The calculated cube edge of this phase is 6.395A, somewhat larger than that of ß-manganese (6.30A). Besides this phase, the anodic residue also contains free carbon from the matrix and amorphous WO,, although the X-ray powder pattern of the residue shows the presence of only this phase. This makes it impossible to determine directly the composition of this phase from the residue. Attempts to prepare an alloy containing only this phase have hitherto been fruitless. The following experiments serve to show that this phase can only be obtained by drastic quenching from the liquid state and that its tungsten and carbon contents must be lower than those in the Fe,W,C carbide. On air cooling from 1325oC, the liquid metal solidifies into a eutectic consisting of austenite and the Fe3W3C carbide. The nature of this dark-etching Fe3W3C has also been ascertained by X-rays. This eutectic becomes coarser on furnace cooling. The solidification of a specimen cooled for 5 min from 1325" to 1200°C and water quenched is still not complete and the fine eutectic is formed during the quenching. Since this new phase can be replaced by a eutectic of austenite and the Fe,W,C carbide, its composition must lie somewhere between the latter two phases. The special features of this phase are: 1—it can only form directly from the liquid state by drastic quenching and 2—it is a ternary phase of iron, tungsten, and carbon. The ß-manganese structure of this phase is also interesting. In the Periodic Table, iron and tungsten lie on opposite sides of manganese; a certain combination of these two elements, in the presence of carbon, may have average properties similar to those of manganese. It has already been established that the x phase, a ternary one of iron, chromium, and molybdenum, has the a-manganese structure."' A similar phase has also been found in the ternary system Fe-Cr-W and in the following binary systems: Re-Cb, Re-Ta, Re-Mo, and Re-W.6 References 1 G. D. Preston: Philosovhical Magazine 11928) 5. 7th Series, p. 1207. - K. W. Andres: Nature (1949) 164, p. 1015. 35. G. McMullin, S. F. Reiter, and D. G. Eberling: Trans. ASM 11954) 46, p. 799. ' J. S. Kasuer: Acta Metallurgica (19541 2, p. 456. • H. J. Goldschmidt: Trans. ASM (19541 46, p. 807. P. Greenfield and P. A. Beck: Private communication.

Jan 1, 1957

By N. E. Grosvenor

Several methods have been proposed for determining the tensile strength of rock. These have been tried out over the past several years, but the results have been erratic and of doubtful value. The tensile strength of rock is its weakest property, and this property apparently enters into all failure phenomena, whether underground or on the slope of an open pit. Therefore, it is essential that detailed quantitative information is known about the tensile strength of rock if the design engineer is going to select the proper pit slope, pit orientation, or orientation of underground workings so as to give the most economical and safest mining condition. This quantitative information may be used to orient the pit in such a manner as to allow steep slopes along two sides. This information possibly may be used to orient the direction of either underground workings or open pits so as to decrease powder consumption and to increase blasting efficiency. Hence it is of prime importance that a method of determining accurately the tensile strength of rocks be developed. The U. S. Bureau of Mines states' that no standard methods have been proposed by the ASTM for testing the tensile strength of rock. The method described in the Bureau publication is said by them to be unsatisfactory. A similar test that has been used in our laboratory in place of the USBM test is shown in Figs. 1 and 2. h this test the core is placed in a set of grips that has been designed for one particular size core. The grips are designed to distribute the stress around the core if they are tightened correctly. A universal joint or a flexible cable may be used in conjunction with the apparatus to prevent bending or twisting of the specimen. The main difficulty encountered with the system shown is the failure of the specimen within the grips. The possible cause of the failure within the grips may be due to a stress concentration set up by the uneven tightening of the grips. This method can be used only for tests on cores, and even then has been found to be totally unsatisfactory because of the failure within the grips. The U. S. Bureau of Reclamation has been using a test similar to the sketch shown in Fig. 3. Sulfur is cast around each end of the specimen to form a bearing surface and then a ring grip is used to apply a tensile stress. The grips are in contact with the sulfur cast and do not touch the specimen. This method is unsatisfactory, apparently because a large number of the specimens appear to break within the sulfur cast. Professor Wuerker of the University of Illinois uses the test shown in Fig. 4.' Professor Wuerker states2 that this method has given definite and reproducible results with the weakest as well as with the strongest rocks. The test is a supplement in all cases where cores cannot be obtained. The principle and equipment are the same as for the test for tensile strength of hydraulic-cement mortar. Soft

Jan 1, 1961

By W. C. Winegard, C. Elbaum, T. Ojala

NONOCTAHEDRAL slip was observed in poly- crystalline aggregates of aluminum by Boas and Ogilvie.&apos; These authors indicate that the non-octahedral slip takes place on (100) or (110) planes. Ogilvie2 studied the continuity of slip lines across grain boundaries in polycrystalline aluminum. Non-octahedral slip was observed by him, but it was not reported to occur in the continuous slip lines across the grain boundaries, which were identified as octahedral slip in all cases. The present note reports the observation of non-octahedral slip in the grain boundary region of an aluminum bicrystal and tricrystal, both deformed in tension at room temperature. An analysis is made, which leads to a probable identification of the non-octahedral slip planes as (110) and (331). The specimens used were of rectangular cross section, approximately 5x10x200 mm. They were prepared by growth from the melt, using aluminum reported by the manufacturer to be 99.994 pct pure. The grain boundaries were in a plane perpendicular to the wider face and parallel to the long dimension of the specimens. The axis of tension was also parallel to the long dimension of the specimen. The orientations of the specimens studied were determined by the Laue back-reflection method and are given in Fig. 1. The nonoctahedral slip was first observed after about 6 pct extension in the bicrystal, and after about 2 pct extension in the tricrystal. The micrograph, Fig. 2, of the grain boundary region of the bicrystal shows two active slip planes throughout each of the two crystals, with a third plane active at the grain boundary in each crystal. Two major sets of slip traces observed in grain No. 1 are consistent with the operation of the slip systems (ill) [oil] and (111) [011]. The nonoctahedral slip takes place on a plane belonging to a <111> zone, as determined by drawing trace normals. Assuming that slip will take place only in the <110> direction, the planes in the <111> zone, which do not contain that direction, need not be considered. Among the remaining prominent planes of that zone, the (011) plane has a common slip direction—the [011]—with the (111) plane, which acts as one of the octahedral slip planes. In grain No. 2, a similar situation to that in grain No. 1 is observed. As indicated previously, the (oil) plane in the <111> zone, to which the nonoctahedral slip plane belongs, has a common [Oil] slip direction with the acting (ill) slip plane. Also, the orientation of the (oil) plane in grain No. 2 almost coincides with the orientation of the acting (111) slip plane in grain No. 1. Similarly, the orientation of the (oil) plane in grain No. 1 almost coincides with the orientation of the acting (111) slip plane in grain No. 2. It is, therefore, possible that the nonoctahedral slip was induced, in both cases, by octahedral slip in the neighboring grain. It is important

Jan 1, 1957

By N. Cabrera

IN a recent paper Kuczynski&apos; studied the rate at which the crack between a metallic plane and a spherical particle of the same material is filled up gradually when heated at temperatures near the melting point. If x is the radius of contact between plane and sphere (fig. I), Kuczynski shows experimentally that x5 = At [1] where t is the time. Assuming that the mechanism of transport of matter is the volume diffusion of vacant lattice sites, he is also able to prove Eq 1 theoretically. The constant A contains as a factor the self-diffusion coefficient of the metal and he shows that the values for this coefficient deduced from his experiments yield the same activation energy as that calculated by other methods, which is a confirmation of this point of view. Kuczynski has also considered theoretically the law of growth of x which would be expected if surface diffusion were the important mechanism. He suggests that x should then obey a law of the form x7 = At, and claims to be able to decide the mechanism involved from the observed law of growth., The purpose of this note is to prove this incorrect. On the contrary, when the mechanism is surface diffusion Eq 1 is also obeyed, but with a different constant A. Following Kuczynski, we suppose the bottom of the crack (surface A A) to have an average radius of curvature p. As a result of this curvature the concentration of adsorbed atoms in this surface, n(p) per cm2, will be smaller, and the concentration of vacant lattice sites in the neighborhood, N(p) per cm3, will be larger than the corresponding concentrations, n(w) and N(w), for a flat surface. For all practical cases we can write Thomson&apos;s formula in the form n(co)— n(P) N(P)—N(cc) _ 2a-a" n(oo) JV(co) kTp [2] where u is the surface energy of the metal and a the interatomic distance. 1. Let us now consider the mechanism of surface diffusion. We suppose the concentration of ad-

Jan 1, 1951

By S. Beatty

RECENT experimental results&apos; on the superconductive properties of vanadium indicate that the magnetic behavior of the metal is greatly affected by internal strains caused by mechanical work, and particularly by oxygen and nitrogen impurities. These result in an increase in the hardness of the metal such that metallurgists&apos; have used hardness as a measure of the impurities. An increase in the impurities should also be reflected in a change of lattice parameter with increasing impurity content. The lattice parameter of vanadium prepared by the thermal decomposition of the iodide has been determined by two workers. Neuburger3 obtained a value of a, =3.0338 ± 0.0003A for the body-centered cubic lattice by means of the powder method. The work of Katelaar is referred to by van Arkel4 in which a value of a0 = 3.025 is given. Four samples were used for this investigation. Sample A, the vanadium of the highest purity in the group, was obtained by means of the thermal decomposition of vanadium diiodide and deposited on a 3 mil diam tungsten filament in the form of crystals. The second sample, labeled B, was obtained by the calcium reduction of the pentaoxide at a sufficiently high temperature to give a melt. A third sample, C, was obtained in the same manner as B but remelted in a pure argon atmosphere. The last sample, D, was prepared by the calcium reduction method and the fine powdered vanadium was then sintered by means of applied heat and pressure. Samples A, B, and C were thus essentially free of mechanical strain in their preparation. Sample D was annealed in a high vacuum at 800°C. The samples were prepared for X-ray diffraction analysis such that all additional strain by cold work or by contamination with oxygen and nitrogen was kept at a minimum. Powder obtained from filings was deemed unsuitable since this would require annealing to get rid of the cold work. A heat treatment up to 1000°C at 10-6 m pressure might still increase the impurity content by means of adsorbed oxygen from residual gas in the vacuum chamber. The most satisfactory samples were prepared for back-reflection film techniques. Samples were cut to size, etched with hydrobromic acid, and mounted in Bakelite. They were then lightly polished on 3-0 paper and lightly etched. Chemical and Hardness Analysis of Samples Spectrographic analyses were made of the four samples and indicated similar metallic impurities for the group. The major metallic impurity in each sample was iron, which was less than 0.01 pct. The sum of the other metallic impurities was approximately 0.1 pct. The carbon content was assumed low by virtue of the methods of sample preparation. The principal impurity difference between the samples was in the oxygen and nitrogen content.

Jan 1, 1953

By H. W. Maynor, C. J. McHargue

DURING the course of an investigation of materials suitable for use as thermocouples at elevated temperatures by one of the authors, several nlolybdenum-rhenium alloys were prepared. Micrographs of an annealed alloy containing 25 pct Re (intended concentration; analysis not obtained) showed a number of twins, Fig. 1, suggesting a face-centered cubic structure. This note reports the structure and recrystallized wire texture of an alloy containing 25 wt pct Re. Alloys were prepared from 99.9 pct Mo (Fansteel Metallurgical Corp.) and rhenium obtained from the University of Tennessee (purity unreported). Powders were combined and briquetted at 56,000 psi and sintering was carried out at 2400°C for 5 hr in vacuum. Ingots so prepared were swaged at 982.2" to 1037.8oC into wires 0.036 in. diameter, a reduction in diameter of 85.6 pct. These wires were vacuum-annealed 1 hr at 2000°C. A North American Philips 114.59 mm powder camera and nickel-filtered copper radiation were used for structure determination. For the texture determination a Laue-type camera was used with zirconium-filtered molybdenum radiation and, because of the high background, aluminum foil was mounted next to the film. Exposures were taken with the wire perpendicular to the X-ray beam and tilted by 10". It was found that the X-ray pattern could be indexed on the basis of a face-centered cubic structure. Because of difficulties associated with obtaining a good X-ray pattern for this material, accurate parameter determinations were not made. An indicated parameter value of 3.70A was obtained. The X-ray data are given in Table I. The annealed wire texture was observed to be a sharp [111] texture. The spread about this fiber axis was k8" at the surface of the 0.036 in. wire. The annealed wire textures of aluminum have been reported as retention of the [Ill] deformation texture for anneals below 500°C and a new [1121 texture for anneals above 600°C.1 In copper wires, with a [Ill] plus [loo] deformation texture, results indicate a retention of this texture for annealing at lower temperatures and new components or the disappearance of components for annealing at higher temperatures.&apos; The presence of the strong [I111 texture in the molybdenum-rhenium alloy after a 2000 °C anneal suggests that the deformation texture was the same. Acknowledgment The wires used in this study were prepared and heat-treated at the Institute for Atomic Research, and Ames Laboratory, Iowa State College, and the authors wish to express their thanks to the Institute for allowing the use of the material and permission to publish the results.

Jan 1, 1954

By C. D. Starr

IT is well known that the martensite reaction can be induced to occur isothermally above the M, temperature by plastic deformation of an alloy in its austenitic state, and also that as the test temperature is increased above the M. temperature, plastic deformation under a given set of conditions merely causes additional slip with a corresponding tendency toward the formation of less martensite per unit of strain. Thus it appears that a maximum temperature exists above which martensite cannot be formed isothermally by plastic deformation. This temperature is commonly designated as the equilibrium temperature Te. Attempts to determine experimentally the equilibrium temperature have indicated that a critical temperature is observed, under a given set of conditions, above which martensite cannot be formed isothermally by plastic deformation. But the observation of a "so called" critical temperature, Te, should not be confused with the equilibrium temperature, Te. In order to clarify this anomaly, true stress-strain curves were obtained for a series of type 304 stainless steel specimens (manufacturer&apos;s analysis, 0.08 pct C, 18 to 20 pct Cr, 8 to 10 pct Ni, balance Fe) over the temperature range 67" to 300°K.&apos; Since martensite is magnetic, a quantitative measure of the amount of martensite that was produced by plastic deformation was obtained by determining the magnetic permeability as a function of strain. The results of these tests are given in Fig. 1. They appear to indicate that a plastic critical point does exist at about 240°K for the stainless steel under investigation here. But that 240 °K is not the equilibrium temperature nor even a true plastic critical temperature can be seen from Fig. 2 wherein the permeability of the same material is shown to increase with cold rolling at 293 OK. Consequently the observation of a "so called" plastic critical temperature is dependent on the mode of deformation and has no theoretical significance. Acknowledgment This work was sponsored by the Office of Naval Research. Permission to publish this note is gratefully acknowledged.

Jan 1, 1954

By R. R. Morral, F. M. Krill, K. T. Aust

THE occurrence of twins in aluminum ingots cast under certain conditions has been well established. For instance, Herenguel and Lacombe1,2 have observed a twinned columnar structure in 99.5 and 99.9 pct Al, solidified by continuous or semicontinuous casting. The structure, which they termed "basaltic," appears in the form of elongated crystalline fibers of alternating luster. Herenguel and Lacombe2 found sections of flat crystalline plates composed of twin crystal plates, in which the twin plane (111) and a [I121 direction contained in the twin plane are parallel to the principal heat gradient. This orientation relationship is different from the usual orientation texture observed in cast face-centered cubic metals, where the [100] direction is approximately parallel to the long columnar axes lying in the direction of growth." A large amount of twinning has also been observed by the present authors in semicontinuous cast aluminum of 99.2 pct purity, Fig. 1. Mondolfo4 has suggested that the twinned cast structure forms by a deformation twinning process as the result of uneven cooling stresses within the ingots. This suggestion appears to be inconsistent with the large amount of twinning observed in the semicontinuous cast ingots and with the large difference of dendritic

Jan 1, 1953

By O. P. Arora, J. B. Darby, Paul A. Beck

LAVES and Wallbaum&apos; reported that the phases occurring at the compositions TiFe, TiRu, and TiOs, which are stable over a wide range of temperatures and are separated from neighboring phases by wide two phase fields, have a CsC1-type ordered structure. For TiRu and TiOs, this was recently confirmed by C. B. Jordan.2 Recent results of Greenfield and Beck3 show that solid solutions with ruthenium of the body-centered-cubic elements vanadium and tantalum (and presumably also of colum-bium) in group Va of the periodic table undergo CsC1-type ordering. Although detailed phase diagrams for these systems are not yet available, it would appear that these ordered structures are separated from the neighboring body-centered-cubic solid solutions by relatively narrow two phase fields.

Jan 1, 1957