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By J. H. Mallery, J. H. Keeler

THE crystal structure of Zral, the compound richest in zirconium (91.03 pct Zr by weight) in the system Zr-Al, has been found to be ordered face-centered-cubic. This compound is of particular interest, since it is encountered as the precipitated phase in potentially useful zirconium-rich alloys. It forms peritectoidally from body-centered-cubic zirconium and Zr,Al at about 975°C. The Zr-A1 constitution diagram has been reported by McPherson and Hansen.' For the primary determination a 100 g ingot was prepared by arc-melting in a water-cooled copper crucible under purified argon. The raw materials were crystal-bar zirconium (a purity of better than 99.7 pct) and spectroscopically pure aluminum. The ingot was double melted, examined metallographi-cally, and found to be quite uniform as shown in Fig. 1. The hardness of the as-cast button was VHN 390 to 445. A 20 mil diam specimen was prepared from annealed (900°C) filings of Zr,Al. The specimen was mounted in a 5 cm radius powder camera and an 8 hr exposure was taken using copper radiation with a nickel filter. The structure of the compound Zral was found to be ordered face-centered-cubic of the Cuau type, with an a,, value of 4.37220.003A. Its calculated density is 5.976e0.013 g per cu cm. The relative intensities for the lines were calculated using the formula 1+cos2 20 I oc----------------- • p • /F7 sin2 0 cos 0 1 + COS' 20 where----------------is the Lorentz polarization fac- sin2 0 cos 0 tor, p is the multiplicity factor, and F is the structure factor. The X-ray data are given in Table I. The compound has exhibited plasticity when present as particles in a matrix of a zirconium. During hot working at about 900°C, the compound has been found to deform plastically to the extent that some of the particles exhibit a length-to-width ratio greater than 4:1 as shown in Fig. 2. In answer to the discussion of ref. 1, McPherson and Hansen pointed out that the compound may be cold rolled and reduced as much as 33 pct. Zr,Al has also been found2 under certain conditions to precipitate in lamellar form at grain boundaries of the a phase of hexagonal-close-packed zirconium. Acknowledgment This work was carried out under Contract W-31-109-Eng 52 for the United States Atomic Energy Commission.

Jan 1, 1956

By F. H. Ellinger

TI HE crystal structure of neodymium has been re-A ported by Quill1 and by Klemm and Bommer"s to be hexagonal-close-packed, Strukturbericht-type A3, with a, = 3.650.4, c, = 5.890.4, c/a = 1.614. Klemm and Bommer,% owever, pointed out that the observed intensities of the lines of the neodymium powder pattern agreed only in part with the intensities calculated for the type A3 structure, and that the neodymium powder pattern showed extra lines which could not be traced to impurities. They found that these extra lines could be accounted for by doubling the c-axis, but apparently they did not consider their evidence to be sufficiently conclusive to justify reporting the doubled c-axis. In the present work, the structure of neodymium was found to be double hexagonal-close-packed. The neodymium metal used in the present investigation was obtained through the courtesy of F. H. Spedding of the Ames Laboratory. Its major impurity was stated to be 0.03 pct Ca. The author's spectrographic analysis indicated high purity and carbon was determined to be less than 30 ppm. X-ray powder specimens were prepared from filings stress relieved in vacuum at 200°C for 50 hr. Powder photographs were taken in an 114.6 mm diam camera (Straumanis film mounting) at room temperature and in a 19 cm diam Unicam high temperature camera at elevated temperatures. Copper x-radia-tion was used for all the photographs. The powder pattern of neodymium was found to index to a hexagonal unit cell with dimensions, as determined from the high angle Ka doublets, of: a.= 3.655+0.001.4; c, = 11.796+0.004.4; and c/a = 3.227 at room temperature. The measured density of neodymium shows that this cell contains 4 atoms, the calculated density is accordingly D, = 7.02 g per cu cm. The diffraction data for the first 15 lines of the powder pattern are listed in Table I. In a double hexagonal-close-packed unit cell, the 4 atoms would be in the positions (0,0,0), (0,0,%), (1/3, 2/3, 1/4), and (2/3,1/3,%) of space group P 6,/mmc. On the basis of these positions, the relative intensities of the reflections were calculated using the expression: 1+cos2 20 I oc \Frp 1 ' sin2 0 cos 0 where F is the structure factor and p is the multi- plicity factor. Since absorption was not taken into consideration, comparison of observed and calculated intensities should be made only for neighboring reflections. Each atom has 12 neighbors, 6 in the basal plane at a distance of 3.655.4 and 3 above and 3 below at the closer distance of 3.626.4. These distances correspond to an average radius of the neodymium atom of 1.820.4. The description of this structure in terms of A, B, and C close-packed layers of atoms is ABAC ABAC. ...... The structure repeats every fourth layer and the stacking sequence of the second, third, and fourth layers corresponds to cubic-close-packing of atoms. A series of powder photographs taken at successively increasing temperatures up to 680a10"C revealed that the double hexagonal-close-packed structure is stable up to this temperature. Acknowledgments The authw wishes to thank W. H. Zachariasen and A. S. Coffinberry for their helpful comments on this work and also Marion Gibbs for measuring the diffraction films. This work was sponsored by the United States Atomic Energy Commission.

Jan 1, 1956

By C. B. Jordan

LAVES and Wallbaum' have described TiRu and TiOs as having the same structure as TiFe; they had previously described the latter compound as having the CsCl structure. On the other hand, a careful investigation of the structure of TiFe by Duwez and Taylor- ailed to reveal the ordered CsCl structure, finding instead a random arrangement of titanium and iron atoms on the points of a body-centered-cubic space lattice. Consequently, it is not clear whether Laves and Wallbaum proposed the ordered or the disordered structure for TiRu and TiOs. In order to settle this question as to the structural type and to obtain values of the lattice para- meters (thereby completely determining the structures), the present investigation was undertaken. Samples having the compositions TiRu and TiOs were weighed out accurately from iodide titanium supplied by the New Jersey Zinc Co., ruthenium powder from Goldsmith Brothers Smelting & Refining Co., and osmium powder from Wildberg Brothers Smelting & Refining Co. No analysis was made of any of these metals. According to the respective analyses of the suppliers, total impurities amount to less than 0.03 pct in the titanium and to less than 0.5 pct in the osmium. The purity of the ruthenium is not known. The alloys were prepared by arc melting in a furnace of the type described by Schramm, Gordon, and Kaufmann.9 pecimens for X-ray diffraction were obtained by crushing the ingots and passing the resulting powders through a 200 mesh screen. Diffraction patterns were made with a powder

Jan 1, 1956

By Edward I. Salkovitz

RECENTLY a set of crystallographic angles for bismuth was calculated and a standard (111) projection was constructed. Since these calculations

Jan 1, 1957

By A. Taylor, S. Leber

WHEN studies of deformation texture, lattice stress, and crystal orientation are made, it is frequently required to know the interplanar angles and subsequently to embody the results of the investigation in a stereographic projection. Tables of

Jan 1, 1955

By Edward I. Salkovitz

THE determination of the orientation of metal single crystals and the studies of plastic deformation are greatly facilitated by the use of the stereographic projection. To draw a standard projection of the crystal it is necessary to have a tabulation of the angles between the various crystal-lographic planes of the particular crystal studied. Bozorth' has published such a table for the cubic system which can be found in many reference books; such convenient tabulation for the hexagonal metals, however, does not appear to be in the literature, although scores of workers have calculated these angles. Therefore, Table I of angles for magnesium, zinc, and cadmium has been compiled. Since the c/a ratio is different for each of these metals, three separate calculations are necessary. The angles 4 between (HKIL) and (hkil) were calculated by means of the formula: Hh+Kk+½(Hk + hK)1+~3aLl cos The c/a ratios were calculated from data given in the 1948 edition of Metals Handbook. Fig. 1 is a typical (0001) standard projection of zinc. For all practical purposes, it serves for cadmium as well, as can be seen from the table. For magnesium, however, it is necessary to construct another net. R. M. Bozorth: Physical Review. (1925) 26, 390.

Jan 1, 1952

By W. J. Romanow

RECENT papers by Williams, Sherwood, and Boothby,1 Seybolt et al.2 Heikes; and Roberts4 attest to the increasing importance of the hexagonal ferromagnetic compound MnBi. Since the magnetic properties of MnBi crystals are highly anisotropic, it is useful and necessary to have appropriate aids for determining their orientations—a (00.1) standard stereographic projection and a corresponding table of crystallographic angles for this structure. The tables of crystallographic angles for the hexagonal system available in the literature5 are computed for c/a ratios greater than that of MnBi and cannot satisfactorily be used to find the crystallographic angles of MnBi. A table of angles between the crystallographic planes (HK.L) and (hk.1) was calculated for MnBi from the formula0 F=are cos Hh+Kk+ 1/2(Hk+hK) + 3/4 (a/c)2Ll/v(H2 + K2 + HK + 3/4 (a/c)2L2) (h2+ k2+hk + 3/4 (a/c)2l2) on an IBM Type 650 Magnetic Drum Data Processing machine. The lattice constants used are listed in Table I and are those determined by Willis and Rooksby7 at 20°C. More recently published values obtained by both X-ray and neutron diffraction"' show no difference from these significant to the calculation. From the crystallographic angles between the basal plane (00.1) and the general plane (hk.1) in Table I, an (00.1) standard stereographic projection was made for MnBi which is shown in Fig. 1. Acknowledgments The author wishes to thank R. G. Treuting and J. N. Hobstetter for their technical assistance, and Miss D. P. Booth for programing the IBM machine for the calculations. He appreciates the opportunity to read the paper of B. W. Roberts of General Electric Co. prior to its publication. References 1H. J. Williams, R. C. Sherwood, and 0. L. Boothby: Bulletin Amer. Physical Soc., 1956 vol. 1, p. 132. 2 A. U. Seybolt, H. Hangen, B. W. Roberts, and P. Yurcisin: AIME Trans., 1956, vol. 206, p. 605: Journal oF Metals, May 1956. 3R. R. Heikes: Physical Review, 1955, vol. 99, p. 446. .B. W. Roberts: A Neutron Diffraction Study of the Structures of Manganese B.W.Roberts:ANeutronDiffractionBismuthide, Physical. Review, 1956, vol. 104, p. 607. 5 A. Taylor and S. Leber: AIME Trans., 1954, vol. 200, p. 190; JouRNal of Metals February 1954. « C. S. Barrett: Structure of Metals, 2nd Ed., p. 635. McGraw-Hill Book Co. New York and London, 1952. 7B. T. M. Willis and H. P. Rooksby: Proceedings Physical Soc., London, 1954, vol. 67B, p. 290.

Jan 1, 1958

By R. B. Russell

SINCE Cahn's¹ paper on plastic deformation in orthorhombic (a) uranium an increasing amount of work is to be expected on orientation of single crystals and preferred orientation in this metal. It would seem desirable to have a table of angles between crystallographic planes (hkl) and (HKL). Table I shows these angles as distances from (loo), (0l0), and (00l), and in Fig. 1 as a standard (001) stereographic projection. Only the locations of poles whose diffracting planes produce Cu Ka reflections up to 0 = 70.5" (i.e. (154) ) are given." The relative reflection of these planes are represented by circle diameters. It is hoped that the projection may also be used in making inverse pole figures, originally suggested by Harris.' Values of 4 were calculated from the expression hH kK 1L cos = hH/a²+kK/b²-lL/c² where the lattice parameters a, b, c, and the spac-ings d were taken from the work of Jacob and Warren." (They report a = 2.852 kX (2.8578 A), b = 5.865 kX (5.8768 A), c = 4.945 kX (4.9550 A).) The parameters reported by them may be subject to revision,4,5 accordingly the interplanar angles are listed to only the nearest tenth of a degree. References ¹R. W. Cahn: Acta Metallurgica (1953) 1, p. 49. ¹G. B. Harris: Philosophical Magazine (1952) 43, p. 113. 3C. W. Jacob and B. E. Warren: Journal ACS (1937) 59, p. 2588. 4J. S. Lukesh: Acta Crystallographica (1949) 2, p. 420. ³ J. Thewlis: Nature (1951) 168, p. 198.

Jan 1, 1954

By J. F. Nicholas

THE angles between the crystallographic planes in cubic metals were originally given by Bozorth and have been republished many times. Recently, Salkovitz2 tabulated the angles for the hexagonal metals (magnesium, zinc, and cadmium). he most commonly used metal which does not fail into either of these groups is tin, which has a tetragonal structure with an axial ratio of c/a = 0.54558 (99.99 pct purity, 25°C).² ccordingly, Table I has been prepared giving the possible values for the angle, 4, between planes of the types {HKL) and {hkl). The formula used was: Hh + Kk + LI — cos? = —--------------—-----------— A [(H2 + K2 + L2-a2c2(h2 + k2 + r;)] All angles are given correct to the nearest minute as this is sufficient for all practical purposes. Every angle depends in a different way on variations in the value of c/a, but even in the worst cases a variation of about 0.0003 in this ratio is needed to vary an angle by l', which corresponds to a temperature change of 20 °C or can be caused by impurities.

Jan 1, 1952

By C. J. McHargue

THE angles between the crystallographic planes in cubic crystals have been given by Bozorth,¹ in magnesium, zinc, and cadmium by Salkovitz,² and in tin by Nicholas. The determination of the orientation of single crystals and the study of plastic deformation require the knowledge of these angles and are often facilitated by use of a standard projection. Tables of these angles and standard projections have not been published for titanium or zirconium which have c/a ratios considerably less than those hexagonal metals for which this data is available. Accordingly, Table I has been prepared giving these angles. Fig. 1 presents a standard (0001) projection of titanium. The angle between (h1k1i1l1) and (h2k2i2l2) was calculated by means of the formula: h1h2 + K1K2 + 1/2 (h1k2 + h2k1 + cos 4 = [(hi2 + K + h1k1 + 3/4 l12 (h2² + C" a² 3/4 — l1 l2 C² k2²+ h2k2 + 3/4 —l2²) ] 1/2 c² The c/a ratio for titanium is taken from the data

Jan 1, 1953

By P. Pietrokowsky

RECENTLY a comprehensive investigation of the various sigma binary alloys was published by Duwez and Baen.1 It was shown that the following conditions are necessary for the formation of the sigma phase: (1) the difference in atomic diameters of the two alloying metals must not be more than about 8 pct; (2) of the two elements which form sigma, one must exhibit a body-centered cubic structure while the second metal must be face-centered cubic, at least in one of its allotropic forms. In addition, a tetragonal unit cell was proposed and powder patterns of six sigma phases were indexed for d spacings greater than 1.640 kx. Since the indexing, based on tetragonal symmetry, led to only fair agreement, the possibility of sigma being orthorhombic was investigated. Various methods for indexing orthorhombic powder patterns are de- scribed in the literature.' The method used in this investigation was a graphical examination of the differences in values of sin' 9 for the adjacent lines of the powder diffraction pattern. This method led to a complete indexing of the Cr-Co (60-40) pattern. Because of the strong similarity between the various sigma alloys, it was then possible to assign indexes to the patterns of Fe-Cr (50-50), Fe-Cr-Mo (30-30-40), Fe-V (50-50), Co-V (50-50), and Ni-V (50-50). The values of sin' 9 and indexes of the six sigma alloys, together with visually estimated intensities, are presented in table 1. In general, the similitude between the six patterns is quite good. For spacings greater than 1.75 kx a few differences are noticeable. In the Ni-V pattern, no (320) exists and the two strong lines (030) and (031) are separated by only two lines of lower intensity, unlike any of the other sigma patterns. However, very little is known about the Ni-V phase diagram and it is possible that the equal atomic percentage composition in this system lies in a two-phase region. At lower spacings there is a close analogy between the patterns. The planes

Jan 1, 1951

By Martin F. Littmann

FOR magnetic devices employing reactors with high rates of flux change very thin magnetic tapes have been employed. One of the more interesting of

Jan 1, 1957

By T. P. Meloy

In a recent paper, Gaudin and Meloy1 derived a size distribution function for single, impact fracture. Mular2 extended the use of this size distribution to describe the output of carefully controlled grinding experiments. As it stands, the function is difficult to compute. Consequently, a series of tables of the function are presented below: where M(x) is the cumulative fraction finer than size x when x is particle size. Weight percents are tabulated for the single parameter, r, in three different size ranges: from 0 to 1, from 1 to 10 and from 10 to 100. Tables I, II and III are cumulative percent finer and Tables IV, V and VI are for weight percent passing screen size x, retained on the screen below. A number of conditions from the table are plotted in Figs. 1 and 2. Fig. 1 is a plot of the cumulative percent finer vs. size, and Fig. 2 is the weight per-

Jan 1, 1963

By J. H. Westbrook

IT is always of interest to document the origin of real microstructures which closely approach various idealized morphologies. Such instances constitute excellent bases for experimental studies of the effect of microstructure on properties. Typical examples include the eutectoid steels (lamellae) used by many investigators and the two phase Cu-Cr alloys (spheres) recently employed by Hibbard and Hart The present note describes a structure with cylindrical particles. In a study of certain alloys in the Cr-C system, an alloy was arc melted whose composition was very close to the aCr-Cr,C, eutectic (3.2 wt pct C, according to the latest phase diagram published by Bloom and Grant2). The alloy was not analyzed but previous experience with the melting technique employed indicates good correspondence between intended and analyzed compositions with negligible tungsten contamination from the electrode. The phases present in the alloy were identified by X-ray powder patterns as a chromium and Cr,C,. Typical micrographs, presented in Fig. 1, show unmistakable evidence of the cylindrical geometry of the carbide phase. The eutectic grains are randomly oriented and, consequently, only a few show the true fibrous nature of the carbide particles, most being cut so as to show slightly elliptical cross sections. Within any particular grain, remarkable uniformity is to be observed with respect to the size, shape, spacing, and orientation of the carbide particles. Length to diameter ratios have been estimated from the micrographs to be at least 250:1, with diameters of about lp. This alloy may be of further interest from different viewpoints. On the one hand, it might be used to check the applicability of the equations derived by Fullman3 for computing true particle dimensions of cylindrical particles from opaque random sections. On the other hand, it might be possible to extract the carbide particles from this alloy and repack them in a ductile matrix to form a synthetic structure of the type discussed by Metcalfe et al.4 With the large l:d ratio and the small diameter of the carbide fibers, it is likely that the interdefect distance in each fiber is sufficiently great to permit realization of a large fraction of the presumed high strength of the carbide. References 1W. R. Hibbard, Jr. and E. W. Hart: Dispersion Hardening of Copper-Chromium Alloys. AIME Trans., 1955, vol. 203, p. 200; Joun-nal of Metals, January 1955. 2D. S. Bloom and N. J. Grant: The System Chromium-Carbon. AIME Trans.. 1950. vol. 188. p. 41; JouRnal of Metals, January 1950. aR. L. Fullman: Measurement of Approximately Cylindrical Particles in Ooaaue Samples. AIME Trans.. 1953, vol. 197, p. 1267; Journal of Metals. ~ebtember 1953 4 A. G. Metcalfe, C. H. Sump, and W. C. Troy: Fiber Metallurgy. Metal Progress, 1955, vol. 67, p. 81.

Jan 1, 1958

By Charles Barron McIntosh

BECAUSE of the well known relationship between a low atmospheric pressure and increased amounts of methane in coal mines, attempts have been made to find associations between low pressures and coal mine explosions. An early study by F. Able disclaimed this relationship. He found that half the explosions took place during a rising barometer when methane content in a ventilated mine would be decreasing. A more recent study by C. L. Hosler revealed a close relationship between anthracite mine explosions and low atmospheric pressure. Bituminous coal mine explosions, where coal dust as well as methane can be exploded, were found to be more closely associated with a rising pressure following a low barometer than with the falling or low pressure period. Emphasis on rising pressure periods led the present writer to investigate the effect of the post-frontal or post-cyclonic weather on coal dust. Dust samples of uniform mesh were exposed in an Illinois mine. Analyses of the dust taken before and after the passage of cold fronts and their accompanying low pressure troughs indicated an increase in coal dust moisture prior to a frontal passage and loss of moisture from coal dust following the time of lowest pressure. Thus the warm, moist air (Tropical Maritime)found over the mine during the falling pressure period was cooled in the mine and moisture added to the dust. Cold, dry air (Polar Continental) accompanies' the rising barometer following a frontal passage and the air, being heated in the mine, subtracted moisture from the coal dust. A similar but seasonal phenomenon occurs from summer to winter, the dry dust period in winter being recognized as the more dangerous period. The question arose as to how the short period or daily changes in moisture content of coal dust compared with the seasonal changes. Temperature and humidity statistics were obtained from the surface and mine entry for the months of July andJanuary. The gain and Ioss of mdisture. to the hine were calculated for these two morths as were the gain and loss associated with mT (Tropical Maritime) and cP (Polar Continental),air masses as observed in the investigatiynsl. Temperature and humidity statistics tigatiynsl.taken from [the two air masses represent atimp span of only 34 hr. The redultant changes as presented in the accompanying table verify the supposition that short period changes in coal mine moisture may attain the magnitude of recognized dangerous seasonal changes. Statistics for the mT air and the July air have been placed next each other and those for cP and January air together for easier comparison of the two warm and two cold air units. The last column readily reveals that there is little difference in the amount of moisture being deposited in the mine from the mT air and the July average air. A similar conclusion is reached regarding the loss of moisture from the mine when it is affected by the cP air mass or the average January air. This comparison would be particularly true from late fall through early spring when strongly contrasting air mass changes are a common occurrence. The invasion of cold, dry air following a cold front thus produces a drying period that could well receive more attention as a danger period for coal dust explosions. This drying period would compare with Able's explosion period during a rising barometer. The drying period is also perltinent in Hosler's findings, where it was noted that the average explosion day (for bituminous coal mines) followed the day of lowest atmospheric pressure. Moreover, the author's investigation of some 365 coal mine explosions also indicates that this post-frontal period should receive special attention in connection with mine safety measures. Two comparatively recent major explosions in Illinois (Centralia and West Frapkfort) occurred after the mines had been under the influence of cold-dry air for 25 to 30 hr-following a deep low pressure passage. Dust was the important explosive element in both these explosions.

Jan 1, 1958

By S. Weinig, E. S. Machlin

THE mechanism of the martensitic transformation has been the subject of a remarkable number of papers in recent years.' Because the task of evaluating all the available theories is a formidable one, the authors will confine themselves merely to the presentation of results of an experimental investigation of the habit orientation, lattice relations, magnitude and direction of average transformation shear strain, and orientation of subband markings for a single variant of the possible habit systems in an 11 pct Mo-Ti alloy. It is hoped that these data will assist in the establishment of a rigorous theory for the mechanism of the martensitic transformation. Experimental Procedure Specimen Preparation: A sample, approximately 1/2 x 1/4 x 1/4 in., was cut from a double arc-melted ingot composed of commercial-process A titanium and high purity molybdenum (nominally, 11 pct Mo). It was capsuled in evacuated Vycor at 10.-3 mm Hg subsequent to a double argon wash and homogenized for 48 hr at 1100°C. After a direct quench into H2O at room temperature, a large-grained specimen resulted, which, by X-ray diffraction and metallographic means, was subsequently shown to be in the body-centered-cubic phase, ß. Two adjacent, approximately perpendicular faces were polished and the ends of the specimen were ground parallel in a V-block. Fiducial lines were inscribed at 45" to the common edge of the polished surfaces in order that they would be perpendicular to the habit traces of the subsequently formed a plates.2 The specimen was then compressed between the ground ends in a Buehler press to stress induce the transformation ß to a'. Experimental Measurements: The habit-plane orientation, the orientation of subband markings, the orientation relation between the parent ß and the product a', and the transformation strain for the same plate were determined. To further establish the nature of the subbands, one surface was repol-ished and etched. The bands in the a' were still visible and were found to be optically anisotropic under polarized light. Back-reflection Laue patterns were obtained from the ß matrix and from a region comprising both a' plates and adjacent ß matrix (a Cu target was used). By superposition of the two X-ray diffraction patterns, it was possible to obtain a tentative orientation relationship between the two phases. This result was confirmed by a pattern taken after the specimen was rotated to make the basal-plane pole of the hexagonal a' phase strike the film. This necessitated cutting the specimen to expose the a' plate in the new position relative to the X-ray beam. Analysis of Experimental Measurements On the basis of the aforementioned X-ray patterns, the orientation between parent and product

Jan 1, 1955

By J. H. Hamilton, J. R. Lewis, J. H. Dismant, W. M. Fassell

RECENTLY this laboratory undertook the task of preparing some low carbon metallic cobalt by the carbon reduction of precipitated cobalt oxides. The oxides came in two lots and had the compositions given in Table I. Industrially, cobalt rondels' are made by the carbon reduction of cobalt oxide in small reverberatory furnaces at temperatures near but not above 1050 °C. This is a slow and tedious small batch process but does give cobalt metal which is low in carbon (1 pct C). Inasmuch as these cobalt oxides were relatively low in copper and iron it was decided to reduce them with petroleum carbon in a small three-phase electric arc furnace of about 3 to 5 Ib of metal capacity. It was hoped such a procedure would save considerable time and perhaps also indicate an improved commercially feasible process. The furnace was preheated by using small pieces of carbon electrodes to maintain the arc until a temperature of 1500°C was reached. The broken pieces of electrodes were then removed and 500 g of the cobalt oxides and 60 to 100 g of petroleum coke added. At the end of the reduction reaction, a high lime flux was added to the furnace to facilitate the removal of sulphur. Due to the fineness of the cobalt oxide powder used and also to the presence of chlorides there was considerable dust lost in charging the furnace. This was overcome by preparing briquettes composed of the cobalt oxides, charcoal, and a little bentonite to serve as a binder. The results obtained are summarized in Table 11, which shows that the cobalt metal produced in the arc furnace was high in carbon varying from 2.5 to 3.5 pct. This, of course, is much too high. For certain uses, such as in the preparation of permanent magnets, the carbon content of cobalt must be low. It was necessary therefore to find an effective method of reducing the carbon content of the cobalt that had been prepared in the arc furnace. Van Arkel3 recommends the use of Co2O3 as a means of removing carbon from cobalt. Experiments by the authors indicate that carbon is removed with difficulty by this method. Other methods used, including lancing of the molten high carbon cobalt with a jet of oxygen, proved to be ineffective. The method finally used makes use of the fact that cobalt metal is decarburized by carbon dioxide at the temperature of the molten metal. Two methods were used: 1—carbon dioxide was bubbled up through the molten cobalt, and 2— molten cobalt was maintained in a carbon dioxide atmosphere. In the first method the gas was introduced below the surface of the molten metal by means of a quartz tube. A high frequency induction furnace was used to keep the cobalt molten in both of these experiments. This kept the metal somewhat agitated and no doubt was an important factor in hastening the decarburization 'process by the second method. Both methods gave satisfactory results as shown in Table 111. An interesting observation in connection with this 'work was that a small sample of carburized cobalt metal could be decarburized by heating it with an acetylene torch adjusted to give an oxidizing flame. This may have been due to the presence of carbon dioxide in the products of combustion. Samples of molten high carbon steel were decarburized by the same method and it is suggested that nickel and perhaps manganese can be decarburized in a similar manner. Additional work, including rate studies and other theoretical aspects of this problem, is in progress in this laboratory.

Jan 1, 1953

By W. R. Clough, M. E. Shank

IT has been noted in a study of the flow and fracture of nodular cast iron under biaxial stress conditions (complete results of which will be published later) that when this metal is subjected to stress it may undergo a striking density change. Such behavior was first determined by strain gage measurements made on tensile test specimens, and has since been substantiated by other types of measurement. The chemical analyses and mechanical properties of several nodular irons to be discussed here are given in Tables I and 11. Tensile data for iron A was obtained from a hollow cylindrical combined stress specimen of the same dimension as those used by L. F. Coffin, Jr.1 in his investigation of gray iron properties. Standard 0.505 in. solid tensile-test bars were used for irons B and C. On each specimen type, A-8 wire resistance strain gages were used—two diametrically opposing gages in the axial direction, two in the tangential or hoop direction. By subtracting elastic strains from the measured strains, the plastic strains could be calculated. By assuming that radial and tangential strains are numerically equal, a measure of permanent volume change can be obtained by summing the plastic strains. This appears to be a good assumption, since the metal either fractured, iron A, or readings were discontinued, irons B and C, long before necking took place. This calculated variation of volume increase with stress is given for irons A and B in Fig. 1. Data for iron C is almost identical with that for iron B. The volume change indicated by Fig. 1 has been substantiated by a more direct type of density measurement. A method developed by S. G. Fletcher and' Morris Cohen,' and completely described in the discussion of their article, has been used. The accuracy of specific volume measurement has been estimated as 0.00002 cu cm per gram. Essentially the method consists of weighing a sample in air and then immersed in water. Measurements were made before and after straining the material. The results shown in Table I11 were obtained by means of half-size (0.252 in. diameter, 1 in. gage length, 3/8-16 threads) tensile specimens. Initial measurements were made on the whole specimen before stressing. After stress-

Jan 1, 1955

By W. A. Backofen

THE texture of cold-drawn copper wire has been described most often as a composite of [Ill] and [loo] directions aligned parallel to the wire axis.' Hibbard2 suggested that sufficient reduction will result in a single [111] texture and reported that after a reduction in area of 96.4 pct, such a texture was nearly obtained. Other work3-4 has shown that recrystallization within the temperature range of 300" to 1000°C does not alter the texture established by cold-drawing. In general, however, the texture of cold-drawn end annealed copper wire is not as well defined as the deformation texture. In the work reported here it was found that the double-fiber, deformation texture persists even after a reduction in area of 97.3 pct, and after recrystallization the texture is practically all [l00]. The wire used in this work was prepared in the following way. A 3/4-in. diam length of annealed OFHC copper was cold-drawn to a diameter of 1/8 in., a reduction in area of 97.3 pct. Each step in the drawing operation brought about a reduction in area that varied from 6 to 10 pct. Short lengths of this wire were etched in a 50-pct solution of nitric acid to a diameter of approximately 0.01 in. The texture of the cold-drawn specimens was determined with the conventional X-ray transmission diffraction technique using filtered copper radiation. The X-ray beam was directed perpendicularly to the wire axis and the diffraction rings were recorded on a flat film. Fig. la is typical of the photo-grams obtained and reveals that the cold-drawing schedule described above introduces a distinct, double-fiber texture with both [Ill] and [l00] directions aligned parallel to the wire axis. Supplementary measurements with a Geiger-Mueller counter of the intensity of reflection from (111) planes showed that the [111] component was much more predominant than the [l00]. Additional specimens of the drawn and etched wire were annealed in a salt bath at temperatures from 300" to 450°C. The texture of the recrystal-lized wire was studied with the same technique applied to the cold-drawn wire. Fig. lb is an X-ray photogram of a specimen annealed for 1 ½ at 300°C and is typical of those obtained from re-crystallized specimens. The photogram shows that recrystallization of this material is accompanied by the almost complete elimination of the [111] component of the deformation texture. A pronounced strengthening of the [100] component was evident from intensity measurements with a Geiger-Mueller counter. In summary, the deformation texture of cold-drawn OFHC copper wire, after a reduction in area of 97.3 pct, may still be described as a composite of [Ill] and [loo] directions aligned parallel to the wire axis. Recrystallization of such wire at temperatures from 300" to 450°C introduces a texture which consists almost entirely of a [loo] alignment. Acknowledgment Sidney Rolle of the Scomet Engineering Co. generously supplied the OFHC copper used in this work. References 'C. S. Barrett: Structure of Metals. p. 382 (1943) New York. McGraw-Hill Book Co. 2 W. R. Hibbard, Jr.: Trans. AIME (1949) -185, p. 598; Journal of Metals (Sept. 1949) TN 19E. 3 P. 422 of ref. 1. 'E. Schmid and G. Wasserman: Ztsch. Physik (1926) 40, p. 451.

Jan 1, 1952

By A. E. Schuetz, A. E. Roswell, W. R. Hibbard

THE drawn wire texture of body-centered cubic iron,' tungsten,' and molybdenum~ as been determined to be a [110] direction parallel to the wire axis. The purpose of this study is to extend the available information on body-centered cubic wire textures to other metals and alloys. Wires were produced using hand wire rolls and dies as given in Table I. In addition, attempts were unsuccessful to draw wires from chromium, vanadium (Vanadium Corp. of America), and tungsten (Cleveland Tungsten Inc.). Although it is known that wires can be made from these materials, suitable techniques were not readily adaptable. Where necessary, wires were polished and etched to form flat ribbons 0.005 to 0.007 in. thick, and transmission X-ray patterns were taken using molybdenum radiation with the specimen tilted 0 degrees from the perpendicular toward the beam to critically cover the wire axis. Analyses were made of (110), (002), and (112) reflection circles. In all cases reflection maxima indicated the texture to be a single [1101 deformation fiber, as illustrated by Fig. 1 for molybdenum. In the case of the hot-worked ß brass, a second texture, [loo], was also found, but this is believed to be the result of recrystallization since it has been reported for re-crystallized molybdenum wires' and it was not present in the cold-drawn ß brass. The difference in drawability between the 51.92 pct Cu ß brass and the 62.5 pct Cu ß brass (containing some grain boundary a due to incomplete quenching) is quite striking, since the latter could be cold worked readily while the former had to be hot worked to avoid cracking. Summary The deformation texture of drawn body-centered cubic wires of ß brass, iron, molybdenum, niobium, and tantalum is essentially a single [110] fiber as predicted by theory.' Acknowledgment The authors wish to thank the suppliers of the metals listed in the text, and the Grant-in-Aid from the Research Fund of the Society of the Sigma Xi and Scientific Research Society of America which made possible the purchase of X-ray equipment.

Jan 1, 1952