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By Paul A. Beck

IN several recent investigations1 ' considerable evidence was accumulated to show the predominance in various face-centered cubic metals of a certain relative orientation, corresponding to a rotation of 30" to, 40" around a [111] axis, between a matrix with a strong single orientation texture and grains growing in this matrix." This relative orientation was found to occur both in recrystallization and in coarsening, "secondary recrystallization", so that one is inclined to look for an explanation applicable in both cases. The abundance of growing grains in the described orientations proves that suitable "nuclei" are present in the matrix material and that they have the capacity to grow. The scarcity of growing grains in other orientations may be explained in one 'of two ways. Either the number of nuclei or the rate of growth must decrease strongly for orientations deviating from that predominating among the growing grains, Fig. 1. Both the "oriented nucleation" and the "oriented growth" theory found support in the literature. Because the frequency of nuclei as a function of orientation is in most instances not amenable to direct experimental investigation, a definitive decision is difficult to achieve. However, it is now known with great certainty that the rate of boundary migration is strongly dependent on the relative orientation of the two grains meeting at the boundary and that the orientation favored by high boundary mobility closely corresponds to that predominating in most cases of recrystallization and coarsening. Thus, it was found that, in general, the mobility is very low for boundaries between grains of nearly identical orientation, or for coherent twin boundaries. On the other hand, the boundaries between two grains of a relative orientation correspending to a [1111 rotation of 30" to 40" have the highest mobility in face-centered cubic metals. If a large variety of nucleus orientations are produced grow- by means of a highly inhomogeneous local deformation, nuclei close to the above orientation are found to grow fastest.z4 In view of this evidence and of the fact that the preferred orientation relationship is the same in recrystallization and in coarsening, the oriented growth theory appears by far the more promising one. Since the origin of nuclei in primary recrystallization is certainly different from that in coarsening, the occurrence of the same orientation relationship in the two processes would be difficult to explain on the basis of oriented nucleation. other advantages of the oriented growth theory are its capability of accounting for the often observed sharpening of the texture in coarsening, and its suitability for explaining the role in the formation of the ''cube texture,, of the most important variables, such as the degree of rolling, the penultimate grain size, and the time and temperature of the last anneal: No similarly consistent explanation of all these effects has ever been offered in terms of oriented nucleation. An important problem in connection with the oriented growth theory is the following: In the ce-c entered system there are four [111] axes and

Jan 1, 1952

By M. J. Sinnott

WITH the advent of nodular iron as an engineering material, considerable interest has been shown in developing this material for various applications. Generally the strength, hardness, or ductility are the more common properties used for design purposes but occasionally applications involving a knowledge of the thermal conductivity of the material is required. A search of the literature showed, rather surprisingly, that relatively little work has been done on this property for all types of cast iron. Insufficient data are available on thermal and electrical conductivities to develop the Weidemann-Franz ratio, or the Lorentz relationship, for estimation purposes. There are no data on nodular irons and the published data on malleable irons are quite sketchy. For these reasons the conductivity of the group of nodular irons listed in Table I were measured. Irons I to IV were made in such a fashion as to maintain the carbon and alloy content essentially the same while varying the silicon content. Test specimens were cut from the mid-section of 4-in. keel castings. Iron V is a commercial casting of nodular iron. The test specimen of this iron was cut from the center of a large cast billet 3x10x26 in. All alloys were tested in the as-cast condition. A microstructural examination showed that each iron had spheroidal graphite but the size and distribution varied with the silicon content of the iron. The spheroid size decreased while the number of graphite nodules increased as the silicon content of the iron was increased. The matrix structures of each iron consisted of pearlite and ferrite with the proportions varying from predominantly pearlite in the low-silicon iron to mostly ferrite in the high-silicon iron. The commercial heat, iron V, was predominantly pearlite probably because of its higher manganese and phosphorus content. Two methods for measuring the thermal conductivity were used. The first was a modification of the techniques described by Powell and Hickman and Van Dusen and Shelton,² the second method was a simpler technique described by Jakob and Hawkins." Since the agreement of both methods as tested on two sets of duplicate samples was excellent, the simpler experimental technique was used. The results of the measurements are given in Table II along with a summary of the microstructural constituents. These conductivity data indicate that as the percentage of silicon increases there is a corresponding decrease in the thermal conductivity even though the structure is changing from pearlitic to ferritic. Such a change in microstructure is usually accompanied by an increase in conductivity. A third factor involved in the behavior of these irons is the size and distribution of the graphite nodules. The relative amounts of graphite do not change greatly but the size and distribution do. Generally graphite improves the conductivity but in the present case such an effect is probably masked by the alloying effect from the silicon and its dispersion through the matrix. The thermal conductivity of the nodular irons studied is less than that of regular foundry irons by some 10 to 30 pct and is less than that of regular malleable irons.' The cause of the decreased conductivity is probably the more highly alloyed fer-rites obtained in these irons and the changed mode of distribution of the graphite as compared to the regular foundry irons. References R. W. Powell and M. J. Hickman: Journal Iron and Steel Inst. (1946) 154, No. 2, p. 99. 'M. S. Van Dusen and S. M. Shelton: U. S. Bur. Standards Journal of Research, RP668 (1934) 12, p. 429. ³M. Jakob and G. A. Hawkins: Elements of Heat Transfer and Insulation. 2nd Ed. (1950) New York. John Wiley and Sons. ' J. W. Donaldson: Journal Iron and Steel Inst. (1933) 128, No. 2, p. 255.

Jan 1, 1954

By J. L. Weeks

THERMAL conductivities of several samples of uranium and uranium alloys were determined using an apparatus previously described.' The value previously reported for uranium,' 0.035 cal per sec per cm per "C at 70°C, is in error due to the failure of a thermocouple during the determination on uranium. The defective thermocouple was detected after a reanalysis of the data obtained during the run and since has been replaced. Subsequently, runs on several samples of uranium show the thermal conductivity of uranium to be 0.069 cal per sec per cm per 'C at 70°C. The accuracy of the determinations was checked by measuring a sample of synthetic sapphire whose thermal conductivity was previously reported and found to be in agreement with other values."-" The values given in Table I are believed correct to % 3 pct or 0.003 cal per sec per cm per "C, whichever is larger. The samples were provided by J. H. Kittel of the Argonne National Laboratory, Metallurgy Div. References J. L. Weeks and R. L. Seifert: Apparatus for the Measurement of the Thermal Conductivity of Solids. Review of Scientific Instruments (1953) 24, pp. 1054-1057. J. L. Weeks and R. L. Seifert: Note Regarding the Thermal Conductivity of Synthetic Sapphire. Journal American Ceramic Society (1952) 35, p. 15. :' J. Francl and W. D. Kingery: Thermal Conductivity: IV, Apparatus for Determining Thermal Conductivity by a Comparative Method; Data for Pb, Al2O3, BeO, and MgO. Journal American Ceramic Society (1954) 37, No. 2, Part 11, pp. 80-84. (Part 11: special issue on thermal conductivity.) ' W. D. Kingery, J. Francl, R. L. Coble. and T. Vasilos: Thermal Conductivity: X, Data for Several Pure Oxide Materials Corrected to Zero Porosity. Journal American Ceramic Society (1954) 37, No. 2, Part II, pp. 107-110. (Part 11: special issue on thermal conductivity.) Edwin Ruh: New Jersey Ceramic Research Station, Rutgers University. Private communication.

Jan 1, 1956

By J. L. Weeks, K. F. Smith

IN order to determine the magnitude of thermal conductivity changes resulting from alloying vanadium with titanium and a few other elements, several sam~les were PrePared and measured. The thermal conductivity -values reported herein in Table I were determined with an apparatus previously described.' As in recently reported2 determinations on uranium and uranium alloys, whose thermal conductivities are in the same range as vanadium," the accuracy of the values was checked by using synthetic sapphire." The error in the measurement is estimated to be '-3 pct or 0.003 cal sec-1 cm-l "C-1, whichever is larger. The vanadium used in preparing the samples was the calcium-reduced type and was supplied by the Electro Metallurgical Co. as 99.6+ pct pure. All alloying elements used in the preparations were 99+ pct pure. A nonconsumable tungsten electrode arc furnace was used for melting the alloys and, without opening the furnace, each ingot was re-melted a number of times to insure homogeneity. The samples as prepared by the Armour Research Foundation were machined from as forged material without annealing. Acknowledgment The note is based on work performed under the auspices of the AEC. References 'J. L. Weeks and R. L. Seifert: Apparatus for the Measurement of the Thermal Conductivity of Solids. Review of Scientific Instruments (1953) 24, pp. 1054-1057. 2 J. L. Weeks: Thermal Conductivity of Uranium and Several Uranium Alloys. Trans. AIME (1955) 203, p. 192; Journal of Metals (January 1955). 3C. A. Hampel: Rare Metals Handbook. (1954) p. 593. New York. Reinhold Publishing Corp. Thermal conductivity of vanadium is given as 0.074 cal sec-1 cm- '°C-1 at 100°C. 4 J. L. Weeks and R. L. Seifert: Note Regarding the Thermal Conductivity of Synthetic Sapphire. Journal Amer. Ceramic Soc. (1952) 35, p. 15. At 70°C, K = 0.071 cal sec-l cm-l °C-1.

Jan 1, 1956

By G. J. Wolga, W. W. Tyler, A. C. Wilson

THE physical properties of uranium have been reviewed by Katz and Rabinowitch.1 Their review includes thermal conductivity data for ternperatures above 375°K. Recently, Mendelssohn and Rosenberg' have published data on the thermal conductivity of uranium from 2" to 20°K. Our measuremerits indicate the temperature dependence of the thermal conductivity in the temperature interval from 20" to 300°K. Electrical resistivity and thermoelectric power were measured on the same sample. The material studied was normal uranium which had been heated at 700°C in a lead bath for 10 min and then quenched in a water bath held at 50°C. From this material a rod M in. in diameter and 2 1/2 in. long was machined. Two 0.040 in. holes were drilled into the rod 1 3/4 in. apart. Copper-constantan thermocouples for temperature and potential measurements were soldered to copper pins which were pressed tightly into these holes. Details of the equipment and experimental techniques used in making the measurements have been described elsewhere." Fig. 1 shows micrographs of a section of the sample studied. Fig. la was taken with unpolarized light and shows impurity inclusions, probably uranium carbide. Fig. lb, showing the same field, was taken with polarized light and gives some indication of the grain size and twinning within the grains. Experimental Results Thermal conductivity and electrical resistivity data are shown in Fig. 2. Table I shows values of

Jan 1, 1954

By E. E. Duncan, G. Derce

REVIEW of the literature on hydrogen in steels indicates that inadequate consideration has been given to the influence of temperature gradients on segregation of this element. Even when segregation has been taken into account, the interpretation of the data has been seriously handicapped by incomplete understanding of the mechanism by which it occurred. Recognition of a mechanism which will be described as "thermal segregation" appears to rationalize many of the observed effects so well that it will be reported here with some preliminary experimental evidence. The complete quantitative evaluation of the factors controlling the mechanism will require extensive experimentation. The operation of the mechanism can be described in relation to fig. 1, which shows the temperature dependence of the solubility of hydrogen in iron at

Jan 1, 1951

By A. T. Corey, J. H. Henderson, M. R. J. Wyllie, C. H. Rathjens

The results of three-phase relative permeability tests on nine water-wet consolidated Berea sandstone samples are presented as composite ternary diagranls showing isoperms of oil, water and gas. Capillary pressure control was exercised over the flow of gas and oil in the presence of water. The water saturations ranged from 17 to 71 per cent pore volume. A method of calculating both the oil and water permeabilities of a three-phase system from the easily measured gas relative permeability is presented. EXPERIMENTAL PROCEDURE AND RESULTS A renewed interest has been shown in three-phase relative permeability as a result of recent developments involving underground combustion processes, steam injection, and other multiphase displacement processes. The experiments and results described here involved simultaneous flow of oil and gas in consolidated Berea sand with brine present as the wetting phase. Gas and oil relative permeabilities were measured on nine cores with CaC12 brine present as the wetting phase in saturations ranging from 17 to 71 per cent. The average residual liquid saturation of the cores was approximately 20 per cent. In order to make certain that brine was the wetting phase, the test cores were saturated with brine before contact with hydrocarbons. As an added precaution to avoid having oil displace brine from the wetting position as a result of changing wettability, each core was only used twice, i.e., first with a fixed percentage of brine and then for a gas-oil permeability determination with no brine present. The results, therefore, are presented as composite ternary diagrams representing the flow tests on nine individual cores having very similar properties. All tests were made using a modification of the capillary pressure techniquc described elsewhere. The effective oil permeability was measured before gas was introduced using a very small pressure gradient (a few centimeters of oil). This determination was made without selectively wet barriers in contact with the core. The cores were then placed between capillary barriers and gas-oil relative permeability curves obtained. The capillary barriers had been made water repellent with a silicone treatment. In determining gas-oil-water relative permeability in this fashion, control was exercised over the capillary pressure existing between the gas and oil. No control was exercised over the pressure difference existing between the oil and water. Athough an equal pressure gradient was applied to the gas and the oil phases, this pressure gradient does not exist in the water phase. Since the pressure gradient across the core was always much less than the displacement pressure of the fully saturated core, the pressure gradient can have caused only a very slight distortion of the oil-water interfaces. This slight distortion of the oil-water interfaces had a negligible effect on the validity of the oil permeabilities measured. The oil permeability, measured in the presence of water but with no gas present, was in every case equal. within experimental error, to the gas permeability of the gas-oil system when the oil saturation was the same as that of the water. Gas and oil relative permeabilities were plotted as a function of total liquid saturation. It was found that the gas relative permeability curves obtained on cores with brine present were identical with those obtained on the same cores with no brine present. The denominator for calculating oil relative permeabilities was the permeability found by extrapolation to infinite mean pressure (A la Klinken-berg). Fig. 1 illustrates gas-oil relative permeability results obtained on a typical core. The solid permeability curves represent the experimental data. The dashed oil relative permeability curve was calculated using the relationship;

Jan 1, 1957

By R. I. Jaffee, H. R. Ogden

AT the present time, there appear to be two conflicting opinions on the solubility of boron in titanium. P. Ehrlich' has indicated from X-ray diffraction work that boron is soluble in titanium up to TiB0.8 (17.8 wt pct, 44 atomic pct). The X-ray diffraction pattern for titanium was found in compositions up to TiB0.05_0.07 (1.1 to 1.6 wt pct); then, without a phase gap, superlattice lines appeared up to TiB0.8 On the other hand, Craighead, Simmons, and Eastwood' have estimated the solubility of boron in both alpha and beta titanium to be less than 0.1 wt pct, based on results of metallographic analysis. In some recent work done at Battelle, results were obtained which shed more light on the titanium-rich end of the titanium-boron system. Iodide-type titanium and high-purity crystalline boron were used in this investigation. The boron was prepared by hydrogen reduction of boron tri-bromide and deposition on a hot tungsten wire. The alloys were prepared by arc melting in an argon atmosphere of 10 cm Hg pressure on a water-cooled copper hearth. The ingots were hot rolled to strip at 850°C. Alloys containing up to 1 pct B could be hot rolled. Those containing 2 pct or more B could not be hot rolled. Metallographically, it was found that a second phase was present in alloys containing as little as 0.4 pct B, and that the quantity of second phase increased with increasing boron content. This is illustrated in Figs. la and lb, which show the microstructures of a Ti-0.4B and a Ti-1B alloy annealed in argon at 850°C. X-ray diffraction patterns of alloys containing 1 and 5 pct B revealed the presence of extra lines which correspond to the superlattice lines reported by Ehrlich.' However, no evidence was found of a shift in the lattice constants of alpha titanium indicating that there is very little, if any, solubility of boron in alpha titanium. This fact, coupled with the fact that the alloys were definitely two-phase, indicates that the extra lines are not superlattice lines, but are more probably the result of a second phase of a hexagonal structure almost identical in cell

Jan 1, 1952

By H. Margolin, E. Ence

Two versions of the Ti-Mn binary diagram have been published recently.' , -0th diagrams show two compounds in the region between 40 and 70 wt pct Mn, but disagree as to the reaction in which these compounds are involved. The investigation of the manganese-rich portion of the Ti-Mn binary diagram was undertaken at New York University as part of an investigation of ternary systems with titanium and manganese in order to determine which of the proposed diagrams is correct. A number of alloys between 31 and 70 pct Mn were prepared in a manner similar to that described by Cadoff and Nielsen; except that low currents (110 amp in argon atmosphere) and long melting times (up to 20 min) were used to prepare the alloys. Compositions were determined from weight-loss data, assuming all loss as due to manganese. Heat treatments were carried out with relatively large pieces, since there was a tendency for manganese to be lost during heat treatment. When X-ray diffraction data was to be obtained, the central parts of heat-treated specimens were used to make filings or powders which were not heat treated. Specimens were heat treated from the as-cast state. Heat-treatment times were as follows: 1150°C, 1 day; ll00°C, 2 days; 1000°C, 5 days; and 900°C, 15 days. It should be noted that equilibrium was not attained at 900°, 1000°, and in one case, at 1150°C. Metallographic specimens were electrolytically polished and strain etched by a technique described elsewhere.' At least four, and possibly six, phases were found in the region investigated. On the basis of information available at this time, a completely self-consistent diagram cannot be constructed, and therefore data are presented only for those phases which have been identified by both X-ray and microstruc-ture. Of the compounds detected, the one highest in manganese is the Laves phase, TiMn,, which is hexagonal with a MgZn, type of structure.V he diffraction data for TiMn2 from a 70 pct Mn alloy annealed at 1150°C are shown in Table I. The c/a ratio and parameters of TiMn2 agree well with those of Wall-baum hnd Rostoker et al. The values obtained here are c/a = 1.641, a = 4.825A. Another compound is the y-phase which is estimated to contain about 60 pct Mn. The y-phase has a structure which is identical to that of TiMn, with c/a = 1.639, a = 4.906Å. The fact that y has a Laves-type lattice would suggest that TiMn, has a range of solubility which extends from the composition of TiMn2 (69.6 Mn) to that of y (60 pct Mn). However, this could not account for microstructures which, in the 60 to 70 pct Mn region, show several phases in both the as-cast state and after annealing at 1150°C. Fig. 1 shows a two-phase structure of a 60 pct Mn alloy annealed at 1150°C. The phases present are y (white) and e (dark). If y were TiMn, then, according to Rostoker et al.,' the second phase of Fig. 1 should be P-Ti. The diffraction data for the 60 pct Mn alloy of Fig. 1 are shown in Table I. The starred d-values are from the e-phase and these lines do not correspond to those of &Ti. Comparison of as-cast and 1150°C microstructures of the 60 pct Mn alloy indicates that e precipitated from y. Since y has a

Jan 1, 1955

By W. A. Backofen, B. B. Hundy

THE pole figure interpretation in a recent paper' on the torsion texture of copper was questioned in discussion,2 nd a simpler alternative interpretation was proposed. In the hope of reaching a positive decision in favor of one or the other, further studies were undertaken with 70-30 brass and Armco iron. This additional work has not answered all the questions about torsion textures, but the new pole figures do offer support for the original interpretation and show that the texture is more complicated than the alternative suggests. From the previous paper,' the appropriate method of describing the texture in a twisted bar is known to be a pole figure plotted on a plane tangent to the surface of the bar. The axes of the pole figure are chosen to coincide with directions in the tangent plane which are parallel and at right angles to the bar axis (the longitudinal direction, L.D., and the transverse direction, T.D.), for these directions define symmetry axes of the texture. Therefore any ideal orientation that might be selected to represent the texture gives the crystallographic plane parallel to the tangent plane and the crystallographic direction parallel to the axis of the torsion specimen. A unique texture was assumed in the original interpretation, and the four ideal orientations, (112) [111], (111) [112], (110) [001], and (112) [131], were used in its description. Of the four orientations, the first three provide possible slip directions along the direction labeled T.D. in the pole figure, which is one of maximum shear stress in a specimen being twisted. The alternative, however, simply considered the texture to be made up of two components, one a [Ill] alignment along the specimen axis with a random orientation about the axis as in the wire texture, and the other a superimposed orientation (110) [0011. Experimental evidence for this simpler interpretation was derived from two observations: 1—twisting did not alter the orientation of a single-crystal torsion specimen of a brass in which an octahedral plane was perpendicular (and a [Ill] direction parallel) to the axis, and 2—deformation bands with approximately the (110) [001] orientation were seen to develop in the crystal during the test. The new pole figures were obtained with a brass and an iron torsion specimen of 3/4 and 1 in. gage length diameter, respectively. After annealing, polishing, and twisting, seven rods, about 0.030 in. in diameter and with different orientations, were prepared from material near the surface of each specimen; these were required for the method of constructing pole figures by using a Geiger counter as developed by Norton.5 Since the shear strain gradient in plastic torsion is linear, it was readily computed that the material supplying the brass rods had been subjected to a shear strain of about 3.2, and that supplying the iron rods had received a shear strain of about 2. All details concerning specimen design, testing procedure, rod preparation, and use of the Norton technique can be found in ref. 1. Only this procedure was followed in working out the (111) and (100) pole figures for brass, Figs. 1 and 2. However, X-ray photograms were also involved in the construction of the (110) pole figure for Armco iron, Fig. 3. The photograms were made according to the conventional transmission diffraction technique using a small sheet taken parallel to the specimen surface and etched to a thickness of about 0.0025 in. They were especially important in locating the boundaries

Jan 1, 1954

By Nicholas J. Grant, Chih-Chung Wang

TO phase of the Ti-0 system has the structure of NaCl and has a wide range of solid solubility.' In the course of studying the Ti-Cr-0 ternary system, binary alloys were made of iodide titanium and high purity TiO,. It was found from X-ray studies of the binary alloys that a transformation of the TiO appears to take place at a temperature near 925°C. Evidence of this phase change is best seen in Fig. 1. Fig. 1A shows the X-ray spectrometer pattern (CUKa radiation) of an alloy of 25 wt pct 0 corresponding to the stoichiometric composition of TiO.

Jan 1, 1957

By W. C. Ellis

IN an ingot of germanium solidified progressively from the bottom by a method' devised by J. H. Scaff and H. C. Theuerer, examination discloses ex- IH. C. Torrey and C. A. Whitmer, Crystal Rectifiers. p. 364. 1948. New York. McGraw-Hill Pub. Co. tensive twin relationships. A slice taken about midway in a cylindrical ingot approximately 3/4 in. in diameter and 1 1/2 in. in length, after etching and polishing to delineate different orientations, is shown in fig. la. The orientations of the regions designated with letters were determined by Laue X-ray back-reflection methods and plotted on stereograms. The orientation relationships of the designated components were determined by comparing the values for the nine angles between the three respective cube poles of each orientation with the values calculated in a formal treatment of octahedral multiple twinning in cubic crystals. Germanium, diamond cubic in structure, has the octahedral twinning habit. I am indebted to K. H. Storks for the calculation of the angular relationships of cube poles in octahedral twinning to four orders. The set of values for the nine angles is distinctive of the order of twinning. Confirmation for a multiple twin relationship is obtained from the determined indices of the mirror planes. These exist for all orders of twinning through the third and for some of the fourth." If the orientations are not those for twinning, then the nine angles for the cube poles do not correspond in value and distribution to those formally calculated. Since all nine angles must correspond in values and distribution of values to the calculated ones, the Laue method with a precision of one or two degrees is adequate to establish or deny with confidence the existence of multiple twins. Regions of the same orientation can also frequently be identified by the optical reflections. For example, the narrow twin bands in A at 2: 00 o'clock have orientation B1. The interesting twin relationships shown schematically in fig. lb were found for the section in fig. la. Most of this slice was made up of orientation, A, appearing in widely separated regions. Of the four possible first order twins of A, three were present in this slice and are designated by B with subscripts. Four second order twins of A are designated by C with subscripts. It is worth emphasizing that two of these, C, and C,, are second orders of A through the first order missing in this section. Two regions, designated by D with subscripts are third order twins of A. D2 is a sixth order twin of D,. All orientations found were ascribable to multiple twinning, as if the orientations in this section originated earlier in solidification from a single nucleus. The presence of extensive multiple twinning to- gether with the absence of other orientations appears to be a characteristic result in many instances of solidification of germanium. Fertile conditions for twinning probably exist in the array of atoms in the diamond cubic structure. The high order twins in the section shown, it is reasonable to presume, are the result of progressive octahedral twinning through several generations in the material freezing earlier. Some of these generations do not appear in this section, it is suggested, because their orientations with respect to the growth direction were unfavorable for survival. The extensive twinning is probably promoted during solidification by constraint imposed by volume increase, and to an irregular growth front. Twinning may also be due, in part, to the attempt of the solidifying region to attain the orientation most favorable to the growth direction (maximum thermal gradient). The nucleus for a twinned orientation could have its origin in a "stacking fault" on the close-packed octahedral plane. Further work is being done in which the course of twinning throughout an ingot is being studied. The results appear to be important in the general theory of solidification.

Jan 1, 1951

By Peter Haasen

INDIUM antimonide has the zincblende structure. A possible defect that does not disturb the indium tetrahedron surrounding any antimony atom in this lattice (or vice versa) is obtained when neighboring

Jan 1, 1958

By E. I. Salkovitz, F. W. von Batchelder

AS Slawson1 and others have already shown, from a geometrical view twinning in the diamond structure may be considered as a reflection across a (111) plane or as a reflection across a (112) plane. An analysis by Ellis and Treuting2 showed that the twinning plane must be the (111) plane, but that a twin might have lateral boundaries along (112) planes. Earlier Slawson1 and Ellis3 had shown that only (111) twinning was present in diamond and germanium respectively. Since an ingot of silicon, 1 in. in diam and 1 1/2 in. long, prepared from Dupont silicon to which 0.2 pct Be had been added was available, it was examined for twinning. The ingot had been cooled slowly from the bottom. A section 1/16 in. thick was ground off from the bottom and then the ingot was sliced vertically through the center. Spectrographic analysis indicated only faint traces of iron and silver, in addition to the beryllium. The sample was first etched with a hot solution of 10 pct NaOH in water.and photographed. Back-reflection Laue patterns were made of the vertical and horizontal sections in the regions designated in Fig. 1. Orientations were obtained for each twin using the Greninger technique. Several regions of the same orientation were found; thus regions A and K were identical, similarly N and P, and C, G, J, and L. Knowing the angles between the traces of the twinning plane on the surface and the specimen axis, the indices of the twinning plane were deduced. In all cases the twinning plane was found to be (111); lateral boundaries, however, were found which were (112) such as the one indicated in Fig. 1. Therefore, as in the case of diamond1 and germanium' only (111) twinning occurs in silicon. We wish to thank Mr. Hino for the use of the ingot as well as for its metallographic preparation. References 1C. B. Slawson: American Mineralogist (1950) 35, p. 193. 2 W. C. Ellis and R. C. Treuting: Trans. AIME (1951) 191, p. 53; Journal of Metals (January 1951). 3W. C. Ellis: Trans. AIME (1950) 188, p. 886; Journal of Metals (June 1950).

Jan 1, 1953

By Murray F. Hawkins, W. J. Ainsworth

In all types of subsurface pressure gauges the extension which occurs in the pressure-sensitive element is a function of the difference between the external (well or calibration) pressure and the internal pressure within the gauge, rather than a function of the external pressure only. The internal pressure is near atmospheric and depends upon (a) the quantity of air sealed within the gauge at the time of calibration or measurement, (b) the quantity of moisture (liquid water), if any, sealed within the gauge, and (c) the temperature at which the calibration or well measurement is made. Part of this correction for the change of internal pressure with temperature is taken care of by the customary temperature coefficient of the gauge. However, part of it is not, and while this portion may be only a few psi, it is nevertheless predictable or preventable, and should be considered in precision measurements. ERROR NO. 1 If air is sealed in the gauge at the same temperature and pressure for both the calibration and the well measurements, the usual temperature correction will take care of any difference between calibration and well measurement temperatures. However, if air is sealed within the gauge at temperature T1 and pressure P1 at calibration but at temperature T2 and pressure P2 for a well measurement, because different amounts of air are sealed within the gauge in each case, the internal pressure at. or corrected to, calibration temperature Tr will he different by where all temperatures and pressures are absolute. The calibration temperature is used, and not the well measurement temperature, because the usual temperature correction reduces the well measurements to calibration temperature. The correction term as calculated by the above equation is separate from. and in addition to, the usual temperature correction. Example: T, = 540°R, sealing temperature at calibration P, = 14.7 psia, sealing pressure at calibration T2 = 460°R, sealing temperature at well P2 = 14.7 psia, sealing pressure at well Tr = 660°R, calibration temperature AP = 660 [14.7/460 — 14.7/540] = 3.1 psi While this error is small even under these somewhat maximal conditions, it nevertheless represents a practical situation which did occur, and which as a matter of fact gave rise to this note. Where AP is positive, as above, the correction is added to the measured pressure; where negative, subtracted from the measured pressure. This correction should also be considered in successive calibration runs where the gauge, for example, may be warm from a previous calibration at an elevated temperature. ERROR NO. 2 Where a small quantity of moisture (liquid water) is sealed within the gauge at atmospheric conditions, the increased vapor pressure of the water at higher well or calibration temperatures will cause an increase in internal pressure. This moisture will come presumably from condensation within the gauge following temperature changes, from moisture on the operator's hands, and from atmospheric moisture (rain, mist, fog, etc.). Calculation shows that approximately 0.2 cc of water (three to four drops) is sufficient to saturate the air within an Amerada RPG-3 Gauge at 160°F, at which temperature the vapor pressure of water is about 5 psia. As the vaporization occurs in a sealed volume, the increase in internal pressure will be in excess of this 5 psi. At higher temperatures the pressures will be higher; however more water will be required to saturate the air within the gauge. Some experimental work was carried out with an Amerada RPG-3 Gauge at 200°F fitted with a 1,000 psi element, both with a dry recording chamber and with a small amount of water added. The results directly proved the existence of the error due to the presence of moisture, and, it is felt, indirectly, due to the differences in sealing temperatures and pressures, as both effects may be ascribed simply to an increase in the moles of gas within the recording chamber. SUMMARY In precision measurements the error introduced by sealing the gauge during a well test at a different temperature and pressure from that of calibration may be corrected for by using the equation presented, or it may be prevented by taking care always to seal the gauge at near calibration conditions. The error introduced by sealing moisture in the gauge may be prevented by taking care to keep moisture out of the gauge, or by removing the moisture by either warming or evacuating the gauge. Both of these errors are independent of the range of pressure measurement and the type of gauge, and are in addition to the usual temperature correction. ACKNOWLEDGMENT Appreciation is expressed to W. B. Kendall, Geophysical Research Corp., Tulsa, Okla., who pointed out the error from differences in sealing temperatures during some winter work in Canada. ***

Jan 1, 1956

By R. L. Segall

AN unusual thermal etch figure in copper is described and an explanation in terms of twinning is suggested. A flat polycrystalline specimen of OFHC copper cut from a rolled sheet was electro-polished in orthophosphoric acid and annealed at 950°C in a vacuum of approximately 10-3 mm Hg for 2 hr. The specimen was found to be thermally etched, the markings on the surface being consistent with the assumption that they were the traces of the (111) planes which are developed preferentially because they have the lowest free energy. However, on one grain (the grain shown in Fig. 1) the traces formed an almost regular pentagon and at first sight it seemed unlikely that they could all be (111) traces. These traces were studied further because it was thought that they might be a type of growth spiral. A fringe pattern showed that this was not so, the grain being sensibly flat and the only features having steps were the striations and the faint curved line passing out from the center of the pentagons. To obtain some additional information, the specimen was deformed in tension. The effect of the stress was first to cause the appearance of lines running from the centers to the apexes of the pentagons and then to tilt the five segments so formed. At a much greater stress, appreciable slip appeared on the grain; these effects can be seen in Fig. 2. The micrograph was taken at a fairly late stage in the deformation and the tilting is quite marked. The magnification is the same as in Fig. 1, and although some slip can be seen it could be observed better by varying the illumination and using higher magnifications. In each segment of the grain, slip (which takes place on the (111) planes) was parallel to the side of the pentagon in that segment. The marked changes in direction of slip from segment to segment seemed to be incompatible with the presence of a regular array of subgrains. These results suggest that some of the five segments were twins. If this is so, since the twinning plane in copper is the (111) plane, the radial lines must be traces of the (111) planes on the surface. From the symmetry of the striations about the radial lines, these planes must be almost perpendicular to the surface. The angle between <III>directions in face-centered-cubic copper is 70&apos;32&apos;. If, in Fig. 3, OAB (triangle 1) is taken as matrix and OA, OB are (111) planes viewed edge on, then AB is in the correct direction to be the trace of either of the other two (111) planes on the surface. If triangle 2 is the twin (about the (111) plane perpendicular to the surface and containing OB) of triangle 1, then once again it can be shown that all lines are traces of (111) planes. Similarly, triangle 3 is the twin of triangle 2, 4 of 3, and 5 of both 4 and 1. (The sequence is, of course, quite arbitrary.) However, if this were the case there would be a discrepancy of 7&apos;20&apos; to be accounted for. It is suggested that the faint curved line passing outward from the center of the pentagon represents either a low angle boundary or a sixth small twin. The slight step shown by the fringes at this line might be an indication that the former is the case. This explanation does not account for the coincidence of obtaining a grain whose surface must be so close to (110) and obtaining the curious twinning described previously; it would be of interest to find a specific mechanism for this.

Jan 1, 1958

By P. A. Toynbee, D. G. Wilson

The combustion performance of sub-bituminous slack coal is greatly improved by the removal of the smaller size fractions. Screening processes are not well suited to the size separation, at 1/8 in. or 1/16 in., with coals which are normally wet, and the use of an alternative size-separation device has been investigated. It is felt that this classifier might be applied equally well to other minerals in cases such as this, where precise size limits are not essential. Coal is dropped as a curtain onto a curved metal plate, shaped rather like a ski-jump. The smaller particles, slowed up in their free fall to the plate and also by contact with the metal, leave the plate with a lower horizontal velocity; they can be separated from the larger particles by virtue of their shorter trajectory. The principle of the classifier is obvious from the diagram (see Fig. 1) which shows also the positions, relative to the curved plate, of the point of coal feed and of the dividing plate which separates the streams of coal particles. The horizontal distance between the curved plate and the dividing plate is varied in the tests. It is designated in the general case, by X. Tests were carried out using slack coal with a free moisture content higher than that expected in any commercial operation. The results given in Table I. show the percentage recovery of upgraded product, and the cumulative screen analysis of both the upgraded and reject material, for three different positions of the dividing plate. The results show, for example, that the original coal can be upgraded, with a recovery of 80%, to reduce the minus 1/8 in. frac-

Jan 1, 1965

By Jean Herenguel

THE published work of Lacombe and Beaujard&apos; has demonstrated the interesting application of etch figures to the determination of crystal orientations in aluminum by a purely micrographic method. The geometry of these figures leaves no ambiguity and the method has the added advantage of being applicable to very small crystal units. These authors applied the technique to the study of high purity aluminum, and it has now been adopted buy Heren-guel and his collaborators to various researches on commercial aluminum, containing up to 1 pct Fe and Si. This must modify the opinion point,ed out by

Jan 1, 1953

By William L. Grube

PECIMEN preparation for electron metallography involves several steps, such as polishing, etching, replicating, mounting, and shadowing. Although each step must be done with care, the operation requiring the utmost attention is etching. Proper etching is important because the relief pattern developed on the surface of the specimen by the etchant, and reproduced as minute differences in thickness of the replica, determines entirely the amount of detail seen in the final micrograph. The characteristic colored stains, sometimes used in light metallography to simplify identification of certain microconstituents, cannot be tolerated because there is danger of introducing artifacts in the replicating operation. It is also quite difficult to remove plastic replicas from stained specimens. A suitable etchant for electron metallography must, therefore, in all cases exhibit a preferential attack upon each of the microconstituents present sufficient to result in a difference in surface elevation. When only two microconstituents are present, it is not too difficult to find a suitable etchant since their physical or chemical properties are generally sufficiently different to result in a marked difference in attack by the etchant. For example, picral (a saturated solution of picric acid in methanol used as an immersion etch) is a satisfactory etchant for the specimen shown in Fig. 1 consisting of iron carbide particles embedded in a ferrite matrix.&apos;

Jan 1, 1952

By Charles W. Oxford, R. L. Huntington

During the past 20 years (1932-1952), many condensate reservoirs have been discovered in the United States, particularly in the Gulf Coast region. Most of these reservoirs have been produced by a combination of gas cycling and slow pressure depletion in order to recover the liquefiable components from the single-phase fluids originally existing within the Although a record of the composition of the produced fluids has been kept on some of these reservoirs, very little laboratory work has been done on small scale replicas so as to obtain some idea of the effect of such variables as fluid flow withdrawal and cycling rates, pressure, temperature, percentage of liquid hydrocarbon and water saturation within the reservoir. Weinaug and Cordell have shown experimentally that condensates can be revaporized within a sand reservoir; however, they studied only the effect of fluid withdrawal rate. In this investigation the above mentioned variables were studied experimentally in small scale reservoirs both in the case of vaporization of condensate by batchwise pressure deple-

Jan 1, 1953