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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

By G. H. Miller

With the recent advances which have been made in science and technology and the increased use of mathematics in this area, the question of the best mathematics courses for a mining engineer to take is of major importance. The question becomes even more difficult to answer due to the recent increase in the number of different mathematics courses in the last two decades offered by the mathematics departments. Therefore, the National Study of Mathematics Requirements for Scientists and Engineers (NSMRSE) was designed to provide some answers to these questions. Approximately 10,000 scientists and engineers were selected for the Study, These individuals were placed in two categories: (1) The Awards Group, recipients of national honors or awards and those recommended by the members of the Board of Advisors as having national and international reputations in their areas of specialization and (2) The Abstracts Group, persons exceptionally productive in their research, based on the number of journal articles listed in the last five years in the Engineering Index, Scientific and Technological Aerospace Reports, Chemical Abstracts, Biological Abstracts, and the Physics Abstracts. The NSMRSE Course Recommendation Form and the Instruction and Course Content Sheet were constructed with the aid of the Board of Advisors and other consultants. For the Study, 40 courses were selected by the mathematical consultants. In order to make sure that the basic content of the mathematics courses was the same for all respondents, a brief resume of each of the 40 courses was given. The NSMRSE Course Recommendation Form consisted of seven sections. These sections were as follows: Section 1, 38 different specializations; Section 2, orientation of work (applied through theoretical); Section 3, highest degree obtained; Section 4, place of employment (academic, nonacademic); Section 5, administrative capacity (administrative or nonadministrative); Section 6, age groups (five-year intervals). Section 7 contained the 40 courses which were to be marked according to five categories: (1) Course Length, 3 to 36 weeks; (2) Applied-Theoretical Orientation, a five-point scale; (3) Course Level, freshman through graduate; (4) Knowledge of Course; and (5) Use of Course Content in Work. The Analysis The report of the data is based on the replies received from 44 mining engineers. This group was part of the Awards and Abstracts Group for all engineers. The resume of the recommended courses is reported in quintiles (upper fifth to lower fifth), since recommendations of this kind are not precise. The results of the Study are based on recommendations of the most active research men in engineering in the U.S. today; therefore, the reader should realize that these course recommendations represent an upper bound of mathematics requirements for the Ph.D. in both undergraduate and graduate work. Conclusions and Recommendations 1) Mining engineering students who plan to be active research specialists should take all those courses which are "very highly recommended" (80-10070) and "highly recommended" (60-79.9%). Those courses in the upper two quintiles and recommended by most mining engineers are: first-year calculus, third-semester calculus, elementary differential equations, applied statistics, and machine computation. Courses of "moderate recommendation" (40-59.9%) are: vectors, intermediate ordinary differential equations, the first course in partial differential equations, elementary probability, and linear programming. 2) The great majority of mining engineers indicated that they prefer a course which is concerned primarily with applications. Only the standard courses such as first-year college mathematics, calculus, differential equations, and advanced calculus received a recommendation for 50% theory and 50% practice. Therefore, all mathematics courses given to mining engineers should contain many applications and little theory. Engineers in both the applied and the combination (ap-plied-theoretical) groups indicated a definite need for applications in all courses. 3) In general, recommendations were for mathematics courses to be given for short intervals of time such as 3, 6, or 12 weeks. Only the standard courses mentioned previously received the usual one-semester or one-year recommendation. Therefore, it is of value to combine several related courses into a one or two-semester course so that the mining engineering student could acquire important mathematical knowledge at an early date in order to prepare him for his research. 4) There was little use for the newer courses in modern mathematics such as the functional analysis sequence, the modern algebra sequence, and the group theory sequence. In addition, there were uniformly very low recommendations (0-19.9%) for multilinear algebra, complex variables, mathematical logic, special functions, integral equations, approximation theory, analytic mechanics, integral transforms, and geometric algebra. Therefore, these courses should be given a low priority. 5a) Comparisons among mining engineers with different backgrounds showed that the combination ap-plied-theoretical group recommended more mathematics than the applied group. 5b) There was little difference in recommendations between the administrative group and the nonadminis-trative group. 5c) Analysis of age groups showed that those in the lower age groups gave significantly higher recommendations to courses such as the first course in partial dif-

Jan 1, 1971

By C. W. Spencer, J. Singer

A PARTIAL phase diagram for the As-Te system is given in Hansen.&apos; The only compound reported is As2Te3, melting at 362°C. Stoichiometric quantities of reagent-grade elements were reacted in evacuated quartz and directionally cooled. The resulting ingot consisted of very thin threadlike crystals from which only very small single-crystal fragments were isolated. A powder diffraction diagram disclosed nonisomorphism with the analogous V-VI compounds insofar as these have been reported; Sb2S3, As2S3, Bi,S,, and Bi2Te3 data in the ASTM index of powder patterns, together with the single-crystal data on Sb2Se3,2 were used for the com- parison with the observed spacings. Single-crystal data confirmed the uniqueness of the As2Te3 structure. Single-crystal Weissenberg diagrams have so far yielded the following data: As2Te3 is monoclinic, space group C-m (OkO data still lacking), a = 14.4A, b = 4.05A, C = 9.92A, ß = 97". The cell volume is about 5802. The set of isomorphous ortho-rhombic cells of Sb2Se3, Sb2S3, and Bi2S, are apparently related to As,Te, in having one lattice constant close to 4.0 and with cell volumes as large as 540A8. Assuming Z = 4 for As2Te3 also, the density is calculated as 6.1 which agrees well with a roughly determined value of 6.0. A complete structure analysis is under way.

Jan 1, 1956

By D. A. Vaughan

COMPOUNDS in the U-N system have received little attention since the work of Rundle, Baen-ziger, Wilson, and McDonald in 1948.&apos; They described the three nitrides UN2, U2,N2, and UN as the only phases in this system. The region between UN and U,N, was reported to consist of the two phases while the region between U,N, and UN, is a homogeneous solid solution in which the U,N3, structure transforms with increasing nitrogen content into the UN, structure. This report presents the results of an X-ray diffraction study of the phases present in the region of the diffusion gradient on uranium reacted with nitrogen at several temperatures between 500" and 915°C. Several samples of uranium used in U-N gas-metal reactions by Mallett and Gerds were available for X-ray diffraction study of phase composition through the diffusion gradient. X-ray diffraction data were obtained using filtered iron radiation at intervals through the diffusion layer of the several samples on filings or turnings at approximately 0.001 in. increments down to the base metal. Representative X-ray diffraction patterns from various layers through the case on uranium after nitriding at 850°C are shown in Fig. 1. These data show that three different phases are present in the

Jan 1, 1957

By J. S. Kasper, R. M. Waterstrat

IN view of the recent findings of a pronounced ordering of atoms in s phase alloys containing elements of the first long row of the periodic table (and including molybdenum),l it is of interest to resolve the question of ordering for s phases containing second and third-row elements. Examples of the latter have been provided recently by Greenfield and Beck2 and two of them, Re-Cr and Ru-Cr, would appear to be favorable for a study of ordering by X-ray diffraction methods because of the considerable differences in the scattering factors concerned. In addition, s phase is found to occur in the Os-Cr system, where the difference in scattering factors is even larger. Accordingly, X-ray powder intensities have been measured in an attempt to learn the nature of the ordering, if any, in these three v alloys. Since there is no reported work on intermediate phases in the Os-Cr system, an exploratory investigation was made in this system, and it was found that, in addition to the s phase, the phase with the A-15 or ß-W structure also occurs. Specimen Preparation—The alloys were prepared by compressing mixed powders of —200 mesh size and sintering in an atmosphere of pure dry hydrogen. All alloys were rapidly cooled from the annealing temperature to room temperature in a stream of cold dry hydrogen in a water-cooled chamber. Table I lists the sources and purities of the starting materials, as well as the details of processing for each of the alloys investigated. Intermediate Phases in the Os-Cr System—In the absence of information on intermediate phases in the Os-Cr system, it was suspected that this system would resemble that of Ru-Cr, where a s phase, RuCr2,2 and a phase with the A-15 structure, RuCr3,3,4 have been identified. Both these phases were found in the Os-Cr system and at compositions

Jan 1, 1958

By N. A. McKinnon, J. H. Auld, A. M. Marshall, R. A. Coyle

IN making a study of the slip deformation and strain hardening of single crystals of aluminum, it has been found that considerable information additional to that provided by the usual metal-lographic techniques can be obtained by the use of the microfocus X-ray method described by Schulz.1 This technique has been applied to crystals both in the state as-grown by the strain-anneal method and after they have been subjected to increasing amounts of plastic strain. Kelly and Wei" have recently reported the use of this method for a study of lineage structure in aluminum single crystals grown from the melt. The crystals, prepared from aluminum of 99.99 pct purity supplied by British Aluminium Co. Ltd., were grown in the form of flat tensile specimens with a gage section of 0.3 by 0.1 in. and a gage length of 2.3 in. The microfocus X-ray tube used provided a focus of approximately 50 half width. Examination of a large number of as-grown crystals showed no sign of any macroscopic defects in the majority of cases. However, occasionally crystals grown by the strain-anneal method did show defects similar in nature to those shown by Kelly and Wei to occur in crystals grown from the melt. In some other cases a more regular appearance of black and white lines, corresponding to valleys and ridges, respectively, in the lattice, was obtained, Fig. 1. This particular crystal was slightly deformed as the lines when present in the image of an as-grown crystal are only barely visible. The angle of tilt of the blocks is of the order of 3. It seems likely that these tilt boundaries arise during the growth of the crystal due to the specimen not being perfectly flat on the hearth of the furnace and straightening under its own weight at the elevated temperatures. For the deformation studies the crystals were strained in a Polanyi-type tensile machine. A typical photograph taken after 1.2 pct elongation of a single crystal oriented with its axis fairly close to the center of the stereographic triangle is given in Fig. 2. The reflection, which is from the (111) planes, is traversed by two systems of parallel lines. These have been identified as traces of the primary (111) slip plane and the (110) plane perpendicular to the primary slip direction. The latter lines correspond to kink bands which could not be detected by the ordinary techniques of

Jan 1, 1958

By E. P. Klier, V. Weiss

IN studies of the X-ray diffraction line geometry of iron with chromium radiation using techniques aimed at minimizing the background intensity, Kp and Ka emission satellites* were resolved with three techniques. These satellite lines are present with sufficient intensity to lead potentially to erroneous structure analysis, if not properly interpreted. The techniques used were: 1) film technique with un-filtered radiation and polycrystalline specimen, 2) film technique with unfiltered radiation and single crystal, and 3) counter technique with unfiltered radiation and single crystal. An example of results obtained with technique 1 is given in Fig. 1.

Jan 1, 1958

By J. H. Wernick, D. Dorsi, K. E. Benson

A LTHOUGH a considerable number of experi--ti mental investigations dealing with the roasting of sulfide minerals have been reported in the past,&apos;"" the behavior of the single roasting particle does not appear to have received the attention it perhaps deserves. This is understandable in that the natural sulfide counterpart of the slab or sheet of metal normally used in high temperature oxidation studies is difficult to obtain and prepare, and is, in most cases, virtually impossible to maintain in one piece at roasting temperatures. The employment, on the other hand, of static aggregations of small particles in masses great enough to permit evaluation of the roasting reactions by means of thermobalances or gas analyses introduces other complications, such as localized overheating, sintering, and variable gas-solid contact. In this investigation a compromise between the above extremes was attempted. Closely sized (e.g., 30 to 40 mesh) particles of natural sulfide minerals were isothermally roasted, out of contact with one another, in an air-swept system. The progress of the roasting reactions was followed by examination in polished section of the treated particles and by X-ray and chemical analysis of their residual sulfide kernels. In this way some conclusions respecting the mechanism of roasting reactions were drawn. Roasting Furnace—The vertical tube furnace used for roasting the sulfide particles had a heated zone 10 1/2 in. long in which four retractable light gage stainless steel trays were suspended. Each tray, and an accompanying baffle, was mounted on a 2 in. iength of 3/8 in. stainless steel tubing. These assemblies were axially suspended on a 30 in. length of in. stainless tubing, by means of which they could be lifted from the hot zone to a water-cooled brass chamber at the top of the furnace. Since each tray unit could slide freely on the 30 in. tube, any desired number of the trays could be retained in the cooling chamber by the manipulation of a horizontal plunger during a momentary withdrawal of the four trays from the hot zone. Although three heating coils, each equipped with variable external resistance, were employed, it was found impossible to avoid a drop of 10O to 15OC between the temperature at the top tray and that of the lower three. Consequently, only the bottom three trays were used for roasting. Temperature readings inside the furnace were made by means of a thermocouple inserted down the tray support tube at tray levels, and a separate thermocouple, inserted adjacent to the middle heating coil, was connected to a Micromax temperature control unit. Experimental Method—The sulfide minerals were obtained in a form as free as possible from gangue and contaminating sulfides, and were crushed and screened to the required particle size range. The tray assembly was kept inside the furnace during the heating-up period and, when a steady temperature had been reached, the trays were withdrawn. Each tray was sprinkled with from 200 to 500 mg of the sulfide grains, and the assembly was lowered into the furnace without delay in order to minimize the time required to achieve the operating temperature. The furnace top was then clamped into position and the thermocouple inserted down the center tube to the required level. It was found that, when this procedure was used, the trays achieved their former temperature within 2 min, after which time the flow of dry air was begun at a rate of 1 liter per min, and timing of the run was started. At the required intervals of time the trays were successively withdrawn from the hot zone and stored in the cooling chamber by means of the retention plunger. On completion of the run the treated particles were removed from the trays to be set aside for examination. The roasted particles were mounted in Lucite on a Buehler press operating at a temperature of 146°C

Jan 1, 1958

By T. D. Tiemann

Extraction of silica from the taconites of the Wisconsin Gogebic range by high temperature digestion in caustic solutions has been described.1,2 The ores consist essentially of hematite, goethite, and microcrystalline quartz, detailed descriptions of which appear in the literature.1,3 It is the purpose of this communication to describe some results obtained from a laboratory investigation of an alternative method, that of sintering the ore with sodium carbonate followed by water extraction of the sodium silicate produced. This is analogous to the Deville-Péchiney4,5 soda ash sinter process for the production of alumina from bauxites in which soluble sodium aluminates are formed. Raw mixes of the desired composition were prepared from 10.0 g minus 200 mesh samples of taconite and sintered in nickel crucibles in a muffle furnace controlled to within ±10°F of the operating temperatures. The resulting sinters were pulverized and then leached in distilled water with continuous agitation for 30 minutes at 95°C. The suspensions were vacuum filtered and the residues dried, ignited and weighed. Iron assays on the ignited samples were made by the standard dichromate procedure after dissolution in hydrochloric acid. The percentage of extraction was calculated from the iron assays by the relation:

Jan 1, 1964

By L. Wahl, M. Allard, B. Trentini

REMOVAL of sulfur in steelmaking is presently a problem of utmost importance as requirements on final sulfur contents in finished steels become increasingly strict. This is in spite of often increased sulfur contents in the fuels used during the different stages of steel processing. According to local conditions or current economic factors, sulfur can be removed during one or more of the processing operations; for instance, in a blast furnace operated under high temperatures and with a high slag basicity ratio and also by means of high inputs of manganese into the burden. These methods of proceeding are, however, expensive and in contradiction with the acid practice which is gradually being developed owing to the fact that it allows coke and lime savings and usually permits an increase of productivity. In the melting-shop, desulfurization can proceed in the open-hearth or electric furnace with one or several very basic slags, or with special prefused slags (Perrin process) mixed with steels poured from the open-hearth, electric furnace, or converter. Liquid pig iron has also been treated separately before being used in the melting shop, in order to reduce high sulfur contents. This external desul-furization has been developed in Europe for the basic Bessemer Thomas process, which is again in favor owing to the great flexibility of such installations and to the fact that the steel produced is not polluted by impurities coming from the scrap. Since the basic Bessemer process, as usually practiced, has a low desulfurizing power, external desulfurization is generally carried out in ladles by means of alkalies such as soda ash. This method, which has the advantage of being simple and costing little, has only a medium desulfurizing power, which implies the necessity for repeating the operation several times when a substantial amount of sulfur has to be removed or when very low sulfur contents are desired. Thermal losses are high and there is a considerable decrease in output. Moreover, the resulting fluid and corrosive slag, which is extremely difficult to eliminate, attacks the refractory linings of the mixers and steel furnaces. Therefore, it seems necessary to devise a simple method for external desulfurization which would not only remove substantial quantities of sulfur from the hot metal coming from an acid blast furnace, but which would also bring the sulfur contents down to the low level required in the making of high quality steel and iron. Principle of the Process In this paper a new method will be described for desulfurizing hot metal. It has been perfected by

Jan 1, 1958

By F. W. Luersson

High carbon, low phosphorus steel can now be made from pig iron containing 0.7 pct P or more, in a commercial sized open hearth furnace. No external heat is required for refining, and steel produced is identical with basic open hearth steel. THE classical Thomas process, which requires liquid pig iron containing over 11/2 pct P, yields a product relatively high in phosphorzs and nitrogen. Unless large quantities of recarburizers are added to the refined steel, the product is low in carbon content. Thus, the Thomas process is not well suited to American raw materials, and its product is often not acceptable according to the standards set by American industry. The shortcomings of the Thomas process have long been recognized; with the advent of low cost oxygen, studies were initiated to develop pneumatic processes which would conceivably overcome the inherent objections to Thomas steelmaking. Several such modified basic pneumatic processes have been tested experimentally in commercial trials during the past decade. Probably the most widely publicized of these developments has been the oxygen converter process as practiced in Austrial,2 and in Canada.8 n this process, oxygen is substituted for air and introduced above the liquid bath in order to increase the heat available to the metallurgical system. This avoids the need for high phosphorus raw materials and gives a product low in nitrogen. In this process, the phosphorus content in the final product depends, to a considerable extent, on the total amount of that element in the burden. The rotary furnace4 which is now in commercial operation at Domnarvet Steelworks, Sweden, is producing low phosphorus steel from iron containing 1.8 to 2 pct P. One or more early slags are removed and by this means high carbon steels of open hearth quality can be produced. At this stage of development there is some question as to the applicability of the rotary process to large heats. Another development has been the use of oxygen in combination with either steam6 or carbon dioxide yn the basic bessemer, thus avoiding the introduction of nitrogen gas into the refining system and giving a product relatively low in nitrogen content. A double slag process has been used in Europe7 in conjunction with a regular Thomas converter, by means of which it is possible to obtain a phosphorus content in the product approaching that obtained in basic open hearth steels. The Turbo-Hearth process:&apos; which uses the side blowing principle so as to produce low nitrogen steel from normal American pig irons, has been developed experimentally in this country. A process fitted to U. S. raw materials All of the preceding processes, with the exception of the rotary furnace, suffer from the common shortcoming that they cannot be adapted to the production of high-carbon, low-phosphorus steels unless large proportions of recarburizers are added. In 1947, a program was initiated by the Inland Steel Company1&apos; to study an oxygen steelmaking process specifically designed to utilize the full range of phosphorus analyses encountered in American pig irons and to give finai products with phosphorus and nitrogen contents comparable to steel produced by the basic open hearth process. Some of the objectives of the proposed process are: 1) the process should be able to accommodate molten pig iron conta;rl;rrg up to 1 pct P., 2) sne process should be subject to close control of carbon analysis, 3) the process should be capable of producing high carbon

Jan 1, 1958