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By T. S. Plaskett

A striated structure perpendicular to the growth axis was observed by the copper-decoration tech-nique in dislocation-free, .float-zoned silicon crystals. The striations, which were spaced about 100 p apart, fitted the relationship d = f/u , where d is the spacing, f is the growth rate, and u is the crystal rotation rate. Each stria was resolved into an UNDOPED silicon crystals pulled from quartz crucibles by the Czochralski technique usually exhibit a striated structure perpendicular to the growth axis.'-' This structure has been attributed to oxygen segregation, with the oxygen being introduced from the quartz crucible. If the crucible is rotated, the level of oxygen contamination has been reported as high as 10° atoms per cu cm.10 These striations are similar to solute striations commonly observed in doped Czochralski-grown crystals. The periodic nature of the striations is caused by a periodic variation in the growth rate",12 which is attributed mainly to thermal gradients in the melt.13 A finer striated structure14 attributed to constitutional supercooling is sometimes observed between the coarse striae. The oxygen striations have been observed by infrared transmission techniques,' by the copper-decoration technique,' by X-ray diffraction microscopy,6-8 and by 9 p absorption measurements3 on crystals pulled from the melt both with and without dislocations. In this investigation float-zoned dislocation-free crystals were examined by the copper-decoration technique. The level of oxygen for float-zone material is less than 1016 atoms per cu cm the lower limit of detection by 9 p absorption measurement. EXPERIMENTAL TECHNIQUE The crystals were grown by the float-zone process with the rf heating coil outside of the quartz envelope containing the silicon. All float zoning was done under an atmosphere of purified helium. The Dash technique15 was used to grow the crystal dislocation-free. This involves growing the crystal initially with a diameter between 2 and 3 mm and at array of starlike precipitates of copper. The strucLure was not .found at the surface tor a depth of about 1.5 mm, or in a region of similar width ahead of a dislocation network. The structure is postulated to consist of vacancy clusterings or dislocation loops. very rapid rates, about 20 mm per min, for a distance of about 3 cm. The diameter of the crystal is then increased to the diameter of the source of silicon, which in this case was about 19 mm. Because of the arrangement of the apparatus, the zone was passed downward rather than upward, contrary to the standard float-zoning practice. Also, the source was rotated rather than the seed. ziegler17 has made dislocation-free crystals by a similar technique but has passed the zone upwards. The starting material was zone-refined and had a p-type resistivity of 150 ohm-cm. The major impurity was boron; the total impurity excluding the boron was reported by the supplier (Dow-Corning) to be typically less than 2 x 1013 atoms per cu cm. The crystals were examined by the Dash copper-decoration technique18'19—a method in which about 10" atoms per cu cm of copper are diffused at a temperature between 900" and 1000°C into silicon which is then quenched to room temperature. On quenching, the copper precipitates on crystalline defects which are then visible when viewed by transmission infrared microscopy. The photomicrographs shown were taken either of the infrared image tube screen or directly on infrared film. All sections prior to decorating were chemically polished and, for some sections, given a sirtlZ0 dislocation etch-pit examination. After decorating, the samples were mechanically polished. RESULTS A photomicrograph, taken in transmission of a decorated cross section, is shown in Fig. 1. The portion of the section shown is near the surface of the crystal. The entire cross section showed no dislocation etch pits after being given a Sirtl etch treatment. It is seen that the copper precipitated randomly. Each precipitate, as has been reported by others, was found to have a starlike structure.

Jan 1, 1965

By M. J. Marcinkowski, E. N. Hopkins

An investigation has been made of the ß(fcc) — a(hexagonal) transformation which occurs in lanthanum using both electrical resistivity and transmission electron microscopy techniques. It has been shown that the ß phase can be retained below the transformation temperature by rapid quenching but that the sample immediately begins to transform to the a phase. The transformation is observed to nucleate in the vicinity of inclusions. Based on the above observations, a detailed model of the transformation has been advanced which involves the nucleation of an extrinsic stacking fault bounded by a pair of Shockley partial dislocations in the vicinity of some heterogeneity, i.e., an inclusion. The stress field of the resultant dislocation pair acts to nucleate extrinsic faults in adjacent planes and leads quite naturally to the B-a conversion with a minimum of strain energy induced in the crystal. LANTHANUM possesses an fcc structure ß) (8) upon cooling transforms to a hexagonal modification (a) in much the same way as cobalt. The one exception, however, is that the stacking sequence of the closest packed planes in a La is ABAC ABAC, and so forth,1 whereas in cobalt it is ABAB, and so forth, i.e., hep. Mainly on the basis of transmission electron microscopy techniques, there seems to be little doubt that the 0 — a transformation in cobalt involves a dislocation mechanism2 although its exact nature still remains obscure. Although the ß - a transformation in lanthanum is somewhat more complex than that occurring in cobalt, it was thought that its very uniqueness would be helpful in understanding fcc — hexagonal transformations in general. Such a general understanding of these transformations is important since they represent what are perhaps the simplest of the martensitic class of transformations. The experimental techniques used were those of electrical resistivity and transmission electron microscopy. EXPERIMENTAL PROCEDURE The lanthanum used in this investigation was prepared by the calcium reduction of lanthanum fluoride in a tantalum crucible under an argon atmosphere as described by Spedding et al. The residual calcium was removed by vacuum remelting in a tantalum container. Portions of the metal were then analyzed by emission spectroscopy as well as vacuum fusion. The amounts of the various impurities that were found are listed in Table I. A portion of the lanthanum ingot was swaged at room temperature into 0.030-in.-diam rod for the resistivity samples while the remainder was rolled into 0.010-in.-thick sheet for the transmission electron microscopy phase of this investigation. In order to eliminate the plastic deformation induced in the samples during fabrication, they were sealed in evacuated tantalum lined quartz capsules and annealed for 1 hr at 700° C. Specimen resistances were measured using the conventional "four-wire" technique described by MacDonald, 4 employing a type K-3 Universal Potentiometer and a standard 0.001-ohm resistor, both manufactured by Leeds and Northrup Co. By taking into account all of the possible errors in the apparatus, it was felt that the absolute resistivities of the approximately 0.87-in.-long specimens measured are reliable to 3 pct. Resistances from room temperature to 700°C were measured using a vacuum furnace. In order to avoid sample contamination by the thermocouple, chromel-alumel leads were spot-welded into a tantalum shield which in turn was welded to the lanthanum specimen. Resistances below room temperature were obtained by transferring the sample to a helium gas-filled quench tube and slowly dripping liquid nitrogen into a surrounding dewar flask. A steady reduction of temperature to about —190°C was completed in about 23 hr, and the resistances were measured at various temperature intervals. As will be shown shortly, rapid quenching from above about 350°C was sufficient to suppress the B -a transformation initially but subsequent annealing at lower temperatures leads to a partial ß --a conversion. To investigate this aspect of the transformation, the samples were suspended in the hot zone of a helium-filled furnace from which they could be rapidly dropped into the quench tube mentioned previously which was now

Jan 1, 1969

Discussion of the paper of DR. L. EDELEANU, presented at the Pittsburgh meeting, October, 1914, and printed in Bulletin No. 93, September, 1914, pp. 2313 to 2332. F. W. BUSHONG,* Pittsburgh, Pa.-This process of extraction is particularly advantageous in the case of Roumanian oil, on account of its high aromatic content. I have prepared a paper, which will appear probably next month in the Journal of Industrial and Engineering Chemistry, describing a series of two-degree fractions of oil from the Nowata field in Oklahoma. I have made extractions with liquid sulphur dioxide in accordance with Dr. Edeleanu's method, and found that the Oklahoma oils, for instance the kerosene fractions, are purified in this way, although the quantity taken out does not at all compare with that taken out of the Roumanian oil. I have made careful analyses of separate fractions, before and after extraction, and they show a very distinct fractional separation-. I like the distinction, brought out by Dr. Day in previous discussions, in regard to oils, rather than oil, and his beautiful illustration of fractionation. Just as fuller's earth, and other clays, will enable us to obtain lower-boiling fractional portions of the oils, and eventually retain a residuum which is hard to get rid of, or to remove, so there is an advantage to be gained by the use of a reagent which begins at the other end by taking out these last constituents first, namely, ozone. I have also analyzed the ozonides and they are derivatives of hydrocarbons very much poorer. in hydrogen than we have heretofore supposed. Similar results have been obtained with Roumanian, Russian, and Italian petroleums. Furthermore, I have prepared ozonides from a fraction of Oklahoma oils, both before and after ex-' traction with liquid sulphur dioxide, and found that the ozonide obtained from the extract is the same as that precipitated out of the original oils. In other words, the residual substance, which the fuller's earth retains, is the one first thrown down by the use of ozone, but it may also be extracted by liquid sulphur dioxide- and be thus separated in apparently unaltered condition. The analysis of this extract corresponds to the formula C15H20, which is surprising, since it is lower in hydrogen content than we have been in the habit of considering among the constituents of our oils. The extract was probably contaminated with other hydro-carbons, but I think it is unquestionable that we must look for hydro-carbons in petroleum which correspond to a formula at least -as low in hydrogen as C15H2o, and possibly even as low as C15H16.

Jan 4, 1915

By S. Feuerstein, J. M. Galligan

SURFACE effects in the deformation of metal single crystals have been noted by a variety of workers.&apos; A large majority of these experiments have used surface roughening or a second chemical constituent at the surface. We performed the following experiment to see how the presence of a fine polycrystalline layer influenced the stress-strain behavior of single crystals of zinc. Spherical single crystals oriented for single slip were acid-machined into cylindrical dumbbell-shape shear specimens having a gage length of 3.2 mm and a cross section of 20 sq mm. The crystals were then deformed varying amounts at the surface of the gage section with emery paper. Following this treatment, the crystals were heated for approximately 8 hr at 200°C. This resulted in a polycrystalline surface layer, with an observed grain size of approximately 1/10 mm in diameter. Deformation of these crystals was undertaken at 78°K in pure shear, the shear direction <1120> lying in the basal plane. The deformation apparatus has been described elsewhere.2 The presence of a polycrystalline layer markedly raises the first observed plastic deformation, as can be seen from Fig. 1. This yield stress is then followed by a region of low work hardening comparable to that observed in shear tests on similar untreated zinc single crystals. However, the extent of easy glide is quite seriously curtailed, and is followed by a more rapid increase in work hardening, reminiscent of Stage II observed in the deformation of fcc crystals. The higher yield can probably be attributed to the difficulty of penetrating the grain boundaries by dis locations from sources interior to the boundaries. If we associate this yield stress with this breakthrough, then we might expect that more dislocations would be trapped in the crystal than is normally the case. If there is an increased density of trapped dislocations, this could lead to an increase in the amount of trapping with increasing strain, giving a larger strain hardening in the crystal. Although other explanations can be given, it is quite tempting to characterize the region of increased work hardening as a manifestation of Stage II-type deformation. This seems reasonable if the polycrystalline layer is quite efficient in holding up a large number of dislocations. In zinc crystals, since it is well-known that the slip distance can be as large as the specimen dimensions, one would only expect to entrap a large number of dislocation with very large crystals or by applying surface layers. If this interpretation of increased strain hardening is correct, it might present a method of studying Stage II in single crystals of zinc. This research was supported, in part, by the Office of Naval Research (1959). The encouragement and stimulation given by Professor E. R. Parker is gratefully acknowledged.

Jan 1, 1965

By Tracy C. Jarrett

In 14-karat gold alloys, as in 10-karat gold alloys,3 the addition of such metals as zinc, nickel, copper and silver produces a wide range of physical and chemical properties such as color, hardness, corrosion resistance and melting points. These important factors made gold alloys desirable in the optical work and for jewelry. In 14-karat gold alloys, as well as in 10-karat or 12-karat, it is possible to have two golds of the same color, one of which will corrode more than the other, although it may be harder. Some of these alloys have been investigated by F. E. Carter,&apos; E. M. Wise,= and L. Sterner Rainer.4 In this group of alloys the gold content of 58.3 per cent (14-karat) was held constant, while the copper varied from 36 to 24 per cent. The balance of the alloy consisted of one, two, or three of the metals silver, zinc, and nickel. All the alloys were melted in an induction furnace and cast into an ingot that measured 3 by 1/4 by 3/4 in. The method of determining the melting points, color determinations and acid test have been discussed in previous papers by the author.2, 3 It is necessary to use small test bars (Fig. I). The tensile bars were annealed at 1300oF. for 20 min. and then air-cooled. There being a very marked drop when the yield point was reached, "the drop of the beam" method was used in determining the yield point. Alloys Gold-copper.zilzc A~loys.—Gold-copper-zinc alloys melt, cast, and labricate easily. The low melting points, however, limit their use to some extent. The physical properties of these alloys are not entirely satisfactory. When the ultimate strength is satisfactory, the elongation and reduction of area are too low (Table I). Gold-copper-sinr-nickel A lloys.—In this group of alloys, in which zinc and nickel replace copper in approximately equal parts (Table I), the yield point, hardness, and ultimate strength increase with the increase of zinc and nickel content, while the reduction of area and elongation decrease. The physical properties are desirable, particularly of the white gold alloys. The alloys of this group are not difficult to cast and fabricate, and most of these colors could be used commercially. Gold-copper-nickel A lloys.—Gold-copper-nickel alloys are similar to the gold-copper-zinc and the gold-copper-zinc-nickel alloys. They do, however, possess high yield point, ultimate strength and hardness, somewhat higher than those of the other two groups mentioned (Table I). The difficulty with these alloys is that they fire-crack readily and heavy rolling is necessary between annealings. Being hard to fabricate, many

Jan 1, 1941

By Tracy C. Jarrett

In 14-karat gold alloys, as in 10-karat gold alloys,3 the addition of such metals as zinc, nickel, copper and silver produces a wide range of physical and chemical properties such as color, hardness, corrosion resistance and melting points. These important factors made gold alloys desirable in the optical work and for jewelry. In 14-karat gold alloys, as well as in 10-karat or 12-karat, it is possible to have two golds of the same color, one of which will corrode more than the other, although it may be harder. Some of these alloys have been investigated by F. E. Carter,&apos; E. M. Wise,= and L. Sterner Rainer.4 In this group of alloys the gold content of 58.3 per cent (14-karat) was held constant, while the copper varied from 36 to 24 per cent. The balance of the alloy consisted of one, two, or three of the metals silver, zinc, and nickel. All the alloys were melted in an induction furnace and cast into an ingot that measured 3 by 1/4 by 3/4 in. The method of determining the melting points, color determinations and acid test have been discussed in previous papers by the author.2, 3 It is necessary to use small test bars (Fig. I). The tensile bars were annealed at 1300oF. for 20 min. and then air-cooled. There being a very marked drop when the yield point was reached, "the drop of the beam" method was used in determining the yield point. Alloys Gold-copper.zilzc A~loys.—Gold-copper-zinc alloys melt, cast, and labricate easily. The low melting points, however, limit their use to some extent. The physical properties of these alloys are not entirely satisfactory. When the ultimate strength is satisfactory, the elongation and reduction of area are too low (Table I). Gold-copper-sinr-nickel A lloys.—In this group of alloys, in which zinc and nickel replace copper in approximately equal parts (Table I), the yield point, hardness, and ultimate strength increase with the increase of zinc and nickel content, while the reduction of area and elongation decrease. The physical properties are desirable, particularly of the white gold alloys. The alloys of this group are not difficult to cast and fabricate, and most of these colors could be used commercially. Gold-copper-nickel A lloys.—Gold-copper-nickel alloys are similar to the gold-copper-zinc and the gold-copper-zinc-nickel alloys. They do, however, possess high yield point, ultimate strength and hardness, somewhat higher than those of the other two groups mentioned (Table I). The difficulty with these alloys is that they fire-crack readily and heavy rolling is necessary between annealings. Being hard to fabricate, many

Jan 1, 1941

By W. A. Mudge

This discussion will be limited to malleable, commercially pure nickel and some high-nickel alloys, containing more than 50 per cent of nickel, which are produced by The International Nickel Company, Inc. at its Huntington works, West Virginia, from electrolytic nickel or from a nickel-copper sulphide matte. The principal sources of nickel are sulphides of nickel, copper and iron, which are found in the large deposit of pyrrhotite-pentlandite-chalcopyrite ores in the Sudbury area of Ontario, Canada. Pentlandite, a complex nickel-iron sulphide, is the nickel carrier. These ores are concentrated, roasted, and smelted to remove considerable iron and sulphur and to produce a nickel-copper sulphide matte. Separation of the component sulphides of this matte, followed by electrolytic refining, results in the production of electrolytic nickel and electrolytic copper; direct refining of a selected portion of the matte gives the nickel-copper alloy, Monel. FUNDAMENTAL OPERATIONS Melting of the metallic materials is done in natural gas-fired, acid furnaces of the open-hearth, or reverberatory, type, having capacities of 6 to 20 tons; in three-phase, basic, electric-arc furnaces, having capacities of 7 to 20 tons; and in basic, high-frequency induction furnaces having capacities of ½ to 3 tons. Malleable, commercially pure nickel is melted in the acid open-hearth furnace. The charge is sulphur-free, electrolytic nickel, containing 99.9 per cent nickel* and clean mill scrap. Monel, containing approximately two thirds nickel and one third copper, is produced by roasting the nickel-copper sulphide matte to an oxide, smelting the oxide with charcoal in a 20-ton, acid open-hearth furnace, adding clean mill scrap, duplexing to a 20-ton, basic, electric-arc furnace, and refining in this furnace with a lime-fluorspar, carbide slag. Inconel, containing nickel, 80 per cent; chromium, 14 and iron, 6, is melted in the 7-ton electric-arc furnace or the 3-ton induction furnace. The charge is electrolytic nickel, ferrochromium and clean mill scrap. These are the fundamental operations. High-nickel alloys are produced from one of these three materials by additions of suitable amounts of manganese, aluminum, silicon or copper. For example, the age-hardenable alloy, K Monel, is produced from Monel by the addition of approximately 3 per cent of aluminum, and D nickel is produced from nickel by the addition of approximately 4.5 per cent of metallic manganese. For conversion to rods, bars, sheet, strip, tubing and wire forms, by hot-working and cold-working operations, the molten materials are teemed into ingots ranging in size from 14 by 14 by 60 in., 3300 lb., to 36 by 36 by 48 in., 18,000 lb. All ingots are overhauled mechanically before hot working.

Jan 1, 1946

By M. T. Worley

This paper reports investigative work conducted to develop a method of estimating the groundwater influx from a homogeneous permeable formation into a vertical mine shaft during sinking. A method of analysis was developed using data obtained from pumping tests and a modification of the Theis non-equilibrium interpretation technique. Excess influx of groundwater into mine shafts has long been one of the more important problems encountered in the development of a mining property. Much work has been done on methods of preventing such influx and on pumping schemes to control inflow if preventive measures fail. The fundamental aspects of the problem, on the other hand, seem to have been neglected. The purpose of this paper is to review the fundamentals of groundwater flow and to propose a rapid method of analyzing hydrologic data in order to estimate influx from a homogeneous permeable formation into a mine shaft. Such an estimate of the quantity of water to be encountered is of value in planning grouting, pumping and other programs designed to control that influx. It is emphasized that the proposed method of analysis should be regarded only as a tool to be used in evaluating the problem before investing the capital necessary to begin development of a property. FUNDAMENTALS OF GROUNDWATER FLOW In order to effectively approach the problem of estimating influx into a mine shaft, a knowledge of the fundamentals of fluid flow through a porous medium is necessary. Darcy, in 1856, developed an empirical relationship to explain the flow of water through sand filters. This relationship V = k (dh/dl), is the basis for all other flow formulae. It has been shown that Darcy&apos;s relation is a solution of the Laplace equation and thus is analagous to other natural phenomena such as heat flow. Theis, using the analogy of heat flow by conduction, developed an expression for determining the transient or time-dependent groundwater flow through a homogeneous, isotropic medium. The resulting equation Was also derived by Jacob using hydrologic considerations alone.&apos; The individual terms in the equation are described in Table I. It is important to understand the assumptions upon which this equation is based. 1) The medium through which the fluid flows is infinite in areal extent, homogeneous and isotropic. 2) The well into which the fluid discharges completely penetrates the medium. 3) The characteristics of the medium remain constant at all times. 4) The initial pressure surface is horizontal. 5) The confining media are impervious and horizontal. 6) Fluid is removed from storage instantaneously by a decline in pressure. 7) The diameter of the discharge well is infinitesimal with respect to the drainage radius of the medium.

Jan 1, 1962

By Charles H. Morgan

THE process of wire drawing depends upon the property which certain metals possess, termed ductility, &apos;which is defined in Brande&apos;s Dictionary of Science as a property in consequence of which metals may be drawn out at length without interrupting the continuity of their constituent parts. As defined by M. Tresca, it is the property of flowing when subjected to pressure, and is termed by him the "flow of solids," in his paper, read before the Academy of Sciences in Paris, November, 1865 * In the simple language of the wire shop, it is that quality in certain metals that permit, them to be drawn (or stretched) out through a tapering, hole in a metal block or die, the die being more dense and harder than the metal to be reduced. It is a fact well known to those skilled in the art, that to succeed in drawing iron or steel wire, it is of the utmost importance to have thorough lubrication, as a lack of it would caws abrasion of the wire, or of the walls of the tapering hole in the die or plate, and quickly put an end to the operation. In drawing coarse or large sizes of wire, say 2/10 inch diameter, the pressure upon the sides of the tapering hole, where the wire comes in contact with the die, is so great that an ordinary lubricant is squeezed out when the usual reductions in size are made, and abrasion takes place. In order to meet this difficulty, and secure proper lubrication, it has been&apos; a common practice for years to apply a paste made of rye or wheaten flour, or lime, to the surface of the wire to be drawn, and when the paste is dry, to smear the wire with tallow or grease; the wire is then ready to be drawn, the dried paste serving to prevent the lubricant from being pressed out in the. process. Some years since, when Bessemer metal came largely into use as material for wire, "the writer found that its drawing required so much more power than iron wire, that he was led to institute a series of trials to ascertain the difference in power required. It was found that Bessemer wire required from 100 to 200 per cent. more power to make the same reduction in sizes than soft iron wire, the difference depending upon the amount of carbon and other chemical constitu- * Interesting experiments in the flow of metals have been made, by Messrs. Hoopes Townsend, of Philadelphia, in cold-punching iron, published and illustrated in the Journal of the Franklin Institute, of March, 1878, by Mr. David Townsend.

Jan 1, 1881

By E. C. Houston, H. S. Rankin

Olivine is considered a valuable potential source of metallic magnesium in the chloride electrolytic process. Treatment of olivine with hydrochloric acid can be carried out under conditions that prevent the formation of gelatinous silicic acid, which would inhibit the reaction by forming a covering around the ore particles. It is our hypothesis that the formation of gelatinous silicic acid is avoided by the dehydrating action of the magnesium chloride, which takes up water to form a series of hydrates and leaves the silicic acid in granular condition. Leaching serves to separate the magnesium chloride from the silicic acid and unattacked ore, which can be treated with fresh acid in successive steps until extraction is essentially complete. The leach solution can be i purified by the addition of caustic magnesia and the precipitated impurities removed by decantation or filtration. The resulting magnesium chloride contains: Fe, less than 0.001 Per cent; Mn, 0.012 ; per cent; Ni, none. Chlorination† of olivine has two major defects: (1) a large part of the chlorine goes to form silicon and iron chlorides, (2) the anhydrous magnesium chloride is held by absorption in the finely divided silica. SupplY It is well known that olivine, a silicate of magnesium and iron, is present in large amounts in several localities in the United States. The largest deposits occur in the southeast and on the Pacific Coast.&apos; The southeastern deposits were surveyed by Lewis2 in 1896 and by Hunter3 in the period 1933-1940 It is estimated that high-grade olivine, conveniently located with regard to transportation and power, is present in excess of 230 million tons above local drainage level in western North Carolina and north Georgia. Previous Technical Work In the past few years, olivine has attracted considerable attention in the refractory field. In the chemical processing industry, however, it has long been thought axiomatic that the cost of processing silicates is an economic barrier to their utilization, especially where more reactive minerals, such as carbonates, oxides or salts, are available. This attitude is not entirely justified in connection with olivine. unlike most silicates, olivine is readily attacked by acids, chlorine and other reagents without resorting to fusion to break down the silicate structure. Olivine has been suggested as a raw material for making epsom salt by roasting with pyrites.4 Other processes include acid treatment6 and digestion with calcium chloride.6 Recently a small plant was built near Webster, N. C., for making epsom salt from olivine by treatment with sulphuric acid. This plant is now in commercial operation, producing approximately two tons per day. Olivine is also receiving attention from the fertilizer industry as an inexpensive source of soluble magnesium.

Jan 1, 1942

By F. C. von der Weid

The mining district of Sao Fidelis, in the northern part of the State of Rio de Janeiro, is situated on the Paraiba River, where it crosses the Serra do Mar (Mountain of the Sea), in the center of a mountainous country having numerous graphitic outcrops. For a long time, these outcrops were irregularly explored by local people, who had little means and no technical advice. A few years ago, the Cia. Brasileira de Minerasgo de Grafite took over the control of some of the more important outcrops and entrusted to me the task of studying the ores and establishing a flowsheet for a pilot plant to be situated in São Fidelis—the ore to be concentrated being mostly of a very high grade. Mineralization and Ores The rocks of the district are mostly gneiss and crystalline schists, with occasional interstratification of dolomitic limestone belonging to the Archean Brazilian Fundamental Complex. The general direction of the beds is roughly between 60" and 80°E., with variable dip, generally nearly vertical. Mostly, direction and dip of the graphitic outcrops is concordant with the embanking gneisses or schists. These outcrops seem to be aligned in two or three parallel zones (Pádua, São Fidelis, Mac- abu), the Sao Fidelis zone being the best known and the most important to date. Two outcrops of the São Fidelis zone, Saudade and Sao Benedito, are now being exploited. Mining has been carried out, so far, on a small scale. The mineralization consists of a vein of nearly massive graphite in a very compact, partially granitized gneiss, with vertical dip. The vein is most irregular, with nests and lenses irregularly distributed along the fracture plane. The ore consists chiefly (particularly in Sao Benedito) of massive graphite appearing and disappearing along the main direction of the vein, forming a succession of irregular lenses in a sort of rosary design. The average width is more or less one foot, with variations from zero to 6 feet. The lode minerals are quartz, a little feldspar and garnet (the latter having its origin perhaps in the embedding gneisses), with rare ferruginous clays on the outcrops. In Saudade a little pyrite, pyrrhotite and chalcopyrite is found occasionally, as well as a carbonaceous mineral, very light, black and shiny, with conchoidal fracture, looking like a sort of jet. The composition of this mineral has not yet been established, but it seems to be very complex. The mineralization seems to be hydro-thermal at a rather low temperature, perhaps mesothermal. The paragenesis, according to samples from Saudade, seems to be as follows, the earlier minerals being listed first: pyrrhotite, pyrite, chalcopyrite, with quartz concomitant to the three and graphite formed later. Age of the mineralization is still uncertain, owing to the very in-

Jan 1, 1948

By F. C. von der Weid

The mining district of Sao Fidelis, in the northern part of the State of Rio de Janeiro, is situated on the Paraiba River, where it crosses the Serra do Mar (Mountain of the Sea), in the center of a mountainous country having numerous graphitic outcrops. For a long time, these outcrops were irregularly explored by local people, who had little means and no technical advice. A few years ago, the Cia. Brasileira de Mineracao de Grafite took over the control of some of the more important outcrops and entrusted to me the task of studying the ores and establishing a flowsheet for a pilot plant to be situated in Sao Fidelis—the ore to be concentrated being mostly of a very high grade. Mineralization and Ores The rocks of the district are mostly gneiss and crystalline schists, with occasional interstratification of dolomitic limestone belonging to the Archean Brazilian Fundamental Complex. The general direction of the beds is roughly between 60&apos; and 80°E., with variable dip, generally nearly vertical. Mostly, direction and dip of the graphitic outcrops is concordant with the embanking gneisses or schists. These outcrops seem to be aligned in two or three parallel zones (Padua, Sao Fidelis, Mac- abu), the Sao Fidelis zone being the best known and the most important to date. Two outcrops of the Silo Fidelis zone, Saudade and Sao Benedito, are now being exploited. Mining has beer] carried out, so far, on a small scale. The mineralization consists of a vein of nearly massive graphite in a very compact, partially granitized gneiss, with vertical dip. The vein is most irregular, nith nests and lenses irregularly distributed along the fracture plane. The ore consists chiefly (particularly in Sao Benedito) of massive graphite appearing and disappearing along the main direction of the vein, forming a succession of irregular lenses in a sort of rosary design. The average width is more or less one foot, with variations from zero to 6 feet. The lode minerals are quartz, a little feldspar and garnet (the latter having its origin perhaps in the embedding gneisses), with rare ferruginous clays on the outcrops. In Saudade a little pyrite, pyrrhotite and chalcopyrite is found occasionally, as well as a carbonaceous mineral, very light, black and shiny, with conchoidal fracture, looking like a sort of jet. The composition of this mineral has not yet been established, but it seems to be very complex. The mineralization seems to be hydro-thermal at a rather low temperature, perhaps mesothermal. The paragenesis, according to samples from Saudade, seems to be as follows, the earlier minerals being listed first: pyrrhotite, pyrite, chalcopyrite, with quartz concomitant to the three and graphite formed later. Age of the mineralization is still uncertain, owing to the very in-

Jan 1, 1947

By C. E. Stafford

and tougher, and will carry double the tonnage of any of Dr. Dud ley&apos;s soft mils. C. E. Stafford, Steelton, Pa.: I must confess my high ap preciation of Dr. Dadlq&apos;s conscientious and painstaking work, and of his scientific methds in obtaining the data; but with his method of handling these results and with his conclusions drawn therefrom 1 canuot agree. The reasons for this difference of opinion I will endeavor to explain. It is apparent on inspecting his Plates 6 and 7 that the majority of the slower-wearing rails are from the north track, and generally have a longer time of service, a greater average tonnage per rail, and a smaller avernge tonnage per year per rail than the faster wearing, the majority of which are from the south track, and gener ally have a shorter time of service, a smaller average tonnage per rail, and a greater average tonnage per year per rail. Have these facts any significance Have these different of conditions to which they are subjected any baring on the relative wearing capacity of these rails I venture to say they have. I think, after a study of Table I (page 676), (an arrangement of linee 17 and 18 of Plate a), in connection with Plates 6 and 7, we will find that the slower wear of the 32 best rails is only partly due to qualities inherent in the rails themselves, but is principally due to external conditions favorable to slower wear. In regard to the north and south track, we know that over the rsoiith track come the loaded cam from the West, and that over the north track these cars return, most of them, empty. It is evident that this means for the north track a less average tonirage per rail per year; or, in other words, a lower wheel tonnage. When the load per wheel is less, the resistance and consequently the wear must, necessarily, be less, other things being equal. Time of service, alee, has an important bearing on the question in hand. It has been only within the last five or six years, as Dr. Dudley has pointed out, that the roadbed of the Pennsylvania Rail road has reached its present admirable condition. Before this time the njadbrd was more elastic, more yielding (and probably not uni tbrmly so) than at present. These circumstalices might cause a sofier rail to be more durable than a harder one, owing to the fact that it ulonId yield rnore or less to the bending force of the passing load and would thus get a bearing on each cross-tie. The harder rail, on the other hatid, being stiffer and more. unyielding, would not

Jan 1, 1881

By F. C. von der Weid

The mining district of Sao Fidelis, in the northern part of the State of Rio de Janeiro, is situated on the Paraiba River, where it crosses the Serra do Mar (Mountain of the Sea), in the center of a mountainous country having numerous graphitic outcrops. For a long time, these outcrops were irregularly explored by local people, who had little means and no technical advice. A few years ago, the Cia. Brasileira de Mineracao de Grafite took over the control of some of the more important outcrops and entrusted to me the task of studying the ores and establishing a flowsheet for a pilot plant to be situated in Sao Fidelis—the ore to be concentrated being mostly of a very high grade. Mineralization and Ores The rocks of the district are mostly gneiss and crystalline schists, with occasional interstratification of dolomitic limestone belonging to the Archean Brazilian Fundamental Complex. The general direction of the beds is roughly between 60&apos; and 80°E., with variable dip, generally nearly vertical. Mostly, direction and dip of the graphitic outcrops is concordant with the embanking gneisses or schists. These outcrops seem to be aligned in two or three parallel zones (Padua, Sao Fidelis, Mac- abu), the Sao Fidelis zone being the best known and the most important to date. Two outcrops of the Silo Fidelis zone, Saudade and Sao Benedito, are now being exploited. Mining has beer] carried out, so far, on a small scale. The mineralization consists of a vein of nearly massive graphite in a very compact, partially granitized gneiss, with vertical dip. The vein is most irregular, nith nests and lenses irregularly distributed along the fracture plane. The ore consists chiefly (particularly in Sao Benedito) of massive graphite appearing and disappearing along the main direction of the vein, forming a succession of irregular lenses in a sort of rosary design. The average width is more or less one foot, with variations from zero to 6 feet. The lode minerals are quartz, a little feldspar and garnet (the latter having its origin perhaps in the embedding gneisses), with rare ferruginous clays on the outcrops. In Saudade a little pyrite, pyrrhotite and chalcopyrite is found occasionally, as well as a carbonaceous mineral, very light, black and shiny, with conchoidal fracture, looking like a sort of jet. The composition of this mineral has not yet been established, but it seems to be very complex. The mineralization seems to be hydro-thermal at a rather low temperature, perhaps mesothermal. The paragenesis, according to samples from Saudade, seems to be as follows, the earlier minerals being listed first: pyrrhotite, pyrite, chalcopyrite, with quartz concomitant to the three and graphite formed later. Age of the mineralization is still uncertain, owing to the very in-

Jan 1, 1947

By H. S. Rankin, E. C. Houston

Olivine is considered a valuable potential source of metallic magnesium in the chloride electrolytic process. Treatment of olivine with hydrochloric acid can be carried out under conditions that prevent the formation of gelatinous silicic acid, which would inhibit the reaction by forming a covering around the ore particles. It is our hypothesis that the formation of gelatinous silicic acid is avoided by the dehydrating action of the magnesium chloride, which takes up water to form a series of hydrates and leaves the silicic acid in granular condition. Leaching serves to separate the magnesium chloride from the silicic acid and unattacked ore, which can be treated with fresh acid in successive steps until extraction is essentially complete. The leach solution can be i purified by the addition of caustic magnesia and the precipitated impurities removed by decantation or filtration. The resulting magnesium chloride contains: Fe, less than 0.001 Per cent; Mn, 0.012 ; per cent; Ni, none. Chlorination† of olivine has two major defects: (1) a large part of the chlorine goes to form silicon and iron chlorides, (2) the anhydrous magnesium chloride is held by absorption in the finely divided silica. SupplY It is well known that olivine, a silicate of magnesium and iron, is present in large amounts in several localities in the United States. The largest deposits occur in the southeast and on the Pacific Coast.&apos; The southeastern deposits were surveyed by Lewis2 in 1896 and by Hunter3 in the period 1933-1940 It is estimated that high-grade olivine, conveniently located with regard to transportation and power, is present in excess of 230 million tons above local drainage level in western North Carolina and north Georgia. Previous Technical Work In the past few years, olivine has attracted considerable attention in the refractory field. In the chemical processing industry, however, it has long been thought axiomatic that the cost of processing silicates is an economic barrier to their utilization, especially where more reactive minerals, such as carbonates, oxides or salts, are available. This attitude is not entirely justified in connection with olivine. unlike most silicates, olivine is readily attacked by acids, chlorine and other reagents without resorting to fusion to break down the silicate structure. Olivine has been suggested as a raw material for making epsom salt by roasting with pyrites.4 Other processes include acid treatment6 and digestion with calcium chloride.6 Recently a small plant was built near Webster, N. C., for making epsom salt from olivine by treatment with sulphuric acid. This plant is now in commercial operation, producing approximately two tons per day. Olivine is also receiving attention from the fertilizer industry as an inexpensive source of soluble magnesium.

Jan 1, 1942

By F. C. von der Weid

The mining district of Sao Fidelis, in the northern part of the State of Rio de Janeiro, is situated on the Paraiba River, where it crosses the Serra do Mar (Mountain of the Sea), in the center of a mountainous country having numerous graphitic outcrops. For a long time, these outcrops were irregularly explored by local people, who had little means and no technical advice. A few years ago, the Cia. Brasileira de Minerasgo de Grafite took over the control of some of the more important outcrops and entrusted to me the task of studying the ores and establishing a flowsheet for a pilot plant to be situated in São Fidelis—the ore to be concentrated being mostly of a very high grade. Mineralization and Ores The rocks of the district are mostly gneiss and crystalline schists, with occasional interstratification of dolomitic limestone belonging to the Archean Brazilian Fundamental Complex. The general direction of the beds is roughly between 60" and 80°E., with variable dip, generally nearly vertical. Mostly, direction and dip of the graphitic outcrops is concordant with the embanking gneisses or schists. These outcrops seem to be aligned in two or three parallel zones (Pádua, São Fidelis, Mac- abu), the Sao Fidelis zone being the best known and the most important to date. Two outcrops of the São Fidelis zone, Saudade and Sao Benedito, are now being exploited. Mining has been carried out, so far, on a small scale. The mineralization consists of a vein of nearly massive graphite in a very compact, partially granitized gneiss, with vertical dip. The vein is most irregular, with nests and lenses irregularly distributed along the fracture plane. The ore consists chiefly (particularly in Sao Benedito) of massive graphite appearing and disappearing along the main direction of the vein, forming a succession of irregular lenses in a sort of rosary design. The average width is more or less one foot, with variations from zero to 6 feet. The lode minerals are quartz, a little feldspar and garnet (the latter having its origin perhaps in the embedding gneisses), with rare ferruginous clays on the outcrops. In Saudade a little pyrite, pyrrhotite and chalcopyrite is found occasionally, as well as a carbonaceous mineral, very light, black and shiny, with conchoidal fracture, looking like a sort of jet. The composition of this mineral has not yet been established, but it seems to be very complex. The mineralization seems to be hydro-thermal at a rather low temperature, perhaps mesothermal. The paragenesis, according to samples from Saudade, seems to be as follows, the earlier minerals being listed first: pyrrhotite, pyrite, chalcopyrite, with quartz concomitant to the three and graphite formed later. Age of the mineralization is still uncertain, owing to the very in-

Jan 1, 1948

By George L. Reiter, George B. Clark

Commercial strip mining of coal was first begun in the state of Illinois in 1911.l The annual tonnage of coal produced from coal strip mines in the state was very small until 1924, when the strip mines shipped 1.68 pct of the total state shipping mine tonnage. Since then, strip mines have gradually come into their own by producing a sizable percentage of the coal produced in the state. Table 1 shows the coal tonnage shipped from both underground and strip coal mines in the state of Illinois for selected years. The table illustrates the major role that strip mines play in the state&apos;s coal industry. Today, strip mining is generally conducted in areas where the coal seams lie so close to the surface of earth that a stripping method of mining the coal seam is cheaper than an underground method. Strip mining not only recovers 100 pct of the coal deposit, but may also be used as a method of mining large acreages of coal abandoned by the closing of underground mines. Open cut or strip mining is a very highly mechanized method of producing coal and is carried on in three distinct and separate operations. The first of these is uncovering or exposing the coal seam so that the coal is made available for mining. The second operation is that of actually mining the coal. The third operation is the washing, crushing and grading of the coal according to the producer&apos;s market. Description of Shovel The Marion 5560 power shovel is used in the first of these three operations. The large electric-powered shovel works forward and back across the coal deposits, removing the overburden of dirt, rock, and clay in successive cuts of 30 to 60 ft deep and 40 to 80 ft wide. The shovel has a maximum cutting height of 95 ft, but around 60 ft is considered to be the maximum economical cutting height by the operators. The smaller the depth of cut, the more economically the shovel will operate until a minimum cut of 15 ft is reached, below which the efficiency decreases rapidly. The Marion shovel may be used in tandem stripping in excessive depths of overburden. The other type of excavating equipment used in the tandem team is generally a dragline with a long boom of about 180 ft. In tandem stripping, the dragline is used to remove the upper portion of the cut and to place it at a maximum dumping radius from the place of removal. The Marion 5560 power shovel is then used to remove the overburden left above the coal seam and to deposit it at the shovel&apos;s maximum dumping radius. The Marion 5560 power shovel is of gigantic proportions. It has a 102 ft 6 in. boom and 32 cu yd dipper and is

Jan 1, 1950

By Walter Crafts, C. M. Offenhauer

IN a previous study&apos; of the carbide phase of chromium steels, it was shown that chromium carbide (Cr7C3) is a more stable carbide than cementite (Fe3C) at tempering temperatures above about 500°C. in quenched steels containing from about r1to 7.5 per cent chromium. Below this temperature the carbide phase was found to consist of cementite in all of the steels examined. In the present investigation it was found that a similar change in the carbide phase takes place in molybdenum and in chromium-molybdenum steels at approximately the same tempering temperatures. The approximate ranges of occurrence of the alloy carbides Cr7C3, Cr4C, and Mo2C have been determined in steels containing up to 5 per cent chromium, 1 per cent molybdenum and 0.60 per cent carbon. The experimental steels were made in small high-frequency furnaces from Armco ingot iron, low-carbon ferrochromium and calcium molybdate and were poured into 2-in. ingots, which were forged to 1-in. round bars. Sections of the bars were heated to the carbide-solution temperature and cooled rapidly to induce austenite transformation at relatively low temperatures. The steels were subject to some segregation, therefore comparatively high temperatures were necessary to dissolve all of the carbides. The microstructure of the quenched specimens was examined to verify the belief that the carbides had been dissolved, and also to determine the nature of the nonmartensitic structure of incompletely hardened steels. Ferrite and pseudomartensite were present in some of the specimens, but all specimens were quenched at such a rate that pearlite was not formed, in order to ensure the formation of the carbides at temperatures lower than about 500°C. It had been found previously&apos; that in chromium steels the chromium carbide could be produced by transformation of austenite in the pearlite range above 500°C., and, in order to start the tempering treatment with the carbide present as cementite, the absence of pearlite was considered to be essential. The specimens were tempered for 64 hr. to permit the formation of the stable carbide. After tempering, the specimens were submitted to microscopic and X-ray examination. The carbides were separated either electrolytically in a 5 per cent HCl electrolyte or with an acidified copper-potassium chloride solution. The crystal structure of the carbide phases was determined by the Debye-Scherrer type of X-ray patterns. The X-ray patterns obtained from specimens near the boundaries between two types of carbides were generally weak and diffuse as compared with the other patterns. For this reason, and because the more soluble components may be masked, the boundaries between the phases could not be determined precisely. However, the X-ray analysis of electrolytically separated carbides has given consistently reproducible results

Jan 1, 1943

By L. G. Graper, E. L. Ramsey

THE present program of increased production of armament and lend-lease material for mechanized war has created a problem for the shops that must do the machining. They have naturally turned to the steel producers to provide them with a steel that can be accurately machined with the greatest possible speed. The adding of sulphur to steel as an aid to machinability has long been practiced; however, it may cause red shortness in rolling and may result in billets with seams and cracks, which must be removed before rolling can be continued. This conditioning of billets slows down production and adds to the cost of making steel. Experience with various grades of sulphur steel made to different specifications has shown that Bessemer sulphur steels roll better than similar grades made in the open hearth, and also that low-carbon steels that are open or semi-killed as tapped roll better than completely deoxidized or killed steels. This has led to the belief that oxygen plays an important part in the rolling qualities of sulphur-bearing steels. It is generally held that the red shortness of sulphur steels is due to the low melting point of the sulphide compounds that separate out at the grain boundaries when the steel solidifies. At the rolling temperature of steel these sulphide compounds melt and cause cracking. ADDING SULPHUR AS A SULPHITE These difficulties can be avoided if sulphur is introduced into the steel by means of an anhydrous sulphite, such as sodium sulphite or sodium bisulphite, which-upon decomposition-forms sulphur dioxide. It is assumed that, in this case, the oxygen of the sulphur dioxide forms part of the sulphide inclusions in the steel, and raises their solidification temperature enough so that the formation in the steel of a low-melting eutectic is prevented. The result is the prevention of hot shortness and a more uniform distribution of inclusions. Fig, I shows photomicrographs of steels made with sulphur, while Fig, 2 illustrates the structure of steels made with sodium bisulphite. These samples were cut from the steels as cast-that is, before rolling and were polished and lightly etched to bring out the grain boundaries. Fig. I shows that sulphide inclusions segregate more or less at the grain boundaries, and it can be seen how the continuity of these low-melting inclusions would cause red shortness. Fig. 2 shows that the sulphide inclusions are more or less uniformly distributed throughout the matrix. This arrangement of inclusions has no apparent effect on the rolling qualities of a steel. This statement has been substantiated by the observation of the rolling of over 6000 tons of steel made with a sulphite addition. RESULTS As stated before, the sulphur dioxide is added to steel by means of the decompcsi-

Jan 1, 1942

By R. T. Webber, B. B. Owen

THE vapor phase deposition of molybdenum and tungsten from the hexacarbonyls has been thoroughly investigated by Lander and Germer1 and shown to yield well-bonded coatings on a variety of hot metallic surfaces. They also demonstrated that chromium coatings2.3 could be similarly deposited, but did not investigate this metal extensively. Recently,4 conditions have been described by which this compound can be prepared in quantities sufficient for laboratory scale plating experiments, and it is the purpose of the present communication to outline the results of preliminary experiments upon the plating of chromium from its carbonyl. APPARATUS AND TECHNIQUE The apparatus used in these experiments is shown in Fig I. At one end, connected by a short length of rubber tubing, is a Cenco Hypervac 20 pumping continuously. At the opposite end is a needle valve which allows a small stream of purified hydrogen to flow through the apparatus. Connected in series are a trap T1, maintained at the temperature of dry ice and acetone, the plating chamber, and two traps T2 and T3 containing crystals of the carbonyl. T2 is kept in a constant temperature bath (not shown), while T3 is at room temperature. Stopcock S6 allows the hydrogen flow to by-pass the carbonyl traps. A McLeod gauge is connected so that it can measure the pressure at the pump through Ss, or the pressure at the plating chamber through S9 and S6. The standard (12 liter) volume connected by S5 is used to determine the volume included by S4, S6, Se, S10, the needle valve and the McLeod gauge. Knowledge of this volume allows calibration of the flow of hydrogen. The apparatus* is built entirely of pyrex, except for the needle valve, the rubber connection to the Hypervac, and the cover of the plating chamber. The plating chamber is water-jacketed, with a large brass top allowing insertion of the specimen to be plated. Set into the brass top is a ground glass stopper through which thermocouple leads are sealed. The thermocouple wires (pure Pt, and 87 pct Pt-13 pct Rh) serve the double purpose of measuring the specimen temperature and suspending it in the chamber. Surrounding the chamber is the coil of an induction heater, H. The apparatus is designed to allow variation of the following conditions: I, the specimen temperature, from room temperature to about 1000°C, 2, the carbonyl vapor pressure, from 40 to 220 microns, and 3, the hydrogen flow. In several runs, 0.8 to 1.8 pct of hydrogen sulfide was introduced through a needle valve that replaced S4. The vapor pressure of the carbonyl is

Jan 1, 1948