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By L. L. Handy

The development of a theory for miscible liquid displacement requires evaluation of the variables which affect growth of the mixing zone between solvent and displaced oil. Factors which appear to be important are individual fluid viscosities, viscosity ratios, flood rate, fluid densities, flow characteristics of the porous medium and molecular diffusion coefficients of the fluid components. The primary purpose of this paper is to evaluate diffusion effects. Theoretical treatments to date have been limited to floods for which the viscosity ratio is one. Two principal theories have been proposed. Von Rosenberg adapted for porous media a theory derived for capillary tubes by G. Taylor.' ,' In this theory molecular diffusion perpendicular to the direction of flow is a primary factor in sharpening the flood front. Slow floods give sharper fronts for a given distance traveled than fast floods. An alternative theory considers miscible liquid displacement as a statistical problem.3,4,5 Diffusion is not an important factor in this theory, but it leads to the same general type of equation as von Rosenberg's. Both theories predict S-shaped concentration profiles with the same dependence on distance traveled. The statistical or "dispersion" theory predicts rate independence, however. To supplement rate studies a direct measurement of a diffusion effect would be helpful in evaluating which of the two proposed mechanisms best describes miscible liquid displacement for one-to-one viscosity ratio systems. No quantitative theory has been proposed for floods in which a low-viscosity fluid displaces a high-viscosity fluid. It might be anticipated, however, that the extensive fingering observed in floods with adverse viscosity ratios would increase opportunities for an exchange of components between displaced and displacing liquids by a diffusional process. Even if molecular diffusion were not an important mixing mechanism for one-to-one viscosity ratio systems, it could be significant in systems with adverse viscosity ratios. METHOD FOR EVALUATING DIFFUSIONAL MIXING In solvent flooding the displacing liquid can become mixed with the displaced liquid by a number of processes; in general, either mechanical or diffusional in character. To evaluate the contribution of diffusion, a method was sought that would distinguish diffusional mixing from mechanical mixing. Suppose two soluble tracers are added to the displacing liquid and that one tracer has a diffusion coefficient much greater than the other. Then, if diffusion is important during miscible liquid displacement and if diffusional transport is primarily transverse to the direction of flow, substances with high diffusion coefficients will have sharper concentration profiles than those with comparatively low molecular diffusion coefficients. In order to have material balance the profiles for the two tracers must intersect. For one-to-one viscosity ratios the intersection would occur at the 50 per cent concentration point. It is generally assumed that diffusion in the direction of flow is negligible. This assumption appears reasonable because flow velocities are ordinarily orders of magnitude greater than diffusional velocities. If this is not a valid assumption, however, the shapes of the fronts will be further degraded by longitudinal diffusion. The effects of rate and molecular diffusion coefficients are the opposite for longitudinal diffusion to those for lateral diffusion. Higher rates or lower diffusion coefficients would tend to give sharper fronts. The double tracer method offers several unique advantages in evaluating effect of molecular diffusion. First, the method gives a direct measure of the effect of diffusion on mixing zone size. Second, the effect of a difference in diffusion coefficients is determined from a single experiment. Comparison of several experiments at different rates is not required. Third, the method is applicable for any viscosity ratio. Fourth, the method is unaffected by density differences between the two fluids which might result in rate dependent gravity effects. EXPERIMENTAL PROCEDURE Suitable tracers are substances whose diffusion coefficients differ as widely as possible, but whose adsorptions on rock surfaces is negligible. The two tracers selected were methanol and sucrose in water solutions. The approximate diffusion coefficients for methanol and sucrose, as given in the International Critical Tables, are 1.3 X 10-5 and 0.3 X 10-5 m2/sec, respectively. Concentrations in the water solutions were 200 gm/liter of solution for both methanol and sucrose. These high

By C. Michael Dickinson

In support of the DNA Deep Basing Program, SRI International has been performing scale model experiments on protective structures since 1973. The SRI program includes field and laboratory tests of mini- structure models with surrounding natural or simulated geology. This paper contains a synopsis of some of the results of this research.

Jan 1, 1984

By E. Buehler, J. E. Kunzler

High-pu.1-ity molybdenum has been heat treated, melted, and zone refined and the physical and chemical changes that are produced by these processes have been studied by making resistance ratio measurements. Pronounced effects are observed that are associated with recrystalliza-tion at about 1200°C and with melting. Melting alone is found to result in a substantial purification by the evaporation of impurities such as iron. Zone refining is found to be reasonably effective with four passes producing a three-fold decrease in resistance ratio and a minimum ratio of 0.0003. With the aid of low temperature measurenzents, it has been shown that the build-up of a deposit of the material being zone refined on the radio frequency coil used for heating can lead to contamination of the sample. CONSIDERABLE interest in high-purity refractory metals for the study of mechanical properties has developed during recent years. Also the need for highly pure metals in certain fundamental studies, such as electronic band structure, has become quite widely appreciated. Molybdenum can now be produced with sufficiently high purity to make it attractive for such investigations. The most suitable measure of chemical purity of metals used for many of these studies is its resistance ratio, R,.,o,/Ro, During the purification of molybdenum by zone refining and its subsequent evaluation by this technique, a number of informative observations were made. These observations concern the effectiveness of zone refining, the volatilization of impurities at the melting point, and the recrystallization of molybdenum and appear to be pertinent to other refractory metals. Also, the usefulness of low-temperature resistance measurements as an analytical tool for evaluating the presence of chemical impurities and physical defects in metals is again illustrated. Samples of high-purity molybdenum of known mechanical history were heated to various temperatures between 800°c and their melting point. Resistance ratios of the samples were measured after they had been given a specified treatment. The data were used, along with mass spectrographic analysis, as an aid in interpreting the nature of the processes that occurred in conjunction with each treatment. Changes in the concentrations of chemical impurities and physical defects are typical of things that effect the low-temperature resistivity. SAMPLES The starting material was obtained from Westing-house Corp., Bloomfield, N.J. It was in the form of molybdenum rods, usually 1/8 or 3/16 in. in diameter. These had been previously processed from bars, 5/8 in, in diameter, originally reduced from 4 in. diam arc-cast ingots, by hot swaging at about 1300°c. In the final step, the temperature was lowered to about l lOO°C which resulted in the production of elongated grains. Typical grains were about 0.03 mm thick and 0.6 mm long. The molybdenum was quite pure as is indicated by the results of mass spectro-scopic analysis1 given in Column 2 of Table I. Other nongaseous elements not listed in the table were not detected. ZONE REFINING AND THERMAL TREATMENT OF SAMPLES Several sample rods, 8 to 10 in. long, were zone refined or were heat treated at several temperatures. Both types of operations were performed using 3 me-

Jan 1, 1962

By Robert R. Turner

This paper discusses wet and dry primary autogenous and semi-autogenous grinding, including a description of the equipment and its mode of operation, testing and the scaling-up of test data. Lists of selected literature references are included.

Jan 1, 1982

By Enid C. Plante, K. L. Sutherland

PRACTICAL metallurgists are unanimous in stating that oxidation of mined sulphide ore adversely affects separation of the constituent minerals under standard conditions in a mill. Frequently, the need for different operating conditions in different plants is attributed either to the extent of oxidation of the mineral surfaces or to soluble oxidation products. The investigations reported in this paper study the effect of oxidation on the primary condition necessary for flotation, namely that of adhesion of an air bubble to the mineral. OXIDATION PRODUCTS FROM SULPHIDE MINERALS Weinig and Carpenter1 state that the relative rates of oxidation of some sulphides are: FeAsS > FeS2 > CuFeS2 > ZnS >PbS > Cu2S tetrahedrite. They also show that oxidation is rapid at first, that sulphides of older geological formations are more stable than those of recent date and that mixtures oxidize more rapidly than any one mineral alone. The more rapid oxidation of mixtures is borne out by results of Gottschalk and Buehler2 who found that PbS, ZnS and CuS oxidized 8 to 20 times faster when pyrite was present. Only the end products of oxidation, sulphate and the metal ion, were identified in these tests. Gaudin3 states that pyrite is difficult to oxidize in the laboratory. Winchell,4 using pyrite containing 99.98 pct FeS2, allowed water to percolate through a bed of this ground material. At the end of three months only a trace of Fe +++and S04- were found. Even after 10 months the quantity of Fe+++ was only 7.8 mg and S04- 25.5 mg per liter of percolating solution. Carmichael5 confirmed Winchell's results on the slow oxidation of pyrite. Usually the oxidation of sulphide surfaces has been conducted in neutral or acid solutions, the acidity being caused by the oxidation products. Eliseev and Nagirnyak6 found that treatment of pure pyrite with lime gave only thiosulphate, but considered it possible that thiosulphate was obtained not by oxidation of the pyrite itself, but by oxidation of calcium disulphide. Mitrofanov7 suggested that thiosulphate was formed by the following process: oxidation of sulphide to give free sulphur (this frequently happens with marcasite), followed by oxidation of the sulphur to sulphur dioxide and reaction of the sulphur dioxide with sulphur to give thiosulphate. Ferric and ferrous hydroxides, or similar compounds, were shown to be present. The Research Staff of the United Verde Copper Co.8 treated ore from the United Verde mine with lime. Thiosulphate, sulphide and polysulphides were stated to be

Jan 1, 1947

By John C. Branner

Shales rich in oil are found at several places along the coast of Brazil. The material has been prospected at several places, and samples have been examined and reported upon by competent authorities. So far as I am acquainted with them, these oil-bearing beds are of Tertiary age. A glimpse at the distribution and character of the Tertiary rocks of the region should give us some idea of the possible distribution of these oil-bearing shales. Tertiary rocks skirt the northeast coast of Brazil from the northern part of the State of Espirito Santo almost or quite to the Amazon valley. Here and there this narrow strip is cut in two by the encroachment of the sea, and the underlying gneisses, granites or other crystalline rocks are exposed upon the beach. In other places, the Tertiary belt widens out until it is 80 kilometers or more in width. Fig. 1 is a sketch-map of a part of the coast-area referred to. Along the coast from Prado, in the State of Bahia, northward to Natal, there is a line of bluffs from 15 to 90 meters high, interrupted here and there by stream-valleys. As seen from the sea, these bluffs are rather conspicuous and highly colored yellow, brown, red, white, black, and purple. These colors are often so mingled as to give the beds a mottled or parti-colored appearance. Fig. 2 shows a characteristic bit of the coast in the State of Parahyba do Norte. In some places, especially in the southern part of the State of Sergipe, and in the northern part of Rio Grande do Norte, the immediate coast is covered with sand-dunes. Here and there these sanddunes have been carried inland over the top of the Tertiary beds, and the subsequent encroachment of the sea has exposed the Tertiary rocks again, where they form the bases of the bluffs. This is well shown in Fig. 3, from a photograph taken at Bahia Formosa, on the coast of Rio Grande do Norte.

Jan 1, 1901

By George Stern

THE purpose of this investigation has been to study one method for making ordinary carbon steel by the powder metallurgy technique. This method con- [ ] sists of pressing and subsequently sintering an intimate mixture of iron powder and graphite in a suitable atmosphere to produce a steel. Two types of iron powder have been studied, electrolytic and reduced. The sintering of mixtures of loose carbonyl iron and carbon black for several hours at 1000° to 1100°C. (1830° to 2010°F.), followed by forging of the resultant ingots to bars, has been studied by Offermann.1 Trail' has reported on the properties of hydrogen-reduced and electrolytic iron powders, both containing 0.5 per cent carbon. Methods for making steel bodies by powder metallurgy have also been sug- [ ] gested by Goetzel,3 who recommends the addition of steel powder of well-defined carbon content to pure iron powder, and Volterra,4 who suggests compaction and subsequent sintering of a mixture of steel powder, iron oxide and iron powder. Additional methods for making steel bodies by powder metallurgy have been reported in the literature by Koehring,5 Allen,6 Balke,7 Wulff,8 Boegehold,9 and others. 10,11,12 It is felt that the method of pressing iron powder and graphite, as described herein, lends itself best to production because of the lubricating action of the

Jan 1, 1946

By J. R. Low, M. Gensamer

During the course of an investigation into the drawability of automobile-body sheet steel, it became apparent that certain advantages would be possessed by a deep-drawing steel with a very low yield strength, but almost normal tensile strength, provided a reduction in yield strength could be accomplished without sacrifice of ductility and fine grain size. It would also be desirable to have this steel free from strain-aging; that is, free from the tendency for the yield point to return after it had been eliminated by straining. It was known that, wet hydrogen treatment acted to eliminate aging, but as carried out by other investigators, at relatively high temperatures, this treatment resulted in grain coarsening. It has been established by some of the experiments reported in this paper that all of these objectives can be accomplished by treatment in wet hydrogen at a low temperature, in the neighborhood of 72o°C. The time of treatment is relatively short (about 3 hr, to completion with 20-gauge sheet) if the water content of the hydrogen atmosphere is made fairly high, say aimost 30 per cent by volume. At this temperature. the grain size remains fine in the time required. After this treatment sheet reduced the usual amount by cold-rolling has a grain size of about A.S.T.M. No. 7. The yield point is completely eliminated, and the yield strength is reduced to a very low value, in the neighborhood of 15,000 lb. per sq. in. The stress-strain curve departs gradually from the straight-line elastic part after the fashion of nonferrous deep-drawing alloys. This elimination of the yield point is accompanied by a verv low indentation hardness; for example, 32 Rockwell B or even lower. There is no aging as measured by increase in the yield strength upon aging at room temperature or for 3 hr. at 200°C., after stretching about 10 per cent in tension. Tensile strength is only slightly less than the box-annealed sheet, seldom dropping much below 40,-ooo lb. per sq. in. Elongation is practically unchanged, or increased slightly. The term yield point, as here used, refers to the phenomenon of heterogeneous deformation occurring at a substantiallv constant load, observed principally in annealed low-carbon steels. If such a steel is loaded in tension, the load increases steadily with elastic strain, suddenly falls, fluctuates slightly about some constant value for a time and then begins to rise again as deformation proceeds. The maximum initial load before the sudden drop is generally called the "upper yield point"; the value of the load where deformation proceeds at a

Jan 1, 1944

By J. R. Low, M. Gensamer

During the course of an investigation into the drawability of automobile-body sheet steel, it became apparent that certain advantages would be possessed by a deep-drawing steel with a very low yield strength, but almost normal tensile strength, provided a reduction in yield strength could be accomplished without sacrifice of ductility and fine grain size. It would also be desirable to have this steel free from strain-aging; that is, free from the tendency for the yield point to return after it had been eliminated by straining. It was known that, wet hydrogen treatment acted to eliminate aging, but as carried out by other investigators, at relatively high temperatures, this treatment resulted in grain coarsening. It has been established by some of the experiments reported in this paper that all of these objectives can be accomplished by treatment in wet hydrogen at a low temperature, in the neighborhood of 72o°C. The time of treatment is relatively short (about 3 hr, to completion with 20-gauge sheet) if the water content of the hydrogen atmosphere is made fairly high, say aimost 30 per cent by volume. At this temperature. the grain size remains fine in the time required. After this treatment sheet reduced the usual amount by cold-rolling has a grain size of about A.S.T.M. No. 7. The yield point is completely eliminated, and the yield strength is reduced to a very low value, in the neighborhood of 15,000 lb. per sq. in. The stress-strain curve departs gradually from the straight-line elastic part after the fashion of nonferrous deep-drawing alloys. This elimination of the yield point is accompanied by a verv low indentation hardness; for example, 32 Rockwell B or even lower. There is no aging as measured by increase in the yield strength upon aging at room temperature or for 3 hr. at 200°C., after stretching about 10 per cent in tension. Tensile strength is only slightly less than the box-annealed sheet, seldom dropping much below 40,-ooo lb. per sq. in. Elongation is practically unchanged, or increased slightly. The term yield point, as here used, refers to the phenomenon of heterogeneous deformation occurring at a substantiallv constant load, observed principally in annealed low-carbon steels. If such a steel is loaded in tension, the load increases steadily with elastic strain, suddenly falls, fluctuates slightly about some constant value for a time and then begins to rise again as deformation proceeds. The maximum initial load before the sudden drop is generally called the "upper yield point"; the value of the load where deformation proceeds at a

Jan 1, 1944

By J. Sharshall Grasty, Thomas L. Watson

The users of barite in the United States derive their supply partly from the domestic production and partly from the imports from foreign countries. According to the Mineral Resource division of the U. S. Geological Survey, the domestic production of barite in 1913 was 45,298 short tons, valued at $156,275, or $3.45 a ton, and the imports of crude barite were 35,840 short tons, valued at $61,409, or $1.71 a ton. These figures clearly show a decided advantage in cost of the foreign over the domestic barite to users in the United States. The difference in cost is the only advantage to the consumer of foreign barite, for there are large reserves of the mineral in the United States of good grade. The production of many of the operating mines is capable of decided increase, and it is believed that the operating mines together with the large reserves of undeveloped deposits of barite are entirely adequate to meet the demands of the users in the United States. Deposits of barite are known in California, Idaho, Nevada, and Alaska, but most of them are undeveloped because there is, apparently, no market for the material in that region. The domestic production is derived from Missouri .and the Appalachian States, the greater part being obtained from Missouri. Following the outbreak of war in Europe many users of foreign barite in the United States have been forced to seek their supplies at home. It seems opportune at this time, therefore, that a general review be given of the barite industry in the Appalachian States, one of the two areas from which the domestic supply of the mineral is derived, and that attention be directed to the undeveloped deposits in the region. Briefly, then, this paper reviews the barite industry in the Appalachian States, and describes the occurrence, preparation, and uses of the mineral. General Character Barite, known commercially as barytes or heavy spar, is barium sulphate (Baso4), containing when pure BaO, 65.7 per cent., and S03, 34.3 per cent. The specific gravity is 4.3 to 4.6, and the hardness 2.5

Jan 1, 1915

By R. F. Mehl, J. K. Stanley

THE recrystallization of cold-worked metals is studied ordinarily by determining the temperatures required for complete recrystallization to occur within a given arbitrary time period, usually within 15 min. to 2 hr. The results obtained are conventionally assembled in a three-dimensional diagram relating this temperature to the amount of cold-work (percentage deformation) and the resultant grain size, though sometimes other modes of representation are employed.1 Such three-dimensional diagrams are not complete, for the number of variables exceeds the number represented. The process of recrystallization is characterized by a time-rate, a fact that is not portrayed upon ordinary recrystallization diagrams. It is known that recrystallization consists in the formation of new nuclei and the growth of these nuclei, a process that continues until the matrix is completely consumed and the original set of grains entirely replaced by the new. This knowledge is old.2 Truly heterogeneous reactions invariably proceed by nucleation and growth; the decomposition of eutectoid solid solutions provides an example about which much is known,3 and freezing, originally studied by Tammann, provides the classic example. Although recrystallization is not a heterogeneous reaction within the orthodox meaning of the term, the mechanism of the process is the same. As in eutectoid inversion and freezing, it should be possible to study the rate of isothermal recrystallization as a function of time, and it should also be possible to analyze the isothermal reaction curve into the component rates of nucleation and growth that determine them.* Other methods, not employing the rates of nucleation and growth, have been used to represent the rates of such reactions, but these in general have been artificial and have not led to progress .4,5† The theory of recrystallization is not in advanced state; if recrystallization data were obtained in terms of the rate of isothermal recrystallization, and in terms of the rate of nucleation and the rate of growth of recrystallized grains, and in particular if the temperature coefficients of these rates were measured accurately, an adequate theory should be more readily developed .27 Such an effort requires proper experimental technique, but especially requires suitable methods of mathematical analysis to convert measurements made upon a surface of polish into values for the rate of nucleation and the rate of growth and to combine these into a rate of isothermal recrystallization. These methods are now

Jan 1, 1942

PRESIDENTS DAVID THOMAS 1871 R W RAYMOND 1872-1874 A L HOLLEY1875 ABRAM S HEWITT 1876 T STERRY HUNT 1877 ECKLEY B COXE 1878 - 1879 WILLIAM P SHINN 1880 WILLIAM METCALF 1881 RICHARD P ROTHWELL 1882 ROBERY W HUNT 1883 JAMES C, BAYLES 1884-1885 ROBERT H RICHARDS 1886 THOMAS EGLESTON 1887

Jan 1, 1923

THE metal iron has physical arid chemical properties which are some- what different from those of steels, but a knowledge of the pure metal is a useful starting point in studying the behavior of steels. Solid iron exists in two different crystalline forms, called alpha (a) and gamma (?) iron the former being the ordinary form at room temperature. When heated above the "A2 point," 769 C (1416 F), the metal becomes nonmagnetic, and at the "A3 point," 911 C (1672 F), it undergoes a change in crystalline form to become gamma iron. 111 the range 769 to 911 C, it is sometimes called beta (ß) iron to distinguish it from the magnetic alpha, but the two are identical in crystal structure. When gamma iron is further heated to 1392 C (2538 F), it changes into delta (d) iron, which is identical with beta or nonmagnetic alpha iron. Pure iron melts (in an inert atmosphere) at 1536 C (2797 F); the melting point is generally lowered by alloys or impurities. PHYSICAL AND THERMAL PROPERTIES OF IRON Many of the properties of iron undergo abrupt changes at the transition temperatures.1 For example, in heating through the A3 point, a sudden shrinkage in volume occurs. Similarly, melting is attended by sharp physical changes such as an increase in volume. Table 16-1 contains a summary of the measured physical properties of pure iron at several temperatures. Usually the properties change smoothly with the range of stability of a given form, but this is not always true. For ex- ample, the specific heat reaches a sharp maximum at the A2 point al- though no transformation occurs. (See Fig. 14-1.) Solvent Powers of Liquid Iron. Liquid iron is capable of dissolving most of the other metals and many nonmetallic elements as well. Of the metals that are liquid at the melting point of iron, only lead, silver, and bismuth refuse to dissolve to an appreciable extent. Table 16-2 contains a list of the common elements classified with respect to their solubility in liquid iron. Those which are very soluble or practically insoluble require no further discussion, but several of the nonmetals that are gases and exhibit limited solubility are of considerable importance to us and merit more detailed consideration.

Jan 1, 1964

By Benjamin Lustman, Robert F. Mehl

THE study of the high-temperature oxidation of pure metals, intensively pursued experimentally since the pioneer work of Pilling and Bedworth1 and supplemented by the recent theoretical work of Wagner2 is now well advanced. The important field of low-temperature oxidation-i.e., oxidation extending only through the temper color range of thicknesses with the formation of thin oxide layers in the range from o to 1000-2000 Angstroms-has not, however, reached so satisfactory a state, owing largely to the experimental difficulties that attend the formation and study of thin films; most of the work has been performed on abraded specimens whose surface irregularities approximated the thickness of the films formed. It has been pointed out that the rates of oxidation of different crystal faces are different and that the difference may be related to the orientation relationships that obtain between the metal crystal and the superimposed oxide crystal; it has also been suggested that this orientation dependence should manifest itself in rates of oxidation and perhaps also of corrosion in aggregates bearing preferred orientations. 3,4 An attempt to measure the rates of oxidation of different crystal faces of alpha iron demonstrated this difference in rate,4 but the dependence of rate on orientation was not simple; the method of measuring thickness, consisting of a color comparison with barium stearate multi-films of known thickness, was not wholly satisfactory. For these reasons it was felt that a study of the rate of oxidation of single crystals prepared with surfaces as smooth as possible, using a sensitive method giving true film thickness, should be profitable. Copper was chosen because of the ease of reduction of the primary oxide film and because the orientation relationships between metal and oxide and the composition of the oxide films formed at low temperatures are known; for thin films formed at low temperatures, Cu2O alone occurs.22-24 EXPERIMENTAL PROCEDURE Various methods of surface preparation were attempted in order to obtain a surface that would oxidize uniformly and reproducibly. Electrolytic polishing by the method of Jacquet5 and electrolytic and mechanical polishing followed by annealing in vacuum and in purified hydrogen at various temperatures were tested. The procedure finally adopted consisted in a fine metallographic polish followed by an anneal in purified hydrogen at temperatures of 900º to 1000°C. for 12 hr. or more. The surface so produced was very bright and smooth, with no trace of specular etching (though some grain-boundary etching was observed); indeed, fine scratches produced by the final polish were entirely removed by the high-temperature anneal.

Jan 1, 1941

By W. J. Babyak

The habit planes for hydride precipitation in large grains of alpha zirconium and Zircaloy-4 were determined in specimens containing 161 and 136 ppm hydrogen, respectively. In zirconium, the hydride platelets precipitated on various pyramidal planes inclined to the basal plane at angles ranging from 10 to 50 deg and 75 to 90 deg. Hydrides were most frequent at inclinations of about 20 deg and 90 deg. In Zircaloy-4, hydride plates were inclined to the basal plane at angles vanging from 5 to 25 deg with the predominant inclinatioiz equal to 12 deg; no platelets were found near the prism plane position. In both zircoinium and Zir-caloy-4, hydrides were principally, but not exclusively, parallel to (1011) type planes. When the Zircaloy-4 gmins were subjected to tension stresses of 12,100 psi and 19,400 psi during hydride precipitation, the hydride habit was unchanged except that precipitation favored those habit planes which were inore nearly perpendicular to the stress direction. The stress-orientatioiz effect increased with the magnitude of the stress. THE hydride habit plane in a zirconium has been determined by several investigators. Langeron and Lehr1 in 1956 found platelets parallel to (1010) slip planes. In 1962, Westlake and Fisher2 confirmed these findings and showed that hydride precipitation on twin planes, as reported by Kunz and Bibb,3 was probably due to incomplete removal of worked metal from specimen surfaces. Secondary habit planes, ( 1011) and (1015), were also found by Westlake and Fisher under particular charging conditions where a hydride layer may have existed at the hydrogenation temperature. Most recently, walters4 and westlake5 again observed the (1010) habit exclusively in zirconium. Louthan and hgermans have reported that hydrides precipitate on various ( 101l ) and (112l) planes positioned 31.5 to 90 deg to the basal plane in Zircaloy-2. The present investigation was concerned with the hydride habit in Zircaloy-4 in relation to that in zirconium and the possible change in habit when precipitation occurs under stress. The latter consideration was prompted by the stress-orientation phenomenon originally reported by Marshall and Louthan.7, 8 I) EXPERIMENTAL Materials and Specimens. Chemical analyses of all materials are given in Table I. The zirconium specimen was a 1 by 4 in. section cut from wrought crystal bar that was hot-rolled at 790°C to 0.300 in. and cold-rolled to a final thickness of 0.095 in. All surfaces were mechanically polished and then chemically polished with a solution of H2O, HNO3, and HF (10:10:l by volume) prior to annealing. Grains as long as 0.25 in. were grown by thermally cycling the specimen three times (in 10-5 mm Hg vacuum) between 825" and 1000°C at approximately 125°C per hr. The specimen was isothermally annealed at 825°C for 24, 40, and 120 hr after each cy-

Jan 1, 1968

By H. M. Strong

Nickel and carbon form a metastable nickel-nickel carbide eutectic system which was ohsen)able by freezing latent-heat arvests at pressures 210 khars. The eutectic freezing temperature Is pressure had a slope of -0.9°Cper kbar. At 50 khars, the nickel-nickel carbide eutectic was at 1297° * 5°C and 0.34 mole fraction Ni3C. The composition of the eutectic increased at an initial rate of 0.004 mol fraction per kbar. The carbon content of the a phase also increased with pressure. Seveval illustrations of nickel carbide microstruc-tures are given and data on the lattice expansion of nickel in terms of carbon content are included. IRON, cobalt, and nickel form a variety of carbides with compositions varying between MeC and MC. Of the three, the carbides of iron are most easily recovered. The nickel carbides are so unstable at temperatures above 900°C that their occurrence in Ni-C alloys is unusual. Under sufficient pressure, however, the temperature range for the stability of the ferrous metal carbides is likely to be increased, or their decomposition suppressed (e.g., see Hilliard' on FesC), providing an opportunity to study the unstable carbides more closely. This was found to be true for nickel carbide which, under pressure, formed a eutectic with nickel. This paper describes the conditions of formation of nickel-nickel carbide eutectic compositions and their subsequent recovery. Despite the comparative instability of the nickel carbides, something is already known about them through various chemical reactions at temperatures not exceeding a few hundred degrees, and from their recovery by the very rapid quenching of molten Ni-C alloys from temperatures of about 1450°C or above. At least four carbides of nickel have been reported: A discussion of the state of knowledge about Ni3C is given by ansen.' The studies of Morrogh and williams7 who obtained Widmanstatten nickel carbide structures and of sidorenko8 who first obtained nickel carbide eutectic structures are also of interest. Sidorenko used short heating times for molten nickel in a graphite crucible followed by very rapid quenching to obtain the eutectic structures. Long heating times produced only the nickel-graphite eutectic probably due to the presence of graphite crystals in the melt which nucleated graphite crystallization. According to the early work summarized by anssen,' nickel carbide may form at temperatures far above the melting point and may be recovered by very rapid quenching. More recently, Giardini and Tydings, working on diamond synthesis, found evidence for "free nickel carbide'' in high-pressure reactions carried to temperatures far in excess of the limit for diamond growth, followed by rapid thermal quench. They stated that nickel carbide was not found in association with diamond growth. In the present work, observations were made on the melting and solidification temperatures of Ni-C alloys as a function of composition, temperature, and pressure. The nickel-nickel carbide eutectic was found at pressures above 10 kbar and its variation with pressure followed up to 60 kbar. Nickel-nickel carbide microstructures were recovered by quenching under pressure from temperatures of about 1400°C and higher. The formation of nickel carbide structures under ordinary diamond-growing conditions was usually observed but the role of carbide formation as an intermediate step in diamond growth needs more study. EXPERIMENTAL METHODS The melting and solidification temperatures of various nickel-graphite compositions were observed by latent-heat arrests in the sample holder illustrated in Fig. 1. The samples were composed of mixtures of carbonyl nickel powder and National Carbon Co.'s SP-1 graphite packed to densities of about 6.4 g per cu cm. They were contained within

Jan 1, 1965

By M. E. de Morton

Low frequency-internal friction measurements on annealed chromium have shown a marked increase in damping below - 40°C which is strongly strain amplitude dependent. An interpretation of these results is given in terms of the motion of antiferromagnetic domains assumed to exist below - 40°C. A time effect on internal friction was measured after slight overstraining. After heavy deformation a pemzanent, five-fold increase in internal friction was observed at -45°C and the character of the internal friction us temperature curve markedly changed. Full recovery of damping was not attained until after heating to 800°C. A qualitative interpretation of some of these effects is given. THE aim of this preliminary investigation was to study the internal-friction characteristics of chromium containing comparatively small quantities of interstitial solutes in the fully annealed and heavily worked condition. Marked anomalies in a number of physical properties of chromium at temperatures near 40°C have been observed1 and an investigation by neutron diffraction' has shown that chromium at room teyperature is weakly antiferromagnetic with a Nee1 temperature at approximately 200oC. No irregularities in the degree of antiferromagnetic ordering have been observed at -40°C, the transition temperature, and a complete explanation of this transition in chromium is still awaited. Recently weiss3 has suggested that an ordering effect of nitrogen in the face-centered interstices of the bcc lattice of chromium could be responsible for the superlattice detected below 200 °C in the neutron diffraction experiments. EXPERIMENTAL MATERIAL AND METHOD Specimens 10 by 0.030 in. diam were prepared from ingots of arc-melted electro-deposited chro-

Jan 1, 1961

By T. N. McVay, E. E. Creitz

INTRODUCTION Object RATHER large amounts of titanium minerals and some zircon and monazite are being recovered from dune sands about 10 miles west of Jacksonville Beach, Fla. The Mining Branch of the Bureau of Mines, Southern Experiment Station, has been interested in developing additional large deposits of similar sands in other areas of Florida. The results of a field study have been published1 concerning the sands occurring on Trail Ridge which runs north and south about 30 miles southwest of Jacksonville. This investigation was undertaken in order to identify the opaque titanium minerals occurring in Trail Ridge and because of the economic importance of Florida titanium minerals. Nature of the Problem The minerals present in the heavy fractions (sp gr > 2.94) of the sands are principally opaque minerals; staurolite, zircon, sillimanite, tourmaline, kyanite, rutile, a small amount of corundum, traces of the zinc spinel gahnite and garnet. Epidote, monazite, hornblende and titanite are present in other dune sands but these minerals were not noted in the samples collected on Trail Ridge. All of the minerals except those which are opaque can be readily identified by the usual petrographic methods. However, opaque minerals cannot be examined satisfactorily by transmitted light. Polished sections of the opaque-mineral grains were examined but these sections did not furnish useful information. Consequently, it was necessary to use means other than the usual petrographic methods to identify them. Previous Investigations of Heavy Minerals in Florida Sands Martens2 has described the heavy minerals in the Florida beach sands and has classified the opaque minerals as ilmenite with minor amounts of leucoxene. Miller3 studied a number of sands collected by Ross and Mertie in Florida. He states that the material from the Florida beach and dune sands that commonly has been called ilmenite has essentially the chemical composition of the material that has been called arizonite.4 The X ray diffraction patterns of several samples indicated that the supposed ilmenite is essentially amorphous, with only weak lines corresponding to ilmenite, and hence the material is unlike the type of arizonite from Arizona. Opaque Titanium Minerals Rutile is essentially titanium dioxide. However, as pointed out by Dana,5 important amounts of Fee and Fe3 as well as Cb and Ta are reported in some analyses.

Jan 1, 1947

By Paul L. Burkhart

THOUGH at an earlier period brief studies had been made by the Lehigh Navigation Coal Company Inc., it was not until 1924 that J. B. Warriner, then general manager, called for a comprehensive study of timber treatment, treating solutions, and related operations. Because of the impossibility of procuring accurate costs and other pertinent treating data, the American Wood Preserving Co. agreed to treat a car of mine timber at the Port Reading plant of the Reading Railroad. Fig. I shows the treating data collected at the treating plant on this timber, which was installed in two of the Lehigh mines in 1925. Table i.—Results of Timber Survey in 1925 before Treated Timber Was Introduced Length of tunnels and gangways ft..... 522,987a Length of tunnels and gangways timbered, ft.................................. 224.880 Number of steel mine sets in use......... 2,412 Number of timber sets in use............ 63,834 Number of timber sets with evidence of rot 50: 419 Number of timber sets with evidence of squeeze..... ...................... I3,415 Percentage of all timber sets showing evidence of failure: BY wet rot........................ 6.0 By dry rot........................ 73.0 By squeeze....................... : Average life of wood set in Panther Valley, years............................... 5.3 • 99.05 miles. In the latter part of 1925, a survey of the tunnels and gangways of the company's Panther Valley mines was made to determine the proportion of gangways or tunnels timbered, cause of timber failures, approximate life of the average wood set and the approximate percentage of treated timber that it would be profitable for the company to use. Results of this survey appear in Table I. Because of the high percentage of timber that gave evidence of failure by rot, as noted in Table I, and a further study of the life of the sections where timbering was necessary, it was deemed advisable to fill 25 per cent of the yearly gangway timber requirement with treated timber. Quantities and Treatments OF Treated Timber Purchased In the early days of the program, none of the large treating companies would accept orders for small quantities of treated timber and the company was compelled to state the quantity of timber it would require at each operation in each month of the year. Table 2 is an example of the tabulation given to the various treating companies to assist them in making a yearly bid on the minimum quantity of timber required by the company during the year 1931. A bill of timber was calculated for each car, the weight of which would be between the minimum and maximum weight permitted for railroad-car loading. The treating company was paid for timber upon delivery at the operation specified. As extra cars of timber were required, they were ordered from the treating company, and payment was required On their receipt, on the basis of the piece or tonnage

Jan 1, 1942

By Paul L. Burkhart

THOUGH at an earlier period brief studies had been made by the Lehigh Navigation Coal Company Inc., it was not until 1924 that J. B. Warriner, then general manager, called for a comprehensive study of timber treatment, treating solutions, and related operations. Because of the impossibility of procuring accurate costs and other pertinent treating data, the American Wood Preserving Co. agreed to treat a car of mine timber at the Port Reading plant of the Reading Railroad. Fig. I shows the treating data collected at the treating plant on this timber, which was installed in two of the Lehigh mines in 1925. Table i.—Results of Timber Survey in 1925 before Treated Timber Was Introduced Length of tunnels and gangways ft..... 522,987a Length of tunnels and gangways timbered, ft.................................. 224.880 Number of steel mine sets in use......... 2,412 Number of timber sets in use............ 63,834 Number of timber sets with evidence of rot 50: 419 Number of timber sets with evidence of squeeze..... ...................... I3,415 Percentage of all timber sets showing evidence of failure: BY wet rot........................ 6.0 By dry rot........................ 73.0 By squeeze....................... : Average life of wood set in Panther Valley, years............................... 5.3 • 99.05 miles. In the latter part of 1925, a survey of the tunnels and gangways of the company's Panther Valley mines was made to determine the proportion of gangways or tunnels timbered, cause of timber failures, approximate life of the average wood set and the approximate percentage of treated timber that it would be profitable for the company to use. Results of this survey appear in Table I. Because of the high percentage of timber that gave evidence of failure by rot, as noted in Table I, and a further study of the life of the sections where timbering was necessary, it was deemed advisable to fill 25 per cent of the yearly gangway timber requirement with treated timber. Quantities and Treatments OF Treated Timber Purchased In the early days of the program, none of the large treating companies would accept orders for small quantities of treated timber and the company was compelled to state the quantity of timber it would require at each operation in each month of the year. Table 2 is an example of the tabulation given to the various treating companies to assist them in making a yearly bid on the minimum quantity of timber required by the company during the year 1931. A bill of timber was calculated for each car, the weight of which would be between the minimum and maximum weight permitted for railroad-car loading. The treating company was paid for timber upon delivery at the operation specified. As extra cars of timber were required, they were ordered from the treating company, and payment was required On their receipt, on the basis of the piece or tonnage

Jan 1, 1942