Search Documents

By Che-Yu Li, J. L. Gregg, W. F. Brehm

Oriented, oxygen-doped niobium bicrystals were tested in liquid lithium. The grain boundaries were attacked preferentially. The depth of the penetrated zone varies as (time)2. The penetration was aniso-tropic, had a high activation energy, and increased with the increased oxygen doping level. A possible model was proposed to account for the experimental observations. 1 HE grain boundary penetration of a metallic system by liquid metal has been studied by several investigators. Their results are summarized by Bishop.' Most of these works show that the penetration by liquid metal corresponds to the phenomenon of liquid metal wetting. In the case of a grain boundary, wetting will occur when twice the solid-liquid interfacial tension is smaller than the grain boundary tension resulting in the replacement of the grain boundary by two new solid-liquid interfaces. Other possibilities exist; for example, the atoms of the liquid metal may diffuse into the grain boundary region due to chemical potential gradient. The gradient can be produced by impurity segregation or simply be due to the increase in solubility in the grain boundary region. The penetrated grain boundary in these cases may remain solid at the test temperature. The Nb-Li system has been of considerable interest because of its possible technological applications. For fundamental interest it provides a possibility of studying the grain boundary penetration process which is not controlled by the wetting mechanism. The pure niobium is not attacked by the liquid lithium, but if niobium containing more than 300 to 500 ppm oxygen by weight is exposed to liquid lithium, corrosion occurs at the solid-liquid interface and preferentially at grain boundaries. Previous investigators2-' have proposed that this preferential corrosion at grain boundaries is caused by oxygen segregation there, with subsequent inward diffusion of lithium to form a Li-Nb-0 compound. These investigators also found that the corrosion could be retarded by adding 1 pct Zr to the niobium to precipitate the oxygen as ZrO2 upon proper heat treatment. However, there are no quantitative data on the kinetics of the grain boundary penetration process to test the validity of the proposed corrosion mechanism. In this work an investigation of this penetration process in oriented bicrystals was made as a function of the oxygen doping level in the bulk niobium and the grain boundary orientation. A possible model for the penetration process based on the experimental results was proposed. EXPERIMENTS Oriented niobium bicrystals were grown by arc-zone melting oriented single-crystal seeds.7 These bicrystals contained simple tilt boundary. The [001] directions in the two grains were tilted about a common [110]. The bicrystals were 31/2 in. long and 5 by 4 in. in cross section with the straight, symmetric, planar grain boundary longitudinally bisecting the crystal rod. The bicrystals were doped with oxygen by anodically depositing a layer of Nb2O on the surface in a 70 pct HNO solution at 100 v, using a stainless-steel cathode. The specimens were homogenized by annealing in evacuated quartz tubes at 127 5°C. Oxygen content of the niobium was measured from microhardness values, after DiStefano and Litmman.' Supplementary checks were made with vacuum-fusion analysis.7 Individual test specimens cut from the doped bi-crystal rods, about by by % in. in size, were tested inside double jacket sealed capsules. The inner jacket was niobium, the outer was stainless steel. The niobium inner jacket eliminated the problem of dissimilar-metal mass transfer.' The lithium (99.8 pct pure, obtained from Lithium Corp. of America) was handled only in a purified argon atmosphere in a Blickman stainless-steel glove box. After introduction of lithium, the capsules were sealed by welding. Further detailed experimental procedures are given in Ref. 7. The capsules were heat-treated in vertical Marshall resistance furnaces. Temperatures were controlled to When heating above 1100°C, it was necessary to seal the furnace work tube and flow argon through to prevent failure of the stainless-steel outer jacket of the capsule. Tests were made on 6" 2", 16" 2, and 33" i2" bicrystals at oxygen levels up to 2600 ppm by weight in the 6' and 16" crystals and with 1300 ppm oxygen in the 33' crystals. The oxygen levels were controlled to 100 ppm. Most of the quantitative data were obtained from 16" bicrystals between 800" and 1050°C. The capsules were quenched into water after the test and cut open with a water-cooled abrasive wheel. The capsules were then submerged in water, which dissolved the lithium and freed the specimen. Measurement of the depth of the penetrated zone in the grain boundary was done either on metallographically prepared surfaces or directly on the grain boundary plane after the specimen was fractured in tension in the grain boundary plane. The depth of penetration measured by both methods agreed well. Further details describing these techniques have been reported elsewhere.'p7

Jan 1, 1969

By S. Floreen, R. M. Pilliar, H. W. Hayden

The fracture behavior of a 50 pct Cu-50 pct Fe mi-croduplex alloy, laminated composites of copper and iron and an extruded 50-50 Cu-Fe elemental powder composite was studied. Very low ductile-brittle transition temperatures were achieved in all cases, but for different reasons. In the microduplex alloy both the initiation and also the propagation of cleavage fractures appeared retarded by the very small in-terphase distances. In the composites, crack propagation through the sumples was prevented in most cases by delamination fractures perpendicular to the advancing cracks. These delaminations occurred at different regions and by different mechanisms in the various composites. In the extruded powder composite, de-lamination appeared to take place along preexisting flaws. In the crack arrest geometry of the laminated plates, delamination took place by localized shear fractures within the copper near the Fe-Cu interfaces. In this case delamination was enhanced by thicker laminate layers, and by having the resistance to shear failure of the copper sufficiently low compared to the toughness of the iron. BRITTLE fracture in engineering materials has long been a problem, and many different ways of preventing it have been considered. One method that has been of growing interest lately is to prevent crack propagation by the introduction of mechanical discontinuities into the structure. These discontinuities may act in several ways. They may simply act as crack stoppers. They may introduce secondary fractures such as de-laminations that deflect the initial crack into new, less damaging directions. Alternatively, they may subdivide a fairly large bulk sample that would have been loaded in plane strain, for example, into a number of subunits that are individually loaded in plane stress and thus are more resistant to fracture. Other mechanisms, or combinations of mechanisms, are also feasible. A number of methods exist for introducing mechanical discontinuities into a structure. Composites by their nature have discontinuities in structure, and numerous studies have shown that fracture propagation in materials of this type can be radically changed by suitable control of the composite parameters. Of particular significance to the present work are recent investigations of layered composites made by joining high strength steel sheets by various means.'-4 These studies have shown that through proper control of the mechanical properties of the bonds joining the sheets it was possible to introduce delamination fractures that markedly improved the overall toughness of the composites and in some cases completely prevented through-the-thickness fractures. Another technique for introducing structural discontinuities is simply to use a two-phase alloy. It has been recognized for many years that a small amount of a second phase may improve toughness either by homogenizing plastic flow and thus preventing localized stress concentrations that nucleate fracture, or by interacting with an advancing crack. In most of these studies of two-phase materials, the decreases in ductile-brittle transition temperatures produced by the second phase were relatively small. More recently, work on two-phase stainless steels having a very fine grain microduplex structure has shown that the presence of on the order of 40 to 50 pct of a tougher second phase may lower the ductile-brittle transition temperature of the brittle phase by approximately 300°F. 5-7 In these alloys delaminations were seldom observed. The tougher second phase appeared to minimize the ease of both the initiation and the propagation of cleavage fractures. These results show that both the composite approach and the microduplex alloy approach are effective methods of preventing brittle fracture. Therefore, it was of interest to compare the fracture behavior of a microduplex alloy with composites made from the two-phases that were present in the alloy. To simplify this comparison the 50 pct Cu-50 pct Fe system was selected for study. At low temperatures the equilibrium tie line phases in this system are essentially pure ferrite and pure copper. A 50-50 alloy was cast and hot worked to produce a microduplex structure. Two types of composites were studied; laminated structures prepared by roll bonding iron and copper sheets of the tie line compositions, and an extruded powder composite made from high purity elemental powders. The fracture behavior of these materials was then compared. EXPERIMENTAL PROCEDURE Alloy Preparation. The 50-50 Fe-Cu alloy and the components for the roll bonded composites were prepared by vacuum induction melting 30-lb heats using electrolytic grades of iron and copper as charge materials. A carbon boil was used to deoxidize the melts. Small additions of copper and iron were made to the iron and copper heats, respectively, to approximate

Jan 1, 1970

By N. C. J. Ros

The paper deals with pressure gradients occurring in flowing and gas-lift wells, a knowledge of which can be applied to the determination of optimum flow-string dimensions and to the design of gas-lift installations. The study is based on a pressure-balance equation for the pressure gradient. It appears that a pressure-gradient correlation of general validity must essentially consist of two parts-—one part being a correlation for liquid hold-up and the other part being one for wall friction. Dimensional analysis indicates that both liquid hold-up and wall friction are related to nine dimensionless groups. It is shown that in the field of interest only four groups are really important. On the basis of these four groups a restricted experimental program could be selected that nevertheless covered practically all conditions encountered in oil wells. This experimental program has been carried out in a laboratory installation. Three essentially different flow regimes were found. The pressure gradients in these regious are presented in the form of a set of correlations. Comparison of these correlations with a few available oilfield data showed excellent agreement. INTRODUCTION Prediction of the pressure drop in the flow string of a well is a widely known problem in oilfield practice. Accurate data on the pressure gradient of a simultaneous flow of gas and liquid in a vertical pipe are especially useful for the determination of optimum flow-string dimensions. It is well known that with moderate gas and liquid flows such a vertical string acts as a "negative restriction". The pressure drop decreases (1) when the throughput through a given pipe increases, and (2) when at a given throughput the cross-sectional area is decreased. The reason is that, with increasing velocities, the flow becomes more agitated so that the gas slips relatively more slowly through the liquid. With the resulting increase in gas content in the string, the static head decreases. When the area becomes very small, however, the high velocities entail great wall friction, which causes an increase in pressure drop. For a given flow, therefore, minimal pressure drop is obtained by using a certain cross section. This means that, in principle, each well can be provided with an optimum flow string for minimum pressure drop and, hence, maximum possible production rate. The procedure for the selection of the optimum string has been discussed by Gilbert.' A necessary tool in the procedure, however, is accurate knowledge of the pressure gradient to be expected for various values of the governing variables. Another application of pressure-gradient data lies in the field of gas-lift practice: they provide a means of determining the optimum gas-injection rate, optimum injection pressure and optimum injection depth. Much work has already been done in the study of the pressure gradient of vertical gas-liquid flow. Poett-mann and Carpenter2 presented a pressure-gradient correlation based on measurements in wells. This correlation has been found to provide accurate predictions in high-pressure wells and in high-production wells for flow through both tubing and annuli.2-5 However, when their method is checked on low pressure-low production wells or on wells with viscous crudes, serious discrepancies are found. As we shall see in the next section, this is due to the fact that their correlation factor, representing all irreversible energy losses, is given as a function of only one correlation group. Some important variables, such as gas-liquid ratio and liquid viscosity, are not incorporated in this group so that their specific effects are not accounted for. To study also the mechanism of vertical gas-liquid flow outside the ranges covered by the Poettmann-Carpenter publication and extensions, a laboratory investigation has been carried out. This study is founded on a pressure-gradient equation that is based on a pressure balance. To reduce the number of test runs required, a dimensional analysis has been carried out, followed by a selection of relevant dimensionless groups. These groups guided a subsequent experimental study, and with their aid the experimental program could be minimized while still covering the majority of the situations encountered in oilfield practice. In this paper the choice of a formula for the pressure gradient is discussed first. This is followed by a brief description of the experimental setup. Subsequently, the dimensional analysis is discussed and the relevant dimensionless groups are selected, resulting in the experimental program required. The general relationships of pressure gradient and liquid hold-up are then described; various flow patterns and a certain flow instability (so-called "heading") are discussed and a set of correlations is presented which shows a good agreement with the measurements and a few available field

Jan 1, 1962

Jan 1, 1956

Jan 1, 1938

Jan 1, 1938

Jan 1, 1921

By C. B. Post, G. V. Luerssen

It is generally recognized that non-metallic inclusions in steel come from two principal sources. First are the chemical reactions in the furnace, or in subsequent deoxidation, resulting in slag which does not free itself from the metal. Much information has been published concerning these chemical reactions and their control through proper attention to slag viscosity, composition of deoxidizers, and other qualities. The studies of this subject by C. H. Herty, Jr. and others through the medium of physical chemistry have yielded much information for the steelmaker. The second source is erosion of ladle refractories, such as lining brick, stoppers, nozzles and runners, causing entrapped particles of globules of fluxed silicate material. In contrast with the large amount of information available on the first source, relatively little has been published on the subject of erosion which, in the case of basic electric melted steel, is the principal source of nonmetallics. This is probably due to the fact that the problem was assumed to be one of simple mechanical erosion, which could be solved primarily by modification of ladle practices. Good improvements have been made by elimination of slurries in the ladle, better ladle and runner refractories, and more attention to pouring temperatures. It is doubtful, however, that this problem has been recognized in its true light since it is not one of simple mechanical erosion but rather one of chemical reaction between the metal and the refractories; and in this sense is as much a problem of physical chemistry as the reactions involved in the actual steelmaking process. The influence of ladle refractories on the resulting cleanness of steels was early recognized by A. McCancel who examined large inclusions in steels made by both acid and basic practices. His chemical analyses showed the large influence exerted by the manganese content of the steel on erosion of the ladle and nozzles used in those days. The presence of MnO in such inclusions led McCance to the hypothesis that both basic and acid steels react chemically with the ladle refractories so that small globules of fluxed refractories are carried in the stream into the molds. This early work of McCance was checked by one of the present authors on basic electric bearing-steel, and it was found that on steels containing as low as 0.40 pct manganese the fluxed surface of the ladle lining after delivering such a heat showed as high as 25 pct MnO by actual analysis. Furthermore, by lowering the manganese content of the steel to 0.20 pct, ladle erosion was decreased with a corresponding decrease in silicate inclusions in the steel. Limitations placed on the manganese content for the required inherent properties made it impossible to pursue this line further, and subsequent attention was concentrated on improved ladle refractories, care in keeping the ladle clean and free from loose refractories up to the time of tapping, and pouring the steel at optimum temperature. Our study of the chemical reactions at the metal-brick interface between steel and ladle refractories was revived in 1939 as a result of an experimental observation made on the cleanness of alloy steels of the SAE types. This observation showed that the relative cleanness of such steels made in basic electric arc furnaces of 12 ton capacity and poured in ingots ranging from 1100 to 2200 lb weight was determined to a large extent by the ratio of the manganese and silicon contents, provided other steelmaking variables such as tapping temperature, pouring temperature, pouring time, amount of aluminum added for grain size control, and degree of deoxidation in the furnace were kept reasonably constant. Detailed studies made on the deoxidation and slag practice during the refining period of basic electric furnace practice showed that these two variables exerted some influence on the resulting cleanness of steel in the form of bars and forgings. The important variable, the manganese-silicon balance, was not apparent until heats were made in succession by the best furnace practice kept under fairly rigid metallurgical control. Another observation pertinent to this work concerned the similarity in the microscope of slag particles causing magnaflux or step-down indications in subsequent rolled bars, and the patches of slag frequently seen on the surface of ingots. These patches are generally believed to come from the glassy metal-brick interface in the ladle and represent an entrapment of such glass (both from the ladle brick and nozzle) in the metal as it flows over the refractories in the neighborhood of the nozzle. These glassy particles are carried down into the mold with the liquid steel, and gradually coalesce into a slag "button" which floats on the surface of the steel as it rises in the molds. Periodically the button is washed to the side of the ingot where it is trapped between the surface of the ingot and the mold, later appearing as a slag patch on the surface of the ingot after stripping. Even though most of the small glassy particles coalesce into a slag button while the ingot is being poured, it is logical to suspect this step in the steelmaking process as being a source of slag lines large enough to cause trouble

Jan 1, 1950

By H. Leslie Bullock

From aluminum to zirconium, the quantitative preponderance of quartz as a gangue material is well recognized. lf this material is to be efficiently removed, its variations must be understood. Variations with temperature are especially important. Too little attention has been given to the thermal polarization of quartz. Under closely controlled conditions, electrostatic upgrading is very reliable. For efficient separation, contact charges must be fostered and charges due to radiation, surface coatings, or thermal polarization avoided. This paper lists thermal transition points of quartz and shows their effect on actual separations. Simple separation tests with all factors except temperature held constant are recommended for determining transition points. With silica making up more than 27% of the earth's crust, its oxides comprising more than 59% of all igneous rocks, and quartz accounting for most of the main free oxides, the mining engineer is in constant contact with quartz, which may occur as a valuable mineral to be purified or, far more frequently, as a gangue material to be removed as completely and economically as possible. As a means of effecting such purification or removal, dry beneficiation is becoming more and more desirable owing to local water scarcities, wet waste disposal problems, or freezing conditions. One method that has been gaining particularly rapid acceptance is electrostatic beneficiation, or the separation of dry free-flowing materials by means of opposite surface charges, differences in potential, or differences in conductivity. Electrostatic beneficiation dates back to the 1870's, but only in recent years have newly developed methods and apparatus and a growing knowledge of solid-state physics widened the field for its economical application. Because the term "electrostatic beneficiation" has been rather loosely used in the literature, it has come to include both electrostatic and electrodynamic procedures. Attracting type separators, however, in which oper- ation is based on differences of surface charge or potential, are truly electrostatic, because the separation occurs in a substantially static field set up between oppositely charged surfaces. Separations with this type of equipment may occur at potentials as low as 1000 v and seldom require potentials as high as 30,000 v. In the new contact charge dielectric separators1 the variation in charge is produced by continuous contact and separation of the particles in the moving feed stream and these charges are fostered by the use of non-conducting support and feed surfaces and by handling the feed in the form of streams of appreciable depth. This favors uniformity of feed and allows higher production rates. The distinctive surface charge differences are set up on the separation of the particles according to Coehn's Law,2 which states that equal and opposite charges are generated on the separation of any two materials in contact and that the substance having the highest dielectric constant will be positively charged. The basic contact charge concept is reliable, but all electrical charges are transient and modified by the electrical conditions of the surroundings. Pyro-electric, photoelectric and radiant effects may modify or totally destroy the contact charges necessary for efficient separation, or contact with conducting surfaces may neutralize them. Such hostile conditions must be carefully guarded against, since they have led to many costly failures in the past. The most consistent difference in surface charges to insure good separation is produced by repeated uniform contact and separation of particles in the moving stream. The thickness of the feed stream possible with this method reduces the effect of contact with the supporting surfaces, but as some contact is inevitable, the best results may be assured by having the dielectric constants of the supporting surfaces between the dielectric constants of the substances to be separated. In general, the hard smooth surface of quartz makes it an ideal substance for electrostatic separation from most minerals. For instance, with calcite, starting with a feed containing 1.9% acid insolubles, one can produce a concentrate containing 0.30% acid insolubles with a tailings containing 21.7% acid insolubles and a yield of 92.8%. The color can be held at 92 or above and the tint at 1.7 or lower. Working with specularite iron ore, laboratory work has given a concentrate of 68.8% Fe., with an iron unit recovery of 96.7%. Excellent results are also in pros-

Jan 1, 1969

Jan 1, 1923

Jan 1, 1929

Jan 1, 1923

By Frank Doxey

Louis A. Turnbull (U.S. Bureau of Mines, Washington, D. C.)—This paper is a well-organized concise discussion of progress in mechanization at coal mines in Nova Scotia during the last 50 years. It shows the perseverance and resourcefulness of those responsible for the production of high-quality coal essential to steel production in the area. The development of the Dosco miner and its use in longwall mining at the Sydney

Jan 1, 1955

Jan 1, 1959

By Arvid Holst Mortensen

The rational exploitation of deposits for cement manufacture requires evaluation of the material, the planning of the quarrying and the right choice of quarry machinery. By using a computer for all evaluations and planning work the optimal recovery of material is arrived at and a quarry layout - and machinery is decided upon. The result will be uniform production throughout the lift of the deposits using a rationally chosen quarry equipment.

Jan 1, 1977

By J. H. Keeler

AN alloy of zirconium containing 18 atomic pct Cb was found to be body-centered-cubic and readily deformable at room temperature. The behavior of this alloy provided an opportunity to determine if

Jan 1, 1957

Jan 1, 1913

By Reynold Q. Shotts

Nitric acid oxidation rate analyses of three coals, previously studied microscopically by the Bureau of Mines, revealed three components. Relative quantities agree with those found for the four components given by the Bureau and results are consistent with current ideas of coal constitution. Possible multi-component composition for bright coal and a reactivity-rank relation are suggested.

Jan 5, 1953

By W. V. Bluck, W. L. McMorris

Higher coal quality is being recognized in potentially lowering the cost of power as measured at the bus bar. Assessment of potential coal supplies for most power plants is now going beyond buying at the lowest delivered fuel cost. It is now taking into consideration other factors, such as handling, storage, pulverization cost, boiler fouling, post combustion cleanup, and waste disposal costs. New measurements of quality are being considered now by those producing and those consuming the fuel by assessing numerous variables in the total fuel cycle to achieve the lowest possible power costs.

Jan 1, 1986