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Part VII – July 1968 - Papers - Grain Boundary Penetration of Niobium (Columbium) by LithiumBy 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
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Institute of Metals Division - The Combined Effects of Oxygen and Hydrogen on the Mechanical Properties of ZirconiumBy D. G. Westlake
Polycrystalline tensile specimens of various Zr-0-H alloys have been tested at 298°, 178°, and 77°K. Solute oxygen and hydride precipitates in quenched alloys made individual contributions to the yield strength at 0.2 pct strain which combined to produce a resultant strength increment, a,., Ductility changes which were ohserved can he interpreted in terms of the various oxygen and hydrogen concentrations, testing tem -peratures, and dispositions of the hydride. ADDITIONS of oxygen in solid solution were known to increase the yield and tensile strengths of polycrystalline zirconium as early as 1951.' More recently, the critical resolved shear stress (CRSS) for prism slip in zirconium single crystals was also shown to be affected by the solute oxygen impurity.' This latter work also demonstrated that large increments of strength could be contributed by the finely dispersed zirconium hydride precipitates that are present in quenched Zr-H alloys.3 It was concluded that the combined strengthening due to alloying could be expressed by where to is the increase in the CRSS due to solute oxygen alone and TH is the increase due to finely dispersed hydride precipitates. Eq. [I] is analogous to one used to express the combined strengthening effects of work hardening and neutron radiation damage.4 Eq. [1] was verified only indirectly and for only small amounts of the impurities—up to 0.14 at. pct 0 and 0.63 at. pct H. The present investigation was undertaken to obtain a more direct verification of the validity of the form of Eq. [1] for this system and also to determine the combined effects of oxygen and finely dispersed hydride precipitates on the tensile strength and ductility of polycrystalline zirconium. EXPERIMENTAL PROCEDURE Tensile specimens were machined from the same rolled billet of Kroll zirconium used in the earlier study.' These measured 38 by 4.7 by 0.5 mm and had 10-mm gage lengths which were 2.8 by 0.5 mm. Each specimen was ß-annealed in vacuo at 1173°K for 15.5 hr and a-annealed at 1073°K for 4 hr to D. G. WESTLAKE, Member AIME, is Associate Metal l ur-gist, Metallurgy Division, Argonne National Laboratory, Argonne, III. Manuscript submitted July 17, 1964. IMD______________ give an equiaxed structure with grain diameters averaging 0.06 mm. Oxygen was added by allowing the metal to react with a known quantity of oxygen during the 0 anneal and known quantities of hydrogen were added during the a anneal. Each alloy was encapsulated in Pyrex under vacuum, annealed at 873°K for 4 hr, quenched into ice water, and polished by immersion in a solution of 46.75 vol pct H2O, 46.75 vol pct concentrated HNO3, and 6.5 vol pct HF (49 pct) at 298°K. Special heat treatments given to a few specimens are described in the results below. Tensile tests were done on an Instron machine and were begun within 20 min after the quench, except where specified otherwise. Tests at 298°K were in air, at 178°K in acetone, and at 77°K in liquid nitrogen. All tests were at a strain rate of 8x sec-1. RESULTS AND DISCUSSION Yield Stress at 298°K. The compositions of alloys and the corresponding yield stresses (0.2 pct strain) are given in Table I. A plot of the yield stresses of the oxygen alloys, A, B, C, and D, indicates that varies linearly with CO1/2, where Co is the oxygen concentration, Fig. 1. This is in accord with Fleischer's6 theory for solution strengthening if the oxygen atoms do not cluster, or the cluster size remains constant with increasing oxygen concentration. In Fig. 1, it appears that if one could prepare some oxygen-free zirconium its yield stress would be very low. Therefore, we shall assume that for the oxygen alloys is equivalent to O0, the strength increment contributed by the presence of oxygen. The relationship between0.2and Co is expressed by 0.2 = 31.3 CO1/2, when the yield stress is in kg per sq mm and the concentration is in at. pct. Each of the hydrogen alloys, Al, A2, A3, and A4, contained 0.081 at. pct 0 as an impurity. In Fig. 1, it appears that this small amount of oxygen makes a significant contribution to the strength which cannot be ignored when we evaluate the contribution of the finely dispersed hydride. Let us assume the validity of the following equation: a0.2 = (a2o+a2R)1/2 [2] which is analogous to Eq. [I] for single crystals, and calculate values of UH for the hydrogen alloys by using the experimental values of 0.2 and o (0.081 at. pct) = 8.9 kg per sq mm. For 0.36 at. pct H, oH = 6.47; for 0.72 at. pct H, OH = 11.30; for 2.16 at. pct H, OH = 19.4; and for 3.60 at. pct H,
Jan 1, 1965
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Drilling and Production Equipment, Methods and Materials - Factors Involved in Removal of Sulphate from Drilling Muds by Barium CarbonateBy P. G. Carpenter, H. B. Fisher, W. E. Bergman
The conditions under which barium carbonate can be used to remove sulfates from drilling muds are limited The amount of sulfate remaining in solution in the system after treatment with barium carbonate is shown to be a function of the concentration of the carbonate and barium ions and the concentration of other electrolytes. Barium hydroxide may advantageously replace barium carbonate when the contamination is not entirely due to anhydrite (calcium in the system is then stoichiometrically less than sulfate) or when the carbonate concentration is high. The effect of substances such as quebracho, phosphates, and chromates, which form complexes or precipitates with barium, is discussed. INTRODUCTION As the complexity of the operations in drilling for oil has increased, more attention has of necessity been directed to the problems pertaining to the maintenance of good drilling mud properties. As a result, chemical treatment of muds has become an important factor in recent years. Some of these treatments have been designed to eliminate the deleterious effects of contaminants in aqueous mud systems by precipitation or other means. The most common of substances encountered during drilling include sodium chloride, cement, and calcium sulfate while various other contaminants: usually in small amounts, may be introduced from the water, clays, and other materials used in preparation of the mud. In certain cases, for example where continued salt-water flow is encountered or massive anhydrite is drilled, special muds may be used so that the physical properties of the mud will remain satisfactory for drilling. In other cases, it is desirable to remove the contaminants so that soluble electrolytes in the system are maintained at low values. For sulfate contamination, the conlmon practice in the field is to add barium carbonate to precipitate the sulfate as barium sulfate Ordinarily such a procedure gives satisfactory results. There have been important instances, however, where addition of barium carbonate was not effective in removal of soluble sulfates from drilling muds. and it is to these cases that the present paper is directed. While it is generally known that barium carbonate is not always effective in removing soluble sulfates from drilling muds, certain inconsistencies appear in the literature as to the limitations of its use, and little explanation for the limitations are given. Varnell and Kimbrel state that "the treatment (with barium carbonate for removal of sulfate) is simple and consists in maintaining a pH of 9 with caustic soda and quebracho." They caution that concentrations of quebracho greater than 1 lb./bbl. may inhibit the reaction. In another publication', a pH of 10.5 is considered "the maximum desirable," and the indication is that as much as 2.5 lb. quebracho per barrel may be present in the particular mud under discussion. Lancaster and Mitchell5 state that appreciable amounts of phosphates in the mud will inhibit the reaction with barium carbonate and that the phosphate treatment should be discontinued at least 24 hours before addition of the carbonate. Experimental work was initiated to ascertain the factors involved in using barium carbonate for the removal of sulfate contamination in drilling muds. While the experimental data herein reported are limited, they focus attention on the pertinent factors which must be considered for successful treatment. These factors are discussed from a practical and a theoretical view, the latter being supported by equilibrium data found in the literature. Further, it will be appreciated that the factors involved in this specific study will be closely analogous to those in certain of the other chemical treatments which involve a precipitation of the soluble contaminant. A thorough comprehension of these factors should result in a more fruitful application of this type of chemical reaction to the treatment of drilling muds. EXPERIMENTAL A. Reagents Two muds were used during this investigation. For one series of tests, bentonite suspensions were prepared by dilution of a stock suspension containing 8 per cent by weight of bentonite (Aquagel). For another series, a 6.4 per cent ben-tonitic mud weighted to 9.7 lb./gal. with barium sulfate (Mag-cobar) was used. Distilled water was used in all preparations. The quebracho (72% tannin extract) was obtained from the Thompson-Hayward Co. of Tulsa and contained 11.4 per cent moisture (105 C.). All other materials were reagent grade, and concentrations were corrected for water of crystallization, if any. All concentrations are expressed in pounds per barrel (42 gallons). B. Technique The systems — either mud or water — were contaminated with either sodium or calcium sulfate after treatment with the desired amounts of sodium hydroxide and quebracbo. For treatments with barium carbonate an approximately 3-fold excess (5 lb./bbl.) was used over that computed to be required to precipitate all the sulfate as barium sulfate. Barium hydroxide was used in concentrations of 2 lb./bbl. — about
Jan 1, 1949
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Part VII – July 1969 - Papers - The Mechanical Properties of Some Unidirectionally Solidified Aluminum Alloys Part II: High Temperature Tensile PropertiesBy J. R. Cahoon, H. W. Paxton
The possibility of using unidirectionally solidified, two-phase alloys as an approximation to fiber composite materials is investigated. The short-term me.chanical properties and failure modes of unidirectionully solidified A1 (rich)-Cu alloys containing ap -Proximately 0, 17.5, and 27.7 vol pct of 0 phase 'fibers" are determined at temperatures from 25" to 500" and compared with those obtained for conventionul SAP alloys. In a previous publication,' hereafter referred to as I, the possibility of understanding some of the room-temperature mechanical properties of unidirectionally solidified castings was explored. For Al(rich)-Cu and Al(rich)-Mg two-phase alloys over a substantial range of compositions, the yield and ultimate strengths and common ductility measures were very adequately predicted from the principles of fiber strengthening4 and the analysis of ductility outlined by Gurland and Plateau." The results obtained in I suggest the possibility of using unidirectionally solidified, two-phase alloys to simulate fiber composite materials where the inter-dendritic second phase or constituent acts as the reinforcing material. Recent attempts concerning the fabrication of fiber conlposites have concentrated on producing composites with a good bond between fiber and matrix and with very long fibers so that their maximum contribution to the strength of the composite may be realized. However, these objectives are difficult to attain in practice and present fabrication processes are either extremely laborious or costly.13 The slow, unidirectional solidification of eutectics has received considerable attention as a method for producing composite materials. 5,6 This method can fulfill both of the above objectives but it is currently laborious, expensive, and has the additional disadvantage that the volume fraction of reinforcing phase cannot be easily varied. On the other hand, unidirectionally solidified, two-phase alloys, also with a good bond between the phases, are relatively easy to make and the volume fraction of reinforcing "fibers" can be easily varied by changing the average composition of the alloy. The disadvantage of the cast alloys is that the mechanical effectiveness of the "elongated interdendritic reinforcements" (EIR)* may be reduced due to their rela- tively short lengths, the w factor in Eq. [2] of I. However, if the EIR have a high strength their contribution can be considerable. For composite materials containing discontinuous cylindrical fibers of various lengths the ultimate strength is given by1 where it is assumed that the composite fractures when the fibers fail. In Eq. [I], a, is the stress in the matrix just prior to failure of the composite, Vf is the total volume fraction of fiber reinforcing constituent, Vf(l+) is the volume fraction of fibers whose lengths exceed the critical length, I,, which is defined as the shortest length of fiber in which the stress can build up sufficiently to break the fiber. af is the fracture strength of the fiber material, w is a factor accounting for the discontinuity of those fibers whose lengths exceed I,, 1-/d is the average aspect ratio of those fibers whose lengths are shorter than I,, and t is the shear stress in the matrix at the fiber-matrix interface. The factor w is dependent on the length of the fibers and also on whether deformation of the matrix occurs plastically or elastically. However, for a given length of fiber, w is smaller when elastic deformation of the matrix is assumed.' It is of interest to consider the properties of simple unidirectionally solidified, two-phase alloys at elevated temperatures in view of the possibility of using suitable modifications for high temperature service. Knowledge of the creep behavior of these materials is still rudimentary (although under active investigation) and the present paper concerns itself with short time tensile properties of some alloys similar to those investigated in I (i.e., unidirectionally solidified Al(rich)-Cu alloys). Unidirectionally solidified alloys containing 5.6, 17, and 23 wt pct Cu were tested parallel to the direction of solidification at temperatures from 25" to 500°C. In the present investigation, the alloys were homogenized for 2 days at 535°C giving a matrix of homogeneous a phase (5.2 wt pct Cu) and an interdendritic constituent (EIR) which was completely Q phase (53 wt pct Cu). EXPERIMENTAL Alloys of nominal composition 5.6, 17, and 23 wt pct Cu (containing approximately 0, 17.5, and 27.7 vol pct 8 phase, respectively, after homogenization at 535°C) were prepared by melting 1200 g of A1 (99.99 pct) in a high purity graphite crucible and adding the appropriate amount of freshly cleaned copper chips (99.9 pct). The molten alloy (at 700°C) was poured into a preheated graphite mold (also at 700°C) and the ingot unidirectionally solidified by impinging water on the steel baseplate of the mold. The alloy was degassed immediately
Jan 1, 1970
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Miscellaneous - Mineralogical Studies of California Oilbearing Formations, I - Identification of ClaysBy W. C. Merrill, P. G. Nahin, A. Grenall, R. S. Crog
A progress report of an experimental investigation into the role of clay in reservoir performance is presented. The Paper gives some of the reasons for considering clay as a significant component and outlines the objectives of a broad field of stud) which it is intended to pursue. Descriptions of the analytical methods used are given; these include X-ray diffraction. elec tron miscroscopy, thin section petrography, infrared spec-troscopy, and cation exchange analysis. A suite of the more important clay minerals has been assembled and characterized l~y these methods for use as standards in core analysis. From the data obtained it appears that although no one method of analysis is diagnostic for all of the clay minerals the infrared technique shows considerable promise in this direction. For the present, one or more supplementary methods should be used to confirm the clay mineral identifications. The methods of analysis are applied to field cores taken from repesentative and widely differing strata especially as regards their susceptibility to damage by fresh water. well.; completed in the stevens and Gatchell zones in San Joaquin valley are I,articularly clear-cut examples of this behavior with stevens zone wells being more adversely affected by fresh water. cores from these zones have been studied and are discussed. It appears that differences in this behavior can be ascribed to differences in the nature of the contained clays. The value of the infrarecl spectra of the clay fractions in establishing the identity of the predominant clay minerals is given particular emphasis. INTRODUCTION It is a challenge to the technical resources of the petroleum industry that when the economic limit of production is reached, from 40 to 70 per cent of the oil in California reservoirs remains unproduced even by use of the best presently known methods of recovery. The magnitude of this abandoned volume of oil can be appreciated when it is considered that to 1950 in excess of 8 billion bbll has been produced from California reservoirs with estimated economically recoverable reserves in known fields and pools totaling nearly 4 billion bbl.24 If for every barrel of oil produced there is at least another barrel still in place, it is evident that the revenue obtained from the recovery of only a .few per cent of this volume would repay the cost of the required research manyfold. From well completion experience. production behavior, and a growing body of laboratory data it now appears certain that the mineral composition of a producing stratum has an important bearing on the productivity and ultimate yield. In addition to the organic component and water, the cores con,ist of gravel, sand. silt, and clay" in diverse variety of (a, composition and (b) texture. It is the composite effect of these two factors which is probably responsible in large measure for the way in which the oil flows to the well. The role of the clay and fine-size accessory minerals is not clear but there is a growing opinion, based on their physical and chemical properties, that it is a significant one. of particular importance are the prime facts: 1. The silt and clay fractions of the reservoir matrix possess the highest surface area per gram, and 2. The silt and especially the clay fractions are the most chemically reactive of the inorganic constituents present. Only within the last few years has the knowledge of clay mineralogy and the techniques of identifying the clay minerals reached such a stage as to enable reliable inquiry into the composition of argillaceous sediments.2,8,10,11,12,16,26 It is the purpox of this and succeeding papers to add to the fund of information on the role which these materials play in the production of petroleum from California formations by correlating their presence and associated properties with observed reservoir behavior. In the present paper attention is directed to their possible influence on damage by fresh water. OBJECTIVES The attack on this problem divides naturally into two broad phases: 1. Determination of the nature of the clays and their relationships to the other mineral components, and 2. Determination of the physico-chemical relationships between the clays and the interstitial fluids. In the work described in this paper the emphasis has been on phase 1, which stems logically from the necessity of identifying and understanding the materials to be dealt with in Phase 2. Based on the authors' present opinion that not all of the minerals which occur in oil-bearing formation are of equal importance in their effects on the flow and recovery of oil, it was decided to focus attention first upon the clay minerals content and then. later perhaps. work into the field of the normally larger size non-clay minerals and fractions. The
Jan 1, 1951
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Institute of Metals Division - Dislocation Collision and the Yield Point of Iron (With Discussion)By A. N. Holden
A DISLOCATION mechanism has been described by Cottrell' by which metals can yield locally, I. form Liiders bands, giving rise to a characteristic stress-strain curve with a sharp yield point and appreciable strain at constant or decreasing stress. It is undoubtedly the best mechanism that has been suggested to date." In its present development, however, the dislocation mechanism provides a more satisfying explanation for the sharp yield point than for the extensive localized flow occurring at the lower yield stress. The primary objective in this paper is to extend the dislocation mechanism to account for localized cataclysmic flow by a dislocation collision process and to give experimental evidence to support such a process. Only the yielding of iron containing carbon -will be discussed, although other metal-solute systems are known to behave similarly. Cottrell Mechanism In brief, Cottrell explains the yield point in the following way: The dislocations in iron which must propagate to produce slip usually lie at the center of local concentrations of carbon atoms, since segregation about these dislocatlons relieves some of the local stress resulting from them. A dislocation surrounded by a "cloud" of carbon atoms is thus anchored, and a higher stress is required to set it in motion than to move a free dislocation. Considering all available dislocatlons to be anchored in this fashion, the iron exhibits a yield point when the first dialocations break free and move through the lattice causing slip. This first breaking away of a dislocation enables other dislocations to break loose by "interaction" and the process becomes a cataclysm producing local deformation or Luders bands. The yield point in the stress-strain diagram for iron is absent in freshly deformed material, but returns gradually with time; the phenomenon is one aspect of what is called strain aging. The rate at which the yield point returns following straining depends on the temperature of aging. According to Cottrell the rate of return of the yield point in strained iron is limited by the rate of diffusion of carbon at the aging temperature, the mechanism is onr: of reforming the solute atmospheres around carbon-free dislocations that had stopped moving coincident with the removal of stress. If the specimen is retested immediately after straining and unloading, carbon will not have had time to diffuse to, and re-anchor, dislocations and the yield point will not occur. The carbon diffusion limitation for the rate of strain aging apparently applies if the criterion for strain aging is either the change in hardness" or the change in electrical resistance" of the strained speci- men with aging time. The possibility exists, however, that the yield point actually returns to strained iron at some rate other than that deduced from hardness or electrical resistance data. Therefore, as a preliminary experiment, the rate of yield point return in a rimmed sheet steel strained 6 pct in tension was measured at 27°, 77°, and 100°C. A plot of yield-point elongation for each of these temperatures against aging time appears in Fig. 1. The aging process is described by curves which rise to a plateau value of elongation that seems independent of temperature, but at a rate that depends on temperature. Very long times lead to a further rise in the yield-point elongation above the plateau value. However, if the later increase in yield-point elongation is ignored and the log of the time to reach half the plateau value of elongation is plotted against 1/T, a straight line results for which an activation energy of about 25 kcal pel- mol may be assigned. Within the accuracy of this sort of experiment this is approximately the activation energy for the diffusion of carbon in iron (20 kcal per mol), and the carbon diffusion limitation suggested for the yield-point return on strain aging is valid. The Cottrell mechanism thus explains in a qualitative manner the occurrence of a yield point in iron and its return with strain aging. It fails, however, to explain some of the other experimental observations that have been made of the yielding behavior of iron. For example, it is known that the yield point in iron becomes less pronounced with increasing grain size. Annealed single crystals of iron have very small yield-point elongations .if indeed they have any,' compared to a polycrystalline steel. If the only requirement for a yield point is that the dislocations in the lattice of the annealed. material be anchored by carbon atoms, the difference in the behavior of single crystals and polycrystals is not explained. That a dislocation mechanism may be entirely consistent with little or no yield point in an annealed single crystal will become apparent later when dislocation interaction is discussed. Strain aging produces a definite yield point even in single crystals. This accentuation of the yield-point phenomenon in single crystals after strain
Jan 1, 1953
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Producing–Equipment, Methods and Materials - Evaluation of Valve Port Size, Surface Chokes and Fluid Fall-Back in Intermittent Gas-Lift InstallationsBy K. E. Brown, F. W. Jessen
By utilizing an 8,000-ft experimental field well equipped with 10 gas-lift valves and 10 Maihak pressure recorders, gas-lift tests were conducted with port sizes ranging from 5/16 through I in. The well was equipped to provide accurate means of measuring surface pressures, temperatures, quantity of injection gas and fluid production. The tests were conducted in 2%-in. OD tubing, and the well was making 95 per cent water. A complete evaluation of gas-lift-valve port sizes shows the relationship of per cent recovery, gas-liquid ratios, minimum pressure created at the operating valve and horsepower requirements for each port. The length of time necessary for the fluid in the tubing to reach equilib.rium conditions after each cycle was recorded. Fallback of fluid at depths of 477, 969, 1,685, 2,493 and 4,290 ft was noted. For each port size, pressure loads of 2.50, 300, 350, 400 and 450 psi were lifted with a valve operating at approximately 550 psi at 6,000 ft. Gas-liquid ratios for each load were varied from excess gas to a gas volume per cycle whereby the load failed to reach the surface. Numerous curves are presented in evaluating the accumulated dara. The results show a 1-in. port to be the most efficient under all conditions. The production of intermittent liquid slugs against different-sized surface chokes was evaluated. These tests were conducted from a 7/16-in. ported valve at 4,072 ft. Tests indicate that, when possible, a %-in. in diameter choke or larger should be used at the surface. In the past few years most of the advancement in gas-lift operations has been made in continuous-flow operations. Yet, it is estimated that at least 70 per cent of the wells on gas lift in the United States are of the intermittent type. Since the term "slug flow" is sometimes used in both intermittent- and continuous-flow operations, it would be well to distinguish between the two types of flow. Continuous-flow gas lift is defined as a method whereby the fluids are produced at a continuous rate at the surface. This generally requires a continuous injection of gas through a surface choke; however, various other control devices sometimes are installed to eliminate freezing, to shut-off gas during natural flow periods, etc. The actual flow of fluids in the tubing may be of the slug type (one of many flow patterns known to exist in continuous flow). Intermittent flow is defined as a method of gas lift whereby the liquid is produced in separate piston-type slugs. Perhaps this type of flow could best be thought of as a ballistic-type flow where the liquid leaves bottom as a piston, propelled by a slug of expanding gas. Gas generally is injected through some type of control at the surface at predetermined intervals. However, the valve may have characteristics whereby gas can be injected through a small choke and still result in a ballistic-type flow. The purpose of the experimental work was to evaluate the most efficient port size to be used on the operating valve for the ballistic type of lift and, in addition, to establish the importance of utilizing a surface choke large enough to allow slugs to be produced without detrimental effects. This work is part of a compre- hensive study of both intermittent-and continuous-flow gas lift, representing a joint project conducted by the Ohio Oil Co., the Sun Oil Co., Otis Engineering Corp, and The U. of Texas. The problem of evaluating port sizes has been given little previous attention. Some work undoubtedly has been done which has not been published to date. Some tests were conducted when the wireline, mechanically-opened valve (Nixon) first came on the market. This valve was capable of utilizing full tubing area as its port size. It is known that this was a very efficient valve, but to the authors' knowledge the results of tests have never been published. EXPERIMENTAL EQUIPMENT These tests were conducted on an actual field well, the Ohio-Sun Unit Well No. 2-E, in the North Markham-North Bay City field, Matagorda County, Tex. The well incorporated 23/8-in. OD tubing and produced 95 per cent water. Since the running of equipment was to be quite elaborate and expensive, a well was selected in which both intermittent- and continuous-flow tests could be conducted. This particular well was capable of producing in excess of 1,000 B/D of liquid (95 per cent salt water), yet with a 3/64-in. in diameter bottom-hole choke, production was controlled to 82 B/D. Most of the intermittent tests were conducted at this low rate. Figs. 1 and 2 show all the surface and down-hole equipment. As can be seen, every attempt was made to insure that ample equipment was available for reliable testing procedures. Fig. 1 shows the surface testing equipment. The input gas was controlled first by a regulator, then
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Reservoir Engineering - General - Evaluating Uncertainty in Engineering CalculationsBy R. C. McFarlane, T. D. Mueller, J. E. Walstrom
In evaluating uncertainty, experiments are usually performed repeatedly and then conclusions are drawn from the distribution of results. With the advent of high-speed electronic computers, it is possible to perform experiments using mathematical models constructed to simulate complex experiments or operations. Statistical methods are then applied to the results of the simulated experiments. This procedure forms the busis of this paper. Demonstrated is the need for properly accounting for uncertainty in petroleum engineering problems. How uncertainty affects solutions is evaluated in three example illustrations. The method used to evaluate uncertainty in petroleum engineering studies is the Monte Carlo simulation procedure.'-" INTRODUCTION The solution to most technical problems may be derived from interrelationships among several quantities called variables or parameters. There may be only a few variables or several hundred. Interrelationships among parameters may be explicit or implicit, well established or only approximate. Some variables that fully or partially depend on the magnitude of others are called dependent variables. Input variables for most practical problems are not precisely known; there is usually an uncertainty in their value. The degree of uncertainty may vary from one variable to another. Variables that are known accurately are called determinates.' For instance, the gravity of crude obtained from a particular pool may be known precisely, and therefore is a determinate. The degree of precision with which a quantity can be determined increases as data describing the pool are accumulated during the development of the field and the producing life of the pool. The uncertainty of a parameter may result from difficulty in directly and accurately measuring the quantity. This is particularly true of the physical reservoir parameters which, at best, can only be sampled at various points, and which are subject to errors caused by presence of the borehole and borehole fluid or by changes that occur during the transfer of rock and its fluids to laboratory temperature and pressure conditions. Uncertainty may also result in attempting to predict future parameter values. This type of uncertainty is particularly evident in investment analyses involving future costs, prices, sales volumes and product demand. Uncertainty in the solution to investment problems is often called risk, and its study is called risk analysis.' Uncertainty also enters into biological and sociological analyses in which indeterminate factors are often important due to limited control of the experimental material. It is customary, in evaluating uncertainty, to perform repeated experiments and to draw conclusions from the distribution of the results of these experiments. With the advent of the high-speed electronic computer, it is possible to construct mathematical models which simulate complex experiments or operations and to perform the experiments repeatedly, utilizing the models. Statistical methods are then applied to the results of the simulated experiments This method forms the basis of the investigation reported here. PROBABILITY DISTRIBUTIONS FOR VARIABLES The uncertainty in the value of a variable may be indicated by a probabilistic description accomplished by expressing the quantity by a probability distribution. Many recognized probability distributions can be used to describe physical quantities. Recent studies used various types of distributions to describe core analysis data.',' However, for the examples in this paper, the uniform and triangular distributions are believed to reasonably approximate the data used (Fig. 1). The uniform distribution confines the variable between an upper and a lower limit. The variable may lie anywhere between the two limits. This distribution is used when no one range of values for a variable is more probable than any other, but information or intuitive reasoning indicates the variable will lie somewhere between the chosen limits. The triangular distribution is used for a variable when more data are available to indicate a central tendency of distribution. This allows postulating a "most likely" value to the distribution and upper and lower limits. In this case, as for the uniform distribution, the variable is not expected to assume a value less than the lower limit or greater than the upper limit. However, with improved quality of data it can be postulated that the variable will tend to assume a value close to the most likely value, and that there will be a decreasing probability for values away from the most likely value. The area under either of these probability distributions is equal to unity since it is assumed that there is a 100 percent probability that the variable will lie somewhere under the curve. An ordinate erected at any particular value of the variable divides the area under the curve into two parts: the area to the left of the ordinate represents the probability that the value of the variable will be equal to or less than the value of the variable at the position of the ordinate, and vice versa. The probability is zero that the variable will have any specific deterministic value. If two ordinates are drawn for any two values of the variable, the probability that the variables will have a value lying between these ordinates is equal to the area under the curve lying between the ordinates.
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Iron and Steel Division - What is Metallurgy?By J. Chipman
There is no better way of paying tribute to the memory of a scientist than by developing and carrying forward those ideas which he has contributed to science and which are for us the very essence of his immortality. For a lecturer who has not had the great privilege of stdying under Professor Howe or 'ven of knowing him in person, these ideas must be transmitted through the printed word. It is our great good fortune that Professor Howe left to us a rich heritage of publication, not only in his classic monograph on the "Metallography of Steel and Cast Iron" but in a wealth of earlier hooks and papers in the transactions of this Institute arid of other scientific and engineering bodies. An outstanding characteristic of this published record is the great breadth of interest and of vision which it portrays. His was riot a narrow specialization in only the scientific aspects of ferrous metallographg. On the contra1y many of his important contributions had to do with a far broader field of metallurgicial endeavor. He insisted that his students be well grounded in 1 he fundamentals underlying the whole field and not led into the narrow groove of specific applications. Among his first major publications we find papers on copper smelting, extraction of nickel, the efficiency of fans and blowers, thermic curves of blast furnaces, the cost, of coke, and the manufacture of steel. These are the papers of a metalhurgical engineer and it was among engineers that Henry Marion Howe made his early and well-merited reputation. These early engineering contributions display very clearly the strongly sctientific inclination of their author. The classic work on "The Metallurgy of Steel" published in 1890 contains a thorough and critical discussion of all that was known at the time concerning the alloys of iron and of what we would now call the physical metallurgy of steel. In addition it describes steel-making processes in use and some that had become obsolete, and points out in critical fashion the reasons for success and failure. Steel mill design and layout were included as well as some pertinent discussion of refractories. The book is indeed an embodiment of one of Howe's outstanding characteristics—breadth. It is both the science and the engineering of steel production as known in that day. One of Howe's earliest technical papers was entitled "What is Steel?" That was nearly seventy-five years ago when many new processes and new kinds of steel were being developed. The time was ripe for such a question and the answers which Howe was able to give were helpful in understanding the phenomena of heat treatment. Twenty-five years ago Professor Sauveur repeated the question as the title of the first Henry Marion Howe Memorial Lecture. It seemed to him that this question, "What is Steel?," had served as Howe's motto throughout the remainder of his life. Today I shall present for your consideration a question of another sort: "What is Sletallurgy?" Perhaps it is not too much to hope that in the answer we may obtain a clearer and possibly broader view of the nature of our science and our profession. The time is ripe for giving careful consideration to what we mean by metallurgy. If our Metals Branch is to become in fact an American institute of Metallurgical Engineers, it is essential that we understand what is meant by metallurgical engineering. I am convinced that the best interests of the profession have not been served by a narrow interpretation of these terms. We must now place emphasis on the breadth of metallurgy as a science and as an engineering profession. With its usual brevity and wit. Webster's dictionary definesmetallurgy as "the science and art of extracting metals from their ores, refining them and preparing them for use." I shall riot assume that the words "science" and "art" and "metal" are so well understood as to require no defining but others among our contemporaries are better qualified than either your lecturer or the dictionary to present the broad meanings of these terms. When we say that metallurgy is among the oldest of the arts we are not classing it with painting or sculpture or music but rather with the making of tools or weapons or the building of bridges or chariots or cathedrals. In short we are saying that metallurgy is among the oldest of the engineering professions. The question " What is metallurg ? " has been one of rather more than ordinary concern to those of us who have the task of developing a curriculum for the education of students in this field. This development has been going on in a number of universities over a period of some years. but there seems to be as yet no unanimity as to what such a curriculum should contain. I believe there is fairly complete agreement that it must be founded upon sound
Jan 1, 1950
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Extractive Metallurgy Division - Low Pressure Distillation of Zinc from Al-Zn AlloyBy M. J. Spendlove, H. W. St. Clair
The problem frequently arises, particularly in refining metals or smelting scrap metals, of separating metals in the metallie state. Many metals may be separated by taking advantage of their difference in vapor pressure. Such separations can be made at atmospheric pressure, but the separations are much more selective and can be carried out at considerably lower temperatures if the distillation is done at pressures of a few millimeters or less in an evacuated enclosure. Until recently, this has not been considered feasible as a metallurgical operation, but the recent improvemcnts that have been made in vacuum technology have broadened the applicability of vacuum processes and have prompted re-examination of low-pressurc distillation of metals as a practicable process. The distillation of zinc from lead is one separation that has already been reduced to practice.l This paper is the first of a series of studies being made on separation of nonferrous metals by distillation at low pressures. Although these experiments were confined to the separation of zinc from aluminum, the significance of the results is by no means confined to these two metals. The purpose has been to investigate a metallurgical technique rather than merely to devise a means of separating specific metals. The experimental work on distillation of zinc from zine-aluminum alloys at reduced pressure grew out of earlier work on distillation at atmospheric pressure.2 The earlier work indicated that it would not be practicable to decrease the zinc in the alloy much below 10 pct owing to the high temperature required. Therefore attention was turned to distillation ah low pressures, at which lower temperatures are required. After preliminary tests were made in a small, evacuated tube furnace, a larger furnace having a capacity of 100 to 150 Ib of metal per charge was constructed. Distillation tests were first made on pure zinc and then on aluminum-zinc alloys of various composition. Particular attention was given to the limit to which zinc could be reduced in the residual metal. Data were also taken on the rate of evaporation, and heat balances were made for both the crucible and the condenser. Distillation Furnace The vacuum-distillation unit is illustrated schematically in Fig 1. The major components are the induction furnace, the condenser, the vacuum system, and the power-conversion unit. Power is supplied to the induction furnace from a 50-kw 3000-cycle motor-driven alternator. The pressure in the furnace is reduced by a vacuum pump having a nominal pumping speed of 10 liters per sec. When in operation, the metal vapors travel upward from the furnace to the water-cooled condenser where they are collected in amounts of 50 to 100 lb. The condenser is removed with aid of an electric hoist. When the system is under vacuum, the condenser is made self-sealing by a rubber gasket between the smooth-faced, water-cooled flanges at the top of the furnace and the bottom of the condenser. The pressure of the atmosphere is more than sufficient to insure sealing. At the conclusion of an experiment, the residual metal can be removed from the furnace by removing the condenser and tilting the furnace with the electric hoist. The metal was cast into the molds carried on a mold truck. A photograph of the furnace and auxiliary equipment is shown in Fig 2. The details of the vacuum furnace are illustrated in Fig 3. The furnace proper is made vacuum-tight with rubber gaskets placed at each end of a fused quartz cylinder. A clamping plate at the bottom and a ring at the top are made to squeeze the rubber between the metal and the end of the quartz tube. A large graphite crucible placed inside the quartz cylinder is thermally insulated and physically supported by refractory insulating bricks. A thermocouple in a quartz protection tube is located at the bottom of the crucible: the leads pass through a rubber seal in the bottom plate. The supporting structure for the furnace is an angle iron frame with transite board sides. The condenser is made in the form of a water jacketed cylinder with an opening to the vacuum line at the top. The bottom has a projecting skirt inside the machined flange to provide additional cooling for the rubber gasket. Condenser sleeves are made in the form of two semicylindrical pieces of sheet metal that fit snugly inside the cooling jacket. The split sleeve facilitates removal of the condensate. Measurement of Temperatare and Pressure The metal temperature was measured by a platinum-platinilm rhodium thermocouple inserted in a well extending up into the bottom of the graphite crucible. During rapid evaporation there is a wide difference in temperature between the surface and the main body of metal in the crucible because of the large amount of heat that must be conducted to the surface to supply the heat of evaporation. The heat of
Jan 1, 1950
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Part VII – July 1969 - Papers - Nitrogenation of Fe-Al Alloys. I; Nucleatin and Growth of Aluminum NitrideBy H. H. Podgurski, H. E. Knechtel
Annealed Fe-Al alloys do not react readily to form AlN when held at 500ºC in NH3-H2 gas mixtures, but do so upon the introduction of dislocatims. Nuclea-tion of the nitride phase occurs on dislocation sites. In turn, the growth of the aluminum nitride particles causes the ferrite phase to yield plastically, generating more dislocations for the nucleation process. The nitride phase extracted from an Fe-2 pct A1 alloy nitrogenated at 500°C was identified as stoichio-metric aluminum nitride with a hexagonal crystal lattice. THIS investigation reveals the role that dislocations play in initiating and sustaining the nitriding reaction in Fe-A1 alloys. As early as 1931 the work of Meyer and Hobrock1 suggested that the initiation of the nitriding reaction could involve a nucleation controlled process. Recently Bohnenka2 depicted the gas-phase nitriding process below 600°C as one of mixed control limited by nitrogen penetration through the surface, by nitrogen diffusion, by aluminum diffusion, and by nucleation of the nitride phase, Fig. l(a). In our research in a comparable alloy (0.57 pct Al) at 575ºC, we have observed a nitrogenation which we feel is better described by Fig. l(b). In the case of a 2 pct-A1 alloy partially nitrided at 500°C we propose the profiles shown in Fig. l(c). For a complete and accurate description of the process, a concentration profile of the dislocation density in the test specimen would be needed. EXPERIMENTAL Nitrogenization was conducted between 500" and 575°C in a variety of NH3-H2 gas mixtures on three Fe-A1 alloys: 1) zone-refined iron + 0.16 i 0.2 pct Al—levita-tion melt, 2) zone-refined iron + 0.57 0.02 pct Al— levitation melt, 3) plastiron + 2 pct Al—melted by induction heating. To demonstrate the effect of dislocations on reactivity, both cold-worked and annealed samples were investigated. All nitrogenation rate studies were conducted gravimetrically with a gold-plated invar balance4 contained in a gas-flow system. To avoid contamination of the specimens in the reaction zone of the system, the reaction chamber was constructed of high-purity dense alumina. The activity of nitrogen was fixed by specific NH3-H2 gas mixtures whose compositions were continually monitored by calibrated thermal conductivity gages and checked by chemical analysis. Variations of ± 0.1 pct NH3 could easily be detected by both methods. Throughout this paper the activity of nitrogen is defined as PN3 /PH23/2 , where PNH3, and Ph2 are partial pressures in atmospheres. Electron transmission, density measurements, and chemical analyses were made on specimens before and after nitrogenating in order to reveal structural and chemical changes. Similar studies as well as X-ray diffraction studies were conducted on nitride extractions from the nitrogenated 2 pct-A1 alloy. These extractions were obtained by the use of an anhydrous bromine-methyl acetate solution which dissolves the iron and leaves the insoluble nitrides as a residue. Hardness profiles were obtained on cross-sections of partially nitrided specimens to demonstrate the extent of nitriding through the thickness of the specimens. RESULTS AND DISCUSSION The nitrogen activity in the NH3-H2, atmospheres was never allowed to reach a level capable of producing iron nitride (Fe4N). Hence, the term nitriding as used in this paper refers only to the formation of aluminum nitride whereas nitrogenation refers to the total uptake of nitrogen regardless of how it is distributed throughout the alloy. The weight increases observed during the initial stage of a nitrogenating treatment are due primarily to the solution of nitrogen in the ferrite phase, particularly when starting with annealed specimens. Because this initial nitrogenation rate in the case of the 0.57 pct A1 alloy, see Figs. 2 and 3(a), was most rapid the weight change that occurred thereafter might be attributed to the nitriding reaction with the exception of a small weight increment due to the irreversible pickup of oxygen by aluminum. The oxygen (<70 ppm) came from traces of H2O and 0, in the hydrogen and ammonia gases. On the basis of discrepancies between total weight increase and the increase in the nitrogen content of the sample as determined by chemical analysis, it was estimated and later established by activation analysis, that as much as 200 ppm of oxygen were taken up by a fully nitrided Fe-0.57 pct A1 specimen at 575°C. Most of the oxygen could have been picked up from the nitriding atmosphere on the surface of the samples during cooling to room temperature. Even 50 ppm of water in the gas phase will become oxidizing to iron before the sample has cooled to room temperature. The lack of reactivity* of these alloys in the annealed
Jan 1, 1970
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Part VIII – August 1969 – Papers - Solution Kinetics of a Cast and Wrought High Strength Aluminum AlloyBy S. N. Singh, M. C. Flemings
Results are presented of a detailed study on the combined influences of ingot dendrite am spacing and thermomechanical treatments on the structure and solution kinetics of high --purity cast and worked 7075 alloy. Solution kinetics were found to depend sensitively on ingot dendrite am spacing and on details of therrnomechanical processing, including amount of reduction and extent of' solution treatment before reduction. An approximate analysis is given for rate of solution of nonequilibrium second phase in the cast and worked structres; results of the analysis are compared with experiment. MICROSEGREGATION in high strength aluminum alloys manifests itself as "coring" (composition differences within the primary aluminum-rich phase), and as interdendritic second phase. The mechanism of formation of the microsegregation is understood, and approximate prediction of the amount of second phase is possible for simple binary systems.1,2 When alloy elements or impurities are present in amounts less than their solid solubility at solution temperature, any phases forming from these elements are termed "nonequilibrium" and can be dissolved by appropriate solution treatment. The rate at which the nonequilibrium phases are removed depends sensitively on their spacing (dendrite arm spacing in the cast material, or band spacing in wrought material). When alloy elements or impurities are present in amounts in excess of their solubility at the solution temperature, second phase particles form an "equilibrium" second phase that does not dissolve in heat treatment and may, in fact, coarsen in such treatment. Usual commercial, high strength, wrought aluminum alloys contain nonequilibrium second phases that were not fully dissolved during ingot processing. They also contain equilibrium second phases resulting from impurities present in amounts greater than their solubility. As has been shown by Antes, Lipson, and Rosenthal,3 and will be demonstrated further in a subsequent paper by the authors,4 significant improvements in mechanical properties of high strength alloys can be achieved by reduction or elimination of these second phases. Methods of elimination are 1) to employ high purity materials to minimize amounts of equilibrium second phase, and 2) to employ suitable thermomechanical processing techniques to fully eliminate nonequilibrium second phases. Work reported herein comprises a study of selected thermomechani- cal processing treatments, and of their influence on solution kinetics of wrought high purity 7075 alloy. EXPERIMENTAL PROCEDURE Melting and Casting. The bulk of the work reported was performed on a single ingot of high purity 7075 alloy. The ingot was 4 in. by 4 in. by 8 in. high, uni-directionally solidified following a procedure previously described.5 The mold was heated to 1350°F before pouring the melt. The bottom chill was carbon coated stainless steel. Water was circulated through the chill after the melt was poured. The 7075 alloy was prepared from high purity virgin material (aluminum, zinc, magnesium) and from master alloys (Al-50 pct Cu, A1-15 pct Cr, A1-5 pct Ti). Final measured melt composition (wt pct) was: Zn Mg Cu Cr Ti Fe Si Al 5.70 2.28 1.35 0.18 0.15 <0.002 <0.012 bal Melting was done in a silicon carbide crucible; all tools were coated with zircon wash to minimize iron contamination; degassing was by bubbling chlorine through the melt. che-rmomechanical Treatments. Detailed studies were made on material taken from a location approximately 13 in. from the chill and 51/2 in. from the chill (i.e., from 1 in. thick slices taken between 1 and 2 in. from the chill and between 5 and 6 in. from the chill). Solution treatment was done at 860°F in an air-circulating furnace with a "bottom drop" arrangement to achieve minimum delay time between solution treatment and quench. Samples solution treated in this way were 2 in. by 2 in. by 1 in. Temperature of the quench water was approximately 10°C. Mechanical reduction was by cold rolling. Samples 11/2 and 51/2 in. from the chill were treated for 12 and 24 hr, respectively, before cold rolling. Reduction by cold rolling was then 4/1, 16/1, and 35/1. In each case, several intermediate anneals (1/2 hr at 860°F) were used to permit reaching the final thickness without cracking; two such anneals were used for the 4/1 reduction, five for 16/1, and six for 35/1. After working, materials were again solution treated for various lengths of time from 0 to 48 hr and quenched in water. Structural Measurements. Secondary dendrite arm spacings were measured using procedures previously described.' For each measurement reported, five photomicrographs were first made at X75. Measurements were made of dendrite arm spacings in at least 20 different grains (grain structure was equiaxed). Grain size measurements were made by running a number of random traverses across photomicrographs of the samples and obtaining the mean lineal intercept. Measurement of the volume percent of second phase and porosity was done by quantitative metallography. A two-dimensional systematic point count was used
Jan 1, 1970
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Minerals Beneficiation - Twisted Return Runs for Conveyor BeltsBy J. W. Snavely
WITH all the advantages of handling bulk materials by means of belt conveyor also go some problems, one of the most persistent being that of cleaning. When sticky materials are being carried; the build-up of material on the return idler rolls results in difficulty of belt training. Much attention has been given to the problem of cleaning conveyor belts, and a great variety of cleaning devices have been developed. Even the best involve troublesome maintenance, and none can completely remove the fine particles imbedded in the belt cover, which cause rapid wear of the return idler rolls, and at the same time, of the belt cover as well. One of the major rubber companies has been promoting a two-way belt system, in which the conveyor belt is given two successive 90" twists at each end to enable it to carry material in both directions simultaneously. For many years the flat belt transmission industry has installed quarter-turn and half-turn twists in countless numbers of instances. While quarter-turn and half-turn twists in transmission belts is a familiar application, the 180" twist apparently has never been previously attempted with a conveyor belt. About a year ago, two officials of the National Iron Co. of Duluth, Lester and Lewis Erickson, proposed twisting the return run of a conveyor belt on an installation that they were designing for one of the major iron ore producers. Since then the soundness of the idea has been demonstrated, both in theory and by practical test, with the result that the installation of two conveyor belts involving the twisting of the return run is now under way. These two installations are designed to have the return run of the conveyor belt twisted 180" as it leaves the snub pulley at the head drive. The clean underside of the belt is thus placed against the idlers on the return run as well as on the carrying run. Just before it enters the tail pulley, the belt will be twisted an additional 180°, restoring it to its normal position. Because this twisting of the return run of a conveyor belt is a radical departure from accepted practice, an elaborate and extensive test was conducted early in 1950 to demonstrate that this twisting of the return run could be done successfully, also to establish application data for accomplishing this twisting, and to determine if any special equipment would be required. In studying this concept of twisting the return run of a conveyor belt, a number of problems need to be solved, primarily the ones brought about by deliberately introducing an unequal distribution of stress across the conveyor belt and controlling that maldistribution of stress, while confining it to the return run portion. The tension conditions existing in the return run of a conveyor belt are clear to all designers. First, the return run carries the initial or slack side tension of the conveyor belt, the tension that must be supplied to the return run to provide proper frictional contact between the belt and the driving pulley so that the necessary power can be transmitted from the driving pulley to the belt without slippage. This slack side tension is supplied to the belt by means of takeups, either of the gravity type, which can be vertical or horizontal, or by means of the screw type. With inclined or declined belt conveyors the slope tension also must be considered, which is the tension imposed by the weight of the belt hanging from the top pulley. This slope tension frequently can furnish part or even all of the initial tension required. The maximum value of the slope tension will be at the top pulley, and it decreases in direct proportion to the length. In addition to the foregoing, it frequently is desirable to impose arbitrarily additional slack side tension to provide sufficient tension at the loading point at the tail, so that the belt will adequately support its load between the carrying idlers. Design Conditions for Twisting A number of design conditions exist, which must be satisfied successfully to accomplish the twisting of the return run without exceeding normal working limits in any portion of the conveyor belt. It is obvious that the belt edge, in its relation to the center of the belt, must stretch in making a twist, because as the twist is accomplished, the belt edge travels through a longer path than does the center of the belt. It is further obvious that if the edge of the belt is stretched, a redistribution of stress in the belt is required to allow this edge stretching. Moreover, this stress will be unequal across the width of the belt, having a maximum value at the edges, with a minimum value at the- center of the belt. With correct initial tension in the return run of a conveyor belt, the existing slack side tension will be unequally distributed when a twist is introduced. A condition then exists in which the edge stresses,
Jan 1, 1952
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Drilling and Fluids and Cement - Plastic Flow Properties of Drilling Fluids-Measurement and ApplicationBy J. C. Melrose, W. B. Lilienthal
The application of Bingham's law to the behavior of drilling fluids in a rotational viscometer permits the expression of viscometric data in terms of plastic viscosity and yield value, the flow properties of a plastic fluid. A commercially available rotational viscometer is described, and when modified to a multispeed type viscometer, is shown to provide a simple and convenient instrument for the measurement of these properties both in the laboratory and in the field. The data obtained are shown to be useful in defining and understanding mud control problems relating to chemical treatment and to the hydro-dynamic behavior of muds. INTRODUCTION The highly complex drilling fluids which are required for deep drilling often give rise to new and unusual mud control problems. Rapid and economic solutions to these problems may require, on the one hand, better understanding of the changes which contaminants and chemical treating agents produce in the colloidal and inert solids of the mud, or, on the other hand, closer control of the hydrodynamic behavior of the mud. The latter objective obviously can be achieved only if a correct rheological analysis of the flow behavior of drilling muds is available and if this is accompanied by the appropriate rheological measurements. The purpose of this paper is to describe such measurements in the field, and to show how the resulting data can be of value in solving difficult mud control problems. It is now generally recognized that Bingham's law of plastic flow can be utilized in describing the hydrodynamic behavior of drilling fluids in the non-turbulent flow range. Beck, Nuss, and Dunn' have recently applied this law to the flow of mud in small pipes, and Rogers2 has reviewed the rather extensive literature on this subject. So far, however, the use of Bingham's law has been restricted to the analysis of mud flow in pipes or capillary tubes, and it has not been directly applied to the flow in rotational viscometers. In the work to be reprted, the Reiner-Riwlin3 equation for the flow of a plastic fluid in a rotational viscometer has been utilized to permit the expression of multispeed viscometric data in terms of plastic viscosity and yield value. the two absolute flow properties of a plastic fluid. With regard to the application of these measurements, the calculation of the relationship between pumping rate and pressure drop, both in the drill pipe and annular space, has long been a subject of interest. Beck, Nuss, and Dunn,' following Caldwell and Babbitt: base their calculations for non-turbulent flow on Buckingham's integration of Bingham's law for pipe flow and measurements of the plastic viscosity (rigidity in their terminology) and yield value. In the case of turbulent flow, Fanning's equation is employed, and the pressure drop is relatively insensitive to the flow properties of the mud. Since flow in the drill pipe is likely to be turbulent at usual circulation rates, the plastic flow properties will chiefly influence the pressure drop in the annular space. As pointed out by Beck,' the control of this component of the total pressure drop may be of special importance where lost circulation problems are encountered. Other hydrodynamic problems to which it should be possible to apply measurements of the plastic flow properties include predictions of the velocity distribution in non-turbulent flow and the critical velocity for transition to turbulence. Plastic viscosity and yield value. as abmlute flow propertie.;, will reflect the colloidal or surface-active behavior of the solids present in drilling fluids. Measurements of these properties should therefore find application in developing a better understanding of such behavior and in characterizing the type and condition of these solids. Garrison and ten Brink have utilized multispeed viscometric data in this manner. although their measurements were not expressed in terms of the absolute flow properties. In connection with the application of these measurements, it should be recognized that the presently used one-point viscosity measurements are relative in nature. The API Stormer 600-rpm measurement, for example. is a function of both plastic viscosity and yield value, as well as mud weight, and will often be misleading when its application to mud control problems is attempted. NOMENCLATURE, UNITS, AND DEFINITIONS In Fig. 1 an idealized plot is given of the flow variables involved in any viscometric measurement. It is seen that the flow behavior of plastic fluids is characterized by two constants — plastic viscosity, µp, and yield value, F. Other workers hate used the term rigidity for plastic viscosity or the term mobility for its reciprocal. The term plastic viscosity, however, emphasizes the close relation this property bears to the viscosity of a true fluid and is expressed in the familiar viscosity units of centipoises. The yield value is expressed in lbs/100 sq ft, the units adopted for gel strength measurements with the APT shearometer. Definitions of these properties based on rheological or macrc)scopic flow considerations follow from Fig. 1. The plastic viscosity of a substance obeying Bingham's equation is defined
Jan 1, 1951
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Secondary Recovery and Pressure Maintenance - Experimental Aspects of Reverse Combustion in Tar SandsBy D. W. Reed, R. L. Reed, Tracht
Laboratory experiments on the reverse combustion of tar sands in a linear adiabatic system have shown that a highly upgraded oil can be produced from an exceedingly viscous, immobile oil. The dependence on the air-injection rate of peak temperature, combustion-zone velocity, oil recovery, air-oil ratio, residual coke and oil, fuel burned and distribution of product gases is shown graphically. Eflects of initial temperature, oxygen concentration, oil saturation and heat loss are discussed. Experiments bearing on the coking properties of heavy oils are mentioned and some results exhibited. Field application of the process hinges on the existence of adequate air permeability and the rate of reaction under reservoir conditions. INTRODUCTION It has been established that oil can be recovered from underground reservoirs by means of at least two fundamentally distinct methods involving in situ combustion of a certain fraction of the oil. Characteristic of both of these known methods is the production of oil from one or more wells by means of hot gases formed when a high-temperature reaction zone is advanced through the reservoir. In both cases, the reaction zone is created by heating certain of the wells to a sufficiently high temperature prior to the introduction of air, and the zone is maintained and advanced through the reservoir by appropriate control of the air-injection rate. In the first of these methods, which is called "forward combustion",' the combustion zone advances in a direction which is generally the same as that of the air flow; whereas in the second method, "reverse combustion",' the combustion zone moves in a direction generally opposite to that of the air flow. Forward combustion, on the one hand, is an ideal combustion process in the sense that a minimum of the most undesirable fraction of the oil is consumed as fuel in the form of coke, a clean sand is left behind and generated heat is used as efficiently as possible. However, the applicability of forward combustion is limited. Since the products of combustion, vaporized oil and connate water must flow into relatively cold regions of the reservoir, there is an upper limit on the viscosity of oil which can be moved by this process in a practical and economical fashion.' On the other hand, it is characteristic of reverse combustion that the vaporized oil and water together with the products of combustion are produced through sand which is already hot and has had its mobile liquid content eliminated. This means there is no upper limit on oil viscosity; indeed, the oil may be an entirely immobile semi-solid. However, fuel for the process is an intermediate fraction of the original oil, and the most undesirable fraction remains on the sand surface as a substantial deposit of coke. Since this coked material is not burned during reverse combustion, it represents energy which is available for the production of oil but is not used for this purpose. It follows that one can expect economics to be somewhat less attractive with reverse combustion than with forward combustion. Nevertheless, it is a process which is designed for reservoirs where forward combustion is impossible and, as such, has become a subject of experimental and theoretical investigation. In this paper, only experiments made with tar sands are discussed. DESCRIPTION OF THE PROCESS We proceed, then, to consider the process of reverse combustion in greater detail. Fig. 1 illustrates a temperature profile defining a combustion zone which moves from right to left when air flows from left to right. In Zone 1, the temperature is the initial reservoir temperature, and the tar sand is as yet unaltered. This statement must be modified to the extent that physical properties of the oil may be changed by low-temperature oxidation at reservoir temperature. As air passes into Zone 2, which has been warmed by conduction, it assists in vaporization of the very light ends (if there are any), and oxidation occurs at a significant rate. In this region, there is almost no production of carbon monoxide or carbon dioxide because predominantly addition-type reactions take place with the formation of oxygenated compounds such as aldehydes and acids together with water. The hydrocarbon-enriched and slightly oxygen-depleted gas stream enters Zone 3 where
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Coal - Flotation Recovery of Pyrite From Bituminous Coal RefuseBy K. I. Savage, S. C. Sun
This paper describes a process developed to recover coal, clays and pyrite from coal wastes. The process consists of fine grinding followed by coal and pyrite flotation which leaves the clays in the flotation pulp. A bituminous coal refuse containing 10% sulfur and 30% carbonaceous material was treated by this method to yield a coal product containing 4% sulfur, 10% ash; a pyrite product containing 45% sulfur (84% FeS2), 1% carbonaceous material; and a clay product containing 2% sulfur (3.5% FeS2). The coal yield was about 89%. The pyrite yield was about 77%. The process steps may be entirely flotation, or gravity separation (hydrocycloning) may be used to increase the pyrite : coal ratio in the flotation feed. Cost estimates for the process show a profit of $2.28 per ton of low pyrite grade refuse, but these do not include labor, maintenance, overhead and plant depreciation. The development of this process consisted of three parts: (1) exploratory tests, (2) op-timazation tests and (3) confirmatory tests. The objectionable qualities that sulfur imparts to coal have been commented upon from early times, and they have become more objectionable as the uses of coal have grown. In whatever form coal takes — raw, carbonized or gasified —the sulfur content remains objectionable, and therefore its compounds are removed as completely as possible. It has long been known that sulfur occurs in coal in different forms. In 1861, sulfur was said to exist in the state of sulfuric acid in combination with a base; in combination with iron as iron pyrites; as bisulfides of iron; and in combination with the organic elements of coal.' Pyritic sulfur is a term loosely used to cover the sulfur associated with iron in its various forms. The mineralogically recognized forms are pyrite (FeS2), pyrrhotite (Fe 1-x S) and marcasite (FeS2). The particle sizes of pyrites vary widely. Isolated grains of marcasite smaller than 15 microns have been found disseminated through coal.2 Hair-like "veins" of pyrite filling cracks in vitrain have been found. At the other extreme, lumps or nodules of pyrites large enough for removal by hand picking have been encountered. Organic sulfur, unlike pyritic sulfur, does not exist as discrete particles, but is instead intimately associated with the coal structure and thus it is impossible to remove it or reduce its concentration by physical or mechanical means.2 In the preparation of coal for its various markets, the pyrite minerals (pyrites) are separated from the raw coal feed. This separation process concentrates the pyrites in the tailings or other waste products. It would be desirable to recover these pyrites for three reasons: (1) Pyrites are potential sources of sulfur and iron. In 1967, for the fifth consecutive year, Free World consumption of sulfur exceeded production.3 Propelled by the shortage, the domestic price of sulfur has risen from $24 to $38 per long ton (bright). (2) The refuse, when placed in piles, becomes ignited. The pyrites (FeS2) bum, giving off SO,. Thus, the pyrites are a cause of air pollution. (3) Also, the pyrites undergo chemical reaction when exposed to air. The refuse is leached by waters which result in stream pollution due to the water-soluble iron and acidic reaction products. Coal refuse also contains coal minerals and clay minerals. Therefore, any process for recovering the pyrites must successfully separate them from the coal and clay minerals. In the study discussed here, ten different bituminous coal refuse samples were successfully upgraded in pyrite content. These samples represented a wide variety of coal waste materials from Pennsylvania and other states. The variabilities of the sulfur and coal contents are shown in Table I. The extremes are Sample J, a high sulfur-low coal, and Sample B, a low sulfur-high coal. Definitions of some of the symbols or terms used in this report are given below: Mesh size—Tyler standard mesh screen sieves with an opening based on the square root of two. Fe —Indicates iron, as determined by a stannous reduction-dichromatic oxidation method. S—Indicates sulfur, as determined by the ASTM "Eschka" method for sulfur in coal.
Jan 1, 1969
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PART XI – November 1967 - Papers - Mathematical Heat Transfer Model for Solidification of Continuously Cast Steel SlabsBy Eugene A. Mizikar
A mathetnatical model of heal transfer in continuously cast steel slabs is described. The model, consisting of a unidimensional transient conduction equation and boundary condition equations, has been pvogrammed for computer solution. Temperatuve and solidification profiles calculated for a 6-in. slab, being cast under several conditions of secondary cooling, are presented and compared. Calculated solidification profiles are in agreement with reported expevinle~ztal values. For the mold zone, the predicted slab shell thickness can be described by: Resuilts of the study indicate that multibank spray cooling followed by radiant cooling should be employed when solidifying thick slabs with minimum surface temperature of 1600°F. Under these conditions, a 6-in. slab can be expected to solidify in about 8.3 min. Computer results also indicate that radiant cooling can replace spray cooling during solidification of the final 30 pct of slab with little increase in overall solidification time. CONTINUOUS casting has come to the forefront of the steel industry in recent years because of economic advantages resulting from increased yields and elimination of several processing steps. Considerable work, however, remains to be done regarding modifications to the process and operating procedures. Both a lack of operating plants in this country and the experimental difficulties associated with direct measurements on moving castings have made determination of solidification rates and temperature distributions difficult. An alternate approach is to mathematically simulate heat transfer in a continuously cast section, and then calculate the temperature distributions as a function of the controllable variables of the process. Simulation of heat transfer during solidification requires that a nonlinear mathematical problem be solved. As pointed out by Ruddle,' there are two mathematical approaches to the problem- the analytical approach and the numerical approach. While the analytical approach is certainly the more elegant of the two, it does require a number of inexact assumptions because of the complexity of the problem. For example, noteworthy analytical treatments of heat transfer in continuous casting have been developed by Savage Hills,3 and pehlke4 only by making one or more simplifying assumptions such as invariant thermophysical properties, constant heat-transfer coefficients in the mold, and linear temperature profiles in the shell. Simplifying assumptions such as these can introduce considerable uncertainty in the validity of results calculated with analytical solutions. Numerical solutions, which are considerably more versatile, appear to be better suited for solving solidification problems. Complex variations in the boundary conditions and variable thermophysical properties can be handled readily with this technique. Whereas numerical computations can be long and tedious when done by hand, results can now be obtained quite rapidly with the use of either the digital or analog computer. Several numerical models of heat transfer in continuous casting have been published. In 1963, Adenis, Coats, and Ragones published a numerical model used to calculate temperature distributions in direct-chill-cast magnesium billets. More recently, Donaldson and Hess 6 presented results obtained with a numerical computer model of heat transfer in continuously cast steel billets. In the present study, a model of unidimensional heat transfer in continuously cast slabs is presented. The method of solution on a digital computer is also included. Calculated temperature distributions and solidification profiles for various schemes of secondary cooling along with attempts to verify the model are also discussed. MATHEMATICAL MODEL The schematic representation of the slab continuous casting process in Fig. 1 illustrates that the slab passes through three distinct zones of cooling. Accordingly, the mathematical model consists of three parts: 1) solidification in the mold; 2) solidification in the spray cooling zone ; 3) solidification in the radiant cooling zone. Heat-Transfer Equations. The model was developed bymaking a heat balance on a horizontal slice of slab over the time period required for the slice to proceed from the liquid metal meniscus in the mold to the cutoff station. As shown in Fig. 2, the imaginary slice extends from the center line to the surface of the slab. As the slice moves downward, heat is conducted from the center line to the surface of the slab at a rate governed by the surface boundary condition and thermophysical properties of the metal in the slice. The following partial differential equation describes the conduction of heat in a medium moving at velocity U in direction Z:
Jan 1, 1968
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Reservoir Engineering - General - A Method of Predicting Oil Recovery in a Five-Spot SteamfloodBy B. H. Caudle, L. G. Davies, I. H. Silberberg
This paper presents a method of predicting the recovery and performance of a five-spot steam injection project, in which a realistic approach to pattern sweepout efficiencies is made. Published methods for radial systems were modified for the five-spot pattern by approximating the stream lines with straight lines radiating from the injection well and then converging to the producing well. In each radial segment, the position of the steam front and the temperature profile ahead of the steam front were determined by heat balance equations, which included an estimation of heat losses to surrounding formations. The location of the saturations behind the cold water front was determined from a Buckley-Leverett solution to the material balance equation. Results from this program show steamflood recovery in a five-spot pattern to be considerably less than that predicted for true linear or radial flow systems. For a specific reservoir containing 900-cp oil, a steamflood in a purely radial flow system was predicted to recover more than 75 percent of the original oil in place when 2 PV of water had been injected as steam. A five-spot steamflood with otherwise identical properties was predicted to recover 10 percent of the original oil in place when 0.15 PV of water had been injected as steam and to recover almost no oil thereafter. A cold water five-spot flood in this system was predicted to recover approximately W percent of the oil in place with I PV of water injected. For a five-spot pattern in an example reservoir with 10-cp oil, steam injection similarly showed lower ultimate recovery than water injection but no improvement in recovery rule. Introduction The thermal recovery method considered in this study is steam injection in a five-spot pattern. Pattern steam injection has been given little attention in the past, possibly because of some rather obvious disadvantages. Unless steam temperature is maintained throughout the entire swept area, the process will revert to simple waterflood with all heat being lost prior to reaching the oil bank. Also, the oil viscosity reduction takes place near the steam front and not around the producing wellbore, so that low producing rates must still be endured. This is the reason for the success of the steam stimulation, or cyclic injection, in which the fluids are produced from the same well used for injection. On the other hand, steamflooding can offer some advantages. Oil displacement is by four methods: (1) mechanical displacement by the condensed water, (2) viscosity reduction of the crude oil, (3) swelling of the crude oil, and (4) distillation of the crude oil in the steam zone. Although dependent upon the crude, laboratory experiments have shown displacements up to 80 percent by steamflooding. In addition, steam is a good heat transport medium, since it is cheap and has a high heat content. Previous Investigations Previous publications have reported methods for predicting recovery in a steamflood for linear and radial systems. Since no pattern sweep efficiency is taken into consideration, the recovery even from a radial system must be greater than from more realistic geometries such as the very common five-spot patterns. Probably the broadest coverage is given by Willman who reported experimental results and offered a method of predicting recovery for a radial flow system. They concluded that both hot water and steam injection recover more oil than an ordinary waterflood, and that steam injection could yield recoveries "as much as 100 percent greater than by water flood." They also concluded that both the heat requirements for a reservoir and the residual oil remaining in the reservoir after steam injection were independent of the amount of oil originally in place, that short exploitation times were desirable, and that a high percentage of net sand in the reservoir with a high initial oil saturation was desirable. The method assumes that the flood occurs in three concentric cylindrical zones: (1) an inner steam zone, (2) a central hot water zone, and (3) an outer cold waterflood zone. Displacement in the steam zone is based on laboratory-determined residual oil saturations while the hot water and cold water zones use the conventional Buckley-Leverett equations. Although the results shown by Willman et al. are for a radial system flowing out from the well to an assumed external circular boundary, their equations did
Jan 1, 1969
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Part II – February 1969 - Papers - Secondary Slip in Copper Single CrystalsBy Lyman Johnson
Single crystals qf copper in "single slip" orientatiorzs have been deformed in compression. During defortnation all of the independent deformation parameters have been measured. These parameters consist of thefive strain components and three components descrihing the lattice rotation. By a finite strain analysis these pararmeters , forrming a deformation gradient martrix, are related to the amounts of slip on each of the twelve slip systems. The results show that the amount of secondary slip is about equal to the amount of primary slip. This is an order of magnitude larger than has been believed previoutsly. ACCORDING to early theory and experiments, when a single crystal of a fcc metal is deformed in tension or compression it should deform by slip on only one slip system until the stress axis reaches a symmetrical orientation.' However. the observation of a large increase in the secondary dislocation density during ..single slip" makes it clear that some slip does occur on secondary systems. Knowledge of the amount and distribution of this secondary slip is essential to a complete understanding of the mechanisms of single-crystal deformation. Ahlers and Haasen 2 and Mitchell and Thornton1 have tried to detect the amount of secondary slip in single crystals of silver and copper, respectively. Each simultaneously measured the angle A, between the tensile axis and the primary slip direction and the length 1 of a gage section of the specimen after incremental amounts of deformation in tension. The measured A, was then compared with the theoretical single slip angle hp. given by sin Ap = j sin . hO where ?o was the initial angle between the tensile axis and the primary slip direction and lo was the initial gage length. In both sets of experiments a small but systematic difference between ?e and ?p was found. This difference must be due to the occurrence of secondary slip. However, as Mitchell and Thornton1 pointed out. nothing quantitative can be said about the amount and distribution of this secondary slip from the measurements that they made. The reason that no quantitative conclusions could be made is because no unique solution for the distribution of slip on the twelve fcc slip systems can be determined from only two measured deformation parameters such as A and 1. There are, in fact, eight independent macroscopic deformation parameters that can be measured when a single crystal undergoes a homogeneous deformation. Physically these can be thought of as the five finite strain components and the three angles describing the crystal lattice rotation. All eight of these parameters were measured by Taylor4,5 for aluminum deformed in tension and compression. At that time the concern was to show that slip occurs on {111 (110) systems in fcc metals, and the mathematics were not available to determine what slip distributions were compatible with the measurements. In this paper the mathematics6,7 are developed that allow the slip distribution to be determined from these measurable macroscopic deformation parameters. The analysis is applied to the measurements of the strain and lattice rotation of copper single crystals deformed in compression. The results show that the amount of secondary slip is an order of magnitude larger than had previously been thought. CRYSTALLOGRAPHIC DESCRIPTION OF A HOMOGENEOUS DEFORMATION The deformation of a solid body can be represented by a transformation matrix F that transforms the un-deformed state into the deformed state. Consider a vector X connecting two material points in the unde-formed material and the vector x connecting the same two material points after deformation, where both vectors are referred to the same set of Cartesian axes. The final vector x is related to the initial vector X by the equation: X = FS. [2] Eq. [2] can be considered as the equation defining F, which is called the deformation gradient matrix. Its components are: If the deformation is homogeneous, the transformation is linear and the components of F are constants. Using subscript notation, if P is the unit vector in the initial direction of a material line, the components of the unit vector p in the direction of the same material line after deformation are given by:
Jan 1, 1970
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Part IX - Papers - Temperature Measurements and Fluid Flow Distributions Ahead of Solid-Liquid InterfacesBy G. S. Cole
The temperature has been measured ahead of stationary solid-liquid interfaces under conditions approximating luzidirectional heat flow and therefore unidirectional solidification. Natural convection flow patterns may be deduced from the temperature distributions , temperature fluctuations, and shape of the interface. Fluid flow increases with the height and the rate of heat transfev through the interface and this is further manifested by a deviation of the interface from aflat vertical plane. The influence of fluid flow on solute inhomogeneity during alloy crystal growth can be inferred from the observed temperature distributions. A buoyancy force exists in the liquid ahead of a vertical solid-liquid interface, caused by a difference in density between cold fluid near the interface and warmer fluid in the bulk liquid. When the viscous and inertia forces in the melt exceed this buoyancy force, a flow of fluid takes place, termed natural or free thermal convection. Natural convection in purely liquid systems has been extensively studied for many years. 1"u On the other hand, fluid flow during horizontal crystal growth has oniy recently been the subject of experimental investigation."-25 The requirements for horizontal crystal growth differ from other heat flow systems. The small aspect ratio (ratio of height of cold wall to length of fluid) has never been considered. The uniform furnace gradient which supplies heat radially (and not necessarily symmetrically) differs from previous boundary conditions of uniform heat flux at the cold and hot ends. And most important of all an isothermal s/l interface is present which can adjust its shape and position to conform to heat and fluid flow. All of these boundary conditions involve complexities which cannot be readily solved analytically. Preliminary observation has demonstrated the penera1 shape of the natural convective flow pattern in transparent media.20'24'25 The flow is circulatory, directed toward the interface at the surface of the liquid, down and away from the interface at the bottom, and then up at the hot end of the melt. During crystal growth such a flow may interact with the solute boundary layer at the s/l interface to affect solute incorporation.M'1B|28'i!T Evidence has also been presented recently to show that thermal convective flow will affect the structure of ca~tin~s.~~-~~ The rate of heat transfer (conduction plus convection) in a given fluid system is a function of the temperature difference between the hot end of the liquid and the s/l interface and the height of the interface. At the lowest values of these variables* all heat is *It has been shown' that adverse temperature gradients as low as O.OOS°C oer cm are sufficient to cause convection. transferred by conduction. When the temperature difference or interface height are increased, laminar fluid flow commences and heat transport takes place by laminar convection as well as by conduction; turbulent heat transfer takes place at higher values of these variables. In the transition region between laminar and turbulent flow, boundary layer separation takes place; fluctuations in temperature are also noted and increase in amplitude and frequency as turbulence becomes dominant. In this paper, fluid flow patterns in the melt ahead of a stationary interface are deduced from observations of temperature distribution and fluctuations, heat flow rate, and interface shape. The fluid flow ahead of advancing interfaces and the effect of such flow on solute incorporation may be inferred from these measurements on stationary interfaces. Observations during enforced fluid motion will also be considered. EXPERIMENTAL PROCEDURE The metal was contained in a lava boat 10 cm in length, 1+ cm in width, and 2 cm in height, as shown in Fig. 1. A water-cooled, molybdenum block heat-sink is at one end of the boat; surrounding this assembly is a slotted stainless-steel tube noninductively wound with a nichrome heating element. Temperature was measured by 38-gage Chrome1 vs Alumel thermocouples sheathed in 0.05-cm-diam graphite-coated stainless-steel tubing, which were moved longitudinally and vertically through the melt by means of a two-dimensional motorized micrometer stage. In some experiments the thermocouple junction was exposed, but in the majority of experiments the junction was welded to the sheath tip; no significant difference
Jan 1, 1968