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By R. S. Hoch, Roy A. Bobo

Maintenance of desirable plastic flow properties of weighted drilling muds may be greatly simplified by use of centrifugal classification to control the drilled solids content. The new application of a decanting type centrifuge to separate and reject the low density solids from the weighting material results in a drilling mud of greatly improved quality with lower values of yield and rigidity. Its practicality and economy has been proven in field operation. The degree of separation of light and heavy solids is not limited by the machine, but by the particle size distribution of the solids in the mud. Removal of the low density component of drilling mud that makes chemical treatment necessary permits a marked reduction in chemicals. The main uses of the centrifugal process are the treatment of muds while drilling, the reclaiming of discorded muds, cleaning up of workover muds, and the reduction in lime content of mud for completion. INTRODUCTION Drilling mud in any circulatory system is made viscous and difficult to pump by gradual accumulation of drilled solids which pass through the shale shaker and are continually reground. In a weighted mud containing a large proportion of barite by volume, the amount of drilled solids that may be tolerated is greatly reduced. Much effort has been expended to control by chemical treatment the effects of such solids. Though chemical treatment is quite effective, the time eventually comes at deeper depths after enough drilled solids have entered the system when a portion of the mud must be discarded and replaced with water and more weighting material. Once begun, this process is generally continued at frequent intervals with resultant high maintenance costs. At the termination of drilling, mud highly contaminated with light solids and spent chemicals is poorly suited for completion operations.' It is likewise limited in utility for other drilling operations. This investigation was conducted for the primary purpose of determining an acceptable mechanical means of removing the lightweight solids from weighted drilling muds in order to maintain viscosity at a minimum. A decanting type of centrifuge was selected from the various possible methods of mechanical separation. The centrifugal process has been employed in this country for this purpose in central mud reclamation systems in California in earlier years. It also was used for treatment of weighted muds on the Gulf Coast.' In more recent years only sporadic attempts have been made to employ it in the field on weighted muds. DISCUSSION OF PROCESS Selection of Apparatus Two factors favor mechanical procedure for the separation and removal of drilled solids or clays from the mud circulatory system. First, the greater specific gravity, 4.1 to 4.3, of the barite would promote more rapid settling than the clays whose specific gravity range is from 2.5 to 2.7. Second, the relative coarseness of the barite particles also facilitate faster settling of this phase. A decanting type of centrifuge was preferred for this process over other possible methods for these reasons: 1. Requires no costly additives or excess dilution. 2. Centrifugal force affords greatly accelerated separation as compared to gravity.

Jan 1, 1955

By T. Patching

"COAL MINING at Canmore, Alberta, began in 1886 and continued there until July 1979. A comprehensive review of the Canmore operations is not available, but the following notes have been prepared to accompany references where more complete information about the operations and problems encountered may be found. The coal measures at Canmore occur in the Kootenay formation of Lower Cretaceous age, and at least twelve seams of varying thickness and horizontal extent have been recognized. The coal, of high quality, ranges from semi-anthracite in the lower seams to low-volatile bituminous in the upper seams. The strata of the Canmore area form an asymmetric syncline, the western limb being overturned to vertical by the Palaeozoic strata of the Mount Rundle Range. The eastern limb is more gently sloping, its dip ranging from IO to about 40 degrees. Tectonic movements have created a troubled and complex coal field. The seams were initially not regularly or uniformly deposited, and mountain-building activity folded and faulted the strata and in many places sheared and crushed the original structures of the coal(l,2,3,4,5). The lack of continuity of the seams, and changes in thickness and inclination, made longrange mine planning difficult and necessitated flexible methods of work, and the local disturbances sometimes created problems in roof support and contributed to the occurrence of sudden outbursts of coal and gas. Almost all of the coal was produced from underground operations but a few relatively small V-cut mines were worked along surface outcrops. These have all been filled in and revegetated. The basic method of underground work was by room-and-pillar, but many variations in layout and sequences were employed. Gangways were driven along the strike and pillars were formed by raises or slopes and crosscuts. Pillars were recovered to the extent that ground conditions permitted by splitting or taking 'skips' from the sides of the raises or splits or crosscuts. Because of the variety of conditions that existed in the field a considerable range of cutting, loading and support methods were employed, including hand-loading, slushers and scrapers, duckbills and shaker conveyors, mobile loaders and continuous miners. Except for the coal obtained by continuous miners most of the coal was broken out by blasting when driving narrow working places or by air picks when cutting from a face. In the early years hand loading onto cars or conveyors predominated. A continuous miner was introduced into Canmore in 1959 on a trial basis, and another was subsequently acquired, in order to minimize blasting and hand loading, but problems in operating these machines in inclining seams and difficulties in providing safe roof support for the machines and workers restricted their efficient use. Another major difficulty with the use of continuous miners was the problem of ventilating development headings in the very gassy conditions. In the early 1970s they were replaced by electric and compressed air slushers and scrapers, resulting in a general increase in productivity, roof control, safety, and flexibility of operations(1.6,7,8.9)."

Jan 1, 1985

By John D. Morgan

Introduction The US Bureau of Mines' (USBM) world reserve/consumption ratios (Table 1) indicate that, if the world is relatively peaceful in the next two decades, there should be ample world supplies of minerals to permit rising standards of living for increasing world population. But it must be remembered that most mineral reserve estimates are conservative and that normal mining practice is to develop a ton of ore reserve for every ton mined. It should be noted that "reserve," as used in this paper follows the definition given in US Geological Survey (USGS) Circular 831, 1980; "that part of the reserve base which could be economically extracted or produced at the time of the determination." In addition to accurately determining the geologic parameters of mineral deposits, a judgment as to whether that deposit is a "reserve" per se involves consideration of many other factors. These factors were recognized nearly a century ago by a well-known mining engineer and later President, Herbert Hoover. In "Principles of Mining," 1909, Hoover wrote: "Unfortunately for the mining engineer, not only has he to weigh the amount of risk inherent in calculations involved in the mine itself, but also that due to fluctuations in the value of metals. If the ore is shipped to custom works, he has to contemplate also variations in freights and smelting charges ...In a free market, the law of supply and demand governs the values of metals as it does that of all other commodities. So far, except for tariff walls and smelting rings, there is a free market in the metals under discussion. The demand for metals varies with the unequal fluctuations of the industrial tides. The sea of commercial activity is subject to heavy storms, and the mine valuer is compelled to serve as weather prophet on this ocean of trouble. High prices, which are the result of industrial booms, bring about overproduction, and the collapse of these begets a shrinkage of demand, wherein consequently the tide of price turns back." Current supplies and use There have been ample supplies of most mineral materials to permit several-fold increases of world production of common major mineral based minerals (steel, aluminum, copper, and cement) over the past three decades. Motor vehicle production is a major consumer of mineral materials. However, in the last decade, down-sizing to facilitate improved fuel efficiency and reduce harmful emissions has reduced the weight of the average US-made automobile 15%, to 1.5 t (3200 lbs). Also in the US, there are 92 million dwelling units, or on average, fewer than three persons per dwelling unit. Construction is another major consumer of materials in the industrialized developed countries. It will also be a major consumer of materials worldwide as less developed nations seek to improve their infrastructures by adding roads, bridges, railroads, airfields, ports, and housing. Fortunately, a large number of traditional common materials, many of mineral origin and also many of agricultural origin, are readily available for construction. Traditional construction materials such as steel, aluminum, copper, and cement, are being replaced in many applications by engineered plastic and ceramic

Jan 4, 1986

By B. D. Cullity, O. P. Puri

The magnetostrictia of nickel after increasing amounts of plastic elongation was measured at field strengths up to 1500 oe. In addition, the residual stress was measured by means of X-ray line shifts. The observed decrease in magnetostriction following plastic strain is shown to be associated with residual compressive stress. If a metal bar, whose longitudinal axis is taken as the x direction, is plastically elongated in the x direction and then unloaded, X-ray diffraction measurements will indicate the presence of a residual compressive macrostress 0%. However, stress measurement by means of mechanical relaxation does not reveal any macrostress. In a previous paper1 the fictitious macrostress indicated by X-rays was ascribed to a particular distribution of micro-stress, namely, one in which the bulk of the material was stressed more or less uniformly in compression and a very small portion in tension. It was shown that this distribution would account for Neurath's measurements2 of magnetic losses in silicon steel, because of the effect of residual stress on magnetostriction. The present paper is concerned directly with magnetostriction, in nickel, and with the effect on magnetostriction of the residual stress created by plastic elongation. The residual stress was determined by measurements of X-ray line shifts. MATERIAL AND METHODS Commercially pure "A" nickel was investigated. Its nominal composition, in weight percent, is 99.4 Ni + Co, 0.2 Mn, 0.15 Fe, 0.1 Cu, 0.1 C, 0.05 Si, and 0.005 S. Magnetostriction was measured by means of SR-4 electrical-resistance strain gages mounted on specimens 1/4 in. sq and 8 in. long. Magnetic fields up to about 1500 ce were provided by a multilayer, non-cooled solenoid. A considerable amount of heat was developed at the higher field strengths, and, to avoid errors due to changes in the specimen temperature, the following procedure was adopted. Each measurement of the magnetostriction X at a particular field strength H was preceded by demagnetization and an adjustment of the strain indicator to zero; the field H was then quickly switched on and the strain read immediately. Curves of ? vs H were flat for field strengths above about 750 oe for all specimens, and this constant value of X was accordingly taken as the saturation magnetostriction ?s The X-ray measurements of residual stress were made with a Norelco diffractometer on specimens cut from flat bars 1 1/4 in. wide, 1/8 in. thick, and 12 in. long. These measurements were confined to lattice planes parallel to the surface of the specimen. Two reflections were studied: the 311 CrKß line at 28 = 157 deg, and the 420 CuKal line at 28 = 155 deg. The line centers were determined by fitting a parabola to the peak of the line, as suggested by Ogilvie3 and as modified by Koistinen and Marburger.4 The CuKa doublet from the plastically elongated specimens was first resolved by the Rachinger method5. All X-ray measurements were made by counting at fixed angular positions. RESULTS The results of the magnetostriction measurements are shown in Fig. 1 and Table 1. The magnitude of

Jan 1, 1963

By John J. Sammarco, Edward F. Fries

This report (Independent Functional Safety Assessment 4.0) is the fifth in a nine-part series of recommendations addressing the functional safety of processor-controlled mining equipment. It is part of a risk-based system safety process encompassing hardware, software, humans, and the operating environment for the equipment’s life cycle. Figure 1 shows a safety framework containing these recommendations. The reports in this series address the various life cycle stages of inception, design, approval and certification, commissioning, operation, maintenance, and decommissioning. These recommendations were developed as a joint project between the National Institute for Occupational Safety and Health and the Mine Safety and Health Administration. They are intended for use by mining companies, original equipment manufacturers, and aftermarket suppliers to these mining companies. Users of these reports are expected to consider the set in total during the design cycle. • 1.0 Safety Introduction.—This is an introductory report for the general mining industry. It provides basic system/software safety concepts, discusses the need for mining to address the functional safety of programmable electronics (PE), and includes the benefits of implementing system/software safety program. • 2.1 System Safety and 2.2 Software Safety.—These reports draw heavily from International Electrotechnical Commission (IEC) standard IEC 61508 [IEC 1998a,b,c,d,e,f,g] and other standards. The scope is “surface and underground safety-related mining systems employing embedded, networked, and nonnetworked programmable electronics.” System safety seeks to design safety into all phases of the entire system. Software is a subsystem; thus, software safety is a part of the system’s safety. • 3.0 Safety File.—This report contains the documentation that demonstrates the level of safety built into the system and identifies limitations for the system’s use and operation. In essence, it is a “proof of safety” that the system and its operation meets the appropriate level of safety for the intended application. It starts from the beginning of the design, is maintained during the full lifecycle of the system, and provides administrative support for the safety program of the full system. • 4.0 Safety Assessment.—The independent assessment of the safety file is addressed. It establishes consistent methods to determine the completeness and suitability of safety evidence and justifications. This assessment could be conducted by an independent third party. • 5.0 Safety Framework Guidance.—It is intended to supplement the safety framework reports with guidance providing users with additional information. The purpose is to assist users in applying the concepts presented. In other words, the safety framework is what needs to be done and the guidance is the how it can be done. The guidance information reinforces the concepts, describes various methodologies that can be used, and gives examples and references. It also gives information on the benefits and drawbacks of various methodologies. The guidance reports are not intended to promote a single methodology or to be an exhaustive treatment of the subject material. They provide information and references so that the user can more intelligently choose and implement the appropriate methodologies given the user’s application and capabilities. [ ]

Jan 5, 2003

By P. Lelong, P. Lacombe, J. Herenguel

IN previous studies on the effect of orientation on the rate of anodic oxidation of A1-3 pct Mg mono-crystals of high purity, certain anomalies were observed on the cold-worked metal. These anomalies were shown to correspond to regions of changed orientation within the grains resulting from plastic deformation.' In fact, they are deformation bands revealed by differences in rate of oxidation and produced by more or less continuous bending of the lattice about a [Ill] axis common to the original crystal and the band.2,3 Preliminary observations made after relatively large degrees of cold working revealed an approximate twin relationship between the bands and the surrounding crystal. Fig. 1 shows the etch figures formed on such a band and on the original monocrystal after a 67 pct rolling reduction. It is evidently not a true twinning, since there is a broad transition zone between the two systems, however the two extreme orientations are nearly in a twin relationship. It was decided to investigate these preliminary observations by progressive rolling-reductions on monocrystals of varied initial orientation. From these studies, which form the subject of the present article, it became apparent that the initial observation of an approximate twin relation between the bands and the monocrystal was simply a special case. Our experiments show that deformation in rolling proceeds by a mechanism analogous to those which have already been observed in the simpler cases of tension and compression. Micrography—in particular, the formation of etch figures—has been applied to the quantitative study of these orientations. In addition, observations have been made of slip lines, of thin oxide films yielding interference colors, of thick films in polarized light, and of etchants giving "engraving." These micrographic methods for studying orientation have established the orientation relationship without any ambiguity, whereas X-ray methods would have given only a statistical result because we were often dealing with thin bands (2 to 100 microns) and even narrower connecting zones covering a maximum of 20 microns. Specimen Preparation and Methods The Al-3 pct Mg alloy was prepared from 99.95 pct A1 and is of the type used industrially in France for brilliant anodized finishes under the name of Brillalumag. This material combines the normal commercial properties with an enduring brilliance due to the protection of a thick, but perfectly transparent, film of alumina.' The monocrystals were prepared by the method of critical deformation followed by prolonged annealing. Great care was taken to insure perfect homogeneity of composition, to eliminate included crystals,6,7 and to avoid the formation of undulations during oxidation. The critical deformation for this alloy is about 1.2 pct (1-l0/10x100) and the subsequent annealing was for one week at 500 °C after gradual increase of temperature (35°C per hr). The crystals thus prepared had a section of 10x5 mm and a length of 20 to 40 mm. Each of these crystals was polished electrolytically and etched for the formation of etch-figures with the classical reagent.' The orientation was then calculated from their angles, as measured with a goniometer microscope.

Jan 1, 1954

By Howard R. Keil

Reactor at Carlton mill successfully calcines pyrite-telluride flotation concentrate for cyanidation. CARLTON mill in the Cripple Creek district, 45 miles southwest of Colorado Springs, Colo., has been in operation for approximately three years, treating the custom sulpho-telluride ores formerly handled by the Golden Cycle mill in Colorado Springs. At the new mill the pyrite-telluride flotation concentrates have been roasted, prior to cyani-dation, in a Dorrco FluoSolids reactor, which has proved capable of yielding calcine readily amenable to cyanidation. Incoming ores are crushed at Carlton to % in. and sampled in 30 to 75-ton lots before the individual lots are mixed in the fine ore bin. The composite ore then goes to the grinding circuit. Classifier overflow from the grinding circuit is treated by flotation to produce a concentrate containing approximately 85 pct of the values in 5 pct of the weight. The flotation concentrate goes to the FluoSolids reactor prior to cyanidation. Cyanide solution values are recovered by zinc dust precipitation. Flotation tailings are thickened and cyanided, the values from this part of the circuit being recovered from solution by activated carbon. Gold values in the flotation concentrates consist of a small amount of finely divided metallic gold; the tellurides, sylvanite and calaverite; and gold very intimately associated with the pyrite. The metallic gold and a part of the telluride values can be extracted from the concentrates by cyaniding without roasting. However, extraction on the tellurides by this method is not satisfactory, and the pyrite values are so intimately associated with the pyrite that very fine grinding and cyanidation for a prolonged period under ideal laboratory conditions does not yield good recovery. Upon roasting, the tellurides are oxidized to very finely divided metallic gold which is readily soluble in cyanide. The pyrite is oxidized mainly to a porous iron oxide which allows cyanide solution to penetrate to gold particles and take them into solution. Feeding the Reactor Flotation concentrates move by gravity to a thickener. Thickener underflow is discharged at approximately 60 pct solids, by means of a diaphragm pump, into a storage and blending agitator. From here the concentrates are pumped to a disc filter. The filter cake, at 84 to 88 pct solids, drops directly into a repulper where it is repulped into a slurry of 78 to 80 pct solids. The repulped filter cake flows into a 6x6-ft slurry agitator from which it is fed directly into the reactor by the Moyno pump. The Moyno pump has eliminated a large number of difficulties that were first encountered in feeding a wet concentrate to the reactor. On the original installation in Canada a screw feeder was used to introduce the filter cake directly into the reactor. Since the reactor is under a slight positive pressure it was necessary to have a suitable seal to prevent gas escaping from the reactor at this point. When the concentrates produced in flotation were coarse or granular they could be readily fed to the reactor but when fine-textured, clayey concentrates were produced a great deal of trouble was encountered.

Jan 1, 1955

By A. Vignes, J. P. Sabatier

A study of ternary diffusion at 1315°C in the Fe-Co-Ni system covering the entire ternary phase diagram has been carried out. Experimental values of the four interdiffusion coefficients DFeNico,DFeCoCo, DFeCoNi were computed at 33 points of the ternary diagram. The limiting values of these coefficients on the three sides of the ternary diizgram have also been determined. This set of data is presented as a contour map on the ternary isotherm for each of the four coefficients. Assuming that the Fe-Co-Ni system can be considered as ideal, the phenomenological coefficients Lk ij (with k = Fe) have been computed and the Onsager reciprocal relutions verified. It is shown that, in the Fe-Co-Ni system, the diffusion process can also be described by only two interdiffusion coefficients DFeFe and DCoNiFe, the second cross diffusion coefficient DCoFeNi being equal to zero and the second direct difusion coefficient being given by The values of the cross interdiffusion coefficients and of the Onsager coefficients are explained in terms of atomic mobilities of the three components with the help of a kinetic calculation due to Lane and Kirkaldy.8 It is shown that all the results are explained if the tracer difusion coefficients of the three components are such that DFe > DNi ~ DCo in complete agreement with experimental data on the three binary systems. DIFFUSION in a ternary alloy system is basically and significantly different from diffusion in binary alloys. In binary diffusion, there is just one independent composition variable and only one coefficient Dij is needed to describe the interdiffusion process. In ternary diffusion, we must allow for cross interaction between two independent species, and four interdiffusion coefficients are necessary to describe the transport process. Kirkaldy et al.1,2 have determined interdiffusion coefficients in the systems, Cu-Mn-A1 and Zn-Cu-Al. Guy and Leroy4 have reported intrinsic diffusion coefficients for the r phase at 1300°C of Co-Ni-Cr alloys as a function of composition using the analysis of Philibert and Guy.3 Interdiffusion coefficients were measured at three different compositions at 850°C in the single phase copper-rich corner of the Cu-Zn-Mn system by Dayananda and race.5 Zie-bold and Ogilvie6 have determined interdiffusion coefficients in the single-phase field of the Cu-Ag-Au system at 725°C. Preliminary results on diffusion at 1136°C in the system Fe-Co-Ni have been reported.7 In this study, data are reported on a more complete determination of interdiffusion coefficients in the Fe-Co-Ni system in the entire ternary at 1315°C. There is complete solid solubility with the fcc structures at 1315ºC, and this system can be considered as nearly ideal. This approximation allows the computation of the Onsager phenomenological coefficients. These values can then be used to test a kinetic calculation of the Onsager L coefficients in ternary substitutional solid solutions due to Lane and Kirkaldy.8

Jan 1, 1970

By John McGhee, Jack Newcombe, M. J. Rzasa

A series of water floods was made on laboratory prepared unconsoli-dated sand columns to study the effects on oil recovery of the solid-water-oil contact angle, the oil-water interfacial tension, flood rate, and oil viscosity. A procedure was developed for treating silica sand with silicone polymer to produce surfaces of varying degrees of wettability as evaluated by measuring the contact angle on a flat silica plate that had been simultaneously treated with the sand. Fluid interfacial tensions were changed by the use of surface active agents in the flood water. Water-wet, oil-wet, and intermediate wettability systems were studied at high and at low values of interfacial tension, at several flood rates, and with oils of different viscosities. For both oil-wet and water-wet systems and a low viscosity oil, recoveries were functions of the oil-water interfacial tension; also, increase in flood rate resulted in increased oil recoveries. High interfacial tension floods were more efi- cient than low interfacial tension floods on water-wet systems, while low interfacial tension floods were more eficient on oil-wet systems. Intermediate or neutral wettability systems were less sensitive to rate of flood advance and interfacial tension than either oil-wet or water-wet systems. The eflects of surface forces on oil recovery for high viscosity oils were not so well defined as for low viscosity oils. INTRODUCTION Reservoir rock surfaces vary in their wettability1, some being water-wet while others are apparently oil-wet. The factor of wettability enters into reservoir performance in both primary and secondary recovery, and into laboratory measurements of capillary pressure, connate water saturation, and relative permeabilities.' In theory, the degree of wettability is measured by the contact angle for the system solid-water-oil. A water-wet system is defined as one in which the advancing water contact angle is less than 90". An oil-wet system is one in which the advancing water contact angle is greater than 90°.3 The surface forces in a solid-water-oil system are related by the Young-Dupree equation as follows4: These surface forces are commonly expressed as the difference in adhesion tension, or the product of the water-oil interfacial tension and the contact angle. If the contact angle is less than 90°, the adhesion tension difference is positive and oil displacement by water from a solid surface will be spontaneous and favored by a high oil-water interfacial tension. If the angle is greater than 90" the displacement will not be spontaneous but will require less energy the lower the oil-water interfacial tension. The contact angle and interfacial tension also appear in the capillary pressure equation5: PC = 2ocosejr .... (2) The quantity cos was used by Rapoport and Leas6 s a factor in the generalized form of their "sealing coefficient." Warren and Cal-houn' presented the results of cos on oil recovery in oil-wet systems and correlated their data using a "scaling coefficient" suggested by Jones-Parra and Calhoun.8 The "sealing coefficients" were advanced to help correlate the effects of the variables influencing oil recovery by

Jan 1, 1956

By F. Kurata, A. F. Bertuzzi, P. C. Davis, T. L. Gore

The phase and volumetric properties of 10 very volatile mixtures are presented for temperatures from — 200°F to above the critical points. These mixtures consisted of natural gases and of mixtures of natural gases with methane and nitrogen. Existing correlations of compressibility factors have been extended to apply to these mixtures. Existing correlations of critical pressures and temperatures do not apply to these mixtures. Methods have been developed for estimating critical temperatures of these mixtures to ± 4°F and critical pressures to 2 5 per cent. These methods apply to other volatile and very volatile mixtures. The results of this work are particularly applicable to the separation of nitrogen from hydrocarbons by low-temperature distillation. INTRODUCTION Knowledge of the low-temperature phase and volumetric properties of natural gases and of other mixtures of the light hydrocarbons is becoming increasingly important as interest in low-temperature separation processes increases. Low-temperature distillation has been used to separate ethane and ethylene from natural gas and from refinery gases for petrochemical uses. Removal of nitrogen from natural gas by low-temperature distillation has been proposed 7,20 as a means of increasing the capacity of existing gas transmission lines and of improving the marketability of the gas. Further application of low-temperature separation processes has been retarded by lack of data on the phase and volumetric behavior of mixtures at low-temperatures and at high pressures. This paper presents the results of determination of the phase and volumetric properties of 10 very volatile mixtures at temperatures from - 200 °F to above the critical point. These mixtures consisted of natural gases with methane and nitrogen. Generalized methods are presented for estimating the critical temperatures, critical pressures, and the densities of such mixtures. EXPERIMENTAL APPARATUS AND PROCEDURES The apparatus and the experimental procedures have been described in an earlier paper13. The method consists of displacing the mixture from a reservoir which is maintained at constant temperature and pressure into an agitated glass equilibrium cell which is maintained at constant temperature. The liquid level within the glass equilibrium cell was visually observed, and the pressure was measured to within & 3 psi with a calibrated Bourdon gage. COMPOSITIONS OF MIXTURES STUDIED The compositions of the mixtures studied are summarized in Table 1. The measured properties included in Table 1 will be discussed later in this paper. The sources of these gases are described below: Gas "A-1'' was obtained from the Phillips Petroleum Co. Its composition was reported in connection with earlier work." The properties of this gas were reported in an earlier paper.13 Gases "A-2, A-3, A-4" were prepared by mixing nitrogen with gas "A-1." Gas "AB-1" was prepared by mixing methane with gas "A-1." The properties of this gas were reported in an earlier paper.'" Gases "AB-2" and "AB-3" were prepared by mixing nitrogen with gas "AB-1." Gas "B" was obtained by W. W. Bodle of J, F. Pritchard & Co. from the primary separator of a well in western Kansas. Gas "C" was obtained from a Cities Service Co. pipeline at Lawrence, Kans. Gas "D" was prepared by mixing gas "AB" with gas "C."

Jan 1, 1955

By D. J. Carney, E. C. Rudolphy

Large macroscopic nonmetallic inclusions were related to altered fireclay refractories by chemical and microscopic means. Pouring refractories are discussed as a source of these large inclusions. Nozzles and wells are major contributors. Use of alkali and titania contents as tracers is described. Recommendations are offered to minimize the sources of inclusions from pouring refractories. IN any attempt to improve the cleanliness of plain carbon and alloy steels, consideration must be given not only to the proper deoxidation practice to minimize inclusions, but also to sources of inclusions from pouring refractories. In some cases, the inclusions resulting from deoxidation may be minor in amount, yet a relatively dirty steel may be produced as a result of improper care in the pouring practices for the steel. The number of studies of inclusions resulting from pouring refractories has increased recently and some excellent reports on this subject have already been published.'4 Some of these reports were reviewed briefly in a companion paper by M. P. Fedock.5 Mr. Fedock's contribution is a fine addition to the studies necessary to improve steel cleanliness for the ultimate benefit of all steel producers and consumers. In the interest of constantly improving cleanliness, the authors have been actively engaged for the past two years in experimentation to determine more closely the sources of inclusions in steel. One phase of this work was associated with efforts to define more closely the sources of macroscopic inclusions which have been experienced on occasional heats. The term "macroscopic inclusions" is defined in general as those inclusions which are visible to the naked eye or at low magnifications of the order of less than X25. These inclusions sometimes can be seen in the macro-etch tests of billets and slabs. This report summarizes a few of the field experiments and laboratory studies conducted at the South Works of the United States Steel Corp., which were made regarding nozzles, wells, and ingot scums, as well as inclusions occurring in steel products. The data in the present study, together with the data of Mr. Fedock concerning ladle erosion, should be of value in regard to future studies of inclusions arising from pouring refractories. The knowledge gained as a result of data collected thus far at South Works has been helpful in improving the cleanliness of the products and in pointing the way toward further improvements. Similarity of Large Inclusions to Refractories and Altered Refractories In the routine inspection of billet etch tests, occasional inclusions visible to the naked eye have been observed. These large inclusions most frequently occur near the top of the ingot and near the billet surface. When such material was encountered, careful examinations were made in an attempt to determine the origin of these inclusions. In a relatively few cases, examination revealed that the material was unaltered fireclay refractory of a type similar to that used for hot-top material, with only the surface of the inclusions having an altered appearance under the microscope. However, the great majority of these inclusions were completely altered-refractory material. The term "altered refractory" is defined

Jan 1, 1955

By K. D. Hester, A. W. Fletcher

A nickel-copper sulphide concentrate was treated in a pilot plant at Warren Spring Laboratory during 1961, by a hydrometallurgical roast-leach-solvent extraction process devised to cleanly separate the metal values and produce acid sulphate liquors containing the metals. It is shown that 86 pct of the nickel and 95 pct of the copper could be leached from the calcine, after a sulphatizing roast on finely ground flotation concentrate. Iron was removed from the leach liquor by limestone neutralization with a small loss of values. Copper and nickel were separated by solvent extraction with naphthenic acid in kerosene after partial neutralization of the iron-free liquors with ammonium hydroxide. Hydrogen sulphide and chlorine were used to remove zinc (and residual copper) and cobalt impurities respectively. The recovery of pure copper and pure nickel, by electrowinning, from the acidic solvent extract strip liquors finally produced, appears technically feasible. An economic analysis of production costs shows that small, geographically isolated, nickel-copper sulphide deposits cannot usually be worked profitably by established processes. The requirements for profitable operation on a comparatively small scale could possibly be met by a flotation-roast-leach process. Two difficulties, obtaining satisfactory extraction of nickel from a sulphide concentrate and separating the copper and nickel in solution, have prevented the previous use of this method. A solution to the first problem, dissolution of the nickel, was described in a recent paper by Thornhill.1 It was shown in this paper that copper and nickel in a flotation concentrate could be oxidized to water soluble sulphates by roasting in a fluidized bed with added salt cake. Workers at the Warren Spring Laboratory have shown that the separation of copper and nickel can be accomplished by solvent extraction using a relatively inexpensive carboxylic acid, naphthenic acid. Moreover, the mineral acid required to strip values from the loaded solvent could be produced, and the metals recovered, by electrowinning; thus the latter section of the process was regenerative. The removal of iron from the leach liquor and the elimination of impurities such as zinc and cobalt before nickel electrowinning would be necessary to complete the flowsheet. The process under investigation could therefore be summarized (Fig. 1) as follows: 1) Flotation to produce a bulk sulphide concentrate. 2) Fluidized bed roasting to sulphate the nickel and copper minerals. 3) Leaching of roaster calcine to extract soluble nickel and copper. 4) Precipitation of iron from the separated leach liquor by air oxidation after the adjustment of pH and temperature. 5) Recovery of copper from the iron-free Liquor by pH adjustment and liquid-liquid extraction. 6) Purification of the copper raffinate by removing zinc and residual copper as insoluble sulphides and cobalt as cobaltic hydroxide. 7) Recovery of nickel from the purified liquor by pH adjustment and liquid-liquid extraction. Laboratory and pilot plant studies detailed below, were carried out at the Warren Spring Laboratory, to test the feasibility of each one of the unit processes and to obtain preliminary plant design data. FLOTATION The ore was an altered basic rock containing concentrations of magmatic sulphides.

Jan 1, 1964

By F. Q. Su

Underground Coal Gasification (UCG) is a promising environmentally acceptable clean-coal technology. A typical UCG system has two wells drilled from the surface into a coal seam with some separation of injection from production. The wells are connected underground by various linking techniques. After creating a combustion reactor in an underground coal seam, air and oxygen flow through the injection well. Heat energy and gases are collected from the production well. As gasification progresses, the combustion reactor is moved along the linking hole. Using this process, the fracturing activity inside the coal seam serves an important role for enlargement of the gasification zone because the surface area oxidization increases continuously by coal cracking. For effective coal gasification, fracturing activity must be controlled. Moreover, excess fractures inside the coal seam and surrounding rock can induce gas leakage, underground water contamination, subsidence, etc. Therefore, monitoring and control of fracturing activity in underground areas constitute key technologies for efficient and safe UCG. To monitor fracturing activity, we conducted laboratory and small-scale field experiments of UCG using acoustic emission (AE) measurements. UCG model tests were conducted for linking and coaxial types UCG models. Coaxial UCG systems are compact and are anticipated for application in underground coal seams having a complex geological structure. The UCG model consists of a coal block molded in a steel canister (20 liter capacity) with heat-resistant mortar, with a linking hole or a coaxial-hole passing through the coal block. During coal combustion, coal temperatures, production gas contents, and AE activity were monitored under the control of injection-air and oxygen flow rates. Results show that the combustion propagated inside the specimen along the linking hole. Many AE events were generated during coal combustion. The AE activity was related closely to temperature changes inside the coal block. This AE generation apparently results from crack initiation and extension around the coal combustion area under the influence of thermal stress. However, comparing the results from UCG models of linking and coaxial types, the gasification of the linking type model showed an average calorific value as high as 11.3 MJ/m3. The coaxial type yielded an average calorific value of produced gas as only 5.79 MJ/m3. In the coaxial type of UCG model, the combustion region was limited to the area around the coaxial hole. The AE activity was lower than in the linking type model. For small-scale UCG field experiments, linking and coaxial types were tested at an open pit coal mine in Hokkaido, Japan. Using a linking type UCG, 58.2 kg coal was processed in 39 h, with the calorific value estimated as 11 MJ/m3. However, the coaxial type UCG processed 7.0 kg coal in 9 h, yielding an estimated calorific value of 6.0 MJ/m3. These tendencies resemble those of results of laboratory UCG experiments. Results of these experiments demonstrate that AE monitoring is a useful tool to evaluate combustion reactors for efficient and safe UCG systems. To develop a coaxial UCG system, results show that fracture control around combustion reactors is indispensable.

Aug 1, 2013

By Stephan Fisch, Franz-Werner Gerressen

"The use of cut-off-walls (COW) for the open pit coal mines has been used for decades. They have been used to reduce the negative hydraulic impact to the surrounding area caused by the open pit mining. The pile-guided trench cutting system is a worldwide unique technique, originally developed by the engineers of the mining companies themselves. It guarantees a continuous, joint free, COW during a continuous installation process. At this specific site in Welzow, this technique has been pushed to new limits in order to address the local lake region. Depth capability has been designed to about 430 ft (130m), proven are already depth of about 360 ft (110m) at a constant trench width of 39 inch (1000 mm). This project is approximately. 6.8 miles (11 km) long of COW, scheduled to be completed in 12 years period. About 2.05 miles (3.3km) have been installed, which is equivalent of about 3.5 Million ft² (330,000 m²). The system flushes special clay which forms a filter crust at the inner surface of the trench. Only natural clay resources used, in order to achieve the cut-off effect (colmation effect). The paper explains the installation process of the cut-off-wall as well as the equipment systems developed specifically for this project. After a successful start of the first phase of the project, the next step in the advancement of the equipment is already underway to enable the installation of greater depth to approximately 490 ft (150 m +) and beyond. The next generation equipment system is scheduled to start operation around 2018 INTRODUCTIONThis Serbian saying “Bóh je stworil Lužicu a cert je zaryl brunicu – God created Lusatia and the devil buried brown coal underneath it.” captures local communities’ ambivalence towards lignite.Lusatia is an almost entirely flat stretch of land between the Elbe and Neiße rivers dominated by glacial sands. On the surface, the heathland and woodland is hardly noteworthy. However, three large lignite mining regions, two in Brandenburg and one in Saxony, in the east part of Germany, divert the attention to underground level, down to depths of up to 120 meters. Here, seams crisscross the earth like ribbons. They were formed in the Tertiary around 17 million years ago.The mining of the lignite started almost 200 years ago. To enable open pit mining, a suitable dewatering system was required. At first, wells and drainage system were used. With the increasing demand to go deeper to enable full use of the existing resources with greater mining depth, a decision taken back in the 60th of the last century, the amount of water which had to be pumped increased dramatically. In peak times, approx. 1.57 Billion cubic yards per year (1.2 Billion m³/year) had to be pumped. This led to a lowering of the groundwater level for up to 230 ft (70 m), impacting the regional lake landscape. In order to reduce the influence on the water balance, and bring the water level back to pre1970th, a first development took place to implement the use of specific COW system to depth of about 147 ft (45m)."

Jan 1, 2017

By Adrianus (Adrian) Halim, Tomas Bolsöy, Stina Klemo

"This paper describes the ventilation system used in underground hard rock mines in Sweden and Finland, which is very different than the system used in other major mining countries such as Australia, Canada, South Africa, and USA. The system utilizes auxiliary fans with Variable Speed Drive to distribute primary airflow to working levels instead of regulators that are commonly used in other countries. Descriptions about Ventilation on Demand in this system and ventilation regulations in Sweden and Finland are presented in this paper. This paper also quantifies a comparison between the Nordic and the system used in other countries. KEYWORDS Auxiliary fan, Regulation, Ventilation on demand (VOD), Variable speed drive (VSD) INTRODUCTION The primary objective of an underground mine ventilation system is to provide sufficient airflow to dilute atmospheric contaminants that are produced by mining activities. Typically, a mine ventilation system consists of one to four primary fans, regulators to control primary airflow distribution to levels or panels, and auxiliary fans that distribute airflow to dead-end workings via ducts. Depending on circuit geometry, underground booster fans are sometimes used. This system is widely employed in many countries such as Australia, Canada, USA, United Kingdom, and South Africa. However, mines in Nordic countries such as in Sweden and Finland employ a different system, in which auxiliary fans instead of regulators are used to control primary airflow distribution, as well as distributing airflow to dead-end workings. This paper describes the general layout of Nordic ventilation system, its VOD and heating system, its comparison with the system that is widely used in other countries which is referred as “Non-Nordic ventilation system” in this paper, and the current ventilation regulations in Sweden and Finland. The comparison was quantified by doing simulations using Ventsim Design 5 software. DESCRIPTION OF NORDIC VENTILATION SYSTEM General System Layout Figure 1 shows a schematic of typical ventilation system used in Swedish and Finnish mines. The schematic was drawn by Franzen, Myran, Larsson, and Rustan from Stiftelsen bergteknik forskning (Swedish Rock Engineering Research Foundation) and the English translation is written next to the Swedish terminologies. The system is generally a push-pull system. None of Swedish and Finnish mines use exhaust system. As shown in Figure 1, the primary airflow is distributed to levels by auxiliary fans that are bolted to a bulkhead located in the access to intake raise/shaft. These intake fans are attached to ventilation ducts that distribute airflow to all working faces. The exhaust auxiliary fans, which are not attached to any ducts and also are bolted to a bulkhead located in the access to exhaust raise/shaft, then flow the exhaust airflow into the exhaust shaft. A small quantity of this exhaust air is directed into the ramp, which acts as another main exhaust airway. The deepest level is also equipped with booster fan(s) that draw air from the intake shaft/raise and direct it into the ramp to provide fresh air in the ramp. There is no free split in this system. Figure 2 shows a schematic of a level ventilation layout in the Nordic system. Figure 3 shows a photo of these auxiliary fans."

Jan 1, 2019

By John C. Calhoun, J. E. Warren

A study of waterflood efficiency, given in terms of oil recovery at water breakthrough and u1timate recovery, has been made on short, consolidated Pyrex glass cores rendered oil-wet by chemical treatment. Contact angle. interfacial tension, permeability and porosity were the variables considered. Oil and water viscosities, core length and velocity of flooding were held constant. The data permit interfacial tension, contact angle, porosity, and permeability to be grouped into a scaling coefficient along with viscosity, velocity of flooding and length of core. Correlation of the .scaling coefficient with recovery at water breeakthrough is found to follow prediction; correlations of ultimate recovery demand a scaling coefficient different from that which correlates breakthrough recovery. The work indicates that, with proper control, a group of similar natural cores, of permeability plug size, call he correlated 10 indicate basic flooding performance. INTRODUCTION The fraction of oil recovered from a porous medium is related to both reservoir conditions and production techniques. An investigation of all factors that enter into this relationship is necessary in order to arrive at the optimum method of exploitation for oil reservoirs. To define this relationship, laboratory studies have been made by a great many investigators. However. an important obstacle arises if the results of these experiments on water flooding are to be applied to practice. Ditferences in behavior are to be expected between reservoirs of the dimensions encountered underground and those used in laboratory work. Factors which play an important role under laboratory conditions may be of no consequence in reservoirs. Laboratory operating practices generally differ from field operating practices. Thus. a mere understanding of the mechanism of the displacement of oil by water is not enough. It is just as necessary that the process be analyzed dimensionally to give continuity and validity to the conversion from laboratory to field. The theory of oil displacement that has come to be accepted by the majority of those who are associated with reservoir mechanics had its beginning in the work of Leverett¹ and Buckley and Leverett2. The banking of oil, observed by many previous workers, was described by the "fractional flow" and the "frontal advance'' equations. The validity of the Buckley-Leverett theory was substantiated by the experimental and theoretical work of Terwilliger et al³; moroever, the theory was extended by the introduction of the idea of a "stabilized zone" to describe the banking of oil. Levine5 showed that the Buckley-Leverett equations gave reasonable agreement between calculated and experimental breakthrough recoveries only if the capillary pressure and gravity terms were included. Rapoport and Leas1 investigated the properties of linear floods and showed that both breakthrough and maximum recovery are related to a "scaling coefficient'' derived from the Buckley-Leverctt equations. Jones-Par-ra and Calhoun6 presented another scaling coefficient which included both viscous and capillary variables. Such scaling coefficients should suffice to predicl waterflood efficiency. However, some experimenters report data which does not appear consistent with the healing coefficient approach. For example, Engelberts and Klinkenberg7 conducted an extensive series of experiments on a dimensional model which contained a

Jan 1, 1956

By S. E. Buckley, M. C. Leverett

THE production of oil is accomplished as a result of its displacement from the reservoir by either gas or water, and the amount of oil recovery is limited by the extent to which the displacing gas or water accumulates. This paper describes the mechanism by which the displacement is effected and the advantages of water over gas as a displacing agent. In the light of the results of experimental observations of the flow of mixtures of oil and/or gas and/or water through sands, certain conclusions are drawn relative to the changing character of the displacement as depletion proceeds, and on the effects of the properties of the fluids and of producing conditions on the ultimate oil recovery. INTRODUCTION Crude oil has no inherent ability to expel itself from the pores of the reservoir rocks in which it is found; rather, it must be forcibly ejected or displaced by the accumulation of other fluids. Accordingly, a knowledge of the mechanism by which one fluid is displaced by another is essential to an understanding of the fundamental process by which oil is recovered. The displacing fluids normally available are gas and water, either or both of which may exist originally associated with the oil in a potentially usable form or may be supplied to the reservoir from external sources. Gas is present in most oil reservoirs. If the quantity is relatively small, it may exist originally completely dissolved in the oil, but if the quantity exceeds that which may be held in solution by the oil at the prevailing pressure, the excess will be found in the free state. Most reservoir sands appear to contain some water,1 and in the majority of fields the oil is trapped in the structure and held over water. In certain conditions the entrapping water may advance into the oil zone and displace the oil therefrom. This paper describes in a qualitative manner some of the characteristics of the displacement of oil by either gas or water, with an attempt to elucidate somewhat the mechanism by which such displacement is effected. ROLE OF DISSOLVED GAS When the pressure on an oil containing dissolved gas is reduced to the saturation or bubble-point pressure, gas escapes from solution and expands, imparting to the oil-gas mixture a high degree of expansibility and causing it to flow in the direction of reduced pressure. This expansibility has frequently been attributed to the oil; closer analysis, however, reveals that as gas escapes from solution the oil phase actually contracts. Hence, it is the accumulation and expansion of the liberated gas that supplies the propelling force for the oil. It has been shown experimentally2-5 that within certain limits a sand containing oil, gas and water will permit the simultaneous flow of all three; the readiness with which they may flow depends upon the characteristics of the sand, of each of the fluids, and upon the relative amounts of the fluids in the sand. Thus, in the initial stages of production by the mechanism of dissolved gas drive, the liberated gas is present in the sand in low concentration and is unable to

Jan 1, 1941

By Feng Xue, Mi Xujun, Peng Lijun, Yin Xiangqian, Liu Dongmei, Xie Haofeng, Huang Guojie, Yang Zhen

The Age-hardening Cu-Cr alloys are extensively used in integrated circuit lead frame, railway contact wire, resistance welding electrode and continuous casting mold copper plate, owing to having an excellent combination of high electrical or thermal conductivity and high strength. High temperature performance is very important during the service process. Effect of Magnesium and Zirconium on softening behavior of Cr-Cr alloy are investigated by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). During the softening process in the Cu-Cr alloy, the recrystallization process, grain growth and Cr precipitates coarsening are observed. The addition of Mg or Zr to the Cu-Cr alloy, the resistance to elevated temperature can be significantly improved, owing to being restrained the growth of the precipitates by segregating along precipitates surface. INTRODUCTION Age-hardening Cu-Cr system alloys can be widely uesed in many fileds such as electrodes for spot welding (Hatakeyama et al., 2008; Cheng, Shen & Yu, 2013; Zhou et al., 2016; Chbihi, Sauvage & Blavette, 2012), intergrated circuit lead frame (Hatakeyama et al., 2008; Cheng, Shen & Yu, 2013; Zhou et al., 2016; Liu et al., 2006; Pang et al., Xia et al., 2012; Wang et al., 2009; Huang et al., 2003; Cheng, Yu & Shen, 2014; Zhang et al., 2016; Li et al., 2007) and railway contact wire (Cheng, Shen & Yu, 2013; Zhou et al., 2016; Chbihi, Sauvage & Blavette, 2012; Liu et al., 2006; Pang et al., Xia et al., 2012; Wang et al., 2009; Huang et al., 2003), because it has high strength, good electrical and thermal conductivity. The precipitation behavior of binary or ternary Cu-Cr alloys had been investigated by many researchers (Chbihi, Sauvage & Blavette, 2012; Peng et al., 2017; Batra et al., 2002). In addition, to obtain additional mechanical properties without much deterioration in electrical conductivity, trace addition of alloying elements like Zr, Ag, rare metals (Y and Ce) and Mg are added into Cu-Cr alloy. The addition Mg to Cu-Cr alloy accelerated the process of precipitates nucleation and restrained the growth of the precipitates by segregating along precipitates surface during aging, which enhanced the stability of the deformation microstructure and improved the mechanical properties of the alloy (Zhao et al., 2018). Additional zirconium in Cu-Cr alloy enhances the strength by the decrease in inter-precipitate spacing of Cr precipitates and the formation of Cu5Zr phase (Chihiro, Ryoichi & Kazue, 2008). Owing to the decrease in inter-precipitation spacing of Cr precipitates and to the Ag-atom-drag effect on dislocation motion, the addition of Ag can increase in strength, stress relaxation resistance and without much deterioration in electrical conductivity (Chihiro, Ryoichi & Kazue, 2008). The enhance in strength and electrical conductivity of the Cu-Cr-Zr alloy by adding Ce and Y elements are attributed to removing oxygen and sulfur from as-cast alloy (Li et al., 2006). However, the effect of Mg or Zr element on microstructure and properties of Cu-Cr alloy during the softening process are not clear. Therefore, Microstructure evolution and properties of a Cu-Cr systems alloy were investigated in detail by OM and TEM. The Relationship between microstructure and properties of Cu-Cr systems alloy was also discussed.

Jan 1, 2019

By G. B. Craig, H. E. Rosinger, W. J. Bratina

NUMEROUS studies have been reported on how the mechanical properties of a bcc metal are affected by interstitial solute atoms in the temperature range where appreciable diffusion occurs in finite time. Only recently, though, has work on an "interstitial-free" iron been reported, this by Leslie and sober,' on an Fe-0.15 pct Ti alloy. The data was limited to a maximum temperature of 296°K. This work presents a systematic study of the flow stress and the activation volume of a similar material as a function of plastic deformation over the temperature range 253" to 473°K. The material studied was Ferrovac E iron containing 0.01 wt pct C and 0.0002 wt pct N annealed at 870°C for 1 hr, and the same iron with an addition of 0.15 wt pct Ti annealed at 870°C for 80 hr; cooling rates being 75°C per hr. In the latter alloy depletion of interstitials in the a-iron matrix associated with the second phase formation was expected. The temperature dependence of the flow stress was measured at 6 = 3.33 x 10-5 sec-1 from 253" to 473°K as a function of the deformation in 0.01 intervals from 0.03 to 0.12 strain. Results for two strains, 0.03 and 0.09 are shown in Fig. 1. The flow stress increased and reached a maximum in the Ferrovac E iron with increasing temperature, but showed a consistent gradual decrease in the Ferrovac E-0.15 pct Ti alloy. A yield point and Luders region, observed in Ferrovac E, was absent in the Ferrovac E-0.15 pct Ti alloy. Also, the Ferrovac E exhibited a serrated stress-strain behavior in the temperature range 330" to 400°K; dynamic strain-aging characteristics were absent for the titanium alloy. The activation volume was determined over the same temperature range by the method of stress relaxation at constant strain. Results are shown in Fig. 2. At the temperatures of serrated stress-strain behavior in Ferrovac E the activation volume was found to increase toward infinity and, as the temperature rose, to decrease, to about 100 to 200 v/b3. By contrast, the activation volume for the Ferrovac E-0.15 pct Ti alloy tended to increase continuously from the initial value of approximately 300 at 300°K to more than 800 at 473°K. Above 400°K, then, the corresponding activation volume values of Ferrovac E were less than that of the Ferrovac E-0.15 pct Ti alloy. The activation volumes, Fig. 2, appear to depend on dislocation-interstitial interaction in Ferrovac E and on dislocation-dislocation interaction in Ferrovac E-0.15 pct Ti alloy. The gradual increase in the latter metal is associated with thermally activated motion of dislocation segments.' The decrease of the activation volume in Ferrovac E above 400°K is probably related to the diminishing effect of interstitials on dislocations. Here, the interstitials can be moved along with a dislocation without appreciable drag. As indicated in Fig. 1, removal of interstitials

Jan 1, 1970

By W. R. Opie, O. W. Mole

By confining the electrolytic reduction of TiCl4 to the interior of a porous basket-cathode the electrolyte between the anode and the cathode can be kept free of reduced chlorides of titanium eliminating undesirable reactions of reduced titanium chlorides with brickwork or oxygen in the cell atmosphere. Semiwalls are not needed. Operating conditions are given and discussed. Titanium yields based on TiCl4 introduced are 93 pct. Cell voltage and amperage characteristics are adaptable to multiple cathode-series cell urmngements. EXPERIMENTS conducted in the National Lead Co., Titanium Division, Research Laboratories showed that titanium metal could be deposited in an electrolytic cell in which titanium tetrachloride was introduced through a tubular cathode.' The reduced chlorides as formed were confined to the vicinity of the cathode. They were reduced to form a cocoon-shaped growth of sponge titanium metal at the end of the cathodic tube below the surface of a sodium chloride-strontium chloride electrolyte. No diaphragm was needed.' Although high-purity, coarse crystalline metal was produced in the cocoon growth, the yields of metal removed from the cell, based on the amount of titanium introduced as TiCl4, were usually only 40 to 60 pct. The growth of the cocoon deposits was away from the cathodic tube for introduction of TiC14 toward the anode following the flu lines. The reduced chlorides of titanium diffused through the deposit and were reduced to titanium electrolytically within the deposit or on the outer surfaces. Deposition within the pores of the cocoon was detrimental to further deposition because it plugged the passages used by the reduced chlorides to diffuse away from the point of titanium introduction. As plugging due to deposition in the pores proceeded, the reduced chlorides in the center of the cocoon would force their way out by forming a channel and would escape from the vicinity of the cathode without being reduced to metal. Some work had been done previously1, 2 which indicated that if the end of the cathodic tube for introducing TiC14 was surrounded by a screen connected to the tube so that it too was cathodic, growth could be made to occur within the screen. Direction of growth was observed to be from the screen toward the point of TiCl4 introduction. Through a series of design modifications a cathode evolved which consisted of an introduction tube surrounded by a perforated metal basket as shown in Fig. 1. Modifications of this design are described in Refs. 3, 4, and 5. This basic cathode designa" was incorporated in electrolytic cells containing graphite anodes and constructed of high-silica brick refractory for containing the electrolyte (see Fig. 2). The inner crucible was surrounded by insulating brick and the entire unit contained in a welded steel shell. Suitable cooling chambers with inert gas atmospheres were devised so that the cathode could be removed from the cell without exposing the deposit to air while hot. Various alkali and alkaline earth chlorides were used as electrolytes.

Jan 1, 1961