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Rock Mechanics - The Influence of Geological Factors in the Stability of Highway SlopesBy C. J. Leith
A study of the effect of rock composition, rock structure and degree of weathering on the stability of cut slopes is being sponsored jointly by the U.S. Bureau of Public Roads and the North Carolina Highway Commission. In 58 mountain and piedmont counties of North Carolina the percentage of failed cut slopes is greatest in micaceous metasediments, gneisses, and schists, and in saprolite and soil derived from these rock types. Soil slope failures outnumber rock slope failures by two to one. Joints and similar planes of separation exert a strong influence on size and shape of the sliding mass. They may or may not act as failure surfaces, depending on their orientation with respect to the active forces. Climatological data, though indicative of weathering conditions, do not correlate well with slope failure frequency. Because of the presence of joints and similar planes of weakness in soil and rock materials, conventional methods for analyzing slope stabilities are not directly applicable. Empirically derived modifications of these methods are being investigated. A study of the stability of highway cut slopes, sponsored by the U. S. Bureau of Public Roads and the North Carolina State Highway Commission, began in 1962 at North Carolina State of the University of North Carolina at Raleigh. As part of this study all slides, rockfalls and other types of cut slope failures on Federal and State highways in the 58 mountain and piedmont counties in North Carolina were located and described, and the data catalogued in a punched card file system. A major objective of the project is to relate slope failures to properties and physical conditions of the geological units in which the slopes were constructed, and to correlate soil type and/or geological unit with type and frequency of slope failure. The complexities of the problem of slope stability and the limitations which these complexities impose on methods for analyzing slopes have been recognized for many years. A great variety of factors and processes may lead to slides, often making it almost impossible to analyze theoretically the conditions required for stability of slopes. One of the principal factors determining maximum safe slopes is the shear strength of the material in which the slopes are cut, but unfortunately there are very few data available concerning shear strengths of residual soils. Vargasl tested clay derived from gneiss and granite in southern Brazil; the properties of decomposed granite occurring near Hong Kong were determined by Lumb.2 These data are being used, when applicable, to supplement the test data obtained in the present study by Yorke.3 The locations of the North Carolina slope failures, more than 400 in number, are shown on Fig. 1. This map, adapted from the Geological Map of North Carolina,4 suggests the possibility of a relationship between frequency of slide occurrence and rock type. However, the evaluation of this possibility requires consideration not only of the type of rock, but also of its large and small scale structural features, its susceptibility to and degree of weathering, and the composition and structure of the weathering products. Soil slope failures in thoroughly weathered soil material and saprolite outnumber rock slope failures two to one. INFLUENCE OF ROCK TYPE The agricultural soil type involved in each soil slope failure was identified and each failure was catalogued in terms of the parent material from which the soil was derived. These data indicate that most of the slope failures, whether in the rock or in the derived soil, are associated with metamorphic rocks (see Fig. 2a). The data may be skewed somewhat because of the relative sizes of the total areas underlain by the various rock types, but Leith and Gupton5 have demonstrated that the preponderance of failures in metamorphic rocks is of much greater magnitude than could be accounted for by the areal factor alone. The dominance of metamorphic rocks is emphasized when soil slope failures are considered in terms of the specific rock types from which the soils were derived (see Fig. 2b). In particular, mica schists and mica gneisses account for more slides
Jan 1, 1965
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Institute of Metals Division - Experimental Techniques for the Direct Observation of Fatigue- Induced Deformation Faulting in Thin-Foil Stainless SteelBy L. E. Murr, P. J. Smith
A study has been made by transmission electron microscopy of thin foils of 304 stainless steel fatigued external to the electron microscope in reversed bending, and of thin foils fatigued directly within the microscope in alternating tension. The build-up of stacking faults in the thin foils during fatigue zoas correlated with the dislocatirm structures found in thin films prepared fror fatigued bulk specimens. The performance of the special devices designed for fatigue of thin foils so outlined and the importance of alternative methods of preparation of more uniform fatigue specimens bY vapor deposition are emphasized. INVESTIGATIONS on fatigued bulk aluminum1,' and stainless stee13j4 have revealed the existence of dislocation substructure on examination by transmission electron microscopy of electrolytically thinned foils representative of these bulk specimens. While this technique has proved extremely valuable, it has several shortcomings. First, the method of fatiguing bulk specimens and then thinning to foil for electron-transmission observation allows only one observation of internal structure at any one portion of the fatigue life. Second, thinning the bulk fatigued specimens to foil results in the loss of at least one original surface. Thus, what one sees in the remaining electron-transparent sections is an internal dislocation or fault structure which in many cases cannot be correlated with the original surface markings. This is an undesirable feature, since it is well-known that metal surfaces play an important part in the fatigue process.5 An obvious third undesirable feature of the thinning-from-bulk technique is the fact that static observations have difficulty (in the case of fatigue) explaining the mechanism of a dynamic process. What is required then is a method whereby a selected thin area can be continuously observed either while undergoing cyclic deformation or at various fixed stages of fatigue deformation. While Murr and wilkov6 have reported some success with an apparatus designed to fatigue thin metal foils directly within the electron microscope, the nature of the specimen-mounting procedure and the mechanical features involved in the adaptation of the fatigue device to the electron microscope make this method difficult to operate. It was not possible, for example, to make frequent observations of a selected area because of difficulty in maintaining a chosen area in a stable viewing position inside the electron microscope. Except for the build-up of a dislocation substructure and what are commonly referred to as "slip striations", little else has been reported from observations on thin-foil sections prepared from bulk fatigue specimens. segal17 has found "slip striations" in stainless-steel fatigued specimens which were electropolished from both sides, but gave no explanation as to their origin or identity in terms of lattice imperfections. The research to be reported in this paper was undertaken with the following objectives in mind. First, an attempt was made to devise a technique or techniques whereby thin metal foils could be fatigued and repeatedly observed by transmission electron microscopy. Second, it was hoped that some correlation could be made between deformation striations found in fatigued thin transmission specimens and thin foils prepared from bulk fatigued specimens. These investigations illustrate quite convincingly that a feasible method is available for the direct study of the fatigue mechanism and similar dynamic phenomena in thin transmission specimens inside the electron microscope. I) EXPERIMENTAL METHODS Three modes of specimen fatigue and observation of fatigue damage were used. These involved fatigue of thin-foil specimens in a special arrangement external to the electron microscope and observation of a selected area at various stages in the fatigue life, the fatigue of thin-foil transmission specimens inside the electron microscope, and the fatigue of bulk specimens external to the electron microscope followed by thin-foil preparation for direct observation at predetermined stages. Design of the External Fatigue Clip and Specimen Holder for the Hitachi H.U.11 Electron Micro-scope. The purpose of the fatigue clip was to provide a reversed bending fatigue stress to a thin-foil transmission specimen outside the electron microscope. In order to accomplish this, a flat-bottomed, U-shaped brass clip was made as shown
Jan 1, 1965
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Geophysics and Geochemistry - Progress in Mapping Underground Solution Cavities with Seismic Shear WavesBy J. C. Cook
In solution-mining of underground salt and similar minerals, using drilled wells for access, it is desirable to monitor the lateral growth pattern of the resulting fluid-filled cavern. Therefore, a process of seismic surveying from the surface of the ground has been conceived in which the amplitudes of waves reflected from and transmitted through the soluble formation are measured. The large acoustic impedance contrast between solid and fluid should produce striking amplitude anomalies, especially if shear waves are employed, since thick fluid bodies are opaque to shear waves. Horizontally-polarized (SH) shear waves are best for preventing conversion to P waves at the numerous horizontal interfaces in the ground. Field tests to date have shown that a truck-mounted, half-ton hammer striking horizontally against the end of a trench produces usable SH-wave energy at lateral distances up to about 850 ft. Horizontally-directed explosive wave sources were effective to about 2000 ft. Conventional magnetic-tape recording and processing were used, but with the detecting geophones oriented to favor SH waves. An irregular solution cavity in bedded salt at 500-ft depth has apparently been located by SH-wave and SV-wave reflections. Further field work is planned to corroborate and extend this result. The Brine Cavity Research Group, an association of 11 chemical and salt producing companies, is supporting this work. Major deposits of salt in tabular beds lie beneath some 300,000 sq miles of land in the central and northeastern U.S. This salt is a basic source of soda ash and chlorine, and has been extracted as brine from drilled wells for about a century. During the past two decades, the U.S. solution-mining industry, following the lead of European operators, has greatly improved the extraction process through the application of engineering and science.' In 1957, the Brine Cavity Research Group, an association of 11 chemical and salt producing companies, was formed. This group proceeded to attack certain common problems through the support of research. An outstanding problem has been that of determining the shape and location of the growing solution cavities in the underground salt, so that measures can be taken to maintain operating efficiency. The problem has been partially solved by the Dowel1 sonar mapping service, which employs a pulse-echo device lowered into the cavity through the well.2 However, the working range of this equipment is at present insufficient for large cavities, and echoes are not returned from highly sloping walls nor from behind such obstructions as rock debris. Therefore, an independent means of mapping the cavity, for example, from the surface without interfering with operation of the well, would be desirable. THEORY OF THE METHOD Seismic waves are the only physical agent known to be capable of sufficient resolution and penetration to define typical solution cavities from the surface of the ground. The geometry is unfavorable: cavity widths are generally less than half their depths below the surface; resolution and lateral location of boundaries and channels to within 50 ft at depths of 500 to 3000 ft is desirable. Conventional seismic surveying, as used for petroleum prospecting, is probably not the answer: isopach mapping, for example, is not thought accurate enough to define the cavity by the slight additional delay time it would introduce (of the order of 0.005 sec for a 50 ft-thick cavity in hard Paleozoic rocks). Refraction surveying has also been considered, but seismic specialists see little promise in it for this problem. In 1957, in correspondence with industry personnel, the writer suggested a seismic method based upon careful measurement of reflection amplitudes. As Table I illustrates, seismic reflection coefficients r for typical brine-rock interfaces are considerably higher than those for typical interfaces between different kinds of solid rock. This fact can be utilized in two ways, illustrated in Fig. 1: 1) If the cavity roof is reasonably flat (which it may sometimes be since the unsaturated top brine will be in contact with an insoluble rock stratum), extra-strong seismic reflections will be received from the salt stratum where the solid has been replaced by liquid.
Jan 1, 1964
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Reservoir Engineering–General - Wellbore Heat TransmissionBy H. J. Ramey
As fluids move through a wellbore, there is transfer of heat between fluids and the earth due to the diflerence between fluid and geothermal temperatures. This type of heat transmission is involved in drilling and in all producing operations. In certain cases, quantitative knowledge of wellbore heat transmission is very important. This paper presents an approximate solution to the wellbore heat-transmission problem involved in injection of hot or cold fluids. The solution permits estimation of the temperature of fluids, tubing and casing as a function of depth and time. The result is expressed in simple algebraic form suitable for slide-rule calculation. The solution assumes that heat transfer in the wellbore is steady-state, while heat transfer to the earth will be unsteady radial conduction. Allowance is made for heat resistances in the wellbore. The method used may be applied to derivation of other heat problems such as flow through multiple strings in a wellbore. Comparisons of computed and field results are presented to establish the usefulness of the solution. INTRODUCTION During the past few years, considerable interest has been generated in hot-fluid-injection oil-recovery methods. These methods depend upon application of heat to a reservoir by means of a heat-transfer medium heated at the surface. Clearly, heat losses between the surface and the injection interval could be extremely important to this process. Not quite so obvious is the fact that every injection and production operation is accompanied by transmission of heal between wellbore fluids and the earth. Previously, the interpretation of temperature logs',' has been the main purpose of wellbore heat studies. The only papers dealing specifically with long-time injection operations are those of Moss and White3 and Lesem, et al.' The purpose of the present study is to investigate wellbore heat transmission to provide engineering methods useful in both production and injection operations, and basic techniques useful in all wellbore heat-transmission problems. The approach is similar to that of Moss and White:' DEVELOPMENT The transient heat-transmission problem under consideration is as follows. Let us consider the injection of a fluid down the tubing in a well which is cased to the top of the injection interval. Assuming fluid is injected at known rates and surface temperatures, determine the temperature of the injected fluid as a function of depth anti time. Consideration of the heat transferred from the injected fluid to the formation leads to the following equations. For liquid, Eqs. 1, 1A and 2 are developed in the Appendix. These equations were developed under the assumption that physical and thermal properties of the earth and wellbore fluids do not vary with temperature, that heat will transfer radially in the earth and that heat transmission in the wellbore is rapid compared to heat flow in the formation and. thus, can be represented by steady-state solutions. Special cases of this development have been presented by Nowakl and Moss and White.3 Both references are recommended for excellent background material. Nowak' presents very useful information concerning the effect of a shut-in period on subsequent temperatures. Since one purpose of this paper is to present methods which may be used to derive approximate solutions for heat-transmission problems associated to those specifically considered here, a brief discussion of associated heat problems is also presented in the Appendix. Analysis of the derivation presented in the Appendix will indicate that many terms can be re-defined to modify the solution for application to other problems. Before Eqs. 1, 1A and 2 can be used, it is necessary to consider the significance of the over-all heat-transfer coefficient U and the time function f(t). Thorough discussions of the concept of the over-all heat-transfer coefficient may be found in many references on heat transmission. See McAdams5 or Jakob," for example. Briefly, the over-all coefficient U considers the net- resistance to heat flow offered by fluid inside the tubing, the tubing wall, fluids or solids in the annulus, and the casing wall. The effect of radiant heat transfer from the tubing to the casing and resistance to heat flow caused by scale or wax on the tubing or casing may also be included in the over-all coefficient. According to McAdams, on page 136 of Ref. 5>
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Institute of Metals Division - Evidence of Vacancy Clusters in Dislocation-Free Float-Zone SiliconBy T. S. Plaskett
A striated structure perpendicular to the growth axis was observed by the copper-decoration tech-nique in dislocation-free, .float-zoned silicon crystals. The striations, which were spaced about 100 p apart, fitted the relationship d = f/u , where d is the spacing, f is the growth rate, and u is the crystal rotation rate. Each stria was resolved into an UNDOPED silicon crystals pulled from quartz crucibles by the Czochralski technique usually exhibit a striated structure perpendicular to the growth axis.'-' This structure has been attributed to oxygen segregation, with the oxygen being introduced from the quartz crucible. If the crucible is rotated, the level of oxygen contamination has been reported as high as 10° atoms per cu cm.10 These striations are similar to solute striations commonly observed in doped Czochralski-grown crystals. The periodic nature of the striations is caused by a periodic variation in the growth rate",12 which is attributed mainly to thermal gradients in the melt.13 A finer striated structure14 attributed to constitutional supercooling is sometimes observed between the coarse striae. The oxygen striations have been observed by infrared transmission techniques,' by the copper-decoration technique,' by X-ray diffraction microscopy,6-8 and by 9 p absorption measurements3 on crystals pulled from the melt both with and without dislocations. In this investigation float-zoned dislocation-free crystals were examined by the copper-decoration technique. The level of oxygen for float-zone material is less than 1016 atoms per cu cm the lower limit of detection by 9 p absorption measurement. EXPERIMENTAL TECHNIQUE The crystals were grown by the float-zone process with the rf heating coil outside of the quartz envelope containing the silicon. All float zoning was done under an atmosphere of purified helium. The Dash technique15 was used to grow the crystal dislocation-free. This involves growing the crystal initially with a diameter between 2 and 3 mm and at array of starlike precipitates of copper. The strucLure was not .found at the surface tor a depth of about 1.5 mm, or in a region of similar width ahead of a dislocation network. The structure is postulated to consist of vacancy clusterings or dislocation loops. very rapid rates, about 20 mm per min, for a distance of about 3 cm. The diameter of the crystal is then increased to the diameter of the source of silicon, which in this case was about 19 mm. Because of the arrangement of the apparatus, the zone was passed downward rather than upward, contrary to the standard float-zoning practice. Also, the source was rotated rather than the seed. ziegler17 has made dislocation-free crystals by a similar technique but has passed the zone upwards. The starting material was zone-refined and had a p-type resistivity of 150 ohm-cm. The major impurity was boron; the total impurity excluding the boron was reported by the supplier (Dow-Corning) to be typically less than 2 x 1013 atoms per cu cm. The crystals were examined by the Dash copper-decoration technique18'19—a method in which about 10" atoms per cu cm of copper are diffused at a temperature between 900" and 1000°C into silicon which is then quenched to room temperature. On quenching, the copper precipitates on crystalline defects which are then visible when viewed by transmission infrared microscopy. The photomicrographs shown were taken either of the infrared image tube screen or directly on infrared film. All sections prior to decorating were chemically polished and, for some sections, given a sirtlZ0 dislocation etch-pit examination. After decorating, the samples were mechanically polished. RESULTS A photomicrograph, taken in transmission of a decorated cross section, is shown in Fig. 1. The portion of the section shown is near the surface of the crystal. The entire cross section showed no dislocation etch pits after being given a Sirtl etch treatment. It is seen that the copper precipitated randomly. Each precipitate, as has been reported by others, was found to have a starlike structure.
Jan 1, 1965
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Coal - Coking Properties of Pittsburgh District CoalsBy D. E. Wolfson, D. A. Reynolds, F. W. Smith
IN 1948 the U. S. Bureau of Mines began a three-phase program to evaluate the extent and quality of U. S. coking coal: 1) a factual appraisal of known recoverable reserves in beds of mineable thickness, 2) a study of preparation characteristics, and 3) a study of carbonization properties. A previous paper presented the methods used in assessing reserves.' Although this investigation is only partly completed, data on coking properties of the Pittsburgh district coals are now available. The results are presented in this article. When coals are selected for manufacture of metallurgical coke more factors must be considered than for any other major use, as no basic industry requires coal of such high quality and uniformity. This is particularly true in the Pittsburgh district, where blast furnace practice is based on use of cokes from high quality coals. Although it is true that inferior coals are carbonized in other industrial areas, both here and abroad, the Pittsburgh coals are the best economically obtainable in the required tonnages, even though they are not the most desirable for metallurgical use. In the general evaluation of suitability of coals for coke making, particular attention is given to: 1) reserve, 2) ash and sulfur content, 3) inherent properties of forming strong, well fused coke, 4) expanding characteristics, and 5) blending properties. Items 1 and 2 are covered in detail in the first two phases of the survey, and coking behavior is considered in items 3 through 5. Problems is Coal Evaluation: Although not all coal beds of immediate or potential use to the coking industry in the Pittsburgh area have been tested for their coking properties, enough tests have been made to permit certain generalized statements. Virtually all the coals that will be used in this district are from the Appalachian region, and except for high oxygen coals from outcrops or stripping operations, they are coking coals. Hence the evaluation problem is not so much that of distinguishing between coking and noncoking coals as attempting to measure quantitatively differences in the coking and expanding properties of the better coking coals. Quantitative differentiation between good coking coals, is complex, since differences in their coking abilities are frequently of about the same magnitude as the precision of the test. Small-scale tests are generally unsuitable for measuring these slight differences, and there has been gradual acceptance of pilot-scale tests. Test Methods Employed: All the data reported here were obtained in two units known as the Bureau of Mines-American Gas Association (BM-AGA) carbonization apparatus and the sole-heated expansion oven. The BM-AGA unit, which consists essentially of a cylindrical steel retort about 18 in. diam and 26 in. high, carbonizes enough coal (180 lb) to allow evaluation of the coke by standard methods of the American Society for Testing Materials. The BM-AGA carbonization procedure and methods of testing the gas, liquid, and solid products have been described.' Expanding characteristics of the coals were determined in the sole-heated expansion oven," wherein the coal charge, heated from the bottom only, is carbonized under a constant applied force and the linear expansion or contraction is measured. Although results in this oven have never been quantitatively correlated with the expansion behavior of coals in conventional slot ovens, they are useful in assessing expansion behavior. In this report discussion will be confined to results obtained from these pilot-scale units, although the following data are available for most coals: proximate and ultimate analyses, free swelling index, agglutinating value, and plasticity. Sources of Coals Tested: In selection of coals for coke manufacture, economic considerations are as important as quality, and each coke plant balances these two factors to meet requirements of the most satisfactory coke at lowest price. Although these economic factors may in some instances outbalance small differences in coke quality, they are usually specific to each coke plant and cannot be given in any general statement. Recognizing that coal and plant operating costs are beyond the scope of the survey, the USBM evaluates the coking quality of various coals without regard to their competitive economic status. For the purpose of this article, coals of interest to the Pittsburgh district are arbitrarily defined as
Jan 1, 1958
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Commercial Paper: An Innovative Source Of Financing For Mining ProjectsBy Robert Gillham, Victoria Yablonsky, Grover R. Castle
INTRODUCTION The commercial paper market, unique to the United States, is a direct exchange of funds between high-grade borrowers and large lenders; because it eliminates both the bank's role as middleman and also some significant transaction costs, commercial paper is the lowest cost short term instrument in the world. For this reason, virtually all borrowers would like to enter the market, but only issuers with the highest rating from Moody's and Standard & Poor can attract purchasers at the best rates. COMMERCIAL PAPER The commercial paper market, in existence for over 100 years, has traditionally been used for short-term financings, with most paper maturing within 30-45 days. Under the U. S. Securities Act of 1933, (section 3(a)3) industrial paper can avoid registration only if it matures within 270 days and is used for current transactions. It was first used to finance the short-term seasonal working capital needs of manufacturing companies. Since World War II, commercial paper use has grown steadily, serving in the 1950's as the market in which finance companies financed the explosion in consumer credit purchases of heavy consumer durables. LETTER OF CREDIT BACKING As far as is known, the use of letters of credit to support energy-related commercial paper began about 13 years ago with an arrangement to finance the nuclear fuel for Con Edison's Indian Point 3 Plant. Goldman, Sachs was the architect of this financing and Chemical Bank provided the letter of credit support. After an early burst of interest, this type of financing wobbled severely in the difficult credit markets of the mid-seventies before regaining serious momentum in 1976 and 1977. A mining project would not normally qualify as a borrower in the commercial paper market because of its credit standing and because its large capital needs require long term financing. However, lately, commercial paper has begun to take the place of a bank term loan in limited recourse project financings. L/C backed commercial paper took this new and startling turn in 1982 when it was used as part of the $700 million financing for the development of the Newlands-Collinsville coal mines of Mount Isa Mines Ltd. in Australia. This was the first use of L/C backed commercial paper in a long-term limited recourse project financing. First Boston acted as financial advisor and, again, Chemical Bank provided sole letter of credit support of $155 million. The $785 million BHP financing for the acquisition of the Queensland (Australia) coal assets of Utah International from General Electric Company followed the next year; there we acted with two other Front Banks to provide $270 million of L/C support. These two important transactions indicate that not only has commercial paper become an integral part of a long-term financing package, but also that it is no longer the exclusive domain of the best known U. S. companies. Lesser-rated companies and a multitude of foreign borrowers have gained access to this "exclusive club." How has this become possible? OPERATION OF AN L/C An instrument of the commercial banks, the "direct pay" letter of credit, has enabled lesser-rated companies to issue commercial paper in their own names. The letter of credit allows the issuer to substitute the credit rating of the supporting bank for its own. The L/C in effect allows a lesser-rated company to rent the bank's credit rating. This upgrading is possible because the bank is unconditionally obliged to pay the note-holders at maturity and then turn to the Issuer for reimbursement. The Issuer commonly "rolls over" a new short-term issue and reimburses the supporting bank from the sale of the new issue until cash flows from the project allow the borrower to reduce the level of paper outstanding. The commitment for an L/C facility, up to 12 years in the case of the Broken Hill transaction, governs the life of the commercial paper tranche of the financing. The term of the L/C commitment thus has the power to extend the ordinary 30-45
Jan 1, 1985
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Coal - Remaining Recoverable Coal of a Part of the Southern Appalachian FieldBy R. Q. Shotts
This paper is a review of recoverable reserves of bituminous coal in the Southern Appalachian area, according to the latest published estimates. A few comparisons are made, some apparent trends are discussed, and some comments are made regarding the limitations of present estimates. The definition of Southern Appalachian area used in this report is somewhat arbitrary. It includes all the bituminous coal deposits of Alabama, Georgia, and Tennessee. All of West Virginia has been excluded. The East Kentucky and Virginia counties included were selected in connection with a literature study the writer made in 1959 of possible coal supply areas for the Tennessee Valley Authority. The selected counties were considered to be the only ones from which TVA might expect to obtain coal. The availability of coal from some of these counties is doubtful, but no other East Kentucky counties were considered more than remote possibilities. With these limitations, the Appalachian area covered is that from which producers of electric power and steel and commercial coal users, located in the Southeastern U. S., may expect to obtain their supplies of coal. Of course, it is recognized that coal from the eastern interior fields is also available to many of these same organizations. RANK AND QUALITY OF THE COALS Practically all the coals in the Southern Appalachian region are of high volatile A bituminous rank. An occasional sample indicates a slightly lower rank, but such samples may be oxidized or otherwise not representative. Some thin beds in Lookout Mountain and Sand Mountain in Alabama and Georgia, are low volatile bituminous coals, but they have not been mined extensively in modern times. There is a possibility that some of the deeper beds along the southeastern edge of the Warrior field of Alabama are near the Low-medium volatile bituminous dividing line. The Sewanee bed and some other minor ones of the Southern Tennessee field, some of the lower beds in Virginia, many beds in Sand and Lookout Mountains in Georgia and Alabama, one or more beds in the Coosa field, possibly some lower beds in the Cahaba field, and most of the beds along the southeastern edge of the Warrior field and the southern end of the Sequatchie anticline of Alabama, are of medium volatile bituminous rank. The quality of the Southern Appalachian coals is highly variable. Some of them, particularly such prevailingly thin ones as the Black Creek bed of Alabama and the Straight Creek bed of Kentucky, are unusually low in mineral matter— probably the lowest in the U. S. With the exception of certain beds and local areas, Alabama and East Kentucky coals probably have as low average ash and sulfur content as can be found in any sizeable coal area in the country. The sulfur content of Southern Appalachian coals is also variable, but few beds are consistently high in sulfur. In Alabama, sulfur generally increases from southeast to northwest across the Warrior field, but this trend is not quite as clear in the other states. A few beds in Northern Tennessee are prevailingly high in sulfur. All Southern Appalachian coals are potential coking coals if they can be prepared to meet chemical requirements. Only a comparatively small part of the medium volatile A bituminous coal, but most of the medium volatile bituminous coal mined is actually used for coking purposes. An estimate of reserves of coking coal under the requirements of present practice, could be compiled comparatively easily, but this probably has never been done. The reserve of coal that can be coked as an ingredient of a suitable blend is probably many times the size of the reserves of coal that will yield suitable blast furnace and foundary coke without blending. WHAT CONSTITUTES ECONOMICALLY RECOVERABLE COAL RESERVES? When one first realizes the vast extent of the coal-bearing rocks in the Southern Appalachian area, (see Fig. 1) the thought is likely to occur that the supply of coal is inexhaustible. This is particularly true on realizing that in some of the basins of thicker coal-
Jan 1, 1962
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Winifrede Mine Coal-Handling Facilities (3e82d471-020a-409e-acc1-5306c521c426)By John E. Young
U.S. Steel Corp.'s Winifrede mine is operated by Lynch District in the mountainous region of eastern Kentucky. This region is characterized by narrow finger ridges and precipitous slopes, which present both an opportunity and challenge in the design and selection of coal-handling facilities for the movement of coal from the section belts to the railrod cars. Lynch District selected diesel-powered locomo¬tives and 100-ton articulated cars capable of negotiating sharp curves. The drop¬bottom mine cars are equipped with longitudinally hinged doors that are auto¬matically opened and closed. Lynch District selected a large-diameter steel-lined borehole for lowering the coal approximately 1000 ft from the seam level to the valley floor railroad load-out point. Taking advantage of gravity, the presized coal is "lowered" vertically approximately 720 ft to existing entries of a previously abandoned mine. The coal is then conveyed horizontally into storage. The coal¬handling facility from the mine-car dump to the railroad load-out point is fully automatic through use of tone control. TV cameras are installed along the facility to continuously monitor the strategic points. The diesel locomotives are either directly operated or remotely radio-controlled, depending on the functions Per¬formed. U.S. Steel Corp.'s Winifrede mine is operated by Lynch District in the mountainous region of eastern Kentucky. This region is characterized by narrow mountain ridges and precipitous slopes which present both an opportunity and challenge in the design and selection of coal-handling facilities for the movement of coal from the section belts to the railroad cars. The narrow finger ridges precluded use of under¬ground haulage and, thereby, presented the opportunity to use high-capacity equipment on the outside bench. The precipitous mountain slopes, steepest at the Wini¬frede seam horizon, presented a challenge to select a solution for lowering the coal approximately 1000 ft from the seam level to the valley floor railroad load-out point. It was evident from the start of planning that these two factors predominated; namely, rail haulage and coal lowering, and solutions to these would determine the final design of the Winifrede mine coal-handling facilities. The Winifrede mine derives its name from the Wini¬frede Seam which comprises the total reserve recov¬erable from this facility. The seam is 5 ft high with a good siltstone bottom and competent shale or sandstone roof. The seam is at an elevation of 2700 ft where the mountain ridges are long and narrow. This configuration of the reserve was ideal for conveyor belt installation to transport the coal from the working face to the outside bench. The preclusion of underground rail haul¬age permitted an opportunity to review the type of locomotive power and to select high-capacity equipment without the limitations associated with underground systems. Since the basic electrical design of the mine was al¬ternating current, with rectification to direct current for shuttle cars required only in the face areas, there was no point in bearing the burden of additional cost of dc trolley installation. And, since the haulage would re¬quire only a few tunnels to negotiate sharp points and to reach the back side of the reserves, diesel power was selected for the haulage locomotives. To provide stability on the almost continuously curv¬ing track and to provide the maximum width of haul¬age equipment, both locomotives and mine cars, stan¬dard railroad gage was chosen to offer the largest choice of equipment. The decision was made to select a standard 45-ton railroad diesel locomotive but to lower the cab height to reduce tunnel excavation requirements. The mine car was the next challenge. Past experience in Lynch operations indicated that drop-bottom cars would be a successful application with the free-flowing coal. The search was for a drop-bottom car within the dimensions of the locomotive to discharge the coal in the shortest time. Numerous types were considered and visits made to various sites to observe cars in operation.
Jan 1, 1972
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Part IV – April 1969 - Papers - An Investigation of the Formation and Growth of G. P. Zones at Low Temperatures in Al-Zn Alloys and the Effects of the Third Elements Silver, Silicon,and MagnesiumBy M. Murakami, Y. Murakami, O. Kawano
The formation and growth of Guinier-Preston zones in Al-Zn alloys containing 4.4, 6.8, 9.7, and 12.4 at. pct zn have been studied by the X-ray small-angle scattering method. Particular attention was paid to the effects of small amounts of third elements silver, silicon, and magnesium on the formation and growth of G.P. zones. It was noticed that an appreciable number of G.P. zones were formed during the course of rapid cooling and that the size, volume fraction, and number of these G.P. zones were influenced by the existence of the third elements. During subsequent aging it was also found that the addition of both silver and silicon lowered the temperature for the growth of G.P. zones, whereas the addition of magnesium raised it. These results were explained in terms of the mutual interactions among zinc atoms, vacancies, and the third elements. A number of studies on the formation and growth of Guinier-Preston zones in Al-Zn alloys have been reported.1-4 Panseri and Federighii have found that the initial stages of zone growth take place at temperatures as low as around -100°C. For investigation of the mechanism of the initial stages of zone growth, growth studies must be carried out at low temperatures. In order to investigate the possibility of the formation of G.P. zones by the nucleation mechanism or the spinodal decomposition during quenching which was reported by Rundman and Hilliard,5 the examination of the as-quenched structure must be performed. In this paper the investigation of the early stages of the formation and growth were determined by means of the X-ray small-angle scattering method. With this technique, change of X-ray scattering intensities was measured while quenched specimens were heated slowly from liquid-nitrogen temperature to room temperature. At as-quenched state and after heated to room temperature, investigation of zone size, volume fraction, and zone number per unit volume was carried out. Measurements on these specimens yielded information on the early stages of zone formation and growth. Measurements were made also on specimens quenched to and aged at room temperature. From these measurements the previously reported model6 for the later stages of growth is confirmed; namely, the larger zones grow at the expense of smaller ones. Three elements, silver, silicon, and magnesium, were chosen as the third elements for the following reasons: Silver. In the binary A1-Ag alloy the spherical disordered 77' zones were observed immediately after quenching.7 Therefore, in the Al-Zn-Ag alloys, it is suggested that silver atoms might induce cluster formation during quenching. Also, since the migration energy of the zinc atoms was found to be raised by the addition of silver atoms,' silver atoms may have a great effect of the zinc diffusion, especially during low-temperature agings. Silicon. The effects of the addition of silicon atoms were found to be marked, especially at low-tempera-ture aging. In the binary Zn-Si system, no mutual solid solubilities between silicon and zinc9 and no in-termetallic compounds10 are reported to exist. Shashkov and Buynov11 investigated the behavior of silicon atoms in Al-Zn alloys and showed that silicon was not in the G.P. zones. The interaction between silicon atoms and vacancies is strong enough to increase the quenched-in vacancy concentration.* Magnesium. Magnesium atoms are reported to trap quenched-in vacancies and after much longer aging times these trapped vacancies will become free and act as diffusion carriers.13 Therefore at intermediate aging times, the diffusion of zinc atoms in Al-Zn-Mg alloys will be slower than in the binary Al-Zn alloys, whereas at longer times zinc diffusion will become faster. EXPERIMENTAL PROCEDURE The alloys used in this investigation had compositions of 4.4, 6.8, 9.7, and 12.4 at. pct Zn with or without 0.1 and 0.5 at. pct Ag, Si, or Mg. The alloys were prepared from high-purity aluminum, zinc, silver, silicon, and magnesium, with each metal having a purity better than 99.99 pct. The analyzed composition of the specimens is given in Table I. The measurements of the X-ray small-angle scattering were carried out with foils of 0.20 mm thick. The change of the scattering intensity was always measured at the fixed scattering angle of 20 = 2/3 deg. This angle exists nearly on the position of the intensity maximum. The value of the interparticle interference function14 which has large effect in this range of angles may not change abruptly in the case of the spherical shape of small zones. Therefore, from the above considerations, it is concluded that an increase of the intensity measured at this constant angle corresponds to an increase of the average radius and volume fraction of G.P. zones. The specimens were homogenized at 500°, 450°, and 300°C for 1 hr in an air furnace. For the study of the formation and growth at low temperatures, the foil
Jan 1, 1970
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Part VIII – August 1968 - Papers - Cellular RecrystaIIization in a Nickel-Base SuperalloyBy J. M. Oblak, W. A. Owczarski
A cellular appearing recrystallization product formed by annealing a cold-worked nickel-base super-alloy at 1800°F has been studied by electron nzicroscopy. Prior to deformation, an equilibrium micro-structure of fcc matrix y and cuboidal ,,', Ni (Al, Ti), precipitates of CuzAu structure had been established by an age at 1825°F. The strain-free recrystallization cells consist of very large rodular y' particles in a y matrix. They precipitate is oriented and coherent both before and after recrystallization. The results showed that y' coarsening accompanies recrystallization at 1800°F. However, it does so as a secondary effect and does not necessarily take place at lower temperatures. The structural similarity of this reaction to cellular precipitation in other systems indicates that lattice strain may also play a significant role during some cellular precipitation reactions. THERE have been numerous microstructural investigations of recrystallization in single-phase materials but two-phase systems have received much less attention. The second phase can either remain inert or be altered along with the matrix during recrystallization. If the second phase is an oxidelm3 or a relatively inert pre~ipitate,~, recrystallization is retarded when the interparticle spacing is less than 1 p. Prior to the onset of recrystallization, these materials show a well-polygonized substructure with the subgrain size limited by the interparticle spacing. Since recrystallization by the motion of preexisting grain boundaries6 is not observed, retardation has been related to particle pinning of the subboundaries. This pinning prevents coalescence' or growth8 of subgrains to a critical size (formation of a high-angle boundary) necessary to initiate recrystallization. In a material such as a nickel-base superalloy both y matrix and y' precipitate are altered by the recrystallization reaction. Haessner et al.' studied the recrystallization of a cold-rolled Ni-Cr-A1 alloy by electron microscopy. The material was initially cold-rolled in the supersaturated condition. upon annealing at 750°C, immediate precipitation of 7'occurred. Presence of this 7' greatly retarded the onset of recrystallization which eventually took place by the development of randomly oriented, strain-free grains. The original •/ was dissolved at the recrystallization interface and reprecipitated as oriented, coherent par-tiles in the new grain. Recrystallization caused a refinement of .)' particle size. Recently ~hillips'' investigated recrystallization of Ni-12.7 at. pct Al. Reduction by cold rolling presumably elongated the p' precipitate into lamellae that remained coherent with the matrix. After recrystallization at 600" to 750°C, there was no unusual change in y' particle size al- though there was a tendency toward clustering along the prior rolling direction at 750°C. Above 750°C, the recrystallized grains were generally free of precipitate. Studies in the somewhat analogous Cu-3.23 wt pct CO" and Cu-2 wt pct'2 systems demonstrated that the coherent cobalt-rich fcc precipitate in these alloys obstructed softening, initiation, and completion of recrystallization. The precipitates were deformed into lam~llae during rolling and those of diameter less than 250A remained coherent. Recrystallization took place by the growth of new grains into the recovered or poly-gonized material. In the first study," both matrix and precipitate reoriented in the same manner upon passage of the recrystallization interface. There was no change in particle size or morphology. Tanner and ~ervi,~ on the other hand, observed that motion of the recrystallization fronts was strongly hindered by the pinning action of coherent precipitates in the deformed material. Particles in contact with a pinned boundary coarsened and coalesced leaving a denuded zone in the unrecrystallized region. When the number of pinning points was sufficiently reduced by coalescence, the boundary swept past these particles and through the denuded zone. The authors1' considered this as a variation of discontinuous precipitation with both chemical driving force and deformation strain energy contributing to recrystallization. Preliminary observations by the present authors had revealed that recrystallization in Udimet 700, a nickel-base superalloy, occurred in an entirely different manner. Optical metallography showed that the recrystallized product formed as cellular colonies containing coarse y' particles elongated in the direction of cell growth. In this investigation the structural features of this reaction were investigated by transmission electron microscopy. EXPERIMENTAL PROCEDURE As-received I$-in. rounds of Udimet 700* were (wtpct) 18.4 15.2 4.95 4.42 3.43 0.06 0.031 0.14 Bal. solution-annealed for 4 hr at 2150" and then fast air-cooled. An initial y-~' structure was established by a 4-hr age at 1825°F followed by a fast air,cool. Essentially the equilibrium volume fraction of ?' at 1825°F is precipitated within 4 hr. Microstructural examination showed no measurable increase in the amount of precipitate after longer aging times. Deformation consisted of swaging to 52 pct RA with 6 pct reduction per pass at room temperature. To reduce the precipitation potential to a negligible amount, recrystallization anneals were conducted at 1800"~ (982"~). Microstructures were investigated by optical and transmission electron microscopy. To prepare foils for electron microscopy, the material was first sliced into 30-mil slabs parallel to the swaging direction. Discs were dimpled and electrolytically cut from
Jan 1, 1969
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Part X - Thermal-Dilation Behavior of Titanium Alloys During Repeated Cycling Through the Alpha-Beta TransformationBy Jerome J. English, Gordon W. Powell
An experimental investigation and mathematical analysis of the thermal-dilation behavior of the titanium alloy Ti-7Al-3Cb have shown that the linear dimensional changes associated with the polymorphic transformation need not be isotropic. The absolute magnitude of the linear dimensional change, which may be either positiue or negative, associated with the cr-p transformation is dependent upon the relutzve volumes of different orientations of the transformation product. It is hypothesized that the dilation irregulati-ties that have been observed during the polymorphic transformation of pure, coarse-grained titanium and other titanium-base alloys can be explained in the same manner. When titanium is heated above about 165O°F, the hcp a structure transforms to bcc 0. Thermal-dilatioh measurements have shown that the transformation is accompanied by a decrease in length of 0.16 pct.' Such dilation behavior would be expected because the volume of the hcp unit cell is about 0.3 to 0.4 pct greater than that of the bcc unit cell. A recent investigation2 of the thermal-dilation behavior of an experimental a-p* titanium alloy, Ti- 7A1-3Cb, containing 0.06 wt pct 0 showed that its dilation behavior during the polymorphic transformation differed substantially from that reported for unalloyed titanium. The first time the alloy was cycled through the transformation, the dilation curve closely duplicated that of unalloyed titanium. However, upon repeated cycling through the transformation temperature range, both the magnitude and the sign of the dimensional change associated with the transformation were observed to vary with each cycle. This investigation was undertaken to obtain additional data on the dimensional changes associated with the polymorphic transformation in the Ti-7A1-3Cb alloy and to determine the cause of the dimensional irregularities. After testing, the specimens were examined metallo-graphically. In addition, Laue back-reflection patterns were obtained from selected sections taken perpendicular to the specimen axes to determine the a orientations present in these sections. White radiation from a tungsten target and a 0.1-mm-diam collimator were used to produce the diffraction patterns. RESULTS Dilation Curves. Three types of thermal-dilation curves were obtained when the a-8 titanium alloy was heated and cooled through the transformation temperature range. These three types of curves are illustrated in Fig. 1. The type I curve represents what is considered normal behavior, because the dilation change is what would be expected on the basis of the volumes of the unit cells of a and p. The Type I1 curve is the inverse of Type I. Normal behavior is characterized by an expansion on cooling through the transformation, whereas a contraction takes place in the Type 11 curve. With Type ni behavior, no clearly distinguishable length change occurs during the transformation. No other anomalies that might be indicative of other phase transformations were observed in the dilation curves at lower temperatures. Apparently, the cooling rate was low enough for equilibrium to be reached during the 0 to a transformation. Table I lists the types of dilation curves observed during the polymorphic transformation as a function of the direction of measurement and cycle number. The A1 value was determined by extrapolating the low-temperature (a + 5 pct p) and high-temperature (100 pct p) segments of the dilation curves to a common temperature and measuring the difference in the or-dinates at that temperature, see Fig. 1. The transformation occurs over a temperature range in this alloy, so the magnitude of A1 is not an absolute value but depends on the choice of temperature. A mean temperature, T,, within the transformation temperature range was selected for the measurement. T, on cooling occurred about 100°C lower than T, on heating. The first time each of the three dilation specimens was heated to above the temperature, that is, Cycle 2, normal Type I behavior was observed. In Cycle 3, two deviations from normal behavior occurred. First, during cooling of the longitudinal specimen, a substantially larger expansion, +0.21 pct, was measured as 0 transformed to a compared with +0.03 pct in Cycle 2. Second, the thickness specimen was observed to undergo a contraction instead of the anticipated expansion on cooling. Continued cycling of the three specimens from room temperature to 2500°F produced additional changes in the dilation behavior. These changes did not seem to be related to the fabrication direction of the alloy because the values of a1 for the longitudinal, transverse, and thickness specimens varied unpredictably in magnitude and sign. Furthermore, both the longitudinal and transverse specimens showed all three types of dilation curves at least once during the six cycles that they received. Fig. 2 is a sketch of the transverse specimen after
Jan 1, 1967
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Part VII – July 1968 - Papers - The Ductile-Brittle-Ductile Transition in Columbium-Hydrogen AlloysBy R. D. Daniels, T. G. Oakwood
A study was made of the effects of small quantities of hydrogen on the mechanical properties of colum-bium. Tensile specimens, hydrogenated to concentrations of 20 to 200 ppm, were tested at temperatures of 300°, 191°, and 77°K. Although hydrogen was found to have little effect on the strength of columbium, the ductility of Cb-H alloys was found to be quite sensitive to both hydrogen concentration and temperature. At 300°K, an abrupt loss in ductility occurred at a critical hydrogen concentration, although some ductility was observed beyond the tolerance limit. A similar result was found at a lower hydrogen concentration at 191°K. At 77°K, however, a more gradual loss in ductility with increasing hydrogen concentration was observed. Hydrogenated columbium was thus observed to undergo a ductile-brittle-ductile transition. Metallographic examination of fractured specimens revealed extensive porosity at both 77° and300°K which was a distinct function of hydrogen content. At 191°K, although some secondary cracking was noted, the amount of observed porosity was minimal. These observations are interpreted in terms of hydrogen solubility and mobility as a function of temperature and in the role of hydrogen in promoting growth of microcracks. lHE effect of hydrogen on the mechanical properties of the refractory metals is not, at present, completely understood. A number of studies have shown these materials to be susceptible to hydrogen embrittlement. Roberts and Rogers1 have found that vanadium can be embrittled by hydrogen. It was further demonstrated that fracture undergoes a ductile-brittle-ductile transition as the temperature is lowered from 150° to -196°C; i.e., there is a ductility minimum observed at a certain temperature. The ductility is increased by either raising or lowering the temperature from this point. A more complete study by Eustice and Carlson2 on vanadium containing 10 to 800 ppm placed the ductility minimum at about -100°C with variations reportedly due to hydrogen content and strain rate. Ductility minima have also been found at certain temperatures for tantalum containing 7 ppm H3 and 140 ppm H.4 At hydrogen concentrations above 270 ppm, however, the ductility return at low temperatures was considerably reduced.4 In the case of columbium, some disagreement exists in the literature. Eustice and Carlson,5 Wilcox et al.,6 and Imgram et al.4 failed to find a ductility minimum although a composition-dependent ductile-brittle transition was observed. Hydrogen concentrations in these investigations were 20 ppm,5 1 to 30 ppm,6 and 200 to 390 ppm.4 However, Wood and Daniels7 observed a rather pronounced ductility minimum at hydrogen contents ranging from 19 to 252 ppm. Those theories of hydrogen embrittlement involving the precipitation of diatomic hydrogen which have been applies to ferrous metals8-12 do not seem to be applicable to the case of columbium and other exothermic occluders. Such theories propose that extensive crack formation and propagation occurs by the precipitation and expansion of diatomic hydrogen at internal voids and microcracks. However, photomicrographs of hydrogenated columbium do not show any evidence of damage introduced by the sorption and precipitation of diatomic hydrogen; rather, at high hydrogen concentrations, a hydrogen-rich second phase is precipitated.13'14 In addition, a number of these theories require the development of high hydrogen pressures at voids in the structure.8'10'12 This does not appear to be feasible in the concentration ranges discussed in the aforementioned paragraphs. The possible interaction of atomic hydrogen with microcracks resulting from dislocation pile-ups15,16 remains in doubt since pile-ups have not been observed in bcc metals17 including columbium.18 Wood and Daniels7 have put forth the possibility that a hydride precipitation could be responsible for crack nucleation in columbium. Work by Longson19 has shown that hydrogen embrittlement of columbium parallels the bulk solubility limit; i.e., as the solubility increases, for instance with temperature, the amount of hydrogen necessary to cause embrittlement also increases. Although a hydride precipitation appears attractive as a means of nucleating microcracks in columbium, what require more intensive study are the low-temperature anomalies which have been observed, i.e., the ductile-brittle-d'ictile transition characteristics. Also, the hydrogen concentrations where embrittlement occurs are often below the bulk solubility limits determined by Albrecht et al.13,14 and Walter and Chandler.20 This work is an attempt to determine more definitively the effects of concentration and temperature on the mechanical properties of dilute Cb-H alloys. EXPERIMENTAL PROCEDURE Ultrahigh-purity columbium rods, obtained from the Wah Chang Corp., were cold-reduced by rotary swaging. A chemical analysis is given in Table I. The material was cut into cylindrical blanks 1.50 ±0.005 in. long. Individual specimens were either given a stress relief anneal at 750°C or recrystal-lized at 1200°C. Resulting microstructures were either a "bamboo" structure characteristic of a wrought material or a recrystallized structure with a grain diameter of approximately 100 n. All heat treatments were carried out in a vacuum of 10-5 Torr or less.
Jan 1, 1969
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PART I – Papers - Intermetallic Phases in the Systems of Zinc with Lanthanum, Cerium, Praseodymium, Neodymium and YttriumBy Harold M. Feder, Robert V. Schablaske, Irving Johnson, Ewald Veleckis
The stoichiometry, structure, and stability of the internzediate phases formed between zinc and some of the rare earth (RE) metals were systematically exarnined by means of a recording effusion balance and X-ray diffraction analyses. In the La-, Ce-, PY-, Nd-, and Y-Zu systems, at or below about 600 C, the following sequences of phases (REZnx) were found: La, x = 1, 2, 4.0, 5.25, 7.3, 17/2, 11, and 13.0;' Ce, x = 1, 2, 3, 11/3, 4.3, 5.25, 7.0, 17/2,* and 11; Pr,x = 1,2, 3, 11/3 ,* 4.3, 5.3(?), 7.0, 17/2,* and 11; Nd,x = 1,2, 3,* 11/3,* 4.3, 6.5, 8.5,* and 11; Y,x = 1,2,3, 11/3, 4.5, 5.0, 17/2,* and 12.* The structure types of all these phases were classified. In addition, lattice parameters were obtained for the first time for the pluses denoted by asterisks. In the absence of de tectable valency or electronegativity effects the systesnatic trends in the results have been ascribed to the effects of' the lanthanide contraction. For example, the maximum number of zinc atoms in the coordination polyhedron surrounding the RE atom decreases from twenty-four to twenty-two to twenty as the size of the RE atom decreases. THE structures and compositions of a great many intermetallic phases (e.g., the Laves phases) are known to be based primarily, but not exclusively, on the space-filling efficiency of various modes of packing together atoms of different sizes. The valencies and electronegativities of the constituent atoms are, however, also influential. In extreme cases hypothetical intermetallic phases which fulfill the efficient spacefilling requirements may not be present in the constitutional diagram because of thermodynamic instability brought about by the operation of valency or electronegativity factors. Hence, for a detailed study of the influence of atomic size on alloy structure and composition, it would be desirable to minimize variations of valency and electronegativity. The intermetallic phases formed by the rave earths (RE) with some common partner offer an excellent opportunity for isolating the effects of size from those of valency and electronegativity. The rare earths exhibit a large, but smooth, decrease in size (the lanthanide contraction) in the series from lanthanum to lutetium when inter comparison is made for a common valence state, e.g., isolated atoms or trivalent ions. The elements yttrium and scandium are frequently included as pseudo rare earths; their sizes place them in the vicinity of dysprosium and lutetium, respectively. The electronegativities of RE elements vary by less than 10 pet. The trivalent state is the most common; however, the well-known tendency of cerium, praseodymium, and terbium to achieve higher valencies, and of samarium, europium, and ytterbium to seek lower valencies, requires that caution be exercised in the assumption of equal valencies. In the present study the existence, constitution, and structure of each of the numerous intermediate phases formed by zinc with lanthanum, cerium, praseodymium, neodymium, or yttrium were examined systematically and in detail. The investigation was conducted by a recording effusion balance technique and by X-ray diffraction analysis. The results enrich our knowledge of the phase diagrams of these systems. In addition, they present some clear-cut evidences of the operation of the size factor alone. EXPERIMENTAL PROCEDURE Apparatus. The mode of operation of the recording effusion balance and its application to phase studies have been discussed in detail elsewhere.' In this work, an effusion cell containing a finely divided alloy was suspended within an evacuated tube from the beam of an analytical balance. The tube was immersed in a massive molten salt bath whose temperature was controlled to within 0.5o C during each experiment. The loss in weight of the alloy owing to effusion of zinc* was continuously recorded. Two effusion cells, 1/2 in. diam by 1 in. high, were machined from tantalum rods. Two orifices were drilled laterally into the walls of each cell. The orifice areas were determined by calibration with pure zinc: cell A had a total orifice area of 6.5 x 10-41 sq cm, and cell B an orifice area of 9.8 x 10-3 sq cm. By appropriate choices of orifice area and temperature the wide range of volatilities from pure zinc to pure rare earth metal could be investigated. X-ray diffraction powder photographs were made at room temperature with a 114.6-mm Debye-Scherrer camera with both filtered CuKa radiation and filtered CrKa radiation. Lattice parameters were refined by a computer-programmed least-squares analytical treatment which incorporated appropriate extrapolation techniques.2 Frequent use was also made of a special computer program3 designed to generate a powder pattern from an assumed structure in order to verify structural assignments. Materials. Lanthanum, neodymium, and yttrium were purchased from the Lunex Co., cerium from the Cerium Metals Corp., and praseodymium from the St.
Jan 1, 1968
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Shaft Sinking Today - A Boring Business TomorrowBy Maurice Grieves
The great majority of shafts constructed today are still excavated by drilling and blasting, a method which changed very little in over 100 years until the introduction of the mechanical lashing unit and cactus grab by the South Africans, which enabled muck to be removed as fast as massive hoisting systems could handle it and resulted in very rapid rates of sinking. Record breaking month's performances were achieved at -Hartebeestfontein No. 4 shaft, October 1960-337.1 m; Western Reefs No. 4 shaft, October 1961-340.7 m; and Buffelsfontein eastern twin shaft, March 1962-381.2m. The method was very labor-intensive, requiring a crew of over 60 workers at the shaft bottom during the drill cycle. Safety precautions were strict, but in the drive to achieve rapid advance, cases of personal injury were still somewhat high because of the large number of people engaged in this potentially hostile environment. The South African method, as it came to be referred to throughout the rest of the world, was adopted in the United Kingdom in the late 1950s in a modified form with greatly reduced manpower and nonsimultaneous sinking and lining, which was insisted on by the British Mines Inspectorate. In that instance, it was successfully used to sink the 7.3-m-diam concrete-lined shafts at Kellingley to 770 m depth, with rates of advance of over 90 m/month achieved, a British record at that time. During the sinking of the 1.15-km-deep twin shafts at Boulby potash mine in the UK in 1970, the method was again used, but for the first time ever in Britain exemptions from the mining code permitted the use of crash beams, crash doors, jack catches, and semi-simultaneous sinking and lining techniques. New British shaft sinking records of over 120 m/month were achieved in both shafts. Similar equipment and techniques were used in the early 1970s to sink several deep shafts in Canada, notably Creighton #7 and the Con zinc mine at Yellowknife in the NW Territories. Today, this equipment is standard for deep shafts in the US and the rest of the world. However, with the tremendous escalation in mining labor costs, the impact of health and safety legislation, and environmental regulations, coupled with a very real shortage of miners willing to work in this exposed situation it was apparent that an alternative to the labor-intensive conventional method of shaft construction had to be found. Recognizing the trend is inevitable, one or two major German shaft sinking contracting firms began to take a fresh look at full face boring techniques applied to tunnels and raise bored shafts. The results were most encouraging. Tunnel drivage techniques using moles had developed considerably from Colonel Beaumont's original channel tunnel machine circa 1880 to the superbly engineered Priestley machine selected to cut the British side in 1975 and the double shielded Robbins Grandori borer on the French side of the English Channel. Full face tunnel machines were being successfully used to drive uphill in inclined shafts in Austria and Switzerland. At Mapprag in Switzerland, the Demag mole drove the first (intentional) vertical transition and curve, and then went on to successfully complete the 730-m-long penstock shaft at an inclination of 35°. In Austria, the Wirth mole drove the Kaprun Glacier ski-lift railcar tunnel at record breaking rates of 457 m/MONTH (best 30 m/d) through green schist at an inclination of 29° for a distance of 3.35 km while the Hydro tunnel at Sarrelli in Switzerland was being driven by the Robbin's mole at an inclination of 35°. Simultaneously, extremely promising results were obtained using large assemblies of cutter discs on raise borer heads, such as the 4.87-m-diam X 460-m-deep shaft raised by Teton for Jim Walter Resources Inc. Bearing in mind that most mine shafts in the future (unless in exceptionally competent rock) will require some form of lining, and the trend will be toward deeper shafts as the more easily accessible mineral deposits become exhausted, it was seen that normal raise boring had definite limitations in vertical accuracy, in the limitation imposed by the drill string on the available torque that could be applied to the cutter head, and in the risk of collapse of the unsupported shaft rock wall in friable or jointed and fissured ground, since it is not possible to apply any form of temporary support until the permanent lining is being installed. A further problem was the economics of installing a subsequent lining, necessitating setting up a headgear and hoisting arrangement approaching in size that required for conventional drill and blast sinking and lining. Because of the economics, German contractors opted for a phased transition from drill and blast to the full face, rodless, out of the solid shaft mole, by starting off with a down-the-hole shaft boring machine -without a drillstring-but using a pilot hole to get rid of the muck.
Jan 1, 1982
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Minerals Beneficiation - Comparative Results with Galena and Ferrosilicon at MascotBy J. H. Polhems, R. B. Brackin, D. B. Grove
THE heavy media separation process plays an outstanding role in the concentration of 4000 tons of zinc ore per day at the Mascot mill of the American Zinc Co. of Tennessee. Of the total tonnage, 72 pct is treated in the heavy media separation plant to reject 56 pct of the ore as a coarse tailing, which has a ready market. Concentrates from this separation are beneficiated further by jigging and flotation. Approximately 25 pct of the total zinc concentrate production is made in the jig mill. Jig tailings are ground and pumped to the flotation circuit where the balance of the production is made. Fig. 1 shows a generalized flowsheet of the mill. The Mascot ore is a lead-free, honey-colored sphalerite in dolomitic limestone, with lesser amounts of chert and some pyrite. A mineralogical analysis is given in Table I. After 10 years of successful operation with galena medium and treatment of nearly 10,000,000 tons of ore, a decision to convert to ferrosilicon was made early in 1948 because of the increasing price of galena and consequent high operating costs. The conversion was made on Nov. 6, 1948, and the results obtained since that time have shown remarkable improvement over those made with galena. The Table I. Mineralogical Analysis of Mill Feed, Pct Calcium carbonate 49.5 Magnesium carbonate 35.2 Iron oxide and aluminum oxide 1.5 Zinc sulphide 4.5 Insoluble 9.3 100.0 Table II. Comparative Data, Galena and Ferrosilicon Ferro- Diner-Gelenaa siliconb ence Operating costs per ton milled, ct. 21.21 9.12 12.09 Medium consumption per ton milled, lb 0.80c 0.15 0.65 Reagent consumption per ton milled, lb 0.45 0.02 0.43 Tailing assay, pct Zn 0.310 0.297 0.013 Concentrate. oct Zn 12.08 10.33 1.75 Heavy medla ieparatlon recovery. pct 89.38 90.22 0.84 Mill feed rate, tons per hr 153 166 13 Heavy mesa separation feed rate. tons per hr 100 10 0 Tons milled per heavy media separation man shift 350 620 270 Mill feed to coarse tailings, pct 51.0 56.7 5.7 Lost mill time, pct 5.6 5.0 0.6 Power consumption, kw-hr per ton 2.06 1.92 0.14 a 1947. " First 6 months of 1950. c Net consumption after deducting credit for reclaimed waste galena. Consumption of new galena was 1.320 lb per ton milled. For entire life of galena operation, a credit of 40 pct of the value of the new galena added was realized from the sale of waste galena. comparisons given in this report cover the first 6 months of 1950 as representing the ferrosilicon operation, and the year 1947 as representing the galena operation. This was the last full year in which galena was used exclusively and is representative of the best work done during the 10 years of operation with this medium. After only 2 years' operating experience, with ferrosilicon and treatment of 1,807,585 tons many advantages have been revealed and are summarized in Table 11. Development Prior to the introduction of the heavy media process, all the mill feed was crushed through 5/8 in. and treated by jigging. A finished tailing assaying 0.66 pct Zn was made on rougher bull jigs, and cleaner jig tailings were ground for treatment by flotation. The first test work on the sink-and-float method of mineral beneficiation was carried out at Mascot in 1935, using a 3-ft cone and galena medium for batch tests. The following year a 6-ft cone was installed for pilot-plant work. This unit became a part of the mill circuit on March 1, 1936, and handled a gradually increasing tonnage in the next 2 years as the process developed to the point where it could treat all the + 3/8-in. material in the mill feed. Coarse jigging was then discontinued on March 1, 1939, and all coarse tailings have been made by the heavy media separation plant since that time. Feed Preparation: The original feed preparation plant consisted of a drag washer followed by two 4x10-ft Allis-Chalmers washing screens. A surge bin and two additional 5x12-ft AC washing screens were added in 1943. Use of primary and secondary washing screens was found essential to provide the cleanest possible feed for the cone and thereby avoid excessive contamination of the galena medium. Improved washing was obtained by replacing the drag washer with a 7x20-ft Allis-Chalmers scrubber, shown in Fig. 2, which has been in service since May 1944. Throughout the life of the galena operation, delivery of extremely muddy ore to the mill overloaded the medium cleaning system, and it frequently was necessary to cut off the feed and clean the medium for several hours until its normal viscosity had been re-established. The cleaning circuit
Jan 1, 1952
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Underground Mining - Determination of Rock Drillability in Diamond DrillingBy C. E. Tsoutrelis
A new method for determining rock drillability in diamond drilling is discussed; the method takes into consideration both penetration rate and bit wear. The method is based on drilling a rock specimen under controlled laboratory conditions using a model bit. The technique used for determining the experimental variables is extremely simple, quick, and reliable. Drillability is then determined by the mathematics of drilling. In considering the different factors that affect diamond drilling performance, the nature of the rock to be drilled is of outmost importance since it affects significantly the drilling costs and such other variables as bit type and design, drilling thrust, and bit rotary speed. Many attempts have been made to study this effect by correlating actual drilling performances either to certain physical properties of the rock being drilled1-? or to test drilling data obtained under laboratory conditions.7-13 These attempts were aimed at providing a reliable method of predicting by simple means the expected rock behavior in actual drilling, thus giving the engineer a tool to use in estimating drilling performances and costs in different types of rock. The purpose of this paper is to describe such a method by which rock drillability (a term used in the technical literature to describe rock behavior in drilling) could be determined in diamond drilling. It is believed that the proposed simple and reliable method will cover the need of the mining industry for a workable method of measuring the drillability of rocks. It should be emphasized, however, that since drill-ability depends on the physical properties of rock and each drilling process (diamond, percussive, rotary) is affected by different or partly different rock properties,14-l6 the proposed method of determining rock drillability cannot be extended to the other drilling processes. The results presented in this paper form part of an extensive three-year research program carried out by the author in the laboratories of the Greek Institute of Geology and Subsurface Research. During this period the effects of the physical properties of rocks and of such operational variables as drilling thrust and bit rotary speed in diamond drilling were investigated in detail. DRILLABILITY CONCEPT The literature is not devoid of drillability studies. While there are a number of investigators1,3,5-7,9-0,12-13,17 who have attempted to establish by direct methods (i.e., drilling tests under laboratory conditions) or indirect (i.e., through a physical property of rock) an index from which the drilling performance in a given rock may be estimated, very few6-7,9,12, of the proposed methods seem to be of much practical value to the diamond drilling engineer and none to date has been universally accepted. Commenting on the proposed methods for assessing rock drillability, Fish14 remarks that "for a measure of drillability to be accepted it is essential that penetration rate at a given thrust and bit life are elucidated as otherwise the method is of little value." This statement should be examined in more detail by making use of the penetration rate-drilling time diagram obtained in drilling a rock under constant operational conditions. Furthermore, the merits of using this diagram to describe rock drillability will be pointed out. At the same time reference will be made to this diagram when discussing some previously proposed methods. Fig. 1 illustrates such a diagram for three rocks,A, B, and C, which have been diamond drilled under identical conditions. It is assumed here that rocks A and B have the same initial penetration rate, i.e., VOA = Vog, but since rock B is more abrasive than A, rapid bit wear occurs and as a result the fall of its penetration rate with respect to time is more vigorous than in rock A. This is shown graphically by a steeper V = f(t) (0 curve in this rock than in rock A. Rock C has a lower initial penetration rate, due to higher strength properties16 but since it is not very abrasive, only a slight fall of its penetration rate occurs during drilling (in this category are some limestone and marbles with compressive strength above 1000 kg per sq cm). It follows from the foregoing considerations that the characteristic for each rock curve (I) is a function of (i), the penetration rate of the rock Vo recorded at the instant of commencing drilling, which determines the starting point of the curve (1) on the y-axis and (ii), the abrasive rock properties which determine the rate of fall of Vo with respect to time. Thus, curve (I) provides an actual picture of the rock behavior in drilling for given operational conditions, and it can be used with complete satisfaction to assess rock drillability. It can be seen clearly from Fig. I that proposed methods for assessing rock drillability by measuring the
Jan 1, 1970
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Sunnyside No. 3 - A Case Study In Ventilation PlanningBy Malcolm J. McPherson, Michael Hood
Sunnyside Mines, owned and operated by the Kaiser Steel Corporation, are situated near the city of Price, Utah. The complex comprises three adjacent mines, named simply Nos. 1, 2 and 3, all connected underground. Two seams, the upper and lower Sunnyside have been worked. These dip at about 10 percent to the north-east. The surface cover is variable due to the mountainous nature of the topography. The Sunnyside upper seam varies from 5 1/2 ft (1.7m) to 9 ft (2.7m) In thickness whilst the lower seam remains at about 6ft (1.8m). The separation between the two seams has ranged from 7 to 45 ft over the mined area (2 to 14m). Longwall mining has been practiced at Sunnyside for over 20 years due to difficulties of roof control encountered when using the roan and pillar system. Number 3 mine is bounded on the north and south sides by mines Number 1 and 2 respectively. Whilst current production is concentrated into Number 1 mine, much of the future of the complex lies in the further development of deeper reserves in Number 3 mine. Workings in this latter mine were curtailed in 1978 due to difficulties in ventilation. Present developments are ventilated partially from the neighboring Number 2 mine where no workings are in progress. The layout of Number 3 mine is illustrated on the schematic Figure 1. Trunk airways extend down dip from the surface at No. 2 Canyon and the Water Canyon for a distance of some 9,600 ft. (2930m). The area between the two sets of trunk airways has been worked extensively in both seams as have the corresponding reserves on either side in the connected adjacent mines. At the present time exhausting fans are sited at the top of a shallow shaft in No. 2 Canyon and an 8 ft (2.4m) diameter shaft sunk to a depth of 1013 ft (310m) closer to the current developments (Figure 1). The current airflow system, even with an additional 116,000 cfm (55m3/s) entering from No. 2 Mine, is adequate only for the development work now in progress but will be unable to support new longwall faces further downdip. The basic ventilation problem of this mine may be stated quite simply. In a situation where all intake and return airways pass through extensive old workings, a ventilation system design was required that would be effective, efficient and economic for the foreseeable future of the mine. ORGANIZATION OF THE PLANNING PROCEDURE The procedure followed during the study is illustrated on Figure 2. Initial ventilation surveys established the current state of the airflow system and provided the necessary data for setting up a Basic Network File in a computer store. The data in this file was a mathematical model of the ventilation system of the mine. The basic network was analysed by a ventilation network analysis program in order to correlate the measured and computed airflows and to establish the basic network as a true representation of the mine as it stood at the time of the surveys. The network model could then be extended to simulate the future development of the mine and alternative ventilation designs investigated. The remaining sections of the paper outline the work involved in each of these main phases of the planning procedure. VENTILATION SURVEYS Conduct of Surveys Two types of measurements were conducted simultaneously throughout the air-carrying routes of the mine: (i) Airflow measurements were made by anemometer traverse or smoke tube at 221 selected stations. Anemometer traverses were repeated at each station until at least three gave results to within 5 per cent. (ii) Pressure drop measurements were made across ventilation doors, regulators and, wherever possible, across stoppings. Additionally, frictional pressure drops were measured along airways where such pressure drops were significant (above 0.01 inches of water gauge or 2.5 Pa over a 100m distance). The trailing hose method was used to determine these frictional pressure drops. This involved laying out 100m of abrasive resistant plastic tubing (3 mm internal diameter) with a 4 ft. pitot-static tube facing into the airflow at either end and a low range pressure gauge connected into the line. The trailing hose method was preferred to the alternative barometer technique for this study because of (a) the relative ease of access between measuring points and (b) the greater accuracy within individual airways. The anemometers used were Davis Biram Type A/2-3" (30 to 5,000 ft/min) and Airflow Developments AM-5000 digital (50 to 5,000 ft/min). The pressure gauges employed were Dwyer magnehelic instruments. These were preferred to liquid in glass manometers because of their portability and dependability under adverse mining conditions. A checklist of the equipment used in the survey is given in Appendix 1. The instruments were calibrated before and after the surveys in the mine ventilation laboratory at the University of California, Berkeley. The survey occupied two teams, each of three men, for ten working days. The work consisted
Jan 1, 1982
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Part VII – July 1969 – Papers - Colony and Dendritic Structures Produced on Solidification of Eutectic Aluminum Copper AlloyBy Pradeep K. Rohatgi, Clyde M. Adams
Structures produced upon solidification of the eu-tectic composition (33 wt pct Cu) aluminum copper alloy have been examined as a function of freezing rate dfs /d? , the rate of change of fraction solid (fs) with time (8). Slow (dfs/d? = 0.0016 sec-1), intermediate (dfs/d? = 0.02 sec-1) and rapid (dfs/d? = 0.4 to 7.30 sec-1) freezing rates were used. The lamellar Al-Cual2 eutectic is arranged in the form of rod-shaped colonies at rapid freezing rates. The colonies are aligned parallel to the direction of heat flow, whereas the lamellae within the colonies are aligned at various angles, as high as 90 deg, to the direction of heat flow. The colony spacing (C) is proportional to the square root of inverse freezihg rate. The relationship is C = 15.5(dfs/d?)-1/2 where C is in µ and 8 is in sec. The ratio of colony spacing to lamellar spacing is greater than 20.0 and increases with a decrease in the freezing rate. A duplex dendritic structure is produced at intermediate freezing rates. A fine lamellar eutectic is arranged within the dendrites (exhibiting side branches at an angle close to 60 deg from the main stem) and a coarse irregular eutectic appears in the interdendritic regions. The duplex eutectic structure is also produced at slow freezing rates. However, at slow freezing rates there is a Platelat of CuAl2, along the center of the main stem of each dendrite and the other lamellae are arranged perpendicular to the central platelet. THE eutectic between CuA12 and a! aluminum has been reported to freeze in a lamellar form by several workers.'-3 chadwick4 has measured the interlamel-lar spacing as a function of growth rate. Kraft and Albright2 have reported on irregularities in the lamellar structures, and have proposed growth models which account for the formation of faults during solidification. In certain instances the lamellar eutectic has been found to exist in colonies. The colony formation315 has been attributed to the breakdown of a planar liquid-solid interface due to rejection of impurities. The aim of the present work is to study the structures produced from the eutectic aluminum-copper alloy under relatively fast solidification rates, such as encountered in casting and welding operations. The solid-liquid interface presumably remains planar under conditions of slow unidirectional freezing which produce lamellae aligned parallel to the direction of heat flow. The local growth velocities are the same over the entire interface and are equal to the rate of growth of the all-solid region. The spacing between the eutectic lamellae is inversely proportional to the square root of the growth rate of the all-solid region. Under the freezing conditions used in the present study, the solid-liquid interface is cellular or dendritic and the local growth velocities are different in the different regions of the interface. The relationship between the growth rate of the all solid region and the local growth velocities varies with the location and the shape of the interface. The growth rate of the all-solid region is, therefore, an inadequate parameter to describe the eutectic micro-structures which depend upon the local growth velocities. For this reason the structures have been examined as a function of freezing rate, dfs/d?, where fs is the fraction solidified at time 0. The freezing rate was varied by a factor of 4000. The relationship between the freezing rate, dfs/d?, and the growth velocit of the all solid region depends upon the specimen geometry and the shape of the interface. EXPERIMENTAL PROCEDURES The A1-33 pct Cu alloy used throughout this study was made in an induction furnace, using electrolytic copper and aluminum of commercial purity (99.7 pct), the primary impurities being silicon (0.12 pct), iron (0.14 pct), and zinc (0.02 pct). Three ranges of freezing rates were investigated: 1) A spectrum of rapid freezing rates (ranging from 0.40 to 7.30 sec-1) was obtained in arc deposits made on 2-in. thick cast plates of the eutectic alloy. The arc was operated at constant power and was made to travel at constant velocity on the surface of the plate that was in contact with the chill surface during solidification. The pool of liquid metal formed under the moving tungsten arc solidified rapidly by heat extraction through the unmelted plate. Conditions of unidirectional heat flow were achieved near the fusion zone interface, especially in the center of the arc deposits. The great advantage of the arc technique is that rapid cooling and freezing rates can be varied in a qualitative way. The correlation between the arc parameters and the solidification rate is given by the following relationship:6-8
Jan 1, 1970
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Part II - Papers - Density of Iron Oxide-Silica MeltsBy R. G. Ward, D. R. Gaskell
Using the maximum bubble pressure technique, the densities of iron silicates at 1410°C have been measured blowing helium, nitrogen, and argon. By ensuring equilibrium between the melt and the blowing gas with respect to oxygen potential and by minimizing tempcrature cycling of the furnace, iron precipitation in the melt has been prevented. Thus the previously reported effect of blowing-gas composition on the densities of the melts has been eliminated. Consideration of the oxygen densities of the melts gives an indication of the structural changes accompanying composition change. The density-composition relationship of iron oxide-silica melts in contact with solid iron has been the subject of several investigations1-7 and considerable disparities exist among the various results obtained. Of these investigations, all except one5 have employed the maximum bubble pressure method. In the most recently reported of these investigations1 the density-composition relationship obtained blowing nitrogen differed from that obtained blowing argon. The measured densities obtained under nitrogen were greater than those obtained under argon, the difference being a maximum at the pure liquid iron oxide composition and decreasing with increasing silica content. This observation rationalized the disparities existing among the results of the earlier investigations, showing that two lines, one for nitrogen and the other for argon, could be drawn to fit all the earlier results. No explanation for this phenomenon could be offered. Chemical analysis of rapidly quenched samples of melt for dissolved nitrogen, and direct weighing measurements, excluded solution of nitrogen in the melt from being the cause of the increase in density. The range of blowing gases was extended by Ward and Hendersons who measured the density of liquid iron oxide bubbling helium, nitrogen, neon, argon, and krypton. The measured density was found to decrease smoothly with increasing atomic number of the bubbling gas. The work reported here is a continuation of the program initiated by Ward and Sachdev7 to study the densities in multicomponent melts in which the iron oxide-silica system is the solvent. As such it is necessary to explain or eliminate the anomalous densities of iron silicates under different atmospheres, and the present rede termination was carried out towards this end. EXPERIMENTAL The maximum bubble pressure method of density determination was again employed and the experimen- tal apparatus used was essentially the same as that used by Ward and Sachdev.7 A molybdenum-wound resistance furnace heated an ingot iron crucible of internal diameter 1 in. containing a 2-in. depth of melt. The bubbling gas was blown through a 1/4 -in.-diam mild steel tube onto the end of which was welded a 2-in. extension of 1/4 -in.-diam ingot iron rod, drilled out to 5/32 in., and chamfered to an angle of 45 deg. The blowing tube was introduced to the furnace through a sliding seal and its position was controlled by a vertically mounted micrometer screw which allowed the depth of immersion to be determined with an accuracy of ± 0.01 cm. A Pt/Pt-10 pct Rh thermocouple was located below the crucible and temperature control was effected initially by means of an on-off controller and later by a saturable core reactor. The bubble pressure was determined by measurement of a dibutyl phthalate manometer using a cathetometer. PREPARATION OF MATERIALS Iron oxide was produced by melting ferric oxide in an inductively heated iron crucible in air. The liquid was quenched by pouring onto an iron plate. Silica was prepared by dehydrating silicic acid at 650°C for 12 hr. RESULTS Before any measurements of the density of a melt were made, the density of distilled water at room temperature was measured bubbling helium and argon. Both gases gave the density as 1.00 ± 0.01 g per cu cm which showed that the density of the manometric fluid (dibutyl phthalate) was not affected by contact with the blowing gas. With the furnace controlled by an on-off temperature controller an attempt was made to measure the density of pure liquid iron oxide by bubbling argon. The furnace atmosphere gas and bubbling gas were dried over magnesium perchlorate and deoxidized over copper turnings at 600°C. It was found that the pressure required to blow a bubble at a given depth increased slowly with time, and thus it was impossible to obtain a unique value for the density of the melt. Inspection of the blowing tube after removal from the furnace showed that rings of dendritic iron had precipitated from the melt onto the immersed part of the tube. This is shown in Fig. l(a) where the various "steps" correspond to different depths of immersion. The precipitation of iron was considered to be due to one or both of two possible causes: i) The composition of the liquid iron oxide is that of the liquidus at the temperature under consideration and can be expressed by the equilibrium
Jan 1, 1968