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By D. J. Carney, E. Richard Randolph, E. Van Meter, J. J. Oravec, Stanley H. Ward, Gerald J. Anderson, Rolland L. 203-000-000-005 Blake

DURING the last 30 years the inductive electromagnetic method has been used chiefly in the search for massive sulphide mineralization. This application has met with varying degrees of success and in recent years has resulted in discovery of several large orebodies. Little has been written concerning its use in exploration for soft iron ores, but one of the present authors has reported on experiments with massive magnetic deposits.' To augment the exploration tools available to geologists in delineating iron orebodies, Cleveland-Cliffs Iron Co. and McPhar Geophysics Ltd. undertook in 1953 to apply the inductive electromagnetic method to Cleveland-Cliffs properties in the Lake Superior region. As a result of this project, equipment has been developed that enables simultaneous transmission of two audio frequency waves, and the field technique and interpretative procedure involved have furthered exploration in the district significantly. Thus far, inductive electromagnetic application in the Lake Superior region has been only a development tool, that is, it is used to locate obscured contacts and faults as a part of property expansion and development. However, its application to primary reconnaissance of unexplored areas may be feasible in the future. The method has assisted in placing drillholes efficiently, and the elimination of excess drilling foot-ages and/or actual elimination of unnecessary holes has amply justified the expense of the geophysical survey. Cost of the field work involved is comparable on a per station basis to the cost of a magnetometer or superdip survey. Since observations require no reduction, i.e., are directly interpretable, overall expenditure is low, and the scope and detail of the survey can be adjusted in the field as geological- geophysical correlation becomes evident. To a great extent, this eliminates the second-guessing so commonly arising after office calculations are completed on data obtained with other types of geophysical surveys. This unique feature of field interpretation and its associated intimate feel of the project area, is, perhaps, one of the most valuable aspects of the inductive electromagnetic method as applied to iron ore exploration. Basis of Method Fundamentally, the method involves transmission of an alternating electromagnetic wave, of a chosen audio frequency, which permeates the ground materials in the vicinity of a transmitting, or primary, coil, see Fig. 1. This wave, or field, induces an electric current in any conductor on which it is incident. The flow of an alternating current in a conductor sets up its own, or secondary, radiating electromagnetic field. These two fields form a resultant whose configuration depends on the following characteristics of the subsurface conductors: 1) size, 2) shape, 3) electrical conductivity, 4) magnetic permeability, and 5) frequency of the transmitted wave. To a lesser extent the resultant is also dependent on material adjacent to the conductor, topography, and surface conductivity. For illustrative purposes, the primary, secondary, and resultant fields may be represented by vectors. In operation, the direction of the resultant vector is measured by a small receiving coil tuned to the frequency of the transmitted wave. Generally speaking, the method can be compared to the transmission and reception of the familiar radio broadcast, with special variations permitting measurement of the effect on reception of intervening materials. Field Technique Mechanics of field operation are simple. The mast is set up in a vertical position and is then guyed in place. The transmitting loop then is raised by means of a sheave at the top of the mast and the coil connected to the motor-generator. A special plane table is clamped into position on the mast and the loop is plumbed. The plane table is oriented according to a grid system established over the project area. By means of this plane table it is possible

Jan 1, 1956

By F. V. Lenel, G. S. Ansell, J. A. Dromsky

The growth of aluminum oxide particles in a nickel matrix was studied eve?. the temperature vange of 2140° to 2470°F. The instability of the dispersed alumina was shown to be independent of the crystal structure of the alumina. The activation energy for the growth of the dispersed alumina was found to be 84.7 1 2.0 kcal. The particle radius increased as a function of time. These results indicate that the growth is not diffusion controlled. It is believed that the rate controlling mechanism is the dissolution of the aluminum and oxygen atoms into the nickel lattice. THE strength properties of alloys which consist of a finely dispersed second phase in a metallic matrix depend upon the spacing between the second phase particles. It is therefore desirable to achieve very fine dispersions in these alloys. Furthermore, to retain the properties these very fine dispersions must be stable during fabrication and service of the alloys. The best known of the dispersion strengthened materials, the SAP type alloys, which consist of a dispersion of aluminurn oxide in aluminum, have exceptionally good stability up to the melting point of aluminum. There is evidence, however, that other dispersion strengthened alloys, even those consisting of refractory oxides in a metal matrix, may be less stable. This investigation is concerned with the stability of Ni-Al2O3 alloys in the temperature range in which these alloys are usually fabricated. The mechanical properties of Ni-Al2O3 alloys at elevated temperatures have been previously investigated by Crelnens and rant,' and Gregory and Goetzel.2 The behavior of these alloys in stress rupture tests appears to indicate that at temperatures below 1800°F they are highly stable. There is some doubt, however, as to their stability at the higher temperatures used during the conventional fabrication. Cremens and Grant, in preparing their test alloys, cousolidated, by powder metallurgical techniques, nickel powders as fine as 0.13 µ diam and alumina powders as fine as 0.018 µ. Metallo- graphic examination of the alloys following fabrication revealed that none had interparticle spacings of less than 2 µ. Considering the size of the original component powder particles, it is likely that the dispersions coarsened during fabrication. Gregory and Goetzel, in their studies of extruded alloys of 80 pct Ni—-20 pct Cr matrixes with nonmetallic dispersion, observed a definite coarsening of the alumina dispersions in alloys sintered at 2280°F as cantrasted to those sintered at 2000oF. Similar observations on the spheroidization and growth of thoria particles finely dispersed in a nickel matrix were made by D. K. Worn and S. F. Marton.3 As a result of such coarsening, much of the effort expended in the preparation of very fine powder mixtures would be lost. The mechanical properties of the alloys which had experienced coarsening would be expected to be poorer than if the original dispersions had been retained. EXPERIMENTAL PROCEDURE Ni-Al2O3 alloys were produced from powder prepared by a coprecipitation technique. Aluminum hydroxide and nickel hydroxide were coprecipitated from chloride solutions of the metals. The mixed hydroxides were calcined to form metal oxides and the nickel oxide in the mixture was selectively reduced to nickel by treating it in hydrogen. Specimens were compacted from the resultant powder which consisted of a fine, uniform mixture of aluminum oxide and nickel particles. The compacts were sintered by resistance hot pressing4, a densification technique which requires exposure times of the order of only a second or less at elevated temperatures. A conventional sintering process was not used, since the temperature required for densification would have to be in the region in which the stability of the dispersion was to be studied. A series of hot pressed specimens were treated in hydrogen at temperatures from 2140o to 2470°F (1171o to 1355oC, for times up to 120 hr. Changes in the microstructures were studied by electron microscopy using the two-stage preshadowed carbon replica method.5 In performing a lineal analysis on a series of micrographs from each specimen it was found more convenient to determine the mean free path between alumina particles rather than particle radii as the parameter of growth. Although these quantities are directly proportional for only spherical particles, the alumina particles in these alloys

Jan 1, 1962

By D. W. Loucks

There is plenty of evidence to indi-cate that at least one of man's chief interests in life is to make himself as comfortable as possible. If you doubt this, just watch the fellow next to you for the next half hour trying to find the most comfortable position that a hard chair has to offer. Comfort, however, does not always mean an easy chair. To some, it may mean a wealth of money; to another, freedom from worry. But to most of us, it means first of all a comfortable atmosphere in which to live, and to a great many of us it probably also means freedom from that annoying task of firing the furnace. Today more than ever before. automatic heat is one improvement that is placed high on everyone's list. Perhaps this is because automatic heating is becoming relatively cheaper. Perhaps it is because of a good publicity campaign on the part of the oil and gas men or maybe it is just that we are getting lazier day by day. At any rate, almost every issue of Better Homes and Gardens, House Beautiful, or your other favorite home magazine carries an article extolling the virtues of this or that automatic heating system. If I were to ask you to name the first thing that came to your mind when I said automatic heat, you would prob-ably say either gas furnace or oil burner. Or if you had just been studying heating systems, you might possibly say heat pump. But chances are you would not mention anything about coal, and yet coal is the most common source of the greatest automatic heat of them all. I say this because coal is the fuel used almost universally by the district heating industry in producing and delivering to certain heavily populated areas heat ready to use at the touch of a valve or the click of a thermostat. Although the industry is over a half century old, it has not experienced the widespread development of other utility industries because of certain limitations which I believe you will realize from the next few minutes discussion. District Heating Operations We may define district heating as any operation where two or more buildings are heated from a central heating plant. The method of heat transfer may be hot water or in some cases warm air, but generally the medium of heat transfer is steam. So universally is steam used that the industry is frequently referred to as the district steam industry. The Allegheny County Steam Heating Co. which operates the district heating system in downtown Pittsburgh is a subsidiary of the Du-quesne Light Co. Although organized in 1912 primarily as a means of securing the electric load of downtown buildings, the service has now become so valuable and so popular that it is no longer considered a necessary adjunct to the electric business but rather a separate business standing on its own feet. Fig 1 shows the layout of the plants and distribution system of downtown Pittsburgh. Two generating plants, one known as the Stanwix and the other as Twelfth Street, supply the area. Each has two boilers with capacity totaling 1,350,000 lb per hour. The Stanwix Plant is supplied coal by truck. The coal is pulverized at the plant and burned as powdered fuel. Coal is supplied to the Twelfth Street Plant also by truck but the boilers arc stoker fired. Over 1 1/2 miles of tunnel house a portion of our main lines, but it requires over twelve miles of pipeline, ranging in size from 32 down to 1 in. in diameter, to supply all our customers. The distribution system consists of two systems in a sense, one high and one low pressure with certain interconnections between the two. Our high pressure system supplies steam up to 125 Ib to some but not all customers, while the low pressure system operates in the range of 10 to 20 psi. Note that the two plants are tied together through large steam mains and that the system to some extent is a loop system, making it possible to have a portion of the line shut, down without interrupting service to any customer. Fig 2 conveys a picture of the extent to which steam service is used in the downtown triangle. The black area indicates the buildings which now use district steam. The dotted area indi-

Jan 1, 1950

By John R. Edwards

Introductory.—There are many interesting and important events connected with the petroleum problem. The remarkable men who conceived 'the thought of transporting petroleum by pipe line, conserving the byproducts of the commodity, and conducting extended investigation and research whereby the flash point of the oil was raised, its cost reduced and its supply assured, are deserving of the gratitude of this nation. It was primarily the success attained by Captain Lucas, after his comprehensive search for oil in Texas and Louisiana, that was the impelling cause which prompted the Navy Department to conduct the extensive series of liquid fuel-oil tests that were made from 1901 to 1903. The sensational discovery of oil at Spindle top made a deep impression upon Rear Admiral George W. Melville, then Engineer-in-Chief of the Navy, and the discovery of the vast oil field in Texas convinced him that, within a generation, if not within a decade, crude petroleum was going to play a very important part in warfare, and that the commodity might possibly develop into a necessary munition of war. The United States' Commanding Position as a Petroleum Producer.— In the study of the various problems relating to the world's production of crude petroleum, the position of the United States is one of commanding importance, whether viewed from the industrial or the military aspect. The present yield of this country is practically double that of the rest of the world, and, in view of the productive and prospective fields possessed by various countries, together with the comprehensive and exhaustive search that has been made throughout the world for petroleum, it is extremely probable that this lead will be maintained for the next decade. As regards the character of the crude-oil yield of different countries, America possesses the greater part of the supply that contains a paraffine base, and therefore a considerable portion at least of the American product produces the best illuminant. Of all the crude-oil distillates, kerosene is in many respects thc most important, and the Appalachian product for this purpose is favored, particularly in the Far East, above that of any other petroleum yield of the world.

Jan 1, 1915

By Charles Catlett

My attention having been called several years ago to the possibility of increasing the yield of coke per ton of coal, as obtained in certain bee-hive ovens, I called the attention of the Institute to the matter at the New York meeting in 1899. I have had occasion since to witness the indifference with which this matter is ordinarily considered, and, on the other hand, the marked improvement which comes from even a most perfunctory effort in that direction; and I am almost tempted to say that nothing in connection with the coking of coal is at present so important. There are other factors, which are fundamental and necessary; but they have been considered already ; while the question of yield is, as a rule, absolutely ignored, or some figure is taken as the result of a special burning of one or two ovens, and the assumption is made that the whole battery is yielding at that rate. The uncertainty of this assumption I may illustrate by saying that, in my own observation, the burning of a single oven in a battery frequently gives, by actual weight, as much as 69 or 70 per cent. of merchantable coke, while the battery as a whole was yielding only an average of 63 per cent. Only from careful records, checked at least once a month, of the weight of the coal going to the ovens and the weight of coke produced, can any correct idea of the actual yield be gained, or methods be modified so as to produce good results; yet, as a rule, the crudest estimates are usually the only available data. In many cases there are reasons for this loose practice. The coal is mined by measurement; the payment for drawing the ovens is in proportion to the amount of cod which goes to them; and, not uncommonly, the royalty is so much a ton of coke, not of coal. The mine-manager is tempted to increase the volume of coal mined which is paid for as a ton, and to do the same thing in charging the ovens. Nor does he

Jan 1, 1903

By AIME AIME

REPUBLIC STEEL'S new iron blast furnace in Alabama, shown on the cover of this issue, is the first to be completed of those authorized by the Government last year when a shortage of scrap became acute. In addition to the furnace, the new equipment includes a new battery of by-product coke ovens, a boiler plant, a generating unit, a 3-mile-long 60-in. water line, a huge gas washer, and precipitators in which the dust from the furnace is washed, separated from the water, and fed back into the furnace as raw material. The new unit is a cylindrical steel giant reaching 130 ft. into the air above the ground level. Because of the high humidity in the deep South, the furnace has been air-conditioned to avoid blowing eighteen tons of water into the furnace daily. Designed by Republic engineers who also had charge of the actual construction, the new furnace incorporates the best in modern blastfurnace practice. Orders to proceed with the construction of the furnace were received Sept. 22, 1941. The engineering crew, which was immediately organized, made more than 1500 drawings. Excavation started the next day, and simultaneously work was begun on demolishing existing buildings and preparing the site. The first concrete was poured Oct. 7 and the first piece of steel swung into place by a giant derrick on Jan. 30, 1942. It began operating May 28. A total of 70,000 cu. yd. of earth was moved and 30,000 cu. yd. of concrete poured.

Jan 1, 1942

By R. W. Heckel, R. E. Trabocco

The recovery process in 400 Monel filings was followed, principally, by using the Warren-Averbach technique of X-ray peak profile analysis. The deformation fault probability, a, was 0.006 in samples of unannealed filings. a , the twin fault Probability , was approximately 0.002 in samples of unannealed filings. Both a and 0 were found to "anneal out" at 600°F. The effective particle size and mzs strain increased and decreased in the (111) direction, respectively, with increasing annealing temperature. The actual particle size was found to be almost equivalent to the effective particle size. Tile small values of deformation and twin fault probabilities accounted for the similarity in values of the effective and actual particle sizes. Stored strain energy and dislocation density calculations based on rms strain decreased with increasing annealing temperature. The dislocation density decreased from 10" per sq cm in the unannealed filings to 10' per sq cm in the partially re-crystallized filings. The square root of the dislocation density based on strain to that based on particle size indicated a random dislocation distribution in the unannealed filings. The dislocation arrangement changed to one with dislocations in cell walls with increasing annealing temperature. THE recovery processes which occur in metals are generally thought to be a redistribution and/or annihilation of defects.' Investigators' have shown that recovery processes can be characterized by X-ray line-broadening analyses. Michell and Haig4 measured the stored energy of nickel powder by calori-metry and found the value to be greater by a factor of 2.5 than that from X-ray data obtained by the Warren-Averbach technique.= Minor increases in particle size occurred up to 752°F (recovery), while above 752°F the particle size increased greatly due to recrystalliza-tion. X-ray microstrain values decreased between room temperature and 392"F, remained constant from 392" to 752"F, and decreased from 752°F to a negligible value at 1112°F. Faulkner developed an equation for calculating stored strain energy based on X-ray line-broadening data which gave a closer correlation of measured and calculated stored strain energy based on the data of Michell and Haig. The stored strain energy released during recovery is predominately dependent on the decrease in dislocation density which was p-enerated from cold work.7 Stored energy has been measured8 in alkali halides during recovery and recrystallization and 80 pct of the stored energy was found to be released during recovery. Dislocation distributions have been studiedg in a number of fcc metals by thin-film electron microscopy. Howie and Swann" found the stacking fault energy of copper and nickel to be 40 and 150 ergs per sq cm, respectively. ~rown" has pointed out that these stacking fault energy values should be corrected to 92 and 345 ergs per sq cm, respectively. The dislocation distribution of a metal is directly dependent on the stacking fault energy of the system. Metals of high stacking fault energy such as aluminum cross-slip readily and do not form planar arrays of dislocations. Metals of lower stacking fault energy such as stainless steels" do not cross-slip readily. Cold-worked nickel has been found to form a cellular dislocation structure after annealing.13 The relatively high stacking fault energy of nickel and copperlo to a lesser extent favor cellular structures of dislocations rather than planar arrays after deformation. The present study of recovery was carried out on a Ni-Cu alloy (Monel 400) to compare with prior studies for pure nickel and pure copper. X-ray line-broadening techniques were used to measure the effect of recovery temperature on rms strain and particle size and the results were compared with previous studies on copper'4-'7 and nickel., Calculations were also made on stacking fault probabilities, dislocation density, dislocation distribution, and stored strain energy as affected by temperature. EXPERIMENTAL PROCEDURE The nominal analysis of the Monel 400 used in this investigation was: 66.0 pct Ni, 31.5 pct Cu, 0.12 pct C, 0.90 pct Mn, 1.35 pct Fe, 0.005 pct S, 0.15 pct Si. The annealed material was cold-reduced in two batches, one 50 pct and the other 80 pct. It was originally planned to conduct line-broadening studies of these bulk samples; however, rolling textures that developed produced low-intensity peaks which were not suitable for line-broadening analysis. Filings were prepared at room temperature from both the 50 and 80 pct cold-reduced specimens, series A and series B, respectively, and were not screened prior to heat treatment or X-ray studies. Heating to the annealing temperature, 200" to 120O°F, was accomplished in a matter of minutes in a hydrogen atmosphere. Following heat treatment, some of the filings were mounted and polished for microhardness measurements with a Bergsman microhardness tester, using a 10-g load. A G.E. XRD-5 diffractometer using nickel-filtered Cum radiation was used to obtain all diffraction patterns. Only (111)- (222) line-broadenin data were used in the present study since the {400f peaks were too weak to use. The Fourier analysis of the (111) and (222) peak

Jan 1, 1969

By F. Rosenblum, P. Spira, F. Kitzinger

The possibility of increasing the efficiency of mineral processing plants by means of computer control has prompted metallurgists to examine their flowsheets more critically in order to develop practical control strategies. Control schemes in use to date generally rely on the automation of traditional and previously manually regulated control loops, e.g., the addition of reagents to maintain a constant assay or a constant pH. This approach is predicated on the availability of well established primary sensors such as pH electrodes or on-stream analyzers. Noranda Research Center, in cooperation with Noranda Group concentrators, has developed a froth level monitor and a pulp density meter adaptable to this type of control. Although some of the basic principles on which they are based have been known for some time, their incorporation into the design of reliable, direct-reading instruments which can be interfaced with a computer is believed to be novel.

Jan 4, 1979

No review of underground mining should begin with anything but the new world safety record set at the Grace underground iron mine of Bethlehem Steel at Morgantown, Pa., on Friday, November 12. There had not been a disabling injury (an injury which keeps an employee away from his next scheduled shift) for 550 working days. In all, 2,660,080 man-hours had been worked by nearly 950 employees without a disabling injury. The record was wrested from Johns-Manville's Jeffrey mine at Asbestos, Que. At 3 p.m. Friday, December 3, miner Stanton E. Friend was completely buried under several feet of coarse rock, fortunately sustaining only cuts and multiple abrasions. But with his fall, the accident- free period came to an end at 2,778,600 man-hrs worked without a disabling injury-the new record!

Jan 2, 1966

By R. L. Smith, I. G. Greenfield

The binary system Ga-Sb has been investigated by thermal, X-ray, and metallo-graphic methods. 'The intermetallic compound GaSb melts at 705.9OC and forms a eutectic with antimony at 11.8 atomic pct Ga. This eutectic melts at 589.8OC. A eutectic appears to be formed at 29.8°C but is too close to the composition of pure gallium to be detected. IN the course of an investigation of the semiconducting properties of the intermetallic compound, GaSb, the phase equilibrium between gallium and antimony has been investigated. Recently, the phase diagram of similar systems, such as In-Sb,' In-AS,' and Bi-As3 have been determined. These diagrams have the same general appearance in that an intermetallic compound is formed at 50 atomic pct and a eutectic is formed on both sides of the intermetallic compound. Jenny,& who has been investigating the semiconducting properties of intermetallic compounds, has concluded from thermal data of several alloys that the phase diagram of the Ga-Sb system resembles those mentioned previously. This paper represents a more detailed study of the Ga-Sb equilibrium. Experimental Procedure The gallium that was used to prepare the alloys was obtained from A. D. Mackay Inc. and the Aluminum Co. of America; the latter reported the purity as 99.95 pct. The antimony was obtained from Bradley Mining Corp. who specified a purity of 99.997 pct. Since the intermetallic compound of GaSb was prepared primarily to be used for further studies of the semiconducting properties, additional purification by a standard zone-melting technique under an atmosphere of hydrogen was performed. Hall-effect measurements on this material indicated an impurity content of less than 3 ppm.5 The antimony also was purified by zone melting and used in conjunction with the compound GaSb to make the necessary alloys for the determinations of the antimony-rich side of the phase diagram. The antimony-rich alloys were chill cast in Vycor tubes which were evacuated to a pressure of less than one micron. Since these alloys expand on freezing, precautions were taken to prevent oxidation of the ingot in the event the tube fractured. To insure homogeneity, the brittle alloys were ground and then placed in the furnace for the thermal-arrest determinations. Since the cost of gallium is high, the experimental procedure was complicated somewhat because of the necessarily limited sizes of the melts. In order to economize, the gallium-rich side of the diagram was determined by using a 35 g ingot of pure gallium initially and adding increasing amounts of antimony in order to obtain additional alloys. The furnace used in the determination of the cooling curves is illustrated in Fig. 1. A 2¼ in. quartz tube, sealed at one end, was fitted with a brass flange which was attached with DeKhotinsky cement. The brass collar was water cooled to prevent the cement from softening. An "0" ring was used to provide a seal between the brass collar and the furnace cover. Nichrome ribbon was wound around a 2 ½ in. asbestos-covered copper core which was used to reduce the thermal gradient in the furnace. The insulation consisted of alternate layers of asbestos and aluminum foil surrounded by sil-o-cel refractory and

Jan 1, 1956

By Henry Siegmann

HISTORY OF PRODUCTION AND USE In 1899 the consumption of fluorspar in the United States was reported as 16,000 tons. The invention of the open-hearth method of steel manufacture, plus the beginnings of a fluorine chemical industry, pushed consumption of fluorspar to 250,000 tons by 1918. In contrast to these consumption statistics of the past, the most recent statistics available (1972) indicate a total fluorspar usage in the United States of 1.352 million st (Table 15.4D.1). Fluorspar remains the world's cheapest source of fluorine, and its unique properties make the mineral the most desirable fluxing agent for steel refining. The linking of fluorine with carbon in the late 1930s resulted in the production of fluorocarbon, and constant growth in production over the years has formed the backbone of a strong fluorine chemical industry. For example, in 1972 it is estimated that total fluorocarbon production amounted to 2.113 million tons, and that, in this process, over 1.351 million tons of acid-grade fluorspar was consumed. The producers of primary aluminum long have been concerned about the fast dwindling reserves of natural cryolite. They found the solution to their problem by utilizing fluorspar for the manufacture of synthetic cryolite and aluminum fluoride. Nuclear weapons, as well as the growing number of peaceful uses for atomic reactors, constitute a market for uranium hexafluoride. This chemical and chlorine pentafluoride, used as an oxidizer with rocket fuels, are products that are as much a novelty as fluorocarbons were 25 years ago. Judging from past success in the field of fluorine chemistry research, it is safe to assume that the market for these chemicals will grow in the future. Three major industries account for the bulk of the fluorspar consumption: steel refining, fluorine chemical, and primary aluminum production. These industries have had a pattern of fabulous growth in the past, and their future plans point to a continuation of this pattern. It seems logical that the fluorspar usage also should continue its upward trend. Considering the growth of the fluorspar industry since 1899, and the obvious dependence on imports of fluorspar as a raw material, one of the most puzzling aspects of the past has been the apparent lack of coordination between fluorspar production and fluorspar consumption. A few authoritative voices have spoken out concerning the need to expand fluorspar production in order to meet consumption of the future. During World War II, the U.S. Government took positive steps in this direction by authorizing purchases at attractive prices for its "stockpile program." As a consequence, new fluorspar producing facilities were built, not only in

Jan 1, 1976

By Raymond D. Daniels, Frank E. Rizzo, James D. Gerber

ThIS discussion describes a method for the addition of small amounts of oxygen to columbium (niobium) in an accurate and reproducible manner. The method is based on the complete reduction by columbium of a carefully weighed amount of another metal oxide. The equilibrium Pq associated with Cb-CbO mixtures is extremely low, e.g., 10"25 atm at 100O°C, and the pressures over Cb-0 solutions are even lower. The equilibrium Pq associated with a given metal-metal oxide mixture can be easily obtained, with the aid of a Richardson-Jeffes chart.' Although columbium should effectively reduce almost any metal-metal oxide combination, the proper choice of a metal-metal oxide system is complicated by the low rate of oxygen transport in the gas phase at low oxygen pressures and the difficulty in reducing any columbium suboxide formed during the reduction of the oxygen source material. Thermodynamically, oxide formation on columbium will be avoided so long as the oxygen partial pressure over the columbium is below the equilibrium pressure associated with the mixture Cb-CbO. The logical choice of a source for oxygen would appear to be a mixture of Cb-CbO, since oxide formation would be precluded by nucleation difficulty. But calculations using the kinetic theory of gasses indicate that, for a temperature of 900°C, the reaction would proceed too JAMES D. GERBER, formerly Research Assistant, University of Oklahoma, Norman, Okla., is Research Metallurgist, Air Force Weapons Test Laboratory, Kirtland Air Force Base, N. Mex. FRANK E. RIZZO, Junior Member AIME, formerly Assistant Professor of Metallurgy, University of Oklahoma, is Associate Professor of Metallurgy, University of Texas at El Paso, El Paso, Tex. RAYMOND D. DANIELS, Member AIME, Professor of Metallurgical Engineering, University of Oklahoma, is an NSF Fellow, Institute de MBtallurgie Structurale, Universite de euch:tel, Neuchitel, Switzerland. Manuscript submitted October 28, 1968. IMD

Jan 1, 1970

CRUSHING and concentration flow-sheets of western mills have become greatly simplified and more or less standardized of recent years with the introduction of modern grinding methods and flotation. Improvement has not stopped, however, and advancement is continually being made in crushing and milling practice. A case in point, where remarkable improvements in efficiency have resulted from comparatively minor changes in the flow-sheet, is in the New Cornelia mill of the Calumet and Arizona Mining Co. at Ajo, Ariz. This mill, completed in 1924 for the concentration ,of the sulfide ores of the New Cornelia mine, was originally designed for a 5000-ton capacity. Before recent changes and additions were made the five 1000-ton units were handling 6500 to 7000 tons per day, giving a flotation feed of approximately 14 per

Jan 1, 1930

By J. J. Gilman, T. A. Read

FOLLOWING the deformation 01 zinc monocrys-tals, sharply bent basal planes are observed near several types of inhomogeneities. Three of these in-homogeneities have characteristics which are quite regular so that they can be studied and analyzed. These are compressive kink bands, "deformation bands," and the inhomogeneities near end restraints. The present paper describes experiments in which "deformation bands" were artificially produced, and bend plane phenomena are discussed in terms of dislocation theory. Also, two new bend plane phenomena are described. The importance of bend plane phenomena in the deformation of crystals is not widely recognized. Many phenomena may be explained in a manner similar to the discussion in this paper. Jillson1 has pointed out that the "punching effect" in zinc is a bend plane phenomenon and is not caused by prismatic slip.' Bowles3 has suggested that they may be involved in diffusionless phase changes. Cahn4 has discussed the role of bend plane formation in the polygonization of zinc. Experimental Work Tensile Kink Bands: Because of the geometrical similarity between "deformation bands" and "kink bands" (compare Fig. 1 of this paper with Fig. 1 of the paper by Hess and Barrett"), the band shown in Fig. 1 of this paper will be called a "tensile kink band," and that shown by Hess and Barrett will be called a "compressive kink band." It is felt that the term "deformation band" should be reserved for banded structures in polycrystalline materials such as iron." Tensile kink bands seem to form spontaneously in aluminum crystals deformed by tensile loading.7-10 In zinc and cadmium crystals they do not form in good, carefully loaded specimens.'." However, tensile kink bands can be produced artificially in zinc crystals. The present authors did this by scratching one of the flat surfaces of triangular crystals transversely with a sharp needle. Natural tensile kink bands caused by inhomogeneities sometimes appeared in deformed crystals which were identical in appearance with the artificially produced ones. Zinc monocrystals were grown by the Bridgman method in graphite molds. Chemically pure zinc (99.999+ pct Zn) was used and the molds were sealed inside evacuated pyrex tubes during growth. The crystal cross sections were equilateral triangles with a typical base of 0.210 in. The artificial kink band shown in Fig. 1 is typical of tensile kink bands in zinc. The band lies between two bend planes which run from upper right to lower left and is inclined oppositely to the slip bands which are sharply bent at the two bend planes. The general form of the artificial tensile kink bands was independent of the scratch depth (1 to 5 mils deep) and also independent of which side was scratched. These variables did cause variations, however. Deep scratches produced more localized kink bands than light scratches. Also, if the angle between the slip plane traces and a transverse scratch varied appreciably among the three sides, then localization of the resulting kink bands also varied. Furthermore, if the slip direction lay nearly parallel to the scratched side, the band was more developed near the scratched side than at the opposite edge. Scratches produced tensile kink bands for crystal orientations from xo = 15" to x, = 75". Fig. 2 shows a scratched crystal after deformation. One triangular side lies in the plane of the photograph. The right hand tensile kink band was produced by a transverse scratch on the upper right side. The next two kink bands were the result of scratches on the front surface. The kink band at the left was caused by a scratch on the lower back side. All four bands have the same general form. A longitudinal scratch was also made on the crystal shown in Fig. 2 to determine the effect of a scratch on the critical shear stress. The critical shear stress of the scratched region was 33.9 g per sq mm compared to 24.4 g per sq mm for the un-scratched region above it. Fig. 3 shows Laue patterns of the crystal shown in Fig. 2. Fig. 3a shows the pattern of the undeformed crystal. The orientation was x, = 21°, A, = 31". After deformation, Fig. 3b was made of the homogeneously deformed portion of the crystal. The spots are compact but split into two halves. This region was elongated 45 pct and its orientation was x = 14", X = 20"; the sine law predicts x = 14", A = 20.5". Fig. 3c was taken near the center of the middle tensile kink band of Fig. 2. The pattern shows a range of orientations and polygonization in this region. The spread in orientation was due to the fact that the basal planes were curved (see Fig. 1) rather than flat as in the ideal case. Some may also have been the result of elastic distortions and "local curvatures." The orientation range was x = 23" to 32", A = 30" to 42". It is apparent from Fig. 3 that the material inside and outside the kink band rotated in opposite directions with respect to the tension axis during deformation. The orientation calculated from the ideal configuration of Fig. 9,

Jan 1, 1954

By Shiro Ban-ya, John Chipman

Equilibrium in the reaction was investigated at temperatures of 1500°, 1550°, and 1600°C for sulfur concentrations up to 7.2 wt pct. Multisample crucibles contained the liquid alloys in a resistance-heated furnace using a technique especially designed for the study of more complex alloys to be reported separately. Modern free-energy data are used to correct the H2S:H2 ratio for dissociation of H2S and calculalion of the partial pressure of S2. Published data on the equilibrium are similarly corrected. Thermodynanzic treatment of the data employs the composition variable zs = nS/(nFe — nS) and the activity coefficient Gs = as/zs The data at 1500" and 1550°C are fitted by the equation log s = —2.30zs. Within the limits of experimental error the same coefficient is applicable to the data at higher temperatures. Equations are given for the free-energy change in Reaction [I] as well as for the solution of S, gas in the metal. The heat of solution of 1/2 s2 is -32.28 i2.5 kcal. Uncertainty in the free energy is very much smaller. For dilute solutions of interest in steelmaking, the activity coefficient of sulfur is unchanged from that listed in Basic Open Hearth Steel-making. DETERMINATIONS of the thermodynamic properties of sulfur in liquid iron by Morris and williams1 and by Sherman, Elvander, and chipman' provided a basis for control of sulfur in steelmaking processes. From the standpoint of understanding the chemistry of metal plus nonmetal in liquid solution they left several questions unanswered. The activity of sulfur in dilute solution at about 1600°C was well-established but temperature coefficients were uncertain, due at least in part to the use of the optical pyrometer and uncertainty regarding the effect of sulfur on emissivity. It appeared that deviation from Henry's law increased with increasing temperature, a most unusual behavior requiring either confirmation or disproof. These studies were based on experimental determination of equilibrium in the reaction: At high temperatures H2S is partially dissociated so that the gas mixture contains HS, S2, and S in addition to HS. At the time of the earlier studies the free energies of these constituents were unknown and it was therefore impossible to make adequate correction for dissociation. Observations on the effects of alloying elements by Morris and coworkers1, 3 and by Sherman and Chip-man4 enable us to assess the effects of alloying elements on the activity and to make corrections for incidental impurities in the binary liquid. These studies as well as a number of more recent investigations will be reviewed in detail after out own experimental results have been presented. It was our purpose in planning this study to avoid uncertainties regarding the emissivity of alloys and the errors of thermal diffusion which plagued some of the early attempts,5 by using a resistance furnace and thermocouple in preference to induction heating and optical pyrometer. Modern data on free energies of the gaseous species are to be applied to our data and to those of other investigators to obtain corrected values of K1 and of the activity coefficient and ultimately to relate the sulfur content of the bath to the equilibrium partial pressure of S,. Extension of the study to include ternary and complex solutions will be described in a later section. EXPERIMENTAL METHOD a) Preparation and Calibration of H2-H2s Gas Mixture. The source of hydrogen sulfide was a preparer mixture of 43 pct H2S, balance hydrogen, contained in a large aluminum cylinder. This was passed through anhydrone and through a microflowmeter. Hydrogen was passed through platinized asbestos, ascar-ite, and anhydrone, and through a capillary flowmeter. Argon was passed through copper wool at 500°C, then through ascarite, anhydrone, and a flowmeter. The flow rate of hydrogen was kept constant at 200 ml per min, to which an arbitrary amount of the hydrogen-hydrogen sulfide mixture was constantly added and then the prepared gas mixture was introduced into the reaction tube through a gas mixer. In certain experiments 200 ml per min of argon was added to the hydrogen-hydrogen sulfide gas mixture to increase the total flow rate of gas. The ratio of hydrogen-hydrogen sulfide in the inlet gas was checked for each run by chemical analysis. A sample of the gas taken from a bypass was bubbled through zinc and cadmium acetate solution (4 pct zinc acetate, 1 pct cadmium acetate, and 1 pct acetic acid) to remove hydrogen sulfide from the gas mixture, and the flow rate of the remaining hydrogen was measured by a soap bubble method to determine the volume of hydrogen. The amount of hydrogen sulfide absorbed in solution was determined by titration with iodine against sodium thiosulfate, with starch used as the indicator. The ratio of hydrogen sulfide to hydrogen in the inlet gas could be kept within ±2 pct in the range from 10-2 to 5 x 10"4 which corresponds to from 0.2 to 7.0 wt pct sulfur in liquid iron. b) Furnace Arrangement. Fig. 1 shows the furnace arrangement and the shape of the alumina crucible used in this experiment. A vertical-tube silicon carbide electric resistance furnace contained the reaction tube which consisted of two parts, the gas-tight

Jan 1, 1969

By J. F. Evers, S. Sadiq, F. W. Preston, G. W. Swift

Proper scaling of unsteady-state flow in laboratory gas reservoir models can be achieved if the permeability/fractional porosity ratio is less than 0.5 md. Porous media meeting this specification can be obtained from mixtures of sand and Portland cement provided (1) the water/cement ratio is in the range of 0.35 to 0.40, (2) the sand/cement ratio is in the range of 1/1 to 2/1, (3) the sand grain size is in the range of 48-100 to 18-28 mesh, (4) the mortar curing time is 7 days or more and (5) the cured mortar is dried under vacuum to reduce the temperature level employed during the drying process. The areal homogeneity of the mortars tested is reasonably good, although significant trends in vertical permeability were noted. The Klinkenberg and non-Darcy coefficients of mortar are such that proper scaling of these effects in the laboratory model could be expected. INTRODUCTION A long term deliverability prediction for a gas well is generally based on data determined from flow tests that are of short duration relative to the producing life of the well. These data, together with an estimate of gas reserves in place, form the basis for establishing the parameters of the mathematical model used to predict performance at future times. Results obtained from a mathematical model represent only an interpretation of the physical process being modeled. Experimental verification of the production process from discovery to abandonment is needed where production occurs under carefully controlled conditions. Ideally, one might consider such an experiment to be conducted in the field. Even if the cost of such an experiment could be justified, the time required would make it impractical to consider. However, if the time scaling problem could be handled properly, an experimental model of the gas reservoir production process could provide the necessary data to study the mechanisms of the production process in a reasonable time period. An experimental model has been designed and constructed using the data of this study as a basis. The model reservoir system consists of one producing well located at the center of a right-circular cylinder of porous material. Ten to 15 observation wells are located at strategic offset positions from the producing well. These wells, and the producing well, are fitted with pressure transducers so that the pressure-time history can be recorded at various radial and azimuthal positions in the drainage area during the entire production life of the system. Time is scaled in the model so that the time required to produce gas from discovery pressure to abandonment pressure is about 2 hours. This compares with a 20-year producing life in the model's field counterpart and gives a time scale factor of approximately 1:100,000. DESIGN CRITERIA To establish design criteria for the experimental model, the reservoir is considered to be a finite right-circular cylinder of radius rr, and height h with a producing well of radius rw located at the center and completed through the producing formation. This reservoir consists of a porous medium which has a uniform permeability k and gas porosity and the gas contained in the reservoir has density p, viscosity µ and molecular weight M. Initially, the pressure at all points within the reservoir is uniform at po. and the reservoir temperature is T. Since the reservoir production process has been demonstrated to occur in two distinct transient modes for either Darcy or non-Darcy flow,l it is

By A. P. Coldren, V. Biss

SINCE the r ? a transformation rates of many carbon-free ferrous alloys and low-carbon alloy steels are relatively fast, conventional equipment is not suitable for the dilatometric determination of continuous cooling transformation diagrams. On the other hand, a method based on metallographic analysis of quenched specimens would not be practicable because the various products of shear-dominated transformation are essentially indistinguishable in low-carbon iron-base alloys. Both problems may be avoided by a thermal analysis method employing gas quenching of small specimens austenitized in vacuo. The laboratory equipment employed in the present study consisted of a Tektronix Type 564 Storage Screen Oscilloscope and a Kinney high-vacuum evaporator, modified as shown in Fig. 1, to permit heating a small specimen and cooling it slowly by programmed cooling or rapidly (up to about 8000°F per sec) by a controlled quench with helium gas. The oscilloscope records the electromotive force of a 40-gage (0.003-in.-diam) Chromel-Alumel thermocouple in the specimen during cooling. The temperature at which the cooling curve begins to show the influence of the heat produced by the phase change in the specimen was arbitrarily taken as the transformation-start temperature.*

Jan 1, 1970

By Albert E. Reed

THE development of the modern high-speed vibrating screen, together with the increasing availability of long-lasting stainless-steel screen cloth for relatively fine-mesh separations, means that more screen circuits will be used in the future. It seems pertinent therefore to examine a few characteristics of screen-circuit products, and especially the points of difference as compared with products of classifier circuits. The most noticeable change that takes place when substituting screening for classification in a grinding circuit is a substantial drop in the circulating load, owing to the greater ease with which the "fines" leave the circuit. Where circulating loads of 500 to 600 per cent are considered fairly normal in classifier grinding circuits, the grinding circuit equipped with screens for equivalent work will have a circulating load of only 20 to 75 per cent. As a result, the products of screen circuits will show a minimum of overgrinding or sliming as compared with a classifier circuit. The desirability of this characteristic will naturally vary according to the metallurgical requirement in each case. Because screen separations make a sharper division according to particle size, the products of screen circuits can be expected to show greater crowding of particles near the point of separation. These changes in product characteristics are so important that other factors, both in the grinding and concentration processes must be adjusted if the operator is to take full advantage of the increased tonnages and higher efficiencies available to him through the use of the screen circuit. One factor that too often is overlooked when changing to screen circuits is the importance of adjusting the ball-mill or rod-mill charge, to compensate for: (I) increased tonnage of new feed, (2) decreased circulating load, or (3) more granular character of feed. These same factors should also be taken into consideration for their effect on the various types of concentration or flotation equipment that may follow the screen circuit. Over a period of years, this equipment has generally been designed and adjusted to the product of the classifier, therefore it seems obvious that some research on the adjustment and adaptation of concentrating and flotation equipment to screen-circuit products will be most profitable to the operators. To illustrate the points mentioned above, the results from three recent installations follow, with data on the comparative characteristics of screen and classifier circuits. A range of separation from 10 to 48 mesh has been chosen, using two general types of screening equipment and two types of classifiers. The first of the installations of which the results are to be examined is that of an iron-ore installation where eastern magnetite was being concentrated prior to sintering. Fig. I shows the original grinding circuit, using classification, while Fig. 2 shows the same circuit equipped with a

Jan 1, 1945

By J. A. Snyder, W. L. Finlay

G. Edmunds—Solid solubility is considered to be of either the interstitial or the substitutional type. Is it possible, in a binary alloy as the simplest case, that some of the solute atoms are present in the normal lattice sites (substitutionally or filling lattice vacancies) while simultaneously others are in interstitial positionss One might even ask whether a distribution of the two types may be the normal situation. H. M. Meyer—Metastable states of interstitial atoms occupying vacant lattice sites possibly occur as well as of substitutional atoms squeezed in between regular matrix positions. However (as we know since Hume-Rothery), the solute atoms choose between the two kinds of solutions; consequently, every solute will be unequivocally either substitutional or interstitial in the equilibrium state of the solid solution. M. Balicki—In view of the fact that the authors apparently correlate the analysis of the alloys at the ingot stage with the properties exhibited at the testing stage, I would like to ask whether this is a fully justifiable procedure. In other words, how good are their determinations of solute concentration for correlating them with the mechanical properties. The answer to this question may explain some of the divergencies. Assuming good enough homogenization of the samples and exact determination of mechanical properties the position of the plotted experimental points will depend solely upon the accuracy of composition determination. If this is not accurate, say due to loss or pickup of elements during processing from the ingot to the testing stage, or due to a systematic error in the method employed for obtaining solute concentration data, the points will deviate from their true position and may align themselves along a different curve than the one expected. H. V. Kinsey—We have been studying the creep-rupture properties of titanium-base alloys at 1000°F. In the course of this work, anomalies in behavior of the alloys that would suggest that the material under test was becoming stronger as the test progressed have been observed. If this was so, the most likely explanation that we could think of was that the test bars were absorbing oxygen and nitrogen from the air during the test and were thereby becoming strengthened. In an attempt to determine the strengthening effect of absorbed oxygen and nitrogen the following experiment was conducted. A length of cold-rolled titanium was supplied by the E. I. du Pont Co. Two test bars, having a 1/4 in. diam gauge length, were prepared from this material. One bar was tested in the as-received condition. The second bar was heated in air at 1550°F for 100 hr and subsequently air cooled prior to testing. A testing temperature of 1000°F was employed. The results of these tests are tabulated in table 11. In the author's opinion, is it reasonable to assume that the bar that was exposed to air at 1550°F for 100 hr was stronger because it absorbed oxygen and nitrogen from the air during this heat treatment? W. L. Finlay (authors' reply)—Direct experimental evidence for or against Mr. Edmunds' interesting suggestion will probably never be available. It seems possible, however, that mixed interstitial-substitutional solid solution might well occur with interstitial elements. The less likely possibility of interstitial solution of a normally substitutional element like copper in aluminum was recently discussed at length by the

Jan 1, 1951

By B. J. Steblay

Roof bolts are the primary means of supplemental support in coal mines and are widely used in other mines. Presently, post installation loads are measured infrequently on only about 10% of the bolts by using standard torque wrenches that limit accuracy to about ± 30%. Because mine roof bolts are long, slender, non-uniformly sized, roughly forged, placed in a difficult environment, and subject to severe bending on installation, researchers have been unable to use ultrasonic reflection techniques to measure strain. A complete measurement system has now been assembled by the US Bureau of Mines, Denver Research Center. Obstacles such as bolt preparation, transducer mounting, reliable reflection, and calibration have been dealt with. The seemingly simple concept of measuring the time of flight of an ultrasonic pulse to a reflector is actually complex due to the need to measure to 0.0025 mm (0.0001 in.) accuracy, the sensitivity of velocity to temperature, and stress, and the stability required to make measurements over several years.

Jan 1, 1986