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By Frank C. Aplleyard

The two calcium sulfate minerals-gypsum and anhydrite-occur in many parts of the world, and gypsum has long been of economic importance in the family of industrial minerals. Gypsum, the dihydrate form of calcium sulfate (CaSO4•2H2O) and anhydrite, the anhydrous form (CaSO4) are frequently found in close association, and it is seldom that a calcium sulfate deposit will consist exclusively of one mineral or the other. Although known gypsum deposits are extensive, anhydrite makes up the largest part of total calcium sulfate reserves. However, it has very minor economic use, and most of the following discussion will be devoted to gypsum. Calcium sulfate is one of the principal constituents of evaporite deposits, and when pure, has the following composition: [Sulfur Combined Lime Trioxide Water (CaO) (SO,) (H2O) Gypsum 32.6% 46.5% 20.9% Anhydrite 41.2% 58.8% -] Deposits of pure gypsum or of pure anhydrite which are large enough to be considered commercial have never been found because of both the metastable relationship between the two minerals, and the presence of impurities such as calcium or magnesium carbonates, chlorides, other sulfate minerals, clay minerals, or silica. As a result most mine production of gypsum will range between 85 and 95% pure. Often it is used as mined, although in certain cases, one or more forms of mineral beneficiation are employed to upgrade the product. End Uses The largest use for gypsum is based upon the unique property which calcium sulfate has of readily giving up, or taking on, water of crystallization. With the application of a moderate amount of heat in a process known as calcining, gypsum is converted to plaster of paris (the hemihydrate of calcium sulfate, CaSO4 ½ H2O) which when mixed with water will set or harden as the calcium sulfate returns to the dihydrate form. This semifinished product, usually called stucco, is then manufactured into a large variety of plasters, wallboard, and block for construction use, or into plasters for industrial applications. About 75% of the gypsum used in the United States is calcined for these purposes. Uncalcined uses of gypsum are principally as a retarder for portland cement, as a soil conditioner, as a mineral filler, and other minor industrial applications. About 25% of the gypsum mined in the United States goes into these markets; however, in less developed countries where construction and other industrial uses may be quite limited, the use of uncalcined gypsum for portland cement retarder may well be the dominant-if not the only-market for the mineral. It has often been noted that calcium sulfate constitutes the world's largest reserve of sulfur, and minor use of both anhydrite and gypsum has been made to produce sulfuric acid or other sulfur compounds such as ammonium sulfate. However, because sulfur is readily available at lower cost from other sources, use of calcium sulfate has been limited to only a few locations where it could compete economically. No such use is reported in the United States at this time. Mineralogy Anhydrite, CaSO4 because of its geologically rapid conversion to gypsum, and relatively high solubility (about 0.2 g per 100 g H2O) is not often found outcropping in climates wet enough to support abundant vegetation except on steeply dipping slopes or other places where hydrated material is continuously removed. Anhydrite rock is most often light to bluish gray in color, and under the microscope, varies

Jan 1, 1983

The Colorado School of Mines, Golden, Colo. M F Coolbaugh, President. Since 1906 the School of Mines has issued a journal, known as the Quarterly of the Colorado School of Mines, which carries many articles on matters of general interest as well as other articles of a technical nature There is no regular subscription price to the School of Mines publications Anyone interested in back numbers should write and find out the conditions under which individual copies may be obtained, whether a price is set on them or whether they are free Some back numbers are not now available but efforts will be made to supply copies from the files of alumni or other friends of the School Vol 23, No. 3 of the Quarterly (July, 1928) is an index of the publications complete from July, 1906 to July, 1928. A selected list of the technical articles appearing in the Quarterly is given here: Vol 3, No. 3, Rare metals. uranium and vanadium, by H. Fleck (1909), vol 3, No 4, Tungsten in Colorado, by H R Van Wagenen, vol 4, No 3, Preliminary report of the radioactivity of the carnotite of southwest Colorado, by H Fleck and W. G Haldane (1909), vol. 8, No 1 (1913), Some recent developments at Leadville, by G. M Butler, vol 8, No. 3, Physiography of

Jan 1, 1933

Jan 1, 1922

Jan 1, 1922

By W. J. Maraman, D. R. Harbur, J. W. Anderson

A device for rapidly quenching liquid metals into thin platelets has been developed at the Los Alamos Scientific Laboratory. This rapid quenching equipment is built around the technique of catching a molten drop of metal between a rapidly closing plate and a stationary plate. The design and operation of this unit are described. The closing speed of the smasher plate at impact is 12.6 ft per sec. The quenching rate for this device is controlled by the interface resistance between the plates and the platelet, and is dependent upon the heat content and density of the material being quenched. The initial quenching rate down to the freezing point of the platelet material is lo5º to 106ºC per sec. After an isothermal delay, which is poportional to the heat of fusion of the platelet material, the final cooling rate down to the temperature of the smaslier plates is l04ºto 105cº per sec. RAPID heating of metals by capacitor discharge and other methods has provided the metallurgist with a useful tool for probing into the kinetics of phase changes and the many nonequilibrium phenomena which occur during rapid temperature changes. Equally interesting studies can also be made on metals and alloys which are rapidly cooled from the liquid state.' Studies in this field have been limited, however, because the rates at which metals could be cooled were many orders of magnitude slower than the rates possible for heating. In recent years many new laboratory methods have been developed to rapidly cool metals from the liquid state to ambient temperature and below.2"4 All of these methods involve spreading a liquid drop of metal into a thin foil in a very short time. The methods developed have varied from ejecting a drop of molten metal at the inside surface of a rotating cylinder or stationary curved plate to catching a falling drop of molten metal between rapidly closing plates. The equipment which has been developed at the Los Alamos Scientific Laboratory for rapidly cooling molten materials uses the latter of these two approaches. The basic design, operation, and initial results of this rapid quenching device are given in this report. APPARATUS The drop smasher, which is now being used to obtain rapidly cooled metal foils, is shown in Fig. 1. Basically the device consists of a smasher plate which is driven by a solenoid into a stationary plate. The solenoid is activated by a drop passing through the photoelectric cell and is powered by discharging an adjustable 350-v capacitor bank with a 66-amp peak current into it. This power supply is designed so that the solenoid is powered for 2 m-sec after plate closure to minimize the rebound effect. There is an adjustable time-delay mechanism between the photoelectric cell and the solenoid. Both smasher plates have changeable inserts so that a variety of materials can be used to smash the molten drop. The shaft of the moving plate is guided in an adjustable housing which has ball-bearing walls. The cabinet shown to the left of the drop smasher in Fig. 1 contains the power supply and receiver for the photoelectric cell, the time delay mechanism, and the capacitor bank. The drop smasher can be placed inside a vacuum chamber, for use with radioactive materials, with the upper plate forming the lid, as shown in Fig. 2. On top of the vacuum lid is an induction coil, powered by an Ajax induction generator, which is used to melt drops from the end of the rod extending through the vacuum seal on top the quartz tube. OPERATION The drop smasher shown in Fig. 2 is operated in the following manner. The smasher plates are separated and the unit is lowered into the vacuum chamber using a pressurized cylinder. The induction coil, quartz tube, and lid with sliding vacuum seal are then assembled on top the vacuum chamber. A rod of the material for rapid quenching studies is connected to the rod extending through the sliding vacuum seal. The vacuum chamber is then evacuated and the desired atmosphere established. The photoelectric cell is turned on, and the capacitor bank is charged and armed. Power is supplied to the induction coil, and the rod of material for rapid quenching studies is lowered into the induction field. A molten drop forms on the end of the rod, drops off, falls through the light beam of the photoelectric cell, and is then caught between the smasher plates. .

Jan 1, 1970

By S. A. Falconer

This paper deals with the practical application of the Dutch State Mines cyclone separator for fine-coal cleaning. The more important operating variables are discussed, and results of a number of continuous-scale tests on various fine coals with a 6-in. cyclone separator are given. Descriptions of the Cyanamid Pilot Plant and the 50 tph Cyclone Separator Plant at the Emma Washery in Holland are included. TODAY, as never before, the coal producers of this country are faced with the necessity for obtaining maximum yield of marketable coal of all sizes down to and including the finest. Particular interest is being displayed in a more effective means of recovering the finer sizes which in the past so often have been discarded to waste or treated by inadequate equipment. The reasons for this interest are easily understood. Rising mining costs have resulted in the increased use of mechanized equipment underground for full seam mining. This, in turn, means more refuse in the run-of-mine and also more fines in the feed going to the cleaning plant. Stringent antistream pollution laws now make it necessary at least to impound the fines, and usually it is a paying proposition to recover the coal from these fines before sending them to the storage area. Finally, the market and price of the finer sizes has increased, but at the same time specifications have tightened and the demand is for higher grade products. During the past four years a great deal of publicity has been given to this new process and apparatus for treating fine sizes of ores as well as coal. Excellent discussions of the apparatus itself and the theoretical aspects of the basic operating principles involved in its operation have been presented by M. G. Driessen,1-3 M. R. Geer and H. F. Yancey,4,5 J. W. Hyer6 and more recently by D. A. Dahlstrom8 as well as others.7,9-11 In view of this, it has been decided to include in the present paper only a brief description of the cyclone separator and its operating principles. This paper deals primarily with some of the more practical commercial aspects of the process and equipment required for its operation; the variables in the operation of the cyclone, their effect and means for control; and the results obtained with a 6-in. semicommercial size separator on a variety of fine coals, bituminous and anthracite, using finely ground magnetite for the separating medium solids. A description is included of the commercial-size cyclone separator pilot plant installed by the Dutch State Mines at its Emma mine in Holland, where finely ground slate is utilized as medium solids. Field of Application: The Dutch State Mines cyclone separator operates most efficiently on ores and coal in the size range of % in. to about 48 mesh. On some types of feed, effective separation can be made on sizes as small as 100 mesh, but up to the present, this may be considered exceptional. Depending upon the type of medium used, the specific gravities of separation can be varied within wide limits, up to as high as 2.70, if magnetite is used as medium. Early Development: The development of the Dutch State Mines cyclone as a separator, or cleaner, was the outgrowth of early experimental work by Dries-sen' and others in Holland, just prior to World War 11, in the course of which was discovered the effectiveness of the cyclone in reclaiming and thickening the dense medium used in the "Loess" process of

Jan 1, 1951

By S. A. Falconer

This paper deals with the practical application of the Dutch State Mines cyclone separator for fine-coal cleaning. The more important operating variables are discussed, and results of a number of continuous-scale tests on various fine coals with a 6-in. cyclone separator are given. Descriptions of the Cyanamid Pilot Plant and the 50 tph Cyclone Separator Plant at the Emma Washery in Holland are included. TODAY, as never before, the coal producers of this country are faced with the necessity for obtaining maximum yield of marketable coal of all sizes down to and including the finest. Particular interest is being displayed in a more effective means of recovering the finer sizes which in the past so often have been discarded to waste or treated by inadequate equipment. The reasons for this interest are easily understood. Rising mining costs have resulted in the increased use of mechanized equipment underground for full seam mining. This, in turn, means more refuse in the run-of-mine and also more fines in the feed going to the cleaning plant. Stringent antistream pollution laws now make it necessary at least to impound the fines, and usually it is a paying proposition to recover the coal from these fines before sending them to the storage area. Finally, the market and price of the finer sizes has increased, but at the same time specifications have tightened and the demand is for higher grade products. During the past four years a great deal of publicity has been given to this new process and apparatus for treating fine sizes of ores as well as coal. Excellent discussions of the apparatus itself and the theoretical aspects of the basic operating principles involved in its operation have been presented by M. G. Driessen,1-3 M. R. Geer and H. F. Yancey,4,5 J. W. Hyer6 and more recently by D. A. Dahlstrom8 as well as others.7,9-11 In view of this, it has been decided to include in the present paper only a brief description of the cyclone separator and its operating principles. This paper deals primarily with some of the more practical commercial aspects of the process and equipment required for its operation; the variables in the operation of the cyclone, their effect and means for control; and the results obtained with a 6-in. semicommercial size separator on a variety of fine coals, bituminous and anthracite, using finely ground magnetite for the separating medium solids. A description is included of the commercial-size cyclone separator pilot plant installed by the Dutch State Mines at its Emma mine in Holland, where finely ground slate is utilized as medium solids. Field of Application: The Dutch State Mines cyclone separator operates most efficiently on ores and coal in the size range of % in. to about 48 mesh. On some types of feed, effective separation can be made on sizes as small as 100 mesh, but up to the present, this may be considered exceptional. Depending upon the type of medium used, the specific gravities of separation can be varied within wide limits, up to as high as 2.70, if magnetite is used as medium. Early Development: The development of the Dutch State Mines cyclone as a separator, or cleaner, was the outgrowth of early experimental work by Dries-sen' and others in Holland, just prior to World War 11, in the course of which was discovered the effectiveness of the cyclone in reclaiming and thickening the dense medium used in the "Loess" process of

Jan 1, 1951

By Enrique Touceda

For a number of years prior to the world war, the firm of Geo. H. Thacher & Co., of Albany, N. Y., was engaged in the manufacture of marine and other gray-iron castings. At the outbreak of the war the firm decided to specialize in the manufacture of propeller wheels. It attacked the problem, therefore, from a foundry point of view, seeking to produce a casting that would be so accurate that no subsequent machining would be required on the blades, also from the point of view of the ship builder. There were two general methods of manufacture, the shortcomings of which have been freely acknowledged. In the sweep method, the nowel, or bottom half-mold, for each blade is swept up by a spindle beam and pitch race, while the top half-mold for each blade is built up individually. In the pattern method one individual blade, with the hub or hub portion, is mounted on a spindle and the individual blade mold formed, the pattern is then rotated on the spindle to the position for the next blade, etc. In rare cases wheels were made from a solid pattern. Owing to the cost of the pattern, its failure in many instances to be correctly made, and (when made of wood) its early and sure distortion the disadvantage of this pratctice is obvious, while metal patterns in most instances were prohibitive in cost. In these methods both green-sand and loam molding was practiced. The casting produced by either method can be considered only as a blank from which the propeller must be machined. The back surface of each blade must be chipped to the templet and through this procedure chipped to such accuracy as will be required for a static balance. Inasmuch as the work done by the machine tool is confined to the driving face of the blades, not only is perfection most difficult, but corrosion will be greater because of the removal of the dense skin of the casting and the local strains set up by the pneumatic tool in chipping. To produce a finished 9-ft. propeller for a Navy destroyer required from 8 to 21 days of foundry work and about the same length of time for the machining. Through the use of the Thacher process, only as many hours are required, besides it is possible to produce a finished casting in perfect conformity with any particular propeller-wheel design.

Jan 1, 1922

By Enrique Touceda

For a number of years prior to the world war, the firm of Geo. H. Thacher & Co., of Albany, N. Y., was engaged in the manufacture of marine and other gray-iron castings. At the outbreak of the war the firm decided to specialize in the manufacture of propeller wheels. It attacked the problem, therefore, from a foundry point of view, seeking to produce a casting that would be so accurate that no subsequent machining would be required on the blades, also from the point of view of the ship builder. There were two general methods of manufacture, the shortcomings of which have been freely acknowledged. In the sweep method, the nowel, or bottom half-mold, for each blade is swept up by a spindle beam and pitch race, while the top half-mold for each blade is built up individually. In the pattern method one individual blade, with the hub or hub portion, is mounted on a spindle and the individual blade mold formed, the pattern is then rotated on the spindle to the position for the next blade, etc. In rare cases wheels were made from a solid pattern. Owing to the cost of the pattern, its failure in many instances to be correctly made, and (when made of wood) its early and sure distortion the disadvantage of this pratctice is obvious, while metal patterns in most instances were prohibitive in cost. In these methods both green-sand and loam molding was practiced. The casting produced by either method can be considered only as a blank from which the propeller must be machined. The back surface of each blade must be chipped to the templet and through this procedure chipped to such accuracy as will be required for a static balance. Inasmuch as the work done by the machine tool is confined to the driving face of the blades, not only is perfection most difficult, but corrosion will be greater because of the removal of the dense skin of the casting and the local strains set up by the pneumatic tool in chipping. To produce a finished 9-ft. propeller for a Navy destroyer required from 8 to 21 days of foundry work and about the same length of time for the machining. Through the use of the Thacher process, only as many hours are required, besides it is possible to produce a finished casting in perfect conformity with any particular propeller-wheel design.

Jan 1, 1922

By George T. Wickes

(Washington Meeting, May, 1905.) SEVERAL years ago, Mr. Robert A. Cook described and illustrated in our Transactions 1 a mechanical coke-drawer, patented in 1891 by Mr. Thomas Smith of the Thorncliff Iron Works, Sheffield, England, and first introduced in the United States in, 1896, at the coking-plant of the Latrobe Coal Co., Latrobe, Pa. This machine has not received any very extended application in this country, although it was successfully used in two places for a number of years. The present. paper describes a new and simpler machine, containing few wearing-parts capable of withstanding continued rough usage. Anything which tends to prolong the general use of bee-hive ovens will be welcome to those who are interested in cheapen¬ing the cost of producing coke in such ovens, especially if it provides satisfactory mechanical means, replacing the hard labor involved in drawing coke by hand with the old-fashioned ?duck bill.? The difficulty of finding efficient coke-drawers, especially during the summer season, and in the South, is notorious. Yet, notwithstanding the great improvements that have been made in retort coke-ovens, new bee-hive ovens are continually constructed; and a machine which will successfully compete with hand-drawing, and, at the same time, add to the efficiency of the bee-hive oven, seems to deserve notice. The machine here described was put in operation at the Frick Coal and Coke Co.'s plant, known as Continental No. 1, at Uniontown, Pa., in October, 1904, and is reported to have met successfully all the tests to which it has been subjected. This trial has demonstrated that one of these machines, equipped with an electric motor, and operated by one mart with an assistant, besides two men to " water down " the

Jul 1, 1905

By Francis O. Blackwell

There are few industries in which power is more important to successful operation than mining, and none in which it is so difficult to ohtain power cheaply. Fuel is usually expeusive in mining districts, ana the ma chinery may be widely scattered and located in places difficult of access. The work is often so intermittent and variable as to prevent the economical use of steam. Mining operations are likely to exhibit accumulations of comparatively small and inefficient engines, numerous boilers and long lines of wasteful steam-pipes. Conlpressed air, as a means of transmitting power, is so handicapped by losses in the compressors and piping that it is limited to short distances and to the operation of apparatus requiring power, without regard to cost. To-day, electricity is rapidly replacing other methods of power-distribution, primarily because it is practically independent of distance. By selecting a potential proportional to the length of transmission, the cost of electric conductors and the e5ciency are the same for all distances within reasonable limits. For instance, a given amount of power can be delivered either 528 ft. away at 100 volts, or 50 miles at 50,000 volts, with the same total of copper per H.P. and with exactly the same loss of power in the transmissioo-circuk. This independence of distance permits the selection of the place most advantageous for power-development as a site for an electric power-plant, and the co~~centration there of the generation of all the power required within a radius of many miles. The powel.-site may be at a fall of water, if one is available, or a steam-plant can be built where fuel and supplies are cheapest, or where suflicient water is available for boiler-feed and condensing purposes.

Jan 1, 1904

The Institute conducts jointly with the American Society of Civil Engineers, American Society of Mechanical Engineers and American Institute of Electrical Engineers, certain activities as listed below, and is joint owner with them of certain properties. United Engineering Trustees, Inc. When Mr. Carnegie made his gift which made possible a home for the engineering societies, a separate corporation was organized to act as a holding company and to manage the common property. This was long known as the United Engineering Society but the name has now been changed to one which more nearly reflects the real function of the corporation. It holds title to the Engineering Societies Building and to various funds placed in its charge and is managed by a Board of Trustees of which three are chosen by each of the four societies, American Institute of Mining and Metallurgical Engineers, American Society of Mechanical Engineers, American Institute of Electrical Engineers and American Society of Civil Engineers, which own equal and undivided interests in the property. The land and building cost two million dollars. The interest of each of the Founders societies, aside from especial trust funds, is now valued at $493,352. The A. I. M. E. trustees are Arthur S. Dwight, J. V. N. Derr and George D. Barron. The President of the Board is Francis Lee Stuart and the Secretary, Alfred D. Flinn.

Jan 1, 1923

By A. Gatti

Studies were made on the system iron plus alumina. Various methods of dispersing and various amounts of alumina were used. Powder metallurgy techniques were used to produce the final product. Microstructures and some mechanical properties are presented. Alloys containing up to 16 pct alumina by weight are ductile at all temperatures tested. The ivon-alumina materials have a higher yield stress and improved creep resistance over that of pure iron. SINCE the development of SAP' an A1- Al2O3 powder metallurgy product, great interest has been shown in the development of a SAP-like structure in metals and alloys other than aluminum. The outstanding properties of this class of materials are: 1) Good creep resistance at high temperature. 2) High yield strengths and high hardness at high temperatures. 3) High recrystallization temperature. However, the lack of ductility and formability has thus far limited the applications of SAP-like materials. The following report deals with methods of dispersing A12O3 in Fe, processing of powders into rod, structures produced after processing, and mechanical properties of the iron-alumina material produced. Methods of dispersing the alumina and also the volume fraction of alumina added were varied. MATERIAL Powder Processing— Four methods of obtaining dispersions of alumina in iron were studied. 1) Oxidation-reduction of a Fe + 8 pct Al alloy. .2) Coprecipitation of Fe(OH)3 + Al(OH)3 from aqueous solution. 3) Colloidal mixing of Fe,O3 and Al2O3. 4) Colloidal mixing of Fe powder and A1,O3. Fig. 1 is a processing flowsheet which outlines the processing steps taken to produce a final extruded bar 1/4 in. in diameter and about 30 in. long. The - 100 mesh iron-aluminum alloy was oxidized by placing a thin layer of powder on an alumina plaque. The reduction step was modified to include 1/2 hr at 1000°C since the powders tended to become pyro-phoric unless sintered slightly after low-temperature reduction. Compacting was done in a 1-1/8-in.-diam pressing die. The slugs produced averaged 1 in. in length. The billets were encased in low-carbon steel cans shown schematically in Fig. 2. The blank is included for structure and property comparison purposes. TESTING PROCEDURE All tests were made on as-extruded material.

Jan 1, 1960

By D. Harker, M. J. Murphy

The mechanism by which age-hardening takes .place is still not completely understood. The principal theories range from the extreme of "precipitaiion-hardening" to that of "order-hardening," with many intermediate gradations. In the hope of obtaining new data on which to base a choice among the many theories, the authors have made electron micrographs of formvar replicas taken from metallic specimens at various stages of age-hardening. The results so obtained on an alloy of 2 per cent beryllium in copper and one of 20 per cent molybdenum in iron will be described in the following pages, as well as the technique used in preparing the replicas. Preparation of Formvae. Replicas of Metallic Specimens This section is concerned with the techniques that have roved successful in preparing formvar replicas for studying the microstructure of metals with the electron microscope. Because of its simplicity and accuracy, the formvar replica1 method developed in the General Electric Research Laboratory has been used exclusively, since it is much simpler than the silica replica method of Heidenreich and Peck2 and produces as good results. The formvar method to be described requires a technique acquired only by practice, and no foolproof set of rules can be given. it is a rapid method and a replica can be obtained in less than five minutes under favorable conditions. This does not mean that perfect replicas can be produced every five minutes, but rather that one can well afford to take several strippings* in order to produce a replica of high quality. The metallographic technique required for replica work—very fine polishing and etching with very dilute solutions—is described here. It can be said, in general, that almost any surface that has been carefully prepared for a photomicrograph at 1000 or more diameters can be used to obtain a replica for the electron microscope. Preparation of Metallographic Specimens The preparation of the metallographic specimens is somewhat more exacting than that usually given to samples to be used for inspection under the light microscope. After much experimentation, it was concluded that the best method consists in polishing the metal through to the coarse cloth, then etching and repolishing on final cloth until the layer of distorted metal is removed. After this procedure has been completed, a dilute etch—to approximately the depth necessary for a micrograph at 1000 diameters—usually produces a sur-

Jan 1, 1945

By R. S. French

The purpose of this paper is to present data that have been obtained during the past two years concerning the effects of prior cold-work and temperature and time of anneal upon the recrystallization and grain growth of 70-30 cartridge brass. It was desirable to study certain of these phases so that an accurate picture of the principles of the subject could be shown. The work is not intended to provide explicit annealing data, but to provide material examples that may help to clarify analogous problems concerning this alloy. Specifications often set limitations upon the grain size of annealed materials because of the importance of grain size upon subsequent manufacturing operations. It was, therefore, worth while to study the variables that affect the recrystallized grain size of this material. C. H. Mathewson and A. Phillips,l W. R, Webster,2 and others have presented annealing characteristic curves of this alloy. A recent typical curve presented by R. S. Pratt3 is shown in Fig. I. The tensile properties and grain sizes are shown as functions of the annealing temperature. Such curves serve as a useful guide in determining the physical properties of annealed material, but as they are made generally under carefully controlled laboratory conditions they do not indicate the performance of metal annealed in a mill muffle, where such conditions as amounts of metal, heating time and temperature may differ. Study of the effect of time and temperature upon grain growth and subscquent recrystallization was made with a coil of metal having the following analysis: 70.04 per cent copper; 0.007 lead; 0.007 iron; 0.00 tin; 0.00 silicon; 0.001 nickel; 0.000 phosphorus; balance zinc. The sample coil was obtained from metal that had been rerolled from hot-rolled mill stock, and was received at 0.228-in. gauge, soft, with a grain size of 0.125 mm. This material was then rolled 43.5 per cent to 0.129-in. gauge and annealed to a 0.053-mm. grain size. In this condition, samples were cut and used in all of the experimental work reported in this paper. Time The first study was of crystal growth at a constant temperature over a moderate length of time. Material was cut from the stock coil at 0.129-in. size and rolled 75 per , cent hard to 0.032-in. gauge. From this piece small samples were cut M by 2 in., suitable for grain-size determina.tions. Twelve samples were placed in an electric furnace uniformly across the width, approximately an inch from the floor. A thermocouple was wired to the center sample, so that the approximate metal temperature could be followed. At various

Jan 1, 1944

By R. S. French

The purpose of this paper is to present data that have been obtained during the past two years concerning the effects of prior cold-work and temperature and time of anneal upon the recrystallization and grain growth of 70-30 cartridge brass. It was desirable to study certain of these phases so that an accurate picture of the principles of the subject could be shown. The work is not intended to provide explicit annealing data, but to provide material examples that may help to clarify analogous problems concerning this alloy. Specifications often set limitations upon the grain size of annealed materials because of the importance of grain size upon subsequent manufacturing operations. It was, therefore, worth while to study the variables that affect the recrystallized grain size of this material. C. H. Mathewson and A. Phillips,l W. R, Webster,2 and others have presented annealing characteristic curves of this alloy. A recent typical curve presented by R. S. Pratt3 is shown in Fig. I. The tensile properties and grain sizes are shown as functions of the annealing temperature. Such curves serve as a useful guide in determining the physical properties of annealed material, but as they are made generally under carefully controlled laboratory conditions they do not indicate the performance of metal annealed in a mill muffle, where such conditions as amounts of metal, heating time and temperature may differ. Study of the effect of time and temperature upon grain growth and subscquent recrystallization was made with a coil of metal having the following analysis: 70.04 per cent copper; 0.007 lead; 0.007 iron; 0.00 tin; 0.00 silicon; 0.001 nickel; 0.000 phosphorus; balance zinc. The sample coil was obtained from metal that had been rerolled from hot-rolled mill stock, and was received at 0.228-in. gauge, soft, with a grain size of 0.125 mm. This material was then rolled 43.5 per cent to 0.129-in. gauge and annealed to a 0.053-mm. grain size. In this condition, samples were cut and used in all of the experimental work reported in this paper. Time The first study was of crystal growth at a constant temperature over a moderate length of time. Material was cut from the stock coil at 0.129-in. size and rolled 75 per , cent hard to 0.032-in. gauge. From this piece small samples were cut M by 2 in., suitable for grain-size determina.tions. Twelve samples were placed in an electric furnace uniformly across the width, approximately an inch from the floor. A thermocouple was wired to the center sample, so that the approximate metal temperature could be followed. At various

Jan 1, 1944

By Chung Yu Wang, Guy C. Riddle

There are found in nature upward of II2 minerals containing antimony, but only a few of them, listed in Table I, can be considered as antimony ore-forming minerals. Stibnite (Sb2S3), antimony sulphide or glance, is the principal ore of antimony. The oxide ores—cervantite, kermesite, valentinite, sernarmontite—occur sparingly in nature. Dry methods are generally adopted for the extraction of the metal. Electrometal-lurgical methods have had much attention in America and Germany and have not yet found, on economic grounds, practical or extended application, except in a few places. During recent years, treatment of the poor grades of the ore, especially sulphide, by ore-dressing methods, has commanded some attention and been adopted at a few plants. The impure sulphide of antimony, resulting from the liquation process, is called lLneedle," "liquated" or "crude" anti- mony, and the refined metal itself is called antimony "regulus." The different processes for the treatment of antimony ores are shown in the diagram of Fig. I. Liquation of Crude Antimony The first step in the smelting of antimony is a simple one, the process of LLliquation," which produces crude or needle antimony. Ores containing $ 50 per cent Sb are used in the liquation process for the production of crude. The temperature required for liquation is between 550' and 600°C. Ores to be liquated are broken to about walnut size. If the pieces are larger than this, the low heat used will not penetrate' effectively, and if they are smaller the ore tends to pack too closely for adequate penetration. A packed charge also prevents the free escape of the fused sulphide. Intermittent Liquation in Crucibles The unique type of furnace that is in use in China for smelting is not highly efficient but is simple in construction and operation. The furnace is generally built

Jan 1, 1944

By W. O. Philbrook, R. H. Spitzer, F. S. Manning

A generalized mathematical model has been developed to describe the kinetics of the gaseous, topo-chemical reduction of porous hematite spheres. Gas-solid reduction is permitted at each of three advancing interfaces and is controlled by a complex series-parallel sequence of chemical and transport steps. Despite the fact that transport resistances are significant to the advance of each interface, little deviation from linear advance is predicted for the first 98 pct of reduction. Calculations to predict the movement of magnetite /wustite interface by a solid-state diffusion mechanism have been incorporated into the earlier dense-pellet model.' The porous-pellet model is found to give a better description than the dense-pellet one for McKewan's measurements2 of interface movements in dense polycrystalline hematite reduced in hydrogen-water vapor mixtures. THIS paper reports a continuation of work"3" directed toward the better understanding of gas-solid reactions and the development of mathematical models that may be helpful in the design or control of ore-reduction processes. Laboratory studies of the reduction of single oxide samples in tube furnaces normally employ an abundant excess of pure reducing gas. Reduction may appear to be adequately described by a model assuming gas-solid reaction solely at the iron/wustite interface.''' However, when iron ore is reduced in either a fixed bed or an efficiently operated counter-current column, there are portions of the bed where the partially spent gas is no longer capable of reducing wustite to iron. Nevertheless, the formation of the intermediate reaction products, wustite or magnetite, can and does continue. In order to account for this aspect of the reduction of beds of particles, three semiempirical mathematical models were devised.' One of these was for the limiting case of completely dense particles, and two alternatives were provided for porous particles. For purposes of the analysis, a dense pellet was defined as one in which the wustite and magnetite layers were impervious to the reducing gas when the atmosphere was capable of forming iron. In a porous pellet, the intermediate product layers were assumed to be sufficiently permeable to allow reducing gas to penetrate beyond the iron/wustite interface to form wustite and magnetite by removal of oxygen as a gaseous product rather than by a solid-state redfiction mechanism. Further progress required a better understanding of the reaction of the individual particles with the gas stream. A comprehensive mathematical treatment was developed' to describe the continually changing interplay of transport and reaction steps

Jan 1, 1967

By J. Lindbo, B. Vigeholm

IN transmission electron microscopy, specimen thicknesses quoted are frequently based upon either traditionally familiar values or a few evaluations representing the whole material. Taking aluminum in 100 kv TEM as an example, average and maximum values are widely accepted as being 2000 to 2500 and 6000 to 7OOOÅ, respectively. It is the purpose of this note to revise these figures and to point out the importance of evaluating individual specimens carefully. All evaluations have been based upon slip trace widths and lattice orientations as determined from diffraction patterns. In many cases where two or more slip systems have been operating the geometrical method described by Crocker and Bevis1 has been applied as a check. The foils were usually oriented to within 2 deg from the exact Bragg angle. Kikuchi patterns were used as indications of correct orientations but not applied in the evaluations. The tilt of the foil surface relative to the beam normal may with certain geometrical relations between the tilt axis and the operating slip plane lead to substantial errors.2'3 Where these geometries were inevitable the samples were omitted in the investigations. Various measures were taken in order to overcome ambiguities, e.g., comparison with neighboring grains, tilts, evaluations based upon two or three slip systems,' and comparison with extinction contour evaluations where s = 0 conditions were obtained. Errors caused by misinterpretation of the slip traces on a micrograph are easily avoided by considering the bright-dark sequence on opposite surfaces and by taking into account the tapering of the foil usually leading to a distinguishable divergence of the pair of traces. In the investigations described here the interpretation was further facilitated as the slip trace formation was observed on the microscope screen and sketches taken down. In a few observations slipping was so violent that the distinction of pairs was considered dubious and consequently given up. To assess average values, thickness evaluations carried out in two independent investigations were analyzed: I) 99.998 pct A1 extruded, cold-drawn, and recrys-tallized to grain sizes between 35 and 500 um were deformed in tension at room temperature. In order to determine the dislocation densities as a function of strain,4 specimens prepared by spark machining and electropolishing in a PTFE holder were analyzed in the electron microscope at 100 kv. Thicknesses were evaluated for 569 selected areas. Histogram I in Fig. 1 shows the results, the average thickness being 4900Å. II) Electropolished specimens prepared from 99.9999 pct A1 with magnesium contents from 0.005 to 0.5 pct rolled to foil and annealed were subjected to fission fragment irradiationa2 For volumetric dose and defect concentration determinations thickness evaluations were performed on 123 areas. Histogram II in Fig. 1 shows the thicknesses of these areas averaging 4250Å. Whereas in investigation I no selection related to thickness has been made, some thin as well as thick areas have been omitted from I1 for experimental reasons. This and the application of two different microscopes although of the same type may account for the difference in average thickness. Assuming a mean error of 10 pct for a single evaluation, the error of the average should be negligible. In order to investigate the maximum transmissible foil thickness in aluminum, specimens were prepared from single crystals with (111) and (110) orientations parallel to the beam, and from polycrystalline material. Maximum values of thickness that could be measured were given by the stopping of the dislocations. The visibility often extended far beyond the end of the slip trace, but with no means of knowing the

Jan 1, 1970

By G. Derge, W. Peifer, J. H. Richards

INTRODUCTION A WIDE variety of metallurgical defects in steel have commonly been attributed to the presence of excessive amounts of hydrogen. These defects include flakes in rails and forgings, cracks in welds, and blisters in enameled ware. They have been related to hydrogen largely by circumstantial evidence because the proper sampling and analysis of steel for hydrogen has been known to be difficult and because no general agreement has existed with regard to the relative suitability and accuracy of available methods. The need for a direct approach to these problems has been widely recognized. This general situation has been well described in the publications of the British Committee on the Heterogeneity of Steel Ingots,1 and current approaches to the problem were reviewed in a recent symposium of the AIME.12 The plans described by the present authors at that meeting have now matured satisfactorily and will form the basis of this paper. The principle object of this paper will be to describe the methods of sampling and analysis which have been developed and to illustrate the usefulness and limitations of these methods by citing their application to a specific problem. The first problem selected for investigation was the behavior of hydrogen in rail steel. This was chosen because the occurrence of shatter cracks in rails has received a great deal of study over a long period of time. The defect can be controlled by the expensive procedure of slow cooling. However, it may be hoped that a better understanding of the factors influencing the hydrogen content of rails will lead to a more efficient control of this problem. Rails provide a good starting point for a more general study of hydrogen in steel because they provide a cross section large enough to develop cracks, yet small enough for convenient handling and sampling. Rails were also selected because they are made from plain carbon steel and it was felt that the initial work should not be complicated by the effects introduced by alloying elements. The considerations which determined the original planning of this study should be reviewed. The inherently complex nature of most hydrogen problems requires that a large amount of data must be collected for any particular case. This in turn means that any analytical procedure should be as rapid and simple as possible. The same objective of speed is indicated by the fact that it may finally become desirable to use hydrogen analysis in process control. It is also known that hydrogen is highly fugitive and that any procedure which facilitates early analysis of the sample without prolonged or irregular storage has distinct advantages. The most important previously reported methods of analysis may be classified into three general groups: (I) Vacuum fusion. (2) Vacuum extraction (without melting). (3) Total combustion.

Jan 1, 1948