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By E. R. Dean

A wire-feed mechanism has been employed to fabricute metal alloy film resistors to various sheet resistivities on oxidized silicon substrates. The effect of several thousand hours storage in air at elevated temperatures on the resistance and temperature coefficient of resistance is presented. Unprotected films of- sheet resistivity between 100 and 500 ohms per sq fabricated at 300°C substrate tenzperatures were unstable when stored at 150°Cfor extended periods. The higher sheet resistivity films exhibited the greatest instability; however, even the 100 ohms per sq films drijted excessively for device application. When stored at still higher temperatures, the normalized resistance increases to maximum, then decreases until a minimum value is obtained, then finally increases in resistance until open. The use of a protective overcoating of SiO has had considerable benejicial effects on the film stability, so that 250 ohms per sq films deposited on 300°C substrates are now stable after 1000 hr storage at 250°C and possess a temperature coefficient of resistance less than 200 ppm per C. The use of a low substrate temperature during depositon (100°C) enables the preparation oj resistors with very low tenperature coefficients of resistance (10 to 20 ppnl per 'C). However, these films are less stable than their higher substrate temperatuve counterparts. During extended storage, the resistance of the protected films always decreases with lower substrate films exhibiting larger normalized resistance decreases. This resistance decrease is accompanied by a linearly related increase in the temperature coefficient of resistance. The electrical behavior of these films may be explained by postulating That the structure of the films is in the transition region between thick continuous films and ultrathin island structure films so that the conductivity is the restlt of both electron scattering and tunneling-activated charge carrier creation between neighboring grains. The annealing behavior when thermally aged is the result of defect anneal, grain growth, and selective oxidation. TheRE is a considerable interest in thin metallic films for use as resistor elements in microelectronic circuits.1,2 These resistor films must be stable when exposed to elevated-temperature storage or operating ambient, possess low temperature coefficients of resistance (hereafter referred to as T.C.R.), and be of a high enough sheet resistivity to be useful. The resistivity and T.C.R. of a thin metallic film are determined by the structure and thickness of the film. Hence the stability of the film when exposed to stress would depend on the stability of the structure. The resistivity of a thin film is the result of the electrons' interaction with the lattice vibrations (electron-phonon scattering), scattering of electrons due to impurities, defects, and grain boundaries and specula reflection from the film surfaces.3' All of these effects serve to reduce the electron mean free path and result in a resistivity higher than the ideal bulk. In ultrathin films possessing essentially an island structure consisting of a planar array of aggregates separated by a few to a few tens of angstroms, conduction is dominated by a combination of tunneling and activated charge carrier reation. Thin films would be characterized by relatively low resistivity, positive T.C.R., and reasonable structure stability whereas ultrathin films possess unstable structures, negative T.C.R., and exhibit high resistivity. Feldman6 has investigated films intermediate between the two regions and postulates that the resistivity of a film in the transition region is composed of two linearly additive parts: that due to the resistance of the grains and that due to the gaps. The grain resistivity would represent the scattering of the conduction electrons by defects, surfaces, and phonon interaction while the gap term represents the tunneling contribution. For gold and platinum films, he found as the film structure becomes progressively less continuous, corresponding to thinner films, the absolute value of the T.C.R. becomes progressively smaller until negative values are observed with respective zero T.C.R.'s at about 35 and 150 ohm per sq, respectively. Recently the author7 investigated the behavior of a multicomponent alloy of nickel, chromium, and iron and found the T.C.R.'s of these films decrease with decreasing substrate temperature during deposition. The lower T.C.A. associated with lower substrate temperatures was attributed to an increased contribution to the total resistivity from the negatively temperature-dependent gap tunneling since it is well-known that thin films deposited on low-temperature substrates consist of a higher density of smaller grains than the same sheet resistivity films deposited on higher-temperature substrates. Under conditions of thermal anneal, the author found that, when various sheet resistivity films fabricated at 300°C substrate temperature are exposed to extended storage in air at 300°C, the thinner films increase in resistance until open, while the thicker films

Jan 1, 1967

By D. R. Uhlmann, T. P. Seward, K. A. Jackson, J. D. Hunt

microscopic ohservations on alloys of organic trzaterials show that dendrite arms can melt off under normal conditiorzs of growth. This occurs because of the interactiorz of' heat and matter fluxes during dendritic growth. The re melting occurs where the den-drite arms are joined onto the main deizclrite sterrz. Many detached crystals can be produced in this fashion. It is postulated that this remelting phenornenon occurs in metal alloys, giving rise to the equi-axed region in castings. Experiments peyformed orr castings of transparent materials support remelting as a primary source of detached crystals. Ob~ervations an equiaxed tones in metal castings are discussed in terms of this and other mechanisms. It is concluded that the partial remelting of dendrites is on important mechanisnl for producing the equiaxed regions in castings. THE freezing of a casting can be divided into three regions: a chill zone formed near the mold wall, a columnar region, and a third region, at the center of the casting, which is called the equiaxed zone. The origin of the grains that comprise the equiaxed region is the subject of this paper. We will first outline the mechanisms which have been proposed to account for the origin of the equiaxed region and discuss some recent experiments which cannot be explained by these theories. We will then present some microscopic observations of dendritic growth which have led us to conclude that the equiaxed zone in castings can arise from partial remelting of dendrites. This proposal is supported by observations on transparent castings. Finally, we will discuss several observations on metal castings which could not be explained previously, and which can be accounted for by the present proposal. Previous Mechanisms. Winegard and Chalmers3 pointed out that the molten central region of an ingot could be constitutionally supercooled, because of the solute layer at the growing interface. In this supercooled region, nucleation on particles could occur, giving rise to the equiaxed crystals. Another mechanism has also been suggested,4y5 that the nuclei originate in the chill zone then float or are carried by convection to the center of the casting, where they grow to produce equiaxed crystals. In this case, all the crystals nucleate immediately on casting, so this mechanism will be termed "big-bang" nucleation. Walker's Experiments. J. L. Walker has made observations on the solidification of nickel and Ni-Cu alloys which cannot be accounted for by either of the above mechanisms. In studying the grain size resulting from freezing of nickel at various undercoolings, walker6 found that at large undercoolings the grain size was small, due to mechanical nucleation, as discussed by walker7 and Horvay.' At small undercoolings, the grain size was large, and the growth dendritic. In Ni-Cu alloys, however, for initial undercoolings starting from just below the melting point and extending for a hundred or so degrees of undercooling, fine grains were also observed. Samples were undercooled 200 Centigrade degrees without nucleating, and were then heated 130 Centigrade degrees so that the undercooling was 70 Centigrade degrees, and nucleated. The samples had a small grain size, indicating multiple nucleation. There were no heterogeneous nuclei in the liquid which could operate at the temperature of growth. Constitutional supercooling could not have been greater than the supercooling of the initial melt, since the temperature rose as the freezing continued. walker -as also shown that a Ni-Cu alloy which can be undercooled to below its solidus will produce typical columnar and equiaxed regions when cast into a cold mold. This alloy could not reach a temperature below its solidus by constitutional supercooling. It could not, therefore, have nucleated heterogeneously. Neither the big-bang mechanism nor the Winegard-Chalmers mechanism can account for the fine grain

Jan 1, 1967

By N. N. Breyer

A specially built "hard" tensile machine with characteristics permitting the precise detertnination of the drop of the load at the yield point has been used to study the magnitude of the yield-point phenotnenon in prestrained martensitic 4340 steel. A new phenonzenon, the appearance of a secondary yield point, has been observed by holding the specimen at constant strain in the plastic region. Furthermore, it has been found that a series of yield-point drops could be introduced by successive constant strain holds in the plastic region. The isothermal kinetics of the development of the secondary yielding point lave been studied at four temperatures: 24° 0° -18°, and -79°C. From the results of the kinetic investigation, equations for the In a previous investigation1 it was shown that, contrary to generally held opinion, steels of medium carbon content, such as 4340, 4140, and 86B30, in the as-quenched martensitic condition, can be cold-drawn through a die with reductions in area of up to 10 pct without cracking. Tensile specimens of 4340 machined from bars quenched and prestrained in this manner exhibited tensile strengths of about 400,000 psi coupled with 30 pct reductions in area. In addition, it was found that each sample of such steels exhibited a yield point in the quenched, cold-drawn condition. Since these studies were conducted on a commercial hydraulic testing machine of a type which is not well-suited to detailed study of yield-point behavior, it was decided to study this phenomenon more thoroughly on a rigid straining machine. In this new investigation, use of such a "hard" machine not only allowed study of the magnitude of the yield-point drop but also revealed a new phenomenon—secondary yielding of the martensite introduced by stopping crosshead motion after plastic deformation of the sample had begun. The present paper is a report of these findings. MATERIALS AND PROCESSING The material used was a commercial 4340 steel of the composition shown below: 0.41 0.80 0.013 0.019 0.31 0.85 1.76 0.28 1 0.42 0.77 0.015 0.024 0.30 0.84 1.69 0.28 0.08 2 1 = Ladle analysis. 2 = Laboratory analysis. Bars of this steel were processed in the following way: 1) machined to predetermined diameters; 2) austenitized at 870°C for 1 1/2 hr; 3) oil-quenched; 4) cooled to -115°C for 1/2 hr; onset and increase in magnitude of the secondary yielding in this temperature region have been found to fit the relationship ?Ys = Atn where ?Ys is the magnitude of the secondary yield Point in psi, t is the time in seconds, and A and n are parameter characteris-tics of the material. Although the occurrence of the primary and secondary yield points could be rationalized qualitatively on the basis of stress-induced ordering of carbon atoms in the stress fields of dislocations, as postulated in an earlier paper, the kinetics of the secondary-yield-point development were interpreted to indicate that the ordering involves more than just single jumps of carbon atoms from high-energy to neighboring low-energy sites. 5) pickled and lime-coated; 6) drawn through a carbide die. The predetermined diameters were chosen so that drawing through the same die gave the various reductions desired. Tensile specimens of 0.252 in. diam with a 1 1/4 in. gage length were then prepared from the drawn bars and tested. In order to study the stress-strain behavior at the yield point in detail, a rigid tensile machine with a high spring constant was constructed. Columns of large cross section (relative to the specimen cross section) constituted the machine frame. A dc motor was used to drive a screw via a gear reducing train and a "crane" thrust bearing. In this relatively simple device small deformations could be observed un-blurred by the slow response and lower spring constant inherent in hydraulic machines.' A strain-gage dynamometer permitted load changes as small as 8 lb to be read. RESULTS Tensile test samples machined from bars in the as-quenched condition with no subsequent drawing and samples from bars with 3.8 pct reduction after quenching gave stress-strain curves typified by those shown in Figs. I and 2. The time lapse between predrawing and tensile testing varied but usually ranged between 3 to 6 days at room temperature. The strain rate during testing was 0.003 in. per in. per min. The as-quenched curve is seen to have a broad serrated maximum whereas the stress on the specimen prestrained 3.8 pct rose linearly to point A, Fig. 2, fell abruptly to B, and then gradually to C. The abrupt drop to B was accompanied by evidence of incipient necking. The drop of the stress at the yield point in the prestrained samples (A to B in Fig. 2) changed with the percent prestrain, as illustrated on Fig. 3. Although the tensile strength increased continuously with the amount of previous cold drawing, the magnitude of the yield point drop first increased—up to about 6 pct prior reduction—and then decreased. Specimens from bars predrawn more than 8 pct broke in a brittle fashion in the elastic portion of the stress-strain curve.

Jan 1, 1967

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 E. R. Parker, R. H. Thielemann

The conventional short-time tensile test provides a reliable means of predicting the sustained load-carrying capacity of steels only when the temperature is such that continuous plastic flow does not occur. At elevated temperatures, stresses considerably less than the short-time rupture value may produce continuous flow, with fracture occurring only after long periods of time. The amount of flow or creep accompanying failure varies for different steels, and depends, to a large extent, on the temperature and the duration of the test. Service records of cracking stills, steam superheaters and high-temperature boilers have shown that brittle fractures sometimes occur with little or no warning. In installations of this type, localized stresses are often encountered, and steels must be capable of withstanding a certain amount of deformation without fracture. The sustained-load rupture test determines the expected life and corresponding ductility of steels at various stresses and temperatures. It also yields additional information regarding the effect of micro-structure and metallurgical stability on the high-temperature properties. Present Status of Sustained-load Rupture Test The sustained-load rupture test conducted at elevated temperatures is not entirely new. Dr. Zay Jeffriesl presented in 1919 the results of a large number of rupture tests made on copper, iron and tungsten. These tests were made with various strain rates and at temperatures ranging from the boiling point of liquid air to 1000° C. At that time he observed the interesting phenomenon characteristic of metals, that a temperature exists below which a metal is ductile and breaks with a transcrystalline fracture (through the grain) and above which the metal is brittle and breaks with an intergranular fracture (through the grain boundaries). He observed that this temperature varied with the testing speed, and that a minimum temperature, slightly above the recrystallization temperature, existed at which the cohesion of the grains themselves was

Jan 1, 1939

By R. H. Thielemann, E. R. Parker

The conventional short-time tensile test provides a reliable means of predicting the sustained load-carrying capacity of steels only when the temperature is such that continuous plastic flow does not occur. At elevated temperatures, stresses considerably less than the short-time rupture value may produce continuous flow, with fracture occurring only after long periods of time. The amount of flow or creep accompanying failure varies for different steels, and depends, to a large extent, on the temperature and the duration of the test. Service records of cracking stills, steam superheaters and high-temperature boilers have shown that brittle fractures sometimes occur with little or no warning. In installations of this type, localized stresses are often encountered, and steels must be capable of withstanding a certain amount of deformation without fracture. The sustained-load rupture test determines the expected life and corresponding ductility of steels at various stresses and temperatures. It also yields additional information regarding the effect of micro-structure and metallurgical stability on the high-temperature properties. Present Status of Sustained-load Rupture Test The sustained-load rupture test conducted at elevated temperatures is not entirely new. Dr. Zay Jeffriesl presented in 1919 the results of a large number of rupture tests made on copper, iron and tungsten. These tests were made with various strain rates and at temperatures ranging from the boiling point of liquid air to 1000° C. At that time he observed the interesting phenomenon characteristic of metals, that a temperature exists below which a metal is ductile and breaks with a transcrystalline fracture (through the grain) and above which the metal is brittle and breaks with an intergranular fracture (through the grain boundaries). He observed that this temperature varied with the testing speed, and that a minimum temperature, slightly above the recrystallization temperature, existed at which the cohesion of the grains themselves was

Jan 1, 1939

By Frank Tolonen

IRON-ORE beneficiation is becoming of vital importance to the Lake Superior region, since only a few decades will be needed to exhaust the direct shipping ores even if generous allowances are made for discoveries of new orebodies. If the region is to continue as the chief source of ore to the steel industry of the United States, it must concentrate or otherwise beneficiate the enormous tonnages of available iron formations. A beginning along this line has already been made. About one-fifth of the total shipment, even now, is the product of some sort of concentrating process, while another fifth is improved in physical structure by crushing, screening, drying, sintering, or some other similar method. The amount of material amenable to these processes is limited, however; and, in order to be able to utilize the billions of tons of iron formations that cannot be so beneficiated, an intensive study of their nature and concentration possi-bilities is necessary. As long as high-grade ores are available in ample quantities, ore dressing is economically impossible, but as soon as the supply nears exhaustion it becomes necessary. At first the products of ore dressing must meet as nearly as possible the same specifications as the rich ores in order to be adapted to the reduction processes already established. The future requirements as to quality will depend on the one hand upon the ability of the ore dresser to eliminate undesired constituents and charac-teristics in the material, and on the other upon the adaptation of the reduction processes to the product that can be economically supplied. A better understanding of the blast furnace and other reduction reactions, and improvements in the preparation of raw materials, should enable the Michigan districts to continue to supply ore for a long time to come. The study and testing of the iron formations necessary to bring a utilization of the low-grade ores, though requiring time and effort on the part of all concerned, should not be postponed, especially since the economic situation forces the use of the highest grade ore in preference to the leaner material.

Jan 1, 1933

By Roland D. Parks

Corundum, little publicized as an industrial abrasive, has, in its small way, contributed greatly to the production of many specialized items vital to our war program and to Our allies. Optical elements Of the highest quality for range finders, bombsights, and scientific instruments; precision metal parts for torpedoes and airplane engines; quartz crystal plates for military radios; armorplate and malleable castings for tanks and guns; and eyeglasses for everyone; these are some Of the products that corundum has helped to produce in the quantities needed and on time. Unlike metals and many other raw materials, corundum is not incorporated into any Of these finished products. It is simply a grinding medium used to produce the desired finish or precision; an operating supply or tool, so to speak. With a Mobs' scale index of 9, corundum ranks next to the diamond in hardness among the natural minerals and is superior to emery and garnet. The gem varieties of corundum, including the Oriental ruby and sapphire, are frequently more highly prized as jewels than the diamond. It is the intent Of this paper to deal Only with a description of the corundum industry, the administration of wartime control, and certain economic aspects as seen by the author. Several references are listed to assist anyone who wishes further information on the geological occurrence of the mineral. Ore Production and Consumption For the past two decades, south Africa has been the world's sole producer of corundum ore. A possible exception is Russia, where, it is understood, there was considerable production during the thirties for domestic consumption but for which statistics are lacking. The United States is the world's principal consumer of corundum ore; imports lor the period 1934 through 1940 averaging 3000 Short tons per year, The years 1935 and 1936 were close to the 5000-ton mark, and imports during 1941, the last prewar year for which statistics have been released, were approximately 6000 Short tons. Again lacking statistics on Russia, the United Kingdom ranks second, but far below the United States in consumption of ore. Historically, corundum has been found in some 35 countries throughout the world, but the principal deposits are in South Africa, Canada, Madagascar, Russia and the united States. Deposits are generally small and subject to rapid exhaustion. Thus, the United States was the principal world producer for the period 1870 to 1900, when operations ceased except for two years during World War I. India was a producer of ore from 1898 through 1921, with peak output in 1916 through 1918 Canada came into production in 1901 with substantial output of ore and finished grain until 1914; the production thereafter was smaller until 1921. Madagascar has produced ore since 1910 but has had important output in only a few scattered years. South African production started in 1912

Jan 1, 1948

By Kenneth C. Vincent, A. M. Gaudin

In a study1 of the action of amyl xan-thate on chalcocite in water suspension, it was found that if the xanthate is added in relatively large quantity the xanthate group can be accounted for in three forms: (1) as xanthate ion remaining in water, (2) as benzene-soluble cuprous xanthate on the chalcocite, (3) as a benzene-insoluble coating on the chalcocite. Reduction in the amount of xanthate added leads to disappearance of form I then of form 2. With minute quantities of added xanthate, substantially all the reagent is of the "unleachable" kind. Yet this unleach-able xanthate can be dissolved by pyridine to form a soluble cuprous xanthate complex, and it is sufficient in effectiveness to make chalcocite flotable even if insufficient in quantity to form a complete mono-molecular film on the mineral. In that study it was also found that chalcocite abstracts cuprous xanthate from benzene so1ution, in what may (or may not) be a case of molecular adsorption. It seemed desirable, therefore, to study further the "unleachable" xanthate on the chalcocite, and particularly to ascertain whether it is formed as a result of the benzene leach or is actually formed during the conditioning of chalcocite in aqueous xanthate solution. A 'splendid tool to make such studies has recently been perfected; that is, the use of radioactive spies or tracer atoms. With this tool, it was thought possible to answer the problem stated above, but, unfortunately, this did not prove to be true. Answer to the flotation question was clouded by the existence of rapid and selective diffusion of copper atoms in the solid mineral—a phenomenon that was totally unexpected yet remains interesting and perhaps important. Method of Radioactive Spies The method of radioactive spies is discussed in many places. Two convenient references are the article by Evans2 and the book by pollard and Davidson.3 The method was first developed by van Hevesy and paneth in 1013, when only natural radioactive isotopes were available. These isotopes are few in number, and so the method remained limited in scope. Recently the synthesis of over 350 active isotopes of all the known stable chemical elements4 has opened widely expanded possibilities for the method, A fundamental tenet of the method is that a radioactive atom and a nonradio-active atom are exactly alike until disintegration of the radioactive atom. Then, by its sudden death, the spy reveals its location. The relative abundance of spies at various locations makes it possible to ascertain the relative abundance of the corresponding nonradioactive atoms at the same times and locations. A second fundamental tenet of the method of radioactive tracers is that the radioactivity lies in the nucleus of the atom: transfer of radioactivity from one

Jan 1, 1947

By Donald W. Scott, Nathaniel Arbiter, A. C. Richardson

This paper describes the application of amine flotation to a specific problem—that of increasing the grade of magnetite concentrates derived from an iron ore requiring extremely fine grinding for mineral liberation. Experiments conducted on an iron ore from Wisconsin had shown that concentrates containing 60 to 62 per cent iron and 12 to 14 per cent silica could be produced by magnetic separation. The residual silica occurred as quartz and hornblende, either entrained or locked with magnetite. Most advantageous utilization of the concentrate, however, necessitated that the silica content be reduced to about 5 per cent, equivalent to an iron content of 67.5 per cent. It had been demonstrated that tabling of the magnetic concentrate removed sufficient quartz and hornblende to yield an acceptable concentrate, but disadvantages inherent in tabling dictated that flotation be investigated as a substitute. The goals set for the flotation investigation were: (I) the production of concentrates of about 68 per cent iron content from the magnetic concentrate; (2) an iron recovery of about 85 per cent of that in the feed to flotation; and (3) minimum reagent cost. Both batch and continuous flotation tests were employed; the former, to establish the procedure and the latter to verify it. Although the data were obtained on a specific ore, and with a commercial application in view, it is believed that they have a bearing on other problems where amine flotation is being used or is anticipated. Samples Two samples, designated "(minus 100-mesh magnetic concentrate" and "minus 150-mesh magnetic concentrate," were used for the batch experimental work. They differed only in the degree to which the crude ore was ground prior to magnetic separation. They were stored moist in steel drums in quantities sufficient for all the experimental work reported. This procedure had the advantage of allowing all tests to be made on common samples, but had the disadvantage that the individual flotation samples, because of the difference in storage time, were subject to various stages of surface alteration. Previous work had indicated that common samples were desirable for the batch studies, and it was decided that if these data appeared sufficiently promising the effect of surface alteration could be checked best by continuous tests. The size distributions and the assays of the samples are given in Table I. The minus 150-mesh magnetic concentrate, on which most of the flotation tests were made, assayed 60.9 per cent iron, 13.3 per cent silica, and 0.016 per cent phosphorus. The minus 325-mesh portion represented 78.I per cent of the sample by weight, and assayed 67.9 per cent iron. Thus, the insoluble, mainly silica, was concentrated

Jan 1, 1947

By Robert J. Anderson

DURing the past 5 years no subject has aroused more interest or received more attention among mill operators than flotation. One reason for this is, undoubtedly, the remarkable success of the process in Australia where that country has risen to the position of furnishing one-fifth of the world's supply of zinc. The plant of the Butte & Superior Copper Co., designed by James M. Hyde in 1912, was the first important large flotation plant in this country; other installations have been made since then with considerable frequency, particularly so in the last 2 years. Without going into complete detail, it may be safely said that although flotation is a highly successful commercial process, it is more or less on an empirical basis. Upon scanning the literature, it is found that the flotation investigations have, in the main, dealt with a solution of the problems which accrue to practise; until recently no attempt was made to remove the difficulties in the way of the formulation of a consistent and harmonious theory. Of late this phase of the work has been receiving considerable attention, particularly by the United States Bureau of Mines at its Salt Lake City station, by the Mellon Institute at Pittsburgh, by the General Engineering Co. at Salt Lake City, by many of the mining schools, and private individuals almost ad infinitum. There is, at present, an enormous amount of laboratory work being carried on in flotation research, and probably the time is not far away when a generally acceptable explanation of flotation phenomena can be set forth. However, at this time, it seems as though the current technology is befogged with a superabundance of contradictory evidence; this confusion can only be dispelled as time proceeds and the knowledge of the subject becomes more complete. Many phenomena are supposed to contribute to the flotation of minerals, whether in whole or in part is a mooted question. I shall only sketch roughly the present tendency of ideas and make no reference to the first early and crude notions which have little value other than histori-

Jan 1, 1917

By Roland D. Parks

Corundum, little publicized as an industrial abrasive, has, in its small way, contributed greatly to the production of many specialized items vital to our war program and to Our allies. Optical elements Of the highest quality for range finders, bombsights, and scientific instruments; precision metal parts for torpedoes and airplane engines; quartz crystal plates for military radios; armorplate and malleable castings for tanks and guns; and eyeglasses for everyone; these are some Of the products that corundum has helped to produce in the quantities needed and on time. Unlike metals and many other raw materials, corundum is not incorporated into any Of these finished products. It is simply a grinding medium used to produce the desired finish or precision; an operating supply or tool, so to speak. With a Mobs' scale index of 9, corundum ranks next to the diamond in hardness among the natural minerals and is superior to emery and garnet. The gem varieties of corundum, including the Oriental ruby and sapphire, are frequently more highly prized as jewels than the diamond. It is the intent Of this paper to deal Only with a description of the corundum industry, the administration of wartime control, and certain economic aspects as seen by the author. Several references are listed to assist anyone who wishes further information on the geological occurrence of the mineral. Ore Production and Consumption For the past two decades, south Africa has been the world's sole producer of corundum ore. A possible exception is Russia, where, it is understood, there was considerable production during the thirties for domestic consumption but for which statistics are lacking. The United States is the world's principal consumer of corundum ore; imports lor the period 1934 through 1940 averaging 3000 Short tons per year, The years 1935 and 1936 were close to the 5000-ton mark, and imports during 1941, the last prewar year for which statistics have been released, were approximately 6000 Short tons. Again lacking statistics on Russia, the United Kingdom ranks second, but far below the United States in consumption of ore. Historically, corundum has been found in some 35 countries throughout the world, but the principal deposits are in South Africa, Canada, Madagascar, Russia and the united States. Deposits are generally small and subject to rapid exhaustion. Thus, the United States was the principal world producer for the period 1870 to 1900, when operations ceased except for two years during World War I. India was a producer of ore from 1898 through 1921, with peak output in 1916 through 1918 Canada came into production in 1901 with substantial output of ore and finished grain until 1914; the production thereafter was smaller until 1921. Madagascar has produced ore since 1910 but has had important output in only a few scattered years. South African production started in 1912

Jan 1, 1948

By R. W. Gurry

WHEN a steel in the austenitic state, with all its carbon in solution, is maintained, at constant temperature, in contact with a gas that removes the carbon from the surface, vet without otherwise altering the composition of the steel, the change in weight of the specimen, after any period of exposure, is a direct measure of the amount of carbon it has then lost. The purpose of the present paper is to show how, by application of established mathematical reasoning based on the fundamental diffusion law and on certain postulates, this loss of weight yields a complete picture of the distribution of carbon throughout a specimen of regular shape after any period of exposure, with all the accuracy required in any practical occurrence of decarburization. Precisely the same is true for the gain in weight during the reverse process of carburization, or for the gradual gain or loss of any element, so long as the steel comprises only a single phase at temperature, provided always that the experimental conditions conform to the postulates. The change in carbon content from surface to center of the specimen is always continuous, when everything is in solution, even though under the microscope the decarburized zone (or carburized rim) may appear to be sharply defined. The experimental procedure is described and some typical results are presented, which are then interpreted by application of the diffusion law. EXPERIMENTAL PROCEDURE Initially an endeavor was made to follow the gain of weight during the process of carburization in a hydrogen-toluene atmosphere, but it was soon found that the specimen became coated with graphite, which could not be removed without some loss of metal; therefore it was decided to continue carburization until the steel was saturated throughout, to remove all graphite from the surface of the specimen, and then to follow the loss of weight during decarburization in a moist hydrogen atmosphere at the same temperature as that used for carburizing. The carburizing procedure has been described in an earlier paper;1 it suffices to state here that the carburization lasted about 140 hr. at 760°C. (1760°F.) and 44 hr. at 1110°C. (2030°F.), these periods being long enough-on the basis of the calculations presented later-to ensure that the specimen was about 9.99 per cent saturated at each temperature. The speci¬men was a cylinder about 3.8 cm. long and 0.475 cm. in diameter; the materials were carbonyl iron, a commercial low-metalloid iron, and a steel with 3.6 per cent nickel and the usual proportion of other elements. The fully [carburized] specimen, after cooling at the top of the furnace tube, was placed in a lathe and sandpapered to remove all graphite; then the diameter was measured with a micrometer caliper, and the initial weighing (corresponding to complete saturation) was made. By means of a

Jan 1, 1942

By J. A. Collins

THE process of plastic extension of face-centered cubic single crystal-line rods is so well understood, since the notable studies of Taylor and Elam,1 that the change in orientation of any crystal by slip and rotation may be predicted from the measured elongation. It is customary to assume a very homogeneous deformation, wherein gliding lamellae are free to rotate so that their slip direction continually approaches the axis of the rod, until a second slip system comes into operation; whereupon conjugate slip proceeds quantitatively to an end adjustment with the [112] direction in the axis of the rod. This process has been checked in many face-centered cubic materials and readily permits the preparation of specimens that have been sub-jected to various determinable amounts of shearing action. It is clearly of interest to study in such measurably strained specimens the development of a recrystallized structure on annealing and if possible detect the source of nuclei from which the new crystals grow. Strain-annealing experiments of this character have been performed by others but not in detail sufficient to permit a study, for example, of the number of recrystallized grains vs, the amount of shear. In the experiments now reported, this was done with a wide variety of orientations covering nearly the entire range of slip on a single system and corresponding to amounts of shear (ratio of shearing distance to distance between lamellae) at the conclusion of a test of from 0.08 to 0.57. A particular point was made of determining the crystallite rotation, or small angular range assumed by the octahedral slip plane after these various amounts of shear. The mechanism of recrystallization and the magnitude and effect of recovery on the recrystallization process was investigated.

Jan 1, 1940

By G. P. Connell, R. E. Gilmore, J. H. H. Nicolls

The purpose of this paper is to suggest a procedure for indicating the dividing line between noncaking coals and those that have weakly caking properties. A laboratory agglomerating test as an aid in classifying weakly caking coals is outlined and its merits in comparison with the standard agglutinating method advanced by the U. S. Bureau of Mines are discussed. No attempt, however, is made to discuss in detail either the different methods for determining "caking" and "agglutinating" indices or the various systems of classification. Two methods, differing somewhat in procedure, have been employed and recognized as suitable for determining the caking or agglutinating values of coals; namely, those in which an inert material such as sand, electrode carbon, etc., has been mixed with the coal before being heated, and those in which the coal is carbonized alone. In all such methods, the coal with or without the inert material is in the finely divided state and the index or value sought is derived from the examination of the residue after heating in a closed crucible or other container. The procedure outlined by Selvig, Beattie and Clellandl is the most recent representative of the method using sand as inert material, while the agglomerating test described below is representative of the method in which the coal is carbonized alone. The standard volatile-matter determination affords a means for observing the coking properties of a coal, and this has been described by Rose2 as the simplest of all coking tests. According to him, "the resulting coke button will indicate whether the coal is noncoking, feebly coking or strongly coking," despite the fact that "almost every condition in this test is at variance with large-scale carbonizing practice." Lessing,3 the

Jan 1, 1934

THIS chapter and Chapter 19 deal with the heat quantities involved in open-hearth steelmaking, including the thermal efficiency of the furnace as a generator of high-temperature heat, the heat storage in the steel and slag produced and in the furnace walls, and the heats of the various chemical reactions involved in combustion, in the formation of slag, and the refining of steel. The fundamental laws to be considered are the first two laws of thermodynamics as applied to problems involving sensible and potential (or latent) heat only: 1. Heat input equals heat outflow plus storage. 2. Heat may be transferred only from a hotter body to a colder one. The first of these laws relates to the various heat quantities or the heat balance of the process. No one has as yet made an open-hearth heat balance that came out almost exactly balanced. The cause probably lies in the difficulties of accurate temperature and flow-rate measurements at the high temperatures involved and the inherent complexities in flow distribution and air leakage present in any real open-hearth furnace system. Some idea of the magnitude of the heat quantities involved can be obtained by a brief, crude outline of the heat balance of a 90-ton heat of steel. We will assume a 60 to 70 per cent hot- metal charge in a fairly fast working and only moderately efficient furnace, burning fuel oil, with a fuel consumption of around 4 million Btu per net ton of ingots produced. The time from start of charge to tap is 9 hr. During this period, the oil burned represents 360 million Btu and the sensible heat in the preheated air at the port ends is 117 million Btu, so that the total heat input at the ports is 477 million Btu. Heat stored in the steel and slag at the end of the heat, plus the various amounts absorbed by certain bath reactions, amounts to a total of 195 million Btu, but 120 million of this is supplied by the heat in the hot metal and by various heat-evolving reactions in the bath,

Jan 1, 1951

By Donald W. Scott, Nathaniel Arbiter, A. C. Richardson

This paper describes the application of amine flotation to a specific problem—that of increasing the grade of magnetite concentrates derived from an iron ore requiring extremely fine grinding for mineral liberation. Experiments conducted on an iron ore from Wisconsin had shown that concentrates containing 60 to 62 per cent iron and 12 to 14 per cent silica could be produced by magnetic separation. The residual silica occurred as quartz and hornblende, either entrained or locked with magnetite. Most advantageous utilization of the concentrate, however, necessitated that the silica content be reduced to about 5 per cent, equivalent to an iron content of 67.5 per cent. It had been demonstrated that tabling of the magnetic concentrate removed sufficient quartz and hornblende to yield an acceptable concentrate, but disadvantages inherent in tabling dictated that flotation be investigated as a substitute. The goals set for the flotation investigation were: (I) the production of concentrates of about 68 per cent iron content from the magnetic concentrate; (2) an iron recovery of about 85 per cent of that in the feed to flotation; and (3) minimum reagent cost. Both batch and continuous flotation tests were employed; the former, to establish the procedure and the latter to verify it. Although the data were obtained on a specific ore, and with a commercial application in view, it is believed that they have a bearing on other problems where amine flotation is being used or is anticipated. Samples Two samples, designated "(minus 100-mesh magnetic concentrate" and "minus 150-mesh magnetic concentrate," were used for the batch experimental work. They differed only in the degree to which the crude ore was ground prior to magnetic separation. They were stored moist in steel drums in quantities sufficient for all the experimental work reported. This procedure had the advantage of allowing all tests to be made on common samples, but had the disadvantage that the individual flotation samples, because of the difference in storage time, were subject to various stages of surface alteration. Previous work had indicated that common samples were desirable for the batch studies, and it was decided that if these data appeared sufficiently promising the effect of surface alteration could be checked best by continuous tests. The size distributions and the assays of the samples are given in Table I. The minus 150-mesh magnetic concentrate, on which most of the flotation tests were made, assayed 60.9 per cent iron, 13.3 per cent silica, and 0.016 per cent phosphorus. The minus 325-mesh portion represented 78.I per cent of the sample by weight, and assayed 67.9 per cent iron. Thus, the insoluble, mainly silica, was concentrated

Jan 1, 1947

By Kenneth C. Vincent, A. M. Gaudin

In a study1 of the action of amyl xan-thate on chalcocite in water suspension, it was found that if the xanthate is added in relatively large quantity the xanthate group can be accounted for in three forms: (1) as xanthate ion remaining in water, (2) as benzene-soluble cuprous xanthate on the chalcocite, (3) as a benzene-insoluble coating on the chalcocite. Reduction in the amount of xanthate added leads to disappearance of form I then of form 2. With minute quantities of added xanthate, substantially all the reagent is of the "unleachable" kind. Yet this unleach-able xanthate can be dissolved by pyridine to form a soluble cuprous xanthate complex, and it is sufficient in effectiveness to make chalcocite flotable even if insufficient in quantity to form a complete mono-molecular film on the mineral. In that study it was also found that chalcocite abstracts cuprous xanthate from benzene so1ution, in what may (or may not) be a case of molecular adsorption. It seemed desirable, therefore, to study further the "unleachable" xanthate on the chalcocite, and particularly to ascertain whether it is formed as a result of the benzene leach or is actually formed during the conditioning of chalcocite in aqueous xanthate solution. A 'splendid tool to make such studies has recently been perfected; that is, the use of radioactive spies or tracer atoms. With this tool, it was thought possible to answer the problem stated above, but, unfortunately, this did not prove to be true. Answer to the flotation question was clouded by the existence of rapid and selective diffusion of copper atoms in the solid mineral—a phenomenon that was totally unexpected yet remains interesting and perhaps important. Method of Radioactive Spies The method of radioactive spies is discussed in many places. Two convenient references are the article by Evans2 and the book by pollard and Davidson.3 The method was first developed by van Hevesy and paneth in 1013, when only natural radioactive isotopes were available. These isotopes are few in number, and so the method remained limited in scope. Recently the synthesis of over 350 active isotopes of all the known stable chemical elements4 has opened widely expanded possibilities for the method, A fundamental tenet of the method is that a radioactive atom and a nonradio-active atom are exactly alike until disintegration of the radioactive atom. Then, by its sudden death, the spy reveals its location. The relative abundance of spies at various locations makes it possible to ascertain the relative abundance of the corresponding nonradioactive atoms at the same times and locations. A second fundamental tenet of the method of radioactive tracers is that the radioactivity lies in the nucleus of the atom: transfer of radioactivity from one

Jan 1, 1947

Jan 1, 1919