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By C. K. Gupta, P. K. Jena

Niobium (columbium) metal in the form of a button has been produced by calciothermic reduction of niobium pentoxide using sulfur as the heat booster. In these experiments with 50 g of niobium pentoxide per batch, the influence of percentage of calcium in excess of the stoichiometric, the percentage of sulfur by weight of the niobium oxide, and the outer-wall temperature of the bomb on the quality and yield of the metal has been studied. The maximum yield on this scale was 78 pct using 50 pct excess Ca and 20 pct of S and at a bomb-wall temperature of 600°C. In experiments conducted on 500 g of niobium pentoxide, reduction with 40 pct excess Ca and 20 pct of S, and at a bomb-wall temperature of 500°C, the.yield of the metal improved to 82 to 84 pct. Some of the reduced-metal samples have been electron-beam melted and the button melts thus obtained have been observed to be extremely ductile and capable of cold reduction to 98 pct without intermediate annealing. NIOBIUM, because of its high melting point (2468oC), its ductility, its resistance to corrosion especially in liquid metals, its high-temperature mechanical properties, and its relatively low capture cross section (1.1 barns) for thermal neutrons, has potentialities as a structural material in the field of nuclear engineering. Niobium and its alloys are also gaining importance in high-temperature technology as components in aircrafts, jet engines, and missiles, electronics, chemical engineering, and surgery. In 1904 Weiss and Aichel 1 produced niobium by reduction of its pentoxide by misch-metal. Since then a large number of investigations have been carried out for the extraction of niobium from its compounds. The various routes through which the metal niobium has been extracted from its compounds can broadely be classified into the following groups: a) reduction of its halides, oxides, and fluo-salts with metals like calcium, magnesium, sodium, and aluminum;2-10 b) reduction of its halides with hydrogen and oxides with carbon or carbides;11-18 c) electrolytic winning from its halides and fluo salts;19-25 and d) thermal decomposition and disproportion ion of its halides26-30 Among the processes in commercial use at present are sodium reduction or fused-salt electrolysis of potassium niobium fluoride, carbide or carbon reduction of the oxide, and hydrogen or metallothermic reduction of the chlorides. In 1907 Von Bolton2 prepared niobium by reducing niobium pentoxide with aluminum. Dennis and Adam-sona attempted reducing the oxide with magnesium powder in argon atmosphere and the resulting metal contained as much as 5 pct O. Mondolfo8 claimed a method for the reduction of the oxides with aluminum. In the case of both magnesium and aluminum reduction, it has been stated31 that by-product oxides such as MgO or A12O3 would involve a major separation problem. Further, in the case of alumino-thermic reduction, the solubility of aluminum in niobium and intermetallic formation have to be reckoned with. In 1922 Bridge3 produced niobium by calcium reduction of niobium pentoxide. Dennis and pdamson' obtained the metal by a similar method with an oxygen content of 0.2 pct. In most of the cases of metallothermic reduction of niobium oxides mentioned above, the metal niobium is obtained in the form of powder. In an attempt to produce massive niobium metal, lock' used iodine as the thermal booster in the bomb reduction of niobium pentoxide by calcium. Massive niobium metal was obtained with a maximum yield of 75 pct containing 0.1 pct 0. Joly32 carried out experiments on calcium reduction of niobium pentoxide on a 2-kg scale using sulfur as the heat booster in a sealed bomb filled with argon. In his experiments, the reaction was initiated by passing a current through niobium spiral wire embedded in the charge. In a typical run consisting of 2000 g of niobium pentoxide, 3100 g of calcium, and 800 g of sulfur (S/Nb2O5 = 3.3), he obtained massive metal in the form of a very uneven mass with a yield of -57 pct. With lower amounts of sulfur and calcium, powder niobium mixed with small metal globules was obtained and the yield was also poor. From these experiments he concluded that this method is not a suitable one for industrial development considering the quality and yield of metal obtainable and the possible hazards with higher ratios of sulfur to niobium pentoxide in the -~charere. In the present work, a detailed investigation on the calciothermic reduction of niobium pentoxide in a stainless-steel bomb in presence of sulfur as the heat booster was undertaken on a laboratory scale.

Jan 1, 1964

By J. R. Long, E. T. Hayes, R. S. Dean, F. S. Wartman

THE production of titanium in 15-1b. lots and with a purity sufficient to be consolidated into ductile metal, as described in a previous paper,1 has provided adequate material for a study of the : physical properties of titanium and a more thorough examination of its working qualities. Data on the physical properties reported in that paper were obtained on metal fabricated by a fixed procedure, standardized for the purpose of control of the reduction, and are representative only of material fabricated under those conditions. There are many possible variables in the working schedule, which will have significant effects on the properties of the finished material; and since the previous working methods were not necessarily the best, an investigation of the fabrication of titanium by other methods was undertaken. In this work the consolidation of the powder by pressing and sintering was conducted essentially as outlined in the report cited' and all efforts were centered on fabrication methods for those powders and the properties produced by them. Hardness, density, microstructure, and tensile properties were determined at various stages in the working and annealing; and resistivity measurements were made on a few bars and drawn wire. [ ] CONSOLIDATION OF THE POWDER The screen analysis of the available titanium powder is given in Table I. No attempt was made to alter the size distribution from that noted because this powder, although coarse by normal powder-metallurgy standards, produced acceptable compacts suitable for the present work. Because of their large specific surface, finer powders are more contaminated by oxygen and produce harder compacts, which are difficult to work. The powder as produced is soft, compresses in a normal fashion, and exhibits very little tendency to adhere to the die surfaces. Unlike aluminum and magnesium powders, it can be readily pressed without the use of die lubricants. When compacted at so tons per

Jan 1, 1946

Alfred Stansfield, Montreal, Canada:—In Professor Howe's paper on the position of Ae3, he shows its industrial importance in determining the temperature to which steel should be heated for " grain refining." Several years ago I carried out a research on the " burning " of steel and found that while hypo-eutectoid steel should be heated to Ae3, hyper-eutectoid steel that has been very much overheated must be reheated to the curve Sa on the carbon-iron diagram, in order to redissolve the pro-eutectoid cementite and thus to obtain recrystallization and grain-refining. This treatment was necessarily only partly successful, and I should like to ask whether the conditions of heat treatment for refining overheated high-carbon steels have been ascertained. Speaking of the &'Persistence of Solidificational Segregation " Professor Howe quotes an experiment made by Mr. Stead in which a bar of 1.2 per cent. carbon steel was immersed in a large mass of molten blast-furnace slag and allowed to cool with it. The steel was heated ; above the solidus (curve An on the carbon-iron diagram), but below the liquidus (curve AB). A drop of eutectic carbon-iron alloy, rich in carbon, had liquated out and hung below the bar. This agrees exactly with my own observations on the burning of steel, but my interpretation differs somewhat from that of Professor Howe. Professor Howe considers that the fusion of a part of the metal (rich in carbon) shows that the solidificational irregularities of composition had persisted through the rolling and heat treatment of the steel, as otherwise no part of the steel would have been sufficiently fusible to melt. It does not appear to me that such an explanation is necessary. A piece of steel represented in temperature and composition by any point within the area ABa will ultimately resolve itself into a solid phase and a liquid phase in equilibrium with each other. It may appear that if the steel were absolutely uniform no fusion could take place, but, the smallest nucleus of high-carbon, fusible alloy would ultimately bring about this separation into liquid and solid phases, by diffusion of the carbon from the solid to the liquid areas. A nucleus sufficient for the purpose might be provided by an area of pro-eutectoid cementite which had not become diffused during the

Jan 1, 1914

By A. Paul Bond

Two series of 17pct Cr iron-base alloys with small, controlled amounts of carbon and nitrogen were vacuum-melted in an effort to detertmine the meclz-uniswls of inter granulur corrosion in ferritic stain-less steels. An alloy containing 0.0095 pct N aid 0.002 pct C was very resistant to intergranular corrosion, even after sensitizing heat treatments at 1700" to 2100o F. However, alloys containing more than 0.022 pct Ni and more than 0.012 pct C were quite susceptible to intergranular corrosion after sensitizing heat treatments at temperatures higher than 1700°F. This corrosion was observed after the usual exposure tests and after potentiostatic polarization tests. Electronmicroscopic examination of the alloys susceptible to intergranular corvosion revealed a small grain boundary precipitate; this precipitate was absent in the alloys not susceptible to such corrosion. Thc electronmicrographs indicate that intergranu1ar corrosion of ferritic stainless steels is caused by the depletion of chromium in areas adjacent to precipi-tates of chromium carbide or chromium nitride. It also seems likely that the precipitates themselves are attacked at highly oxidizing potentials. Confirma-tion of the proposed mechanisms was obtained in tests on air-melted ferritic stainless steels containing titanium. The titanium additions greatly reduced susceptibility to intergranular corrosion at moderately oxidizing potentials but had no beneficial effect at highly oxidizing potentials. A major obstacle to the use of ferritic stainless steel has been their susceptibility to intergranular corrosion after welding or improper heat treatment. It appears that sensitization of ferritic stainless steel occurs under a wider range of conditions than for austenitic steels. In addition, a greater number of environments lead to damaging intergranular corrosion of sensitized ferritic stainless steels than to sensitized austenitic steels. The chromium depletion theory of intergranular corrosion is widely accepted for austenitic stainless steels'" although there: are some objections.3 On the other hand, several alternative mechanisms proposed for ferritic stainless steels include precipitation of easily corroded iron carbides at grain boundaries,' grain boundary precipitates that strain the metal lat-tice,5 and the formation of austenite at the grain bound-arie.6 The application of the chromium depletion theory to ferritic stainless steels has been discussed extensively by Baumel.7 The present investigation was undertaken to determine which of the proposed mechanisms can be sub- A PAUL BOND IS Research Group Leader, Climax Molybdenum Co of Michigan, Ann Arbor, Mich. stantiated with experimental data obtained on ferritic stainless steels. High-purity 17 pct Cr alloys containing small controlled additions of carbon or nitrogen were therefore prepared, and then examined electro-chemically and metallographically. EXPERIMENTAL PROCEDURES Materials. Two series of experimental alloys were prepared from electrolytic iron and low-carbon ferro-chromium using the split-heat technique. In this technique, the base composition is melted, and part of the melt is poured off to produce an ingot. To the balance of the melt, the required addition is made and the next ingot cast. This process is repeated until a series of the desired compositions is cast. By this procedure the impurity levels are essentially constant within each series. All the alloys in the carbon-containing series were melted and cast in vacuum. The base composition in the nitrogen series was melted and cast in vacuum; subsequent ingots in the series were melted with additions of high-nitrogen ferrochromium, and cast under argon at a pressure of 0.5 atmosphere. Two additional alloys were produced starting with normal purity materials. They were induction-melted while protected by an argon blanket and cast in air. Table I gives the composition of the alloys. The 2-in.-diam ingots produced were hot-forged and hot-rolled to a thickness of 0.3 in. and then cold-rolled to 0.15 in. All specimens were annealed at 1450°F for 1 hr. The indicated sensitizing heat treat-s s ments were performed on annealed material. All heat treatments were followed by a water quench. Specimen Preparation. For the 65 pct nitric acid test, 1 by 2 by 0.14-in. specimens were wet-surface ground to remove surface irregularities and polished through 3/0 dry metallographic paper. For the modified Strauss test, $ by 3 by 0.14-in. specinlens were similarly prepared. Immediately prior to testing, the Table I. Compositions of the Alloys Composition, pct Alloy Cr hio C N 270A 16.76 0.0021 0.0095 270B 16.74 0.0025 0.022 270C 16.87 0.0031 0.032 270D 16.71 0.0044 0.057 271A 16.81 0.012 0.0089 27 IB 16.76 0.018 0.0089 271C 16.69 0.027 0.0085 271D 16.81 0.061 0.0O71 4073' 18.45 1.97 0.034 0.045 4075† 18.5 2.0 0.03 0.03

Jan 1, 1970

By J. F. Martin, J. E. Friedline, L. M. Melnick, G. E. Pellissier

A method has been developed for determining gases in steel in which the gases are extracted by vacuum fusion and analyzed by mass spectrometry. This method is especially applicable for determining small amounts of oxygen and nitrogen. The lower limit of detection for both oxygen and nitrogen is 0.0001 pct with an average deviation of about 0.0001 pct for oxygen and 0.00008 pct for nitrogen. Hydrogen analyses by this method are in good agreement with analyses by vacuum tin-fusion. A complete analysis of all gases extracted from a steel sample can be accomplished in 40 min. It has long been known that certain of the gaseous elements exert particular effects on the physical and mechanical properties of steel. With the recent advent of new experimental steelmaking practices it is now possible to obtain steels with extremely low contents of such elements as oxygen and nitrogen. Present methods for determining these two gases are of insufficient sensitivity as applied to steels made by these newer practices, and therefore a new technique was considered necessary. A review of the literature showed that the conventional vacuum-fusion method1 was the procedure most suitable for modification to obtain a sensitive method for determining the gaseous elements present in steel simultaneously. However, for trace amounts of gases it is impractical to increase the sample size because of the physical limitations of the apparatus and the increased degassing time which would be necessary. Also, when only one of the desired gases is present in trace amounts, quantitative separation by conventional vacuum fusion is almost impossible. Since small analytical mass spectrometers are now commercially available, it was decided to use this instrument in conjunction with conventional vacuum fusion for both qualitative examination and quantitative determinations of the gaseous elements in steel. This technique has already been used with success for the analysis of copper and lanthanum.2"4 APPARATUS A vacuum-fusion unit was first designed and built, Fig. 1. This unit was designed especially for the determination of small amounts of nitrogen and/or oxygen in steel since an acceptable method (vacuum tin-fusion)5 was already in use for the determination of hydrogen in steel. The vacuum system was con- structed of Pyrex glass throughout. Mercury check valves were used in place of stopcocks in the high-vacuum section of the system. Ferromagnetic samples are normally introduced into the vacuum system through a mercury lift. In case of a break in the lift, the mercury is prevented from entering the furnace by a self-locking, mercury safety check valve, Fig. 2. This check valve, developed at our laboratory, is a modified T/S ball-and-socket joint placed in the sample inlet system between the mercury and the furnace. A sudden entry of mercury or air pushes this valve into the closed position, completely blocking the top of the mercury lift. The check valve is held in the closed position by the vacuum of the apparatus. A separate entrance tube also was placed in the system, so that samples which would amalgamate with mercury, or which are nonmagnetic, could be introduced into the furnace. A slightly modified Guldner-Beach furnace is used in this system.8 The optical flat was connected to the system by a ground-glass joint to facilitate cleaning, a quartz delivery tube was substituted for Pyrex, and the crucible was used uncovered. Fusion takes place in a high-purity graphite crucible insulated by — 200-mesh high-purity graphite powder. The crucible set (crucible and funnel) is suspended in a quartz crucible. The furnace envelope and the sample inlet system are exhausted by 2 single-stage, mercury-diffusion pumps in series. The first of these is a high-speed pump, which will work only with a very low backing pressure. This pump is used to exhaust the gases from the furnace as rapidly as possible. The second mercury-diffusion pump is used as a backing pump for the first; the capacity of this pump is much lower. However, it will work efficiently against a back pressure of 3 mm of mercury. To assure positive pumping, a modified Naughton and Uhlig condenser7 is used. With the use of proper valving the second pump is also used as a circulation pump in the catalyst system.

Jan 1, 1959

By F. H. Wilson, R. M. Brick

WITH the papers of Palmer and Smith1 and of Burghoff and Bohlen,2 published in 1942, understanding of the problem of the development of ears on deep-drawn brass cups was brought to the point where, from a practical standpoint, producers of brass sheet could keep earing under control. However, these very practical results raised questions concerning the reasons for the observed behavior. Since plastic deformation is fundamentally a function of crystallographic slip, these reasons must be considered in the light of the textures to be found in the annealed sheet. Various attempts have been made to interpret the mechanism of ear formation by correlation with the preferred orientation and the anisotropy of the sheet. However, none of these has satisfactorily explained why ears are usually found in the rolling and transverse directions for copper but at 45° to these directions for brass. This paper offers additional data on these two related subjects and has been divided into two sections. The first section provides a survey of the recrystallization textures of brass as affected by annealing temperatures and prior reductions, and an account of the earing behavior which accompanies these textures. The second section reports new data on the anisotropy that accompanies a characteristic texture for brass and endeavors with partial success to establish the factors that account for the difference in earing behavior between copper and brass. EARING BEHAVIOR OF BRASS Review of Textures The recrystallization texture of severely rolled brass was first reported by Bass and Glocker.3 The preferred orientation to which this texture, obtained from metal annealed at 500°C., was most akin was (113)[112]. This texture has been confirmed by Bauer, von Göler and Sachs;4 Brick;* Brick, Martin and Angier;6 and Cook and Richards7 who, in general, used annealing temperatures under 500°C. Bass and Glocker3 also reported the recrystallization texture at 850°C. to be the same as at 500°C. They analyzed their textures by means of single photograms obtained with white radiation. The photograms for both temperatures are reproduced in their paper, and there is a strong similarity between the two. However, for the latter temperature, the number of spots registered on the film was remarkably large for the grain size to be expected, and the authors made no mention of using a technique that would integrate a large enough area of the specimen to produce so many spots. The only other attempt to determine textures resulting from high temperature

Jan 1, 1945

By P. S. Kotval, O. H. Nestor

Stacking fault energy measurements of nickel-base alloys have been mainly confined to binary and ternary systems. In this paper, the stacking fault energy has been measured by the rolling texture method in a series of ten alloys which comprise successive additions of Cr, Mo, Fe, and C to pure nickel, eventually resulting in an alloy of the composition of Hastelloy alloy X. The alloys studied here are single-phase, solid solutions with the exception of two alloys in which some undissolved particles of "primary" carbide have been retained. It is found that successive additions of chromium, molybdenum, and iron all lower the stacking fault energy, with iron having only a minor effect. The stacking fault energy is found to increase when carbon is added in solid solution. The results from the rolling texture measurements are correlated with thin foil observations of dislocation substructures in these alloys. In a recent paper' it was pointed out that the dislocation substructure of various superalloy matrices could be classified into three broad categories based on 'high', 'medium', and 'low' stacking fault energy. It has also been demonstrated2 that the dislocation substructure in each of these categories has a well defined role in the nucleation of strengthening precipitates which is different from the role played by the dislocation substructure in other categories. Thus, it becomes desirable to understand the influence of various solute elements on the stacking fault energy and hence on the dislocation substructure of the matrix, before any further development of superalloys by mi-crostructural predesign can be undertaken. Recently, Beeston and France have studied the influence of increasing solute additions on the stacking fault energy of a series of binary nickel-base alloys relevant to the Nimonic series using the rolling texture method, and have then estimated the effect of a given alloy addition in five commercial Nimonic alloys. However, comparison with stacking fault energy data from other investigations''5 suggests that the influence of a given solute element in a nickel-base binary system is not necessarily the same in a ternary or more complex superalloy system. Accordingly, the present work was undertaken to study the effect of successive addition of solute elements to pure nickel, the final composition being the nominal composition of Hastelloy X. The rolling texture method of stacking fault energy measurement was used since it can be used for the whole range of stacking fault energy values and does not have the disadvantage of, say, the Node method which is only applicable to low values of stacking fault energy. In addition, the rolling texture method provides a means of determining the stacking fault energy which is statistically more significant than that provided by other methods. EXPERIMENTAL TECHNIQUES Button heats of alloys of the compositions shown in Table I were prepared. Each button was remelted not less than four times. After a slight deformation (approximately 5 pct) all alloys were homogenized at 2200°F except alloys, H . I, and J. Alloys H and I were solution heat treated at 2150°F and alloy J at 2282OF. The buttons were cold worked by rolling, using "end-to-end" passes and intermediate anneals at the homogenization temperatures mentioned above. After each annealing treatment the samples were rapidly water quenched to avoid any precipitation. In alloys F and I, however, a few particles of "primary" carbides were retained even after the homogenization treatments at the temperatures mentioned above. Part of the solution heat treated material was cold worked to 0.04-in.-thick sheet and the penultimate reduction was -50 pct of deformation as recommended by Dillamore et al. All annealing was carried out in vacuo within sealed quartz capsules. Some of the material from each alloy was rolled down further to 0.004 in. strip for thin foil transmission electron microscopy specimens. Specimens of this strip were annealed at the homogenization temperature for 1 hr and then strained 7 pct by rolling at room temperature. Thin foils were prepared from the strip specimens by the 'window" technique using an Ethanol-Perchloric acid electrolyte at 32°F and a voltage of 22 v. Stainless steel cathodes were employed. All transmission electron microscopy was performed in a JEM-7 electron microscope using an accelerating voltage of 100 kv. Specimens from the 0.04 in. sheet which had been rolled -60 pct in the final pass were electropolished to remove the surface layers to a depth of approximately 0.002 in. Rolling texture pole figures for all the alloys were determined using a Schulz ring and nickel filtered CuKa radiation at 50 kv and 20 ma. The texture parameter Io/(lo + I,,) (where Io is the

Jan 1, 1970

By MAGNE MORTENSON

IN laboratory work and industrial tests it is important to set forth the results of research, clearly. This is generally achieved by means of some form of diagram or graphical illustration. The most common form for such graphs of flotation research is a simple chart with two curves for percentage and recovery of the concentrate. This may be quite useful, especially for minerals which may be floated: by means of one reagent in variable and another in constant amounts. If both reagents are used in variable quantities the process may be illustrated by means of several diagrams, .keeping one reagent constant in each series of tests. A more useful form of diagram for a. system with two variable - components (reagents) may be established by drawing a chart with the weights of the two reagents as .abscissas and ordinates. Every test is marked down -in the diagram with an indication of the extraction and concentration gained. In this diagram there are drawn lines for equi-extraction and equi-concentration of the mineral that is floated out in the - concentrate. The contour of these lines gives a relatively clear impression of the conditions for flotation by means of .the chemicals used. The best conditions are of course found in diagrams where the 'areas for maximum extraction and high conntration are coincident

Jan 1, 1931

By G. Cartaud, F. Osmond

WE have already devoted two previous memoirs to this question. In the first we collated and discussed the existing literature on the subject; in the second, we described the crystalline forms obtained by the reduction, at different temperatures, of ferrous chloride by hydrogen or by zinc-vapor. The conclusion from these researches was that the three allotropic states of iron-a, stable below A2; 19, stable between A2 and A3; and 7, stable above A3-all crystallize in the cubic system. The differences observed were such as are customarily encountered in the crystallographic records of many minerals of which allotropic varieties or isomerides are not known, but did not conform to the ordinary definition of polymorphism. It is, however, improbable that allotropic transformations, which are placed beyond doubt by a series of positive facts, do not involve some changes in the intimate structure. As a matter of fact, the crystals we did obtain were too small to allow of a precise examination, and this might introduce an element of uncertainty in the firm establishment of our conclusions. Professor H. Le Chatelier was even led to think from some of our results that iron could very well be a rhombohedron simulating a cube, and not a true cube, and it will be remembered that the crystalline form of bismuth was for a long time incorrectly regarded as cubic. Allotropy does not, however, necessarily involve such a deduction. Without departing from the cubic system at all, a whole

Nov 1, 1906

By Jonas Svensson

A new method is described for the production of cold-bonded pellets using a hydraulic binder, such as portland cement. Large-scale pilot-plant tests have proved that self-fluxing pellets of high reducibility and good handling strength can be made by the method. Blast-furnace trials have shown that the pellets are an acceptable burden material, comparable with self-fluxing sinter or heat-hardened pellets. Economic factors of commercial-scale production are discussed. The Grangcold Pellet Process—for which patents have been applied or already granted in a number of coun-tries—uses a hydraulic adhesive such as portland cement, slag cements, pozzolanic cements, etc., for the production of cold-bonded pellets. The idea of using a hydraulic binder for the agglomeration of iron-ore fines is not new. Portland cement was proposed as an adhesive for cold-bonded iron-ore briquettes in patents granted more than 50 years ago.' In a report on the briquetting of iron-ore fines, published in Stahl und Eisen in 1959; it is stated that briquettes bonded with portland cement are used on a small scale at an ironwork in Germany. According to the report, the briquettes showed excellent strength in the blast furnace although their general use was made impossible because they required a long hardening time, during which they are sticky, soft, and difficult to store and handle. The Grangcold Pellet Process has overcome this particular disadvantage by mixing the balls with a suitable amount of the balling concentrate before storing them. The pellets are embedded in the concentrated during storing in such a way that they are isolated from each other and thus prevented from sticking together to form clusters. Thanks to the embedding concentrate, the pellets are subjected to a more or less uniform pressure from all sides which does not deform them. Thus, the mixture can be stored in a stockpile or in a bin until the pellets have hardened sufficiently. The concentrate is separated from the pellets by means of screening. The concentrate is returned to the balling operation and the pellets are either shipped to the blast furnace or stored for final hardening. The binder preferred for the Grangcold Pellett Process is portland-cement clinker, ground without the admixture of gypsum in order to avoid sulfur in the pellets as far as possible. Usually a 10% binder content is used. Two-thirds of the portland-cement clinker consist of lime and the rest is silica, alumina, and ferric oxide. Thus, self-fluxing or overbasic pellets are produced with this binder if the amount of silica in the concentrate used does not exceed 4%. The Grangcold Pellet Process was developed by the mineral Processing Laboratory of the Granges Co. Work started in 1963 with batch-scale tests. In 1966, a small pilot plant was put into operation in which 1800 tons of pellets were produced using 10% of rapid-hardening portland cement as a binder. Favorable results from a blast-furnace test with this batch led to the decision to erect a larger pilot plant which went into production in the summer of 1967. Since then, approximately 100,000 tons of cold-bonded pellets have been produced, mostly with 10% gypsum-free portland cement as a binder. Several full-scale blast-furnace trials have been performed with the pellets. The results of the trials indicate that the Grangcold pellets constitute a satisfactory blast-furnace feed. An industrial plant for the production of Grangcold pellets with a rated capacity of 1.5 million tpy is now under construction at the Granges Co.'s mine at Grangesberg. The plant will come into operation in the summer of 1970. Results from Laboratory Work Pellets made from iron-ore concentrate bonded with portland cement harden slowly and their handling is very critical until they have hardened enough to loose their stickiness. It is therefore especially important to study the progress of the hardening action and the factors influencing it. This is best achieved by investigating the relationship between the compressive strength of the cement-bonded pellets and the curing time under varied conditions. The general course of this relation-

Jan 1, 1971

By J. Murray Riddell, Grover J. Holt, Arthur E. Anderson

Out of the depths of each business cycle we emerge with a stimulus for greater efficiency and a realization of progress in industrial technique. The recent years have not been an exception to this rule, and in retrospect we sense that significant advances have been made in mining practices on the Mesabi Range, with emphasis on speed of production and economy of operation. A survey of such changes does not reveal anything that is fundamentally or basically new, but it is apparent that ideas and machines that have found wide application in industry elsewhere, with necessary modifications, are being put to productive use in mining iron ore. Innovations in transporting and conveying ore from the open pits stand out with greatest prominence, so that, in the main, it will be with these features that this paper will treat, in the review of progress made to this date. The late years have witnessed the development of small deposits for open-pit operation, the cleaning up of pits nearing exhaustion, and in two large operations the approach to the limit for haulage by steam locomotives, owing to grades, making it necessary to recover the ore in slopes, track benches and below the power-shovel limit by a milling and scram operation. For several years small standard-type dump trucks have been used in clean-up or scram operations within the pits, but during the season of 1936 the first effort was made to use heavy truck haulage in the transportation of stripping and iron ore. The new units in use today vary from 15 to 20 tons in capacity, and are equipped with powerful gasoline or Diesel engines and supplemented by trailers or wagons on rubber or crawler treads. The Diesel engine finds favor with most operators because of fuel economy. These units develop upward of 125 hp. in the 15-ton trucks. The speed of these trucks varies from 2 miles per hour in Pow gear to 35 in high gear. The transmission affords 12 speeds forward and 3 speeds in reverse.

Jan 1, 1940

By C. E. Cottrell, G. W. Preckshot, N. D. Delisle, D. L. Katz

Most crude oils contain asphaltic substances that may be naturally or artificially precipitated. In the Greeley field, California, this asphaltic bitumen is precipitated during the flow of the oil from the reservoir to the stock tank The mechanism of such precipitation is not well understood. This paper presents the progress that has been made by using the electron microscope as a new tool and by observing the effects of the streaming potential on the formation of bitumen particles. Crude oils at atmospheric pressure viewed in the electron microscope in very thin films under a vacuum showed no asphaltic particles. A technique of preparing slides of thin films by dilution of the oil with benzene and washing in petroleum ether was used at first, and these observations showed that the solvents caused the formation of the particles, varying from 0.01 to 0.2 micron in diameter. The electrical effects of fluids flowing through porous solid were studied, with emphasis on the formation of colloidal particles by the streaming potential. The streaming potential of crude oil flowing through sand was measured and was shown to be responsible for the formation of bitumen particles. These results bring out a new phenomenon, which may occur when crude oil flows through the porous oil reservoir. mechanisms. Asphalt has been the subject of widespread investigation but, owing to the complexity of the substances being considered, progress has been slow. Investigators working primarily with the asphaltic substances have treated the subject from the colloidal standpoint and have developed theories that picture the asphaltic particles as surrounded by adsorbed materia1s.14,15,17,24 The deasphaltization of lubricating oil by the use of solvents treats the subject primarily from the standpoint of liquid-liquid equilibria.'' A complete understanding of asphaltic substances would make possible the following of the material from its initial state in the crude oil through precipitation processes to the final plastic stage, the most common form of which is used in asphaltic pavements. Since these asphaltic particles are very small, it appears 'hat the electron microscope4 might be a useful tool in studying the precipitation processes. Specimens are examined by the electron microscope in a vacuum and as very thin films, requiring special techniques in preparation of samples. A brief description of the electron microscope and its operation will bring out the difficulties and advantages of its use for this problem. The first work was done with crude oils that had been diluted with solvents for the preparation of the film to be examined. Later a technique was developed by which the undiluted oil film could be made thin enough for direct examination. These two techniques show vastly different results Asphaltic particles have been precipitated from crude oils by a variety of

Jan 1, 1943

By C. W. Binckley, F. R. Burgess, E. R. Haymaker

A method of establishing stabilized back-pressure curves for gas wells producing from formations of extremely low permeability is presented. Actual well performance under many different operating conditions is shown by the stabilized back-pressure curve. By use of the method. it is possible to conduct back-pressure tests with a critical-flow prover on wells that stabilize slowly, and save approximately 88% of the gas ordinarily vented to obtain satisfactory test data, with a great reduction in time required for testing. INTRODUCTION The reasons for establishing dependable back-pressure curves on gas wells have been pointed out by previous publications. The publication most referred to. of course, is the United States Bureau of Mines Monograph 7, titled "Back-Pressure Data on Natural Gas Wells and Their Application to Production Practices". The technique generally established therein has been accepted and used by many engineers; and, when proper tests are conducted, the results can be used for the analysis and solution of several practical problems concerning field operation and development. Even where formations of low specific permeability are encountered, the determination of a well's actual performance by the back-pressure test method permits the engineer to analyze many problems in individual well operation and also to predict necessary future field development. Such problems as the determination of the ability of a well to produce into a pipe line at a predetermined line pressure, the design of gas gathering systems and meter settings, and the determination of the time and the number of wells required to be drilled to meet future market obligations, can be solved, in part., by the use of a reliable back-~ressure curve. In addition, the computed well delivery rates determined by data from backpressure tests ordered by state regtilatory bodies, when compared with the true back-Pressure curve, permit the operator to ascertain whether such data represent unstable or relatively stabilized delivery rates for given pressure conditions of the well. The technique of back-pressure testing, as described in this report, was developed by Phillips Petroleum Company engineers from data obtained during a testing program that started in 1944 and has been continued to date. Three hundred and eleven back-pressure tests were conducted on 299 wells located in the southern part of the Hugoton Field. The gas-bearing zone is composed of several dolomitic formations of the Permian Age; the important ones are the Herington, Upper Krider, Lower Krider, and Winfield. The average bottom-hole temperature is approximately 91 °F.. and the initial wellhead shut-in pressures range from 400 to 440 psig. The spacing pattern is 640 acres per well with each well located near the center of the section. The range of back-pressure potentials on wells tested was from 500 to 23,000 Mcfd. All gas wells were acidized, and the quantity of acid used, expressed in 1574 hydrocloric acid, varied from 12,000 to 22,000 gallons per well. The quantity and concentration of each treatment depended on the stage, the formation being treated, and experience gained from previously completed wells. The gas in the Hugoton Feld is a "dry" gas. It has a gasoline content of approximately 0.25 gallons per thousand cubic feet, as determined by charcoal test, and its specific gravity averages about 0.71 as compared to air (air = 1.00 at 60°F.). Of the wells tested, 71 were completed with 7" casing, 3 with 9 5/8" casing, and 1 with 6%" casing set on top of the upper producing formation with the well bore through the gas bearing formations being open hole. Two hundred and twenty-four were completed with 5 1/2'' O.D. casing set through the gas bearing formations and perforated. For the purpose of establishing reliable back-pressure curves in the area, Phillips Petroleum Company personnel has computed data on the basis of 24-hour flows per point. Early in the program, many tests were actually permitted to flow 24 hours to obtain data for each plotting point, at great expense in man power and time. Presently, however, such tests have been replaced by tests of short duration flows which can be made to effect results that correspond to the tests obtained by flows of much longer duration. METHOD When a gas well producing from a reservoir of low permeability is opened for production through a constant size orifice, both the rate of flow and working pressure decline. first at a high rate and later at a lower rate until after several hours the decline becomes difficult to ascertain. In this paper the rae of flow and working pressure are considered to be stabilized when it becomes difficult to observe changes in working pressure during a period of three hours by the use of a deadweight pressure gage. Stalibization of pressure in the literal sense is never obtained in a producing gas well. In formations of low permeability. such as those in the Hugo-ton Field, most wellhead working pressures approach stabilization closely enough to be used satisfactorily in the determination of a back-Pressure potential curve after flow periods of 24 hours. We shall therefore describe the backpressure curve calculated from ohserved rates of flow and working pressure at the end of 24-hour flow periods.

Jan 1, 1949

By G. W. Preckshot, C. E. Cottrell, D. L. Katz, N. D. Delisle

Most crude oils contain asphaltic substances that may be naturally or artificially precipitated. In the Greeley field, California, this asphaltic bitumen is precipitated during the flow of the oil from the reservoir to the stock tank The mechanism of such precipitation is not well understood. This paper presents the progress that has been made by using the electron microscope as a new tool and by observing the effects of the streaming potential on the formation of bitumen particles. Crude oils at atmospheric pressure viewed in the electron microscope in very thin films under a vacuum showed no asphaltic particles. A technique of preparing slides of thin films by dilution of the oil with benzene and washing in petroleum ether was used at first, and these observations showed that the solvents caused the formation of the particles, varying from 0.01 to 0.2 micron in diameter. The electrical effects of fluids flowing through porous solid were studied, with emphasis on the formation of colloidal particles by the streaming potential. The streaming potential of crude oil flowing through sand was measured and was shown to be responsible for the formation of bitumen particles. These results bring out a new phenomenon, which may occur when crude oil flows through the porous oil reservoir. mechanisms. Asphalt has been the subject of widespread investigation but, owing to the complexity of the substances being considered, progress has been slow. Investigators working primarily with the asphaltic substances have treated the subject from the colloidal standpoint and have developed theories that picture the asphaltic particles as surrounded by adsorbed materia1s.14,15,17,24 The deasphaltization of lubricating oil by the use of solvents treats the subject primarily from the standpoint of liquid-liquid equilibria.'' A complete understanding of asphaltic substances would make possible the following of the material from its initial state in the crude oil through precipitation processes to the final plastic stage, the most common form of which is used in asphaltic pavements. Since these asphaltic particles are very small, it appears 'hat the electron microscope4 might be a useful tool in studying the precipitation processes. Specimens are examined by the electron microscope in a vacuum and as very thin films, requiring special techniques in preparation of samples. A brief description of the electron microscope and its operation will bring out the difficulties and advantages of its use for this problem. The first work was done with crude oils that had been diluted with solvents for the preparation of the film to be examined. Later a technique was developed by which the undiluted oil film could be made thin enough for direct examination. These two techniques show vastly different results Asphaltic particles have been precipitated from crude oils by a variety of

Jan 1, 1943

By A. H. Larson, L. G. Twidwell

The influence which Au, Ag, Sb, Bi, Sn, and Cu have, both individually and collectively, on the activity coefficient of sulfur in liquid lead at 600"C zuas studied by circulating a H2S-Hz gas wlixture over a specific lead alloy until equilibrium was attained. Subsequently, the H2S concentration in the equilibrium gas mixture and sulfur concentration in the condensed phase were deterruined. The elements gold, silver, and antinzony (above 8 at. pct) increased the activity coefficient of sulfur. Bismuth had no apparent effect. Tin (above 3 at. pct) and copper decreased the coefficient. The influence of an individual element, i, on sulfur is best reported as the interaction parameter, riS, which is defined as The values o these first-order interaction zus are: ESzu = —55.0. These interaction parameters are used to predict the activity coefficient of sulfur in six fouv-component alloys and one seven-component alloy. Comparisons are made with direct experimental determinations. INTERACTIONS in dilute solution have been studied by many investigators. Most of the experimental work has been confined to solute-solvent interactions in simple binary systems and solute-solute interactions in ternary systems. Dealy and pehlke"~ have summarized the available literature on activity coefficients at infinite dilution in nonferrous binary alloys and have calculated from published data the values for interaction parameters in dilute nonferrous alloys. Interaction parameters are a convenient means of summarizing the effect of one solute species on another in a given solvent. Only a few investigators have studied interactions of the nonmetallic element sulfur in a metallic solvent. They are as follows: Rosenqvist,~ sulfur in silver; Rosenqvist and Cox,4 sulfur in steel; chipman, sulfur in alloy steels; Alcock and Richardson,% ulfur in copper alloys; Cheng and Alcock,' sulfur in iron, cobalt, and nickel; Cheng and ~lcock,' sulfur in lead and tin. The only reported work on the Pb-S system in the dilute-solution region is that of Cheng and Alcock.' Their investigation involved a study of the solubility of sulfur in liquid lead over the temperature range 500" to 680°C. The results may be summarized by the following relationship: S (dissolved in lead) + Pb(1) = PbS(s) log at. %S = -3388/T + 3.511 Experimentally, it was found that Henry's law was valid up to the solubility limit of sulfur in lead, i.e., at 600°C up to 0.43 pct. Their investigation did not include the study of sulfur in lead alloys. More accurate calculations could be made in smelting and refining systems if activity coefficients of solute species could be accurately predicted in complex solutions. One of the objectives of this study was to compare the experimental data with the values calculated from the equations derived from models for dilute solutions proposed by wagner9 and Alcock and Richardson. A temperature of 600°C was chosen as the experimental temperature to attain reasonable reaction rates and to minimize volatilization of the condensed phase. EXPERIMENTAL Materials. The Pb, Au, Ag, Sb, Bi, Sn, and Cu used for preparation of the alloys were American Smelting and Refining Co. research-grade materials. All were 99.999+ pct purity except the antimony and tin which were 99.99+ pct. The initial alloys prepared for this study consisted of twenty-one binary alloys, eleven ternary alloys, and one six-component alloy. The constituent elements were mixed for each desired alloy and were placed in a crucible machined from spectrographically pure graphite. The crucible was placed in a vycor tube which was evacuated with a vacuum pump and gettered by titanium sponge at 800°C for 8 to 12 hr. After the gettering was completed, the chamber containing the titanium was sealed and removed. The remaining sample chamber was placed in a tube furnace at 800°C for 2 hr and quenched in cold water. The final operation consisted of homogenization of the alloy for 1 to 2 weeks at a temperature just below the solidus for the individual system. The resulting master alloys were sectioned into small pieces and a random choice made for individual equilibrations. Cobalt sulfide (Cogs8) used to control the gas atmosphere in the circulation system was prepared by passing dried HzS for 24 hr over a Co-S mixture heated to 700°C in a tube furnace. This material was then mixed with cobalt metal to give a two-phase mixture which, when heated in hydrogen to a particular temperature, produced a desired H2S/H2 gas atmosphere in the circulation system. A Cu2S-Cu mixture also used in this study was prepared in a comparable manner. Apparatus for Equilibrium Measurements. The experimental technique of this study required apparatus

Jan 1, 1967

By Marius S. Darrow, William B. White, Rustum Roy

The PbS-PbTe systen has been studied by quench-ing and D.T.A. techniques f?om 400' to 1150°C. Runs were made in evacuated silica tubes so that all equilibria are at the vapor pressure of the system. Lattice parameters of the quenched salnples , measured by X-ray diffraction, show a complete crystalline-solution series existing over a narrow temperature range between approximately 805" and 871°C. An exsolution dome extends from a maximum of about 805"C (approximately 30 mole pct PbTe) to 1 and 96.5 pet PbTe at 400°C. A narrow melting region, deternined by D.T.A., extends form 918c (mp PbTe), The shapes of the liquides and solidus curves imply the existence of a minimum at 871°C at approximately 65 pct PbTe. THe exact composition of the minimum could not be established due to the very narrow two-phase region. At compositions containing less than 50 pet PbTe, liquidus temperatures begin to increase, while the solidus remains almost flat to about 15 mole pet PbTe before beginning to vise toward the mp of PbS (1075 C). LEAD sulfide and lead telluride are isostructural (NaC1 type) semiconductors whose electrical and optical properties have been extensively studied and used in recent years. If appreciable crystalline solution exists between these compounds, the variation of physical properties with composition could be of interest. The purpose of this investigation was to determine the extent, if any. of crystalline solution, and to obtain the phase diagram for the system. To the knowledge of the authors, only three studies of the system PbS-PbTe have been reported, and, in chronological order, each investigation found an increasing amount of crystalline solution. In 1956, Yamamoto reported finding no evidence of crystalline solution between the compounds. Sindeyeva and Godov-ikov,' in 1959, found very limited crystalline solution. but only under conditions of excess tellurium concentration. Finally Melevski s3 investigation in 1963 indicated that one solid phase exists in the region from PbS to 7 pct PbTe and from 82 pct PbTe to PbTe at 886'C, with an eutectic at 55 pct PbTe at that temperature. Detailed data on the solvus boundary were not given. EXPERIMENTAL EQUIPMENT AND MATERIALS Commercially produced PbTe and PbS powders were used as starting materials. Batches of specific mole percent composition were accurately weighed and mixed in a plastic bottle, in a shaker mill. An analy- sis of impurity content is given in Table I for pure PbS and PbTe and for two randomly selected batches after the powders were mixed. Individual samples, ranging in weight from 0.2 to 0.5 g, were sealed in evacuated silica tubes which had been thoroughly washed and rinsed with acetone and distilled water. Thus all data taken were at the pressure of the system. Subsolidus relations were studied down to 400°C by heating the samples in a vertical tube furnace for 24 hr. The sealed tubes were quenched in water with quench time from the hot zone not exceeding 1 sec. Temperatures were measured by a chromel-alumel thermocouple and controlled to 53°C for most runs. The number and composition of phases present were determined from powder X-ray diffraction patterns taken at room temperature on a Norelco diffractome-ter, using silicon as an external standard. Above 850°C quenching techniques were, in general, found to be unsatisfactory, and differential thermal analysis (D.T.A.) was used to determine melting relations. The evacuated tubes were recessed about 1 cm at one end to accommodate the differential thermocouple. Al203 was used as the reference material in a similar tube containing the other side of the differential couple. For temperature measurements, a separate thermocouple was placed in the recess of the tube containing the sample to be measured, thus providing an opportunity to obtain thermal, as well as differential, analysis. All thermocouples for these measurements were Pt-Pt 10 pct Rh. Temperature and differential curves were recorded separately on synchronized strip-chart recorders. Thermocouples and recording equipment were calibrated using NaCl and gold standards, using the melting points 801" and 1063 C, respectively, which span most of the temperature range of interest. Heating and cooling rates generally were from 4 to 7°C per min. It was found, in fact. that rates ranging from 1.5 to 25°C per min did not significantly change the data obtained.

Jan 1, 1967

By C. H. Li, R. J. Stokes

This paper compares the fracture behavior of tungsten rods in three conditions: recrystallized. recovered, and wrought. Notched specimens suhjected to a 50 in.-lb impact load showed ductile-brittle transitions at 700, 4.90°, and 440°C, respectinely. The recrystallized material had an equiaxed pain structure and jracbred by simple cleavage from a grain boundary source at all temperatures up to 700°C. The wrought and recovered material had an elongated fibrous structure and at low temperatures fractured by cleavage originating from the notch. As the transition temperature was approached cleavage was preceeded by more and more intergvanular splitting which deflected the crack front into planes parallel to the tensile axis. The enhanced toughness of wrought and recovered tungsten was attributed both to its inability to initiate cleavage because no pain boundaries were suitably oriented perpendicular to the tensile stress and to its inability to maintain cleavage because of intergranular splitting ahead of the crack. It has been appreciated for a long time in a qualitative manner that the room-temperature brittleness of fully recrystallized tungsten may be alleviated by working the material at relatively low temperatures.' More recently this difference in mechanical behavior between wrought and recrystallized tungsten has been examined quantitatively by measurement of the tensile properties as a function of temperature. In these experiments brittleness has been expressed in terms of ductility or reduction in cross-sectional area upon tensile fracture or in terms of the bend radius before fracture under bending.' This work has shown the existence of a fairly sharp transition from brittle to ductile behavior with an increase in temperature. The ductile-brittle transition temperature for recrystallized material is approximately 200°C higher than for wrought material. An increase in strain rate, small additions of impurity,' or an increase in grain size4 shift the respective transition temperatures to higher values, but the difference between them remains approximately the same at 200°C. A number of explanations for this embrittlement by recrystallization have been given. It has been blamed either on the concentration of impurity at the grain boundaries, the increase in grain size, or the change in texture which occurs upon recrystallization. The present paper examines the effect of different heat treatments on the notch-impact behavior of commercial powder-metallurgy tungsten rods. The change in the ductile-brittle transition temperature for this method of loading and the fracture mode has been related to the different mi-crostructures produced by heat treatment. EXPERIMENTAL PROCEDURE Commercial swaged powder-metallurgy tungsten rods 1-3/8 in. in length and 1/8 in. in diameter were machined to introduce a sharp V notch 0.030 in. deep. To change the microstructure from that of the as-received wrought material some of the specimens were subjected to an anneal in nitrogen either at 1300° or 1400°C for 8 hr or at 1600° or 2000°C for 1/2 hr. The notched rods were then placed in a miniature Charpy-type impact machine and struck at their midpoint (opposite the notch) with a hammer designed to deliver 50 in.-lbs of energy. The strain rate at the base of the notch was estimated to be approximately 100 sec-1 at the instant of impact. The specimens were heated in situ to the desired impact temperature. The microstructures produced by the various anneals were studied by both X-ray diffraction and metallographic techniques. Fig. 1 reproduces the microstructures observed metallographically following a 10-sec electroetch in a 10 pct KOH solution. Fig. l(a) shows the elongated fibrous grain structure of the as-received material. Following the anneal at 1300" or 1400°C the grain structure was still elongated as shown in Fig. l(b) but the etch pits delineated dense polygonized dislocation arrays within many of the grains. Occasionally a relatively dislocation-free recrystallized grain was found growing into the matrix. The anneals at 1600° and 2000°C resulted in complete recrystallization and some grain growth. The grains produced at 1600°C were still slightly elongated as shown in Fig. l(c) whereas the anneal at 2000°C produced equiaxed grains. The changes in grain size produced the expected changes in the X-ray back-reflection patterns; there was no indication either in the as-received material or the annealed material of any preferred orientation. RESULTS a) Impact Behavior. Fig. 2 reproduces the ductile-brittle transition curves measured in the manner described in the previous section. It can be seen that under these testing conditions the as-received

Jan 1, 1964

By Mark Malamphy

THE occurrence of outcrops of bituminous schists and sandstones impregnated with heavy asphaltic petroleum first directed attention to the Sao Pedro area as a possible source of commercial production of petroleum. Since 1920, more than 20 wells have been drilled in this area. The discovery of oil shows and small quantities of natural gas in some of the early wells led to the continuation of drilling in the hope that more important findings would result. During the early part of 1934, detailed magnetometer observations were made in this area, and a con-siderable number of torsion balance stations were occupied. The results of these geophysical observations help considerably to clarify the structure of the area and the very considerable amount of geologic information available makes possible a much more exact interpretation of geo-physical anomalies. In presenting the results of these observations, and interpretation of the geophysical data, certain actual case problems are included; i.e., geophysical anomalies due to anomalous masses of which the forms and positions are more or less known. Although anomalies due to igneous intrusions are probably more important to geophysicists in Brazil than in other countries, these data have a certain interest for all geophysicists, particularly because they were obtained in the south magnetic hemisphere, where the lines of magnetic force are directed upward, and in a region of moderately low inclination. This is considered as a geological-geophysical problem, and only passing mention will be given to the petroleum possibilities of the area.

Jan 1, 1936

By K. A. Jackson, G. A. Chadwick, A. Klugert

The diffusion field ahead of a lamellar interfnce is analyzed using an electrical analog. A self-consistent solution is obtained for the shape of the interfnce and the diffusion field by an iterative process. The solutions presented here are for a 50-50 eutectoid or eutectic, The shape of the interface is found to he independent of growth velocity and lamellar spacing, and to depend on the relative values of interfacial free energies at the phase houndaries . The mode of growth of lamellar eutectics and eutectoids has been a subject of much interest for many years.1-4 Mehl and Hagel 1 have shown photomicrographs taken by Tardif when he attempted to determine experimentally the shape of an advancing pearlite interface; the results are completely ambiguous. Brandt' and schei13 have made approximate calculations of the composition ahead of a lamellar growth front. The shape of the advancing front and the composition distribution ahead of the front are difficult to calculate because one depends on the other. It is the purpose of the present paper to describe a method by which this calculation has been done. Lamellar-eutectic growth usually occurs under conditions where the growth is fairly rapid, and the interface temperature is close to the eutectic temperature. The growth rate is usually determined by heat flow. Eutectoid growth, on the other hand, can best be studied by quenching to some temperature, and allowing growth to proceed isother-mally. In both cases the growth is believed to be controlled by diffusion* rather than by the atomic kinetics of the transformation. This being the case, a single treatment of the diffusion equation will apply to both cases, provided the region of the interface in a eutectic may be considered to be isothermal. If a part of the interface could appreciably change its thermodynamic driving force by advancing ahead of or lagging behind the mean interface, then the two cases would not be similar. Eutectics normally grow in temperature gradients of the or-der of a few degrees per centimeter. The normal eutectic spacing is the order of a few microns. Part of the interface would have to extend many lamellar spacings ahead of the mean interface before it experienced sensibly different conditions. The interface temperature is usually a few tenths of a degree below the eutectic temperature so that temperature differences of the order of one-thousandths of a degree (a displacement of one lamellar spacing) would be unimportant. Protrusions large compared to the mean spacing do occur when one phase only grows into a eutectic liquid. This is usually a dendritic type of growth, and easily distinguishable from the lamellar mode of growth. A single treatment of lamellar growth will apply equally well to both eutectic and eutectoid decomposition. At the interface, which as shown above is essentially isothermal, the difference between the equilibrium eutectic temperature Teu and the actual interface temperature Ti, can be divided into two parts: 1) the composition varies across the interface, so that the local equilibrium temperature is not Teu; and 2) the interface is curved, so that the local equilibrium temperature is depressed according to the Gibbs-Thompson relationship. This undercooling can be written as Teu-Ti =?T = mAC(x) + a/r(x) [1] where ?C(X) is the departure of the composition at a point x on the interface from the eutectic composition, see Fig. 1, r(x) is the local radius of curvature at a point x on the interface, m is the slope of the liquidus line on the phase diagram, and a is a constant given by where s is the interfacial free energy, TE is the equilibrium temperature, and L is the latent heat of fusion. The calculations in this paper will be made only for the case where the phase diagram is symmetric, that is, the eutectic occurs at 50 pct, the liquidi have the same magnitude slope m at the eutectic temperature, and C,, the amount of B rejected when unit volume of a freezes, see Fig. 2(a), is the same for both phases. As shown in Fig. 2(b), the composition ahead of the a phase will be rich in B, the composition ahead of the ß phase will be rich in A. The composition at the phase boundary is the eutectic composition. The difference between the local liquidus temperature and the actual tempera-

Jan 1, 1964

By J. Murray Riddell, Arthur E. Anderson, Grover J. Holt

Out of the depths of each business cycle we emerge with a stimulus for greater efficiency and a realization of progress in industrial technique. The recent years have not been an exception to this rule, and in retrospect we sense that significant advances have been made in mining practices on the Mesabi Range, with emphasis on speed of production and economy of operation. A survey of such changes does not reveal anything that is fundamentally or basically new, but it is apparent that ideas and machines that have found wide application in industry elsewhere, with necessary modifications, are being put to productive use in mining iron ore. Innovations in transporting and conveying ore from the open pits stand out with greatest prominence, so that, in the main, it will be with these features that this paper will treat, in the review of progress made to this date. The late years have witnessed the development of small deposits for open-pit operation, the cleaning up of pits nearing exhaustion, and in two large operations the approach to the limit for haulage by steam locomotives, owing to grades, making it necessary to recover the ore in slopes, track benches and below the power-shovel limit by a milling and scram operation. For several years small standard-type dump trucks have been used in clean-up or scram operations within the pits, but during the season of 1936 the first effort was made to use heavy truck haulage in the transportation of stripping and iron ore. The new units in use today vary from 15 to 20 tons in capacity, and are equipped with powerful gasoline or Diesel engines and supplemented by trailers or wagons on rubber or crawler treads. The Diesel engine finds favor with most operators because of fuel economy. These units develop upward of 125 hp. in the 15-ton trucks. The speed of these trucks varies from 2 miles per hour in Pow gear to 35 in high gear. The transmission affords 12 speeds forward and 3 speeds in reverse.

Jan 1, 1940