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By Bruce Chalmers, D. C. Larson

Aluminum crystals with longitudinal-axis orientations of (111) . (110), and (100) were deforined in tension and annealed. The conditions of deformation were controlled so that the re crystallization nuclei originated in either the heavily deformed regions at saw cuts {artificial nucleation) or in the lightly deformed matrix (spontaneous nucleation). The artificial-nucleatioln experiments showed that in lightly deformed (110) and (100) crystals low-angle twist boundaries are most mobile, while in (111> crystals and heavily deformed (110) and (100) crystals high-angle tilt boundaries with near (111) rotations are favored. The spontaneous-nucleation experiments showed the existence of preferred orientations in the (111) crystals. The nonrandomness of the grain orientations is quantitatively determined through a comparison with the results which would he obtained from a randowl set of grain ovientations. PREVIOUS recrystallization studies have been performed on single crystals deformed in tension.1 7 The crystals used in these studies usually had random tensile-axis orientations and the extent of deformation was not a primary consideration. The present study concerns the recrystallization of single crystals with tensile-axis orientations of (Ill), (110), and (100). The emphasis of this work is on the influence of the tensile-axis orientation and the degree of deformation on both the nucleation and growth processes. The multiple-slip orientations were chosen because secondary slip or slip intersection promotes nucleation.1,5,8 These crystals recrystallize at lower strains than the crystals which are oriented for single slip. Also, the greatest variation in deformation behavior is exhibited by the multiple-slip orientations. The stress-strain curves for crystals with tensile-axis orientations of (111) are higher than the stress-strain curves for poly-crystals, and the stress-strain curves for crystals with tensile-axis orientations of (100) are lower (at large strains) than the stress-strain curves for the crystals which deform initially in single slip.g The recrystallization nuclei originated in either 1) the homogeneously* deformed matrix of the crys- tals or 2) the heavily and inhomogeneously deformed regions at saw cuts. The nuclei will be referred to hereafter as spontaneous and artificial nuclei, respectively. The two terms do not imply a difference in the nature of the nuclei; they imply simply a difference in the mode of introduction of the nuclei. During spontaneous nucleation very few (always less than ten) grains nucleate, while during artificial nucleation large numbers of grains nucleate. Only a fraction of the artificially nucleated grains penetrate very far into the deformed matrix during annealing. The grains that penetrate the farthest into the deformed matrix will be referred to as the dominant grains. EXPERIMENTAL PROCEDURE The thirty-five crystals used in this investigation were grown from the melt in milled graphite boats at a rate of 1.6 cm per hr. The crystals had dimensions of approximately 6 by 12 by 80 or 6 by 6 by 80 mm and the aluminum was of 99.992 pet purity. The as-grown crystals were annealed at 610°C for 24 hr and furnace-cooled. They were then heavily etched and electropolished in a solution of five parts methanol to one part perchloric acid. The crystal orientations were obtained by back-reflection Laue photographs and were accurate to ±2 deg. The tensile-axis orientations were (loo), (110), and (111). Two of the side faces of the (111) crystals were (110) lanes. The (110) crystals had both {100) and {110) side faces and the (100) crystals had (100) side faces. The crystals were deformed at a strain rate of 0.003 per min. Shear stress and shear strain were obtained by multiplying and dividing the tensile stress and strain, respectively, by the Schmid factor, m. For the (111) crystals m = 0.272 and for the (110) and the (100) crystals m = 0.408. The Schmid factor is effectively constant during deformation for all orientations. The deformed crystals were sawed into 1-in.-long specimens while the crystals were totally enclosed in a graphite boat. The sawing was performed very carefully in order to limit the plastic deformation to the sawed regions. The specimens were electropolished in the solution mentioned above to remove the sawed-end deformation as well as controlled amounts of surface material. A special stainless-steel grip was used to hold the specimens during the electropolishing treatment. The gripping faces were flat, with no teeth, to prevent the introduction of extraneous de-

Jan 1, 1964

By AIME AIME

Russell B. Paul, Chairman of the Special Committee on Divisional Relationships, presented the interim report of his Committee which was published in the September, 1945, issue of MINING AND METALLURGY and a copy of which is incorporated in the official minutes of this meeting. The following specific actions were taken by the Board of Directors in relation to the six recommendations in the Summary of the Report as published: (1) Mr. Haider, Chairman of the Petroleum Division, presented the formal request of his Executive Committee that the headquarters of the new Secretary of the Petroleum Division be established in Dallas, Texas. After lengthy discussion in which the point was made that the success of this program would depend upon effective co-operation between the Chairman of the Division, the Secretary of the Petroleum Division, and the Secretary of the Institute, the request was approved. The new secretary will be selected by the Division and will be employed by the Institute in the capacity of an Assistant Secretary. (2) The following item in the report was approved:

Jan 1, 1945

By W. T. lsbell

HERCULANEUM, MO., about thirty miles south of St. Louis on the Mississippi River, is the site of the lead smelter of the St. Joseph Lead Co. The lead concentrates come by rail from the Flat River district and from three properties in Madison County, Missouri; from the Balmat division in St. Lawrence County, New York; a small tonnage from the Tri-State district; and occasionally from the Aguilar property in Argentina. The average grade is 67 to 68 percent lead and 1 to 3 oz of silver. The bulk of the material is flotation concentrate, with some gravity or table concentrate. No secondary metals, outside drosses, or any materials high in bismuth, arsenic, or antimony are treated. All concentrate is received in box-caps and is unloaded directly from a trestle into the concentrate bins at the roaster plant. Flux, coke, and any miscellaneous lead-bearing material is either unloaded directly into bins or unloaded with a locomotive crane. All moving and switching of cars is done with two thirty-ton steam locomotives. Shipping facilities for the plant are provided by the Missouri-Illinois Railroad. Water for the plant and for fire protection is obtained from a dam built in a near-by creek. Drinking water both for plant and town is obtained from

Jan 1, 1947

By Colin M. Sargent

ALTHOUGH annealing twins are frequently observed in many fcc metals, their occurrence in aluminum is relatively rare. ~ahn' in his review of twinning has listed only a few references to observations of twins in aluminum, e.g., Refs. 2 and 3. They have also been shown to occur in evaporated aluminum layers.4 During the present work, several annealing twins were studied in aluminum. The specimens of 1099-grade aluminum had the following thermomechanical treatment: deformed 90 pct by rolling, partially re-crystallized, further deformed 60 pct to a final thickness of 100 p, then annealed for 24 hr at 120°C. This treatment produced several annealing twins—-about ten per electron microscope specimen. The specimens were produced by the window technique and examined in a Phillips E.M. 200 operating at 100 kv. A typical twin boundary is shown in Fig. 1. For several of the twins studied the twin plane could be tilted so that it was parallel to the electron beam, e.g., Fig. 2. The associated diffraction pattern, Fig. 3, shows the twinned relationship between the grains. The twinning plane in each case was (111). Use of a reflection common to both the twin and the matrix,* i.e., using reflecting planes parallel in the twin and the matrix, the coherent twin boundary becomes invisible and only the noncoherent segments of the stepped boundary are seen, e.g., Fig. 4. Trace analysis of the boundaries showed that the long straight portions were invariably the twin plane; i.e., these portions are coherent. The planes of the shorter segments are shown by Fig. 5 to be (551 1, (7111, and {211).

Jan 1, 1969

By S. Wiederhorn

The energy and force of interaction between a crack and a slip band have been calculated. When the distance between the crack and the slip band is greater than the dislocation spacing of- the slip band, the force on the cgrack is perpendicular to the slip band. The energy needed to propagate a crack against this force can be lawe enough to pevmit crack propagation parallel to noncleavage planes. SEVERAL recent experiments have demonstrated the occurrence of crack-slip band interaction in ionic crystals having a NaC1-type structure. Stokes, Johnston, and Lil have studied the nucleation and growth of cracks in MgO. From their observations, they conclude that slip bands have the ability to halt and stabilize cleavage crack nuclei. Gilman2 has shown that a crack, propagating along a (100) cleavage plane in a previously deformed LiF crystal, tends, at certain points within the crystal, to switch to (110) planes. He reasons that plastic deformation reduces the cohesive energy of the (110) planes below that of the (1130) planes, making possible (110) crack propagation. Keh3 has demonstrated that when indentations are made in MgO, crkcks form along (110) planes at the indentations. Gilman2 attributes the formation of these cracks to plastic cieformation. There is some doubt as to the formation of cracks on (110) planes. Kuznetsov4 in his discussion of crack propagation in rock salt, shows that splitting along (110) planes requires 1.76 times as much energy as splitting along a stepped (100) surface. Therefore, the observed (110) cracking in LiF and

Jan 1, 1962

By Francois Clerf

IRON ORE fields are situated in both the East and West of France (see maps). The eastern deposit is by far the most important from a tonnage point of view, not only in France, but in all Europe. The ores of this region are known as minette, and are situated in the Lorraine ore fields and the Briey plateau. The iron ores of the West are those of Normandy, Anjou and Brittany. Before the war, a large number of important German companies had acquired considerable interests in these western fields and a heavy trade with Westphalia had begun. Recently, however, conditions have changed and some of the mines of Brittany and Anjou are now idle. From a geological point of view, in Anjou and Brittany, a series of synclines extends from the northwest to the southeast, containing a number of seams of varying thickness and generally intercalated in Silurian and sometimes in Devonian formations. The ore is generally a hematite or a magnetite. The composition varies from 48 to 52 per cent of iron and from 8 to 12 per cent of silica. Con¬servative estimates indicate a con¬siderable tonnage of workable ores (150,000,000 metric tons).

Jan 1, 1936

By B. H. Bergstrom, D. D. Crabtree, C. L. Sollenberger

Experimental data is given for several natural minerals on the load required for the fracture of single specimens over a very wide size range. The experimental results are compared with published data, such as for coal specimens from 30 to 64 in. in size. Correlations of the specific energy (per unit mass) required for fracture with specimen size are given as functions of specimen shape and the experimentally observed load-size relationships. These correlations are discussed with reference to comminution theory. Comminution, through compression or impact, can result only if sufficient force, or energy, is applied to a specimen of a given size. The relation of specimen size to force requirements has not been adequately considered previously. For single particle fracture, it was previously shown 1 that the specific energy (energy, e, per unit mass, M) at fracture of single glass spheres was inversely proportional to the product size modulus, k, as indicated in the equation: e/M = C/k [1] This was found true not only for numerous glass specimens of the same nominal size but was true for all nominal sizes tested from 1/8 to 1 in. Also, it was observed that the smaller spheres required a greater specific energy at fracture than the larger spheres and consequently had a smaller product size modulus. However, the relationship giving the required fracture energy as a function of specimen size was not further elaborated upon. This paper will extend the development of the feed size effect on specific fracture energy for brittle materials. SPECIFIC ENERGY-FEED SlZE RELATIONSHIPS FROM PREVIOUS DATA For the particular glass spheres tested in the previously described experiments,' it can be shown, as on Fig. 1, that the specific energy varied inversely as the 4/3 power approximately of the feed size, F, in the span of nominal sizes ranging from 1/8 to 1 in. The load at which a 3-in. diam glass sphere (a crystal gazer's ball) was broken was within the range predicted by an extrapolation of this energy-feed size relationship. The product size distribution from this

Jan 1, 1963

By D. A. Woodford

In a constant-load creep test, if the density of nlobile dislocations is assumed constant for strains exceeding that corvesponding to the minimum creep rate, it is shown that the creep rate may be approximated by the equation where E is the nominal strain, o0. is the initial stress, and a' the stress fov unit dislocation velocity. The constant C contains the mean density of mobile dislocations and n is a measure of the stress sensitivity of dislocation celocity. This equation is shoum to be applicable to published data on an alloy steel and on nickel. The degree of plastic instability and hence the creep ductility is dependent on the calue of n for these materials. When instability becomes gross and local macroscopic necking occurs, the assumptions are no longer valid. On the basis of this equation, and the strain-time relation derived from it, a method of predicting the creep behavior at different stresses is suggested. MOst analyses of creep data have been concerned with time-dependent transient creep or time-independ- ent secondary creep in constant-stress tests. The far more widely used constant-load test has been neglected in terms of a mechanistic approach. In general, since the strains involved are usually small, the same laws for transient creep may be applied to both types of tests. However, there is no steady-state creep in a constant-load test since the stress increases continuously. Any apparent steady state observed on a strain-time plot is either fortuitous or illusory, and is generally revealed as a continuously varying creep rate on a carefully constructed strain rate vs time plot.* Transient creep may be understood in terms of a simple differential equation representing the change in mobile dislocation density with time:' where p is the density of mobile dislocations. The first term on the right is related to first-order kinetics of dislocation multiDlication and the second to second-order kinetics of exhaustion. On the basis of this equation, several authors2-4 have found good agreement with experimental transient creep curves for a number of materials. When k1p = k2p2, a steady-state creep

Jan 1, 1968

By F. R. Brotzen, L. D. Whitmire

Single crystals of high-purity molybdenum were de-formed at temperatures from 195°to 473°K, and the effect of deformation on the electrical resistivily was deler-mined. To separale the resislivity components of point and line defecls some cryslals were annealed at 473°K. The vale of resislivily increase wilh strain was nearly linear and was strongly dependent upon the deformation temperature. Point dejects are annealed out without any effect on the flow stress. At low temperatures the flow stress is a linear function of the square root of the resistivity increase attributable to dislocations. ELECTRICAL-resistivity measurements have been used successfully to gain information on structural changes in metallic materials. During plastic deformation the electrical resistivity rises because of electron scattering from newly created lattice defects. Such measurements lend themselves, therefore, to corroborating results from direct observation of lattice defects and, to a certain extent, to correlating defect densities and distribution with mechanical properties. Published information on research with single crystals of the bcc metals of Group VI, particularly molybdenum, is still limited. Yet, molybdenum single crystals of relatively high purity can be readily prepared by electron-beam-melting techniques. Furthermore, some valuable information on the defect structure of deformed crystals by direct observation is available. Lawley and Gaigher,1 for example, have examined dislocation configurations in deformed molybdenum crystals by means of transmission electron microscopy. Their results revealed that the dislocation density and distribution were strongly dependent upon the deformation temperature. These findings differed from those by Keh and weissmann,2 who found that the average dislocation density in polycrystalline iron deformed between 138° and 298°K depended only on the degree of strain and not on the deformation temperature. Martin3 and peiffer4 showed that point defects introduced in polycrystalline molybdenum by cold work can be eliminated by annealing at a relatively low tempera-ture. In view of their work it became apparent that resistivity measurements of suitably annealed crystals could disclose changes in their dislocation structure and contribute to the understanding of the work hardening of molybdenum crystals. EXPERIMENTAL PROCEDURE Crystals were grown by electron-beam zone melting5,6 of 0.062-in.-diam molybdenum rods (99.99 pct) supplied by General Electric Lamp and Wire Division, Dover, Ohio. The crystals, about 4 in. long, were prepared by using five zone-refining passes at a speed of about 6 mm per min in a vacuum of about 5 X l0-6 Torr. The resistivity ratio of the crystal, p(4.Z°K)/p(273°K), was generally near 10-3. These crystals were used as tensile specimens of uniform diameter in the "as-grown" condition. They were oriented for maximum shear on the (011)[111] slip system (Schmid factor >0.49). The specimens were held in spherically seated Templin-type grips so as to minimize bending. Samples were deformed on an Instron machine at a strain rate of about 5 X 10-5 sec-1 in an isopentane bath with dry ice at 195°K, in ice water at 273°K, and in a vegetable-oil thermostat at 373° and 473°K. The temperature in the latter was maintained constant within +2°K. Resistance measurements were carried out with a Kelvin double bridge. The resistance of the potential leads was kept low by using large-diameter wires outside the low-temperature bath. Many of the resistance data were checked by measurements made with an ac bridge. Current and potential leads were spot-welded to the specimens. The distance between the potential leads, about 3 in., was also considered to be the gage length for the strain measurements. Diameter and gage length of the samples were measured optically with an error of less than 2 pct. These measurements were used also to insure that the deformation had been uniform over the gage length of the specimen. Resistivity changes were then determined from the resistance measurements at 4.2°K assuming constancy of volume. In the course of a test, the crystal diameter, gage length, and resistance at 4.2°K were determined first in the initial state and subsequently for various amounts of elongation.

Jan 1, 1968

By Davis Baker

The direct-metal cars or ladles of the Maryland Steel Company have a capacity of 18 tons when filled within 12 inches of the top. On account of this large capacity, the formation of skulls in these ladles is by no means as rapid as in smaller ladles; but a skull once formed is a very unwieldy piece of metal to handle, and especially to remove from the ladle. We have found it cheaper to clean ladles often rather than make very heavy skulls. We aim to keep the ring of chilled metal that forms on the surface of the iron chipped off, so that the skull shall form principally at the bottom until it becomes so thick as to render the ladle unfit for service. Sometimes it happens that a ladle may be held for several hours filled with molten metal. This invariably leaves a large amount of chilled metal in the ladle. Frequently the skull will weigh several tons, and will be of the full size of the ladle inside, with a top crust, having perhaps a hole 12 inches square, through which the molten metal was poured. In order to remove skulls that cannot be easily chipped out with a bar, we use what may be called a skull-extractor, consisting of a hydraulic cylinder mounted in the center of a heavy cast-iron plate, standing vertically on a suitable foundation. Figs. 1 and 2 show the construction and operation of this apparatus, Fig. 1 being a view of the extractor with pistons extended to full stroke, and Fig. 2 a view with ladle in position and pistons about to commence the stroke. in both figures, A is the hydraulic cylinder, B the vertical cast-iron plate, and C the foundation. The water-pressure, admitted through the pipe, P, is 750 pounds per square inch, and the inside diameter of A is 14 inches. There are two pistons: D, fitting the bore of the cylinder, and E, 84 inches in diameter, moving inside of D. Both pistons move together when

Jan 1, 1893

By Klaus Detert, Joseph Ziebs

The progress of primary recrystallization has been studied in alloys of nickel with 0.01, 0.1, and 1.0 at. pct Ta. It can be shown that in one particular alloy containing 0.1 Ta and 0.02 02 a large grain structure (0.5 mm diameter) could he developed by primary recrystallization in thin sheetswhich were cold-worked to 97.5 pct reduction in thickness. Electron transmission microscopy demmstrates that this phenonmena was linked to the occurrence of fine precipitates at subboundaries. A discussion of how fine precipitates can exert under certain circumstances a rather distinct retarding effect on nucleation rate is included. IN a former investigation, the recrystallization and texture formation in a series of binary nickel alloys including pure nickel were studied.' Nickel alloys with some tantalum added displayed peculiarities during primary recrystallization which have been studied in more detail by the present investigation. The alloys were prepared by powder-metallurgy techniques similar to the previous investigations.' Pure metal powders were thoroughly mixed to obtain alloys with 0.01, 0.1, and 1.0 at. pct Ta, referred to as alloy A, B, or C, respectively. The metallic impurities were kept below 0.005 at. pct except iron and cobalt with slightly higher values, by using highly purified nickel and tantalum powders.' The mixtures were pressed into bars and sintered at a temperature of 1300°C. The sintering atmosphere was either high vacuum, dry hydrogen, or wet hydrogen. The sintered rectangular bars were rolled 60 pct to a thickness of 3 mm, then annealed under dry hydrogen at 1000°C and again cold-rolled to about 97.5 pct reduction of thickness. After this heavy deformation, the sheet thickness was 0.07 5 mm. In order to study primary recrystallization which occurred in measurable times between 400" and 600°C, samples of the rolled sheets were annealed in a salt bath at various temperatures for various times in order to study the progress of recrystallization by hardness measurements and microscopic examination. For optical observation, the samples were polished and etched in a solution of 65 cu cm HNO3, and 18 cu cm acetic acid in 20 to 100 cu cm H2O, depending of the particular sample and annealing treatment. For transmission electron microscopic observations, thin foils were prepared by the combined window and Bollmann techniques.273 The electrolyte consisted of 23 pct perchloric acid and 77 pct acetic acid held at 15°C. Polishing was performed at a current density of 0.4 amp per sq cm. The examination of the thin films was accomplished by a Siemens Elmiscope-type electron microscope operating with an accelerating voltage of 100 kv. RESULTS The progress of primary recrystallization was very accurately followed in these alloys in order to establish the time when recrystallization started and ended during an isothermal anneal. Table I gives some of the data obtained by these studies. The time for beginning is a mean value, where somewhat less than 5 pct of the matrix has recrys-tallized. The end of recrystallization is the time when at least 95 pct of the matrix has recrystal-lized. Listed are three different B alloys, with 0.1 Ta distinguished by different sintering atmospheres which influence the rate of primary recrystallization. By the above method, the state of the grain structure when primary recrystallization was completed, but grain coarsening had not started, could be clearly defined. The average grain diameter of the recrystallized matrix is also given in Table I. The grain size did not depend on the temperature of the isothermal anneal. With one exception the grain size of the primary recrystallized matrix was found to be rather fine

Jan 1, 1965

All the TECHNICAL PUBLICATIONS and CONTRIBUTIONS published in 1938 are available at Institute headquarters, unless otherwise noted. They are also on file in many public, university and technical libraries and, when so indicated in the list, may be found in the TRANSACTIONS. TECHNICAL PUBLICATIONS in Classes A-Metal A-Lining, B-Milling and Concen-tration, H-Industrial Minerals, and I-Mining Geology are distributed in MINING TECHNOLOGY, which is issued every other month. Technical Publications in Classes C-Iron and Steel Division, D-Nonferrous Metallurgy and E-Institute of Metals Division are distributed in METALS TECHNOLOGY, which is issued twice quarterly. TECHNICAL PUBLICATIONS ill Class G-Petroleum Division are distributed in PETRO-LEUM TECHNOLOGY, which is issued quarterly. TECHNICAL PUBLICATIONS in Classes F-Coal Division, .l-Mineral Industry Education Division, K-Mining Administra-tion, and L-Geophysical Methods of Exploration are issued as separate pamphlets. All Institute member is entitled to one copy of any TECHNICAL PUBLICATION or CON-TRIBUTION. Copies of TECHNICAL PUBLICATIONS listed have been mailed to members of the Institute according to their registration by classes. CONTRIBUTIONS and other TECHNICAL PUBLICATIONS will he sent upon request. A member may purchase an additional copy of a TECHNICAL PUBLICATION or a CONTRIBUTION at one cent. a page; in minimum charge, 256. If the TECHNICAL PUBLICATION has been published in METALS TECHNOLOGY, MINING TECHNOLOGY or PETROLEUM TECHNOLOGY, the number of either magazine containing it will be supplied at the sae cent a page (minimum charge, 25¢) rate for the particular TECHNICAL PUBLICATION requested. Nonmembers may purchase any CONTRIBUTION or a TECHNICAL PUBLICATION Of the F, J, K, or L classes at the same rate, butt the nonmember price per copy for METALS TECHNOLOGY, MINING TECHNOLOGY or PETROLEUM TECHNOLOGY is $1. TECHNICAL PUBLICATIONS (Separate pamphlet form), $2 per annum; Canadian and foreign postage 50 cents extra. METALS TECHNOLOGY, $7 per annum; Canadian and foreign postage 50 cents extra (Iron and Steel Division and Institute of Metals Division ferrous and nonferrous papers). MINING TECHNOLOGY, $6 per annum; Canadian and foreign postage 50 cents extra (metal mining, milling and concentration, Industrial Minerals Division, and mining geology papers). PETROLEUM TECHNOLOGY, $4 per annum; Canadian and foreign postage 50 cents extra.

Jan 1, 1938

By Eugene A. Stephenson

NUMBER of noteworthy events in the petroleum industry may be reported for 1941, of which the most spectacular was doubtless the rise in the daily rate of crude-oil production to a peak of approximately 4,300,000 barrels. This enormous daily rate did not ensue from the furor of flush pools but represented for the most part merely a slight additional daily delivery from many wells that had previously been operated on a more restricted basis, in line with good conservation practice and also from the adroit increase in the number of days per week by the Texas Railroad Commission. Another important fact was the increase in price throughout the Mid-Continent area from the static level of $1.02 for 36°, A.P.I., crude, to $1.17 per barrel. Efforts to elevate the price above this point have met with severe opposition from the O.P.A.. as has also a similar effort by the PennsyIvania Crude Oil Producers' Association, but the vastly increased costs for materials and labor may shortly give the industry the enhanced price which it has long deserved.

Jan 1, 1942

By J. R. Low, D. F. Stein

Single crystals of iron have been grown from three different lots of Ferrovac "E" of somewhat different chemical composition by the strain anneal technique. Using a technique to seed the crystal similar to Dunn's for silicon-iron, it has been possible to orient the crystals grown in both direction and plane of growth. Crystals having the plane of the strip oriented (100) , (110), (111), (112), (123), and (491) have been grown. The growth directions used have been [100], [110], 45 deg from a [110}, and various others of no specific crystal orientation. The usual dimensions of the crystals were 8 by 1 by 0.08 in. Attempts to grow crystals were about 90 pct successful. METHODS of growing single crystals of high purity iron have been reported in the literature.1-4 However, each of these methods was not completely reliable when used on materials having slightly different chemical composition and in some instances a small number of successes were obtained using identical materials. Except for the method used by S. Dohi and T. Yamoshita,1 it has not been possible to reorient single crystals of high purity iron to give any desired orientation. The method to be described has made it possible to grow single crystals from three different lots of material having different compositions, and to orient the crystals with respect to growth direction and surface. STARTING MATERIAL The material used during this investigation was a vacuum melted high purity iron marketed by the Vacuum Metals Corporation designated Ferrovac "E." Three lots of Ferrovac "E" having the following composition were used with equal success: The compositions listed are those of the as-received material; and they may have been modified before the growth of single crystals. Analysis of heat B just before growth and after growth revealed that the heat treatment prior to growth did not change the carbon content, but the oxygen content was changed from 0.0092 pct to 0.0034 pct and the nitrogen content from 0.0003 pct to 0.0001 pct. After growth of the single crystals, the carbon had dropped to 0.001 pct. None of the heat treatments would be expected to change any of the other impurities very markedly. Heat C would be expected to have a metallic impurity content similar to heats A and B. PROCEDURE Ferrovac "E" iron which had been obtained in bar form having a diameter of about 1 in. was rolled into strip for growing single crystals. By passing the 1-in. bar through a cold rolling mill several times, it was reduced to a strip 0.15 in. thick. The strips obtained were then cut into suitable lengths for heat treating (about 9 in. long), annealed at 925°C for 2 hr in dry hydrogen and water quenched. It was then necessary to bake the strip at 200°C for 24 hr in air in order to prevent cracking during further rolling operations. While it was possible to cold roll the 1-in. bar directly to the desired 0.080-in. strip, the intermediate anneal was used because the strip so obtained produced better single crystals. The strip obtained by rolling the 1 -in. bar directly to 0.080-in. strip produced single crystals having a large number of occluded grains. Experiments showed that the optimum reduction in area by rolling prior to the growth of single crystals was about 50 pct. Attempts to grow single crystals from material that had been reduced less than 40 pct were unsuccessful presumably because the matrix did not possess the critical amount of texture necessary for growth. The strip obtained after the rolling operations had very irregular edges which were ground to give a strip with uniform dimensions. The strip was then annealed at 825°C for 3 hr in hydrogen and furnace cooled. Fig. 1 illustrates the grain size obtained. A temperature of 940°C was used for the annealing temperature on one group of strips

Jan 1, 1962

By E. A. Nesbitt

THE important permanent-magnet alloys 15 years ago contained carbon and depended upon it for their permanent- magnet properties. In recent years great, advances have been made in a number of new alloys substantially free of carbon. These include Remalloy,l an alloy of iron, cobalt, and molybdenum, the various iron- nickel-aluminum alloys of the Mishima2 type, and the more recent Alnico V3 in which the best properties are developed by heat-treating in a magnetic field. The Mishima and the Alnico types of alloys are very brittle and after casting must be ground to size. This article describes a permanent-magnet material4 that can be machined as cast, and when handled with some care can be .rolled to thin sheet and drawn to fine wire. Optimum magnetic properties are developed by a simple heat- treatment, and at this time the ductility A of the alloy disappears. If the cast alloy is heat-treated without cold-working the magnetic energy product is about 1.0 X 106. This material is called Vicalloy I (pronounced vicalloy, V for vanadium, I for iron, and C for cobalt). When the alloy is first hot-worked and then considerably reduced in area by cold-swaging, drawing or grooved rolling, it is found that after heat-treatment the magnetic energy product measured in the direction of previous extension can be increased to 2.0 to 3.5 X l06. These higher values have been obtained only after reductions in area of 75 to 95 per cent, and since the material hardens considerably during working, the reduction ordinarily can be accomplished only in fine wires, although larger sizes can be reduced by the use of powerful machinery. When the material has been cold- worked in such a manner as to improve its energy product substantially, it is called Vicalloy II. Commercial use of Vicalloy has been made in the recording of speech. Tape 0.002 by 0.050 in. has been found superior in quality to all others tried, and is now used in the Western Electric Mirrorphone In a variety of forms Vicalloy I or II is useful in many laboratory instruments, and in experiments in which the sizes and shapes required cannot be obtained with the other more brittle permanent-magnet materials. In 1936, during a study of other age- hardening magnetic systems, it occurred to the author that some of the iron-cobalt-vanadium alloys might be suitable for permanent magnets. The proportions of iron, cobalt, and vanadium were varied and a range of alloys of particular interest was found, as shown by the indicated area in Fig. I. The limits of this range of com- position are 30 to 52 per cent iron, 36 to 62 per cent cobalt, and 4 to 16 per cent vanadium. The compositions indicated by points outside this area were also tested. PREPARATION AND PROPERTIES OF VICALLY I The alloys were usually cast in graphite molds into bars ¾ in. in diameter and

Jan 1, 1946

By D. H. Turner, F. A. Crossley

The titanium-rich corner of the system Ti-Al-Si has been studied to determine the phase relationships in the temperature interval 600° to 1200°C. Metallographic examination of long time isothermally annealed specimens was the means of investigation. PART of a program on phase relations and transformation processes of titanium alloy systems included the study of the titanium-rich corner of the Ti-Al-Si system. The investigation covered ternary compositions in the range 2 to 8 pet A1 and 0.1 to 2 pet Si and binary compositions in the range 0.2 to 2 pet Si. Temperatures were in the range of 600" to 1200°C. Alloys containing 6 pet A1-0.1 to 0.5 pet Si were investigated down to 400°C. Partial vertical sections are presented for 2, 4, 6, and 8 pet Al. The Ti-Si system has been reported by Hansen et al.' It is characterized by a eutectoid decomposition, ß = ± a + Ti3Si3, at 860°C. The maximum solubility of silicon in a is reported to be about 0.5 pet at the eutectoid temperature. The solubility of silicon in 0 increases from 0.9 pet at the eutectoid temperature to approximately 3 pet at the eutectic temperature, 1330°C. Several investigations in the composition range of interest have been reported for the Ti-A1 system."' These investigations are in agreement on the phase fields, but differ to small extents on boundary positions. However, very recent, and as yet unpublished, findings" " indicate that there are perhaps two phases which occur at lower aluminum contents than the ? (TiA1) phase, and that the solubility of aluminum in a titanium is less than 6 pet. In the present investigation phase relations found are in agreement with the published literature exemplified by the work of Bumps et al.3 Therefore, it is probable that the partial system reported herein is metastable and does not represent true equilibrium. Experimental Procedure High purity Bureau of Mines titanium sponge of 103 Bhn hardness, granulated aluminum shot of 99.7 pet purity, and silicon powder of 99.8 pet purity were used in making the alloys. For the work in the range from 600" to 1200°C, 100 g ingots were prepared by arc melting. Melting losses were negligible and spot checks by chemical analysis showed good agreement between nominal and analyzed results. Nominal compositions are used throughout this paper. Ingots were forged to 3/8 in. rounds and cut into specimens for heat treatment. Isothermal anneals in the range from 600" to 900°C were preceded by solution treatment at 1000°C for 1 hr, followed by furnace cooling to the annealing temperature. Samples were sealed in evacuated Vycor bulbs for heat treatments up to 1000°C. Higher temperature anneals were done with the samples sealed in quartz bulbs under a partial pressure of argon.

Jan 1, 1959

By B. DE MARE

THE No. 6 open-hearth furnace at the plant of the Worth Steel Co., Claymont, Del., is the first to be rebuilt according to the Kuehn system. This as well as the other five furnaces at Claymont, has a nominal capacity of 75 tons, but the actual charge is about 242,000 lb. No hot metal being available, the pig-iron is charged cold. Oil of low grade with an asphalt base is used as fuel. These two items have to be kept in mind when discussing the actual fuel consumption. Careful records have been kept covering a five weeks run and the following is a brief summary of them The time required to heat the furnace preparatory to charging from the time a wood fire was started until charging commenced was 36 hours. This, I understand, is much less than with furnaces of standard design. The draft of the furnace, as shown by a gage in the stack-flue, is 1.25 in. The maximum draft with new checkers on former runs was 1.50 in., this draft gradu¬ally decreasing as the checkers closed up. Both of the first helpers claim the present draft is all they need for the proper working of the furnace, and, as with the Kuehn regenerators the draft remains practically the same from beginning to end of a run, this is satisfactory.

Jan 1, 1929

By R. Silent, N. A. Rousselot

The first producing wells completed in the Kettleman Hills arca were noteworthy for their high gas-oil ratios. As a result they became the object of criticism, and controversies arose based on their alleged lack of gas conservation. Ultimately protracted hearings ensued in the District Court of the area, and diverse rulings and subsequent modifications have been handed down affecting the permissible gas-oil ratios. When the Kettleman North Dome Association was formed in April, 1931, and the control of the major portion of the North Dome area vested therein, it was decided to produce only those wells which had a relatively low gas-oil ratio. Among the wells having the highest gas-oil ratio were the Milham Elliott No. 1 (the discovery well) and the Continental Elliott 12-8. drilled as an offset to it. Under the numbering system adopted by the Kettleman North Dome Association, these wells are now known as 88-2P and 1-12P, respectively. Milham Elliott No. 1 was originally drilled to 7236 ft., then redrilled to 7108 ft. The upper portion of the Temblor Horizon produces with a very large gas-oil ratio; production which actually consists of light crude oil with an accompanying large.volume of gas. Little was known as to the location of the Temblor formation at that time but it is now generally accepted that its top was encountered at 6180 ft., giving 928 ft. of penetration. Initial production was estimated at 4000 bbl. of oil and 80 to 90 million cubic feet of gas per day, giving a gas-oil ratio in excess of 20,000 cu. ft. of gas per bbl. of oil. This ultimately increased to a ratio of about 48,000 at the time the well was killed when it was producing about 1100 bbl. of oil and 52 million cubic feet of gas, with a flow pressure of 1200 pounds. The Continental Elliott 12-8 was drilled to a depth of 6876 ft. with the top of the Temblor at 6100, giving a penetration of 776 ft. The estimated initial production of this well was 7000 bbl. of oil and 130

Jan 1, 1933

By Haydn H. Murray, Sam H. Patterson

The term "clay" is somewhat ambiguous un¬less specifically defined, because it is used in three ways: (1) as a diverse group of fine-¬grained minerals, (2) as a rock term, and (3) as a particle-size term. Actually, most persons using the term "clay" realize that it has several meanings, and in most instances they define it. As a rock term, clay is difficult to define be¬cause of the wide variety of materials that com¬pose it; therefore, the definition must be gen¬eral. Clay is a natural earthy, fine-grained ma¬terial composed largely of a group of crystalline minerals known as the clay minerals. These minerals are hydrous silicates composed mainly of silica, alumina, and water. Several of these minerals also contain appreciable quantities of iron, alkalies, and alkaline earths. Many defini¬tions state that a clay is plastic when wet. Most clay materials do have this property, but some clays are not plastic; for example, halloysite and flint clay. As a particle-size term, clay is used for the category that includes the smallest particles. The maximum-size particles in the clay-size grade are defined differently on various grade scales, Soil investigators and mineralogists gen¬erally use 2 micrometers as the maximum size, whereas the widely used scale by Wentworth (1922) defines clay as material finer than ap¬proximately 4 micrometers. Some authorities find it convenient to use the term "clay" for any fine-grained, natural, earthy, argillaceous material (Grim, 1968). When used this way, the term includes clay, shale, or ar¬gillite, and some argillaceous soils. Even though no standard definition of the term clay is accepted by geologists, agronomists, engineers, and others, the term is generally un¬derstood by those who use it. Clay is an abun¬dant natural raw material, and it has an amaz¬ing variety of uses and properties which will be discussed in this chapter. Clays rank among the leading industrial min¬erals in both tonnages produced and total value. Their importance is indicated in Table 1, which lists the 1970, 1971, and 1972 production and values according to the U.S. Bureau of Mines (Ampian, 1972). Adequate reliable statistical data on which to summarize world production of clay are un¬available; this paragraph outlines the world re¬quirements for clay only in a very general way. According to one estimate, the world bentonite production in 1972 was 3.5 million tons (Anon., 1973a), but in the authors' opinion it was prob¬ably at least 5 million tons. The total fuller's earth produced was at least 1.5 million tons and may have been as much as 2 million tons. The total world kaolin production in 1972 was more than 10 million tons. Approximately 7 million tons of this total was produced in only two regions-the Georgia-South Carolina kaolin belt in the United States and the Cornwall re¬gion, United Kingdom. The world's 1972 out¬put of ball clay, which is also produced pri¬marily in the United States and the United Kingdom, was approximately 1.5 million tons or perhaps a little more. The total world fire clay production in 1972 was probably about one and one-half to two times and the miscellaneous clay production three times the United States production. As industrial minerals, clays are a complex group that consists of several mineral commodi¬ties, each having somewhat different mineral¬ogy, geologic occurrence, technology, and uses. In this chapter these commodities are organized

Jan 1, 1975

By Ed Van Eeckhout

As part of a U.S. Bureau of Mines-sponsored project on the utilization of "stiff" backfill to minimize potential rock burst hazards, a finite element study was undertaken to predict stresses and displacements around a stope mined up from the 5400 level of the Sunshine mine, Kellogg, Idaho. This stope was to be backfilled using a high-modulus fill. In preparation for that configuration, certain instrumentation was installed near the 5400 level to monitor stress changes. Due to untenable economics, only 2 cuts of the stope were ever made. This paper presents the results of the instrument readings taken during the first cut and compares them with the numerical predictions, as well as presents the modeling results of closure and fill stresses in the stope if it had been mined.

Jan 1, 1984