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By R. L. Slobod, H. A. Blum

A semiquantitative method for measuring the wettability of reservoir rocks has been developed. These data are needed for reservoir analysis and for interpretation of laboratory displacement studies. The wettability of a core sample is measured by the contact angle for the system oil-water-solid. These contact angles are calculated from the displacement pressure (threshold pressure) obtained by use of the centrifuge, using first oil-water and second air-oil in the same core sample. This method is based on the assumption that the air-oil and oil-water interfaces occupy similar positions in the porous medium when desaturation of the wetting phase is initiated. The assumption is also made that the Contact angle for the air-oil-solid system which is close to zero in value does not change appreciably even when the contact angle for the oil-water-solid system experiences marked changes. "Apparent contact angles'' for five different solids ranging from 31" to 82" have been determined, and changes irr the "apparent contact angle" of a given sample with laboratory use from 33" to 53' {lave been observed. INTRODUCTION Reservoir rocks vary in their wettability, 1,2,3,4 some being preferentially water wet while other are apparently preferentially oil wet. The degree of wettability, in theory, is measured quantitatively by the contact angle for the system solid-oil-water, hut in 1)practice this quantity is extremely difficult to determine." The need for obtaining some measure of this quantity has become obvious in recent years as a result of both laboratory. and field observations. Several reservoir.: such as the Bradford Sand in Pennsylvania and the Wilcox' at Oklahoma City are reported to be oil wet. If these report:: correctly reflect the true nature of the surface of the rock in the ground, then these reservoirs probably will not perform as predicted on the basis of a water wet rock. In the laboratory many core samples have been Observed to be oil wet. These samples, while perhaps not correctly representing the reservoir, have markedly different properties from water wet rock. The location of the phases is different (oil is in contact with rock instead of water), and other quantities such as the connate water, the capillary pressure curve; residual oil. relative permeabilities. and the recovery of oil by water flooding are markedly affected by the value of the contact -4 A further complication observed in the laboratory is the chang-ing of the wettability of a rock specimen with use. such changes mean that repeat runs on the same core are not the duplicate tests desired, but represent new experiments on a more oil wet material. The changes in surface characteristics are sometimes so rapid that by the time an experiment requiring several days is completed, the results may not be representative of the core as originally described, The, rock material itself (Silica. carbonates. etc.), whell Clean and uncontaminated, is water wet. There seems b( : little evidence of the presence of oil wet minerals such as heavy metal sulfides. The oil wetness of reservoir samples, therefore, is believed to be caused by the accumulation of an adsorbed film in which the polar group of a large organic. molecule is adsorbed on the surface leaving the organic or hydrocarbon part of the molecule projecting out from the solid. Such a surface is much more readily wet 17" oil than by water. These considerations indicate the need for a method which will provide some measure of tile wettalbility (Contact(angle if possible) for reservoir rock ..samples) The method should be capable of (1.1 distinguishing between tile wettalility of dif. ferent formation,.. (2) detecting (change. ill wettalbility of a core with use. and (3) measuring the changes in Wettability which may be accomplished with cleaning operations. such as the use of sodium silicate for increasing water wrettalbility." A preliminary report on such a method is preseted below. not with the idea that this procedure alone will Solve the wettabil-ity problem. but rather that it may provide encouragement to

Jan 1, 1952

INTRODUCTION Much discussion has been generated over the years among geologists and engineers as to the ideal drill-hole configuration and spacing for evaluating various types of mineral deposits. Little can be found in the literature about the outcome of the programs, probably because of their subjective nature and the then lack of suitable means of scientific testing. In years past the drilling patterns and sequence were almost entirely determined by the experience and personal bias of the senior engineer, geologist, or project manager on the job. However, planning a drilling program- spacing, pattern, sequencing, etc.-is simply a specific case of sample design, or the design of a sampling program. Having been exposed in the preceding chapter to the theory of regionalized variables, and having learned something about the tools for measuring correlation, or lack of correlation, among samples within a given mineralogical population, we are now prepared to apply these concepts and new-found parameters to a scientifically designed mineral sampling program, be it by drilling or other means. FACTORS IN SAMPLING DESIGN It was shown in Chapter 8 that three major factors should be considered in any mineral

Jan 1, 1980

By A. A. Jr. Smith, J. S. Smart

The controlled amounts of phosphorus, arsenic, sulphur or selenium found in commercial coppers perform a variety of highly useful functions. Indeed, a large segment of modern copper technology is essentially dependent upon the presence of one or more of these elements. Consequently, the literature contains many references to their effects but the scope is broad and has been only partly covered. New data are presented herewith directed toward a better understanding of the basic behavior of these elements in copper, with particular emphasis on the composition range o to 0.05 per cent. These data are a part of a general program of research on the effects of impurities on the properties of oxygen-bearing and oxygen-free copper, other portions of which have been reported previously. Schematically, the behavior of individual elements is determined from measurements of conductivity and softening temperature,'v2 and the binary alloys employed are synthesized from high-purity copper in order to eliminate interference from the effects of extraneous impurities. Alloys of selected composition were first prepared in the oxygen-free form by continuously casting the melts in the form of %-in. diameter rod. Oxygen was added subsequently to portions of the alloys, either by remelting or by diffusion at 8jo°C. from a surface scale. Test wires wcre drawn one B. and S. number per pass, using four 30-min. 600°C. anneals at 0.3125, 0.257, 0.204 and 0.162 in., and a final cold reduction of 75 per cent to 0.081 in. Oxygen-bearing slugs made by remelting nere hot-rolled to 4ia in.. drawn to 0.162 in., annealed for 30 min. at 6o0°C. and cold-drawn 75 per cent to 0.081 inch. The alloys containing phosphorus, having been compounded very early in the program, were prepared in the form of 3i6-in. rod, and processed to wire with only the last three intermediate anneals listed above, all of these having been conducted in commercial nitrogen. In addition, the conductivity anneals on these alloys were also performed in the same atmosphere, and the small amount of oxygen present as an impurity in the gas resulted in some loss of accuracy at temperatures of 700' to 8o0°C., as will be shown later. Subsequently, the anneals for all oxygen-free alloys were conducted in hydrogen to prevent oxidation, and purified nitrogen was employed only for oxygen-bearing samples. All conductivity anneals wcre of one hour duration followed by a rapid quench in 10 per cent HZSO*. Effect of Phosphorus The widespread use of phosphorus as a deoxidant has resulted in universal appreci-

Jan 1, 1946

By A. A. Jr. Smith, J. S. Smart

The controlled amounts of phosphorus, arsenic, sulphur or selenium found in commercial coppers perform a variety of highly useful functions. Indeed, a large segment of modern copper technology is essentially dependent upon the presence of one or more of these elements. Consequently, the literature contains many references to their effects but the scope is broad and has been only partly covered. New data are presented herewith directed toward a better understanding of the basic behavior of these elements in copper, with particular emphasis on the composition range o to 0.05 per cent. These data are a part of a general program of research on the effects of impurities on the properties of oxygen-bearing and oxygen-free copper, other portions of which have been reported previously. Schematically, the behavior of individual elements is determined from measurements of conductivity and softening temperature,'v2 and the binary alloys employed are synthesized from high-purity copper in order to eliminate interference from the effects of extraneous impurities. Alloys of selected composition were first prepared in the oxygen-free form by continuously casting the melts in the form of %-in. diameter rod. Oxygen was added subsequently to portions of the alloys, either by remelting or by diffusion at 8jo°C. from a surface scale. Test wires wcre drawn one B. and S. number per pass, using four 30-min. 600°C. anneals at 0.3125, 0.257, 0.204 and 0.162 in., and a final cold reduction of 75 per cent to 0.081 in. Oxygen-bearing slugs made by remelting nere hot-rolled to 4ia in.. drawn to 0.162 in., annealed for 30 min. at 6o0°C. and cold-drawn 75 per cent to 0.081 inch. The alloys containing phosphorus, having been compounded very early in the program, were prepared in the form of 3i6-in. rod, and processed to wire with only the last three intermediate anneals listed above, all of these having been conducted in commercial nitrogen. In addition, the conductivity anneals on these alloys were also performed in the same atmosphere, and the small amount of oxygen present as an impurity in the gas resulted in some loss of accuracy at temperatures of 700' to 8o0°C., as will be shown later. Subsequently, the anneals for all oxygen-free alloys were conducted in hydrogen to prevent oxidation, and purified nitrogen was employed only for oxygen-bearing samples. All conductivity anneals wcre of one hour duration followed by a rapid quench in 10 per cent HZSO*. Effect of Phosphorus The widespread use of phosphorus as a deoxidant has resulted in universal appreci-

Jan 1, 1946

By Charles Y. Clayton

THE general public does not know that there is such a thing as metallurgy and it is very seldom that you see the word metallurgy in print except in technical magazines. Perhaps it is more to the front now than in former years; the Dee. 30, 1929, issue of Time mentioned under the heading of "Science7' certain new achievements in metallurgy, which may be cited as a rare instance of the use of the word in anything but the technical press. Too often the part the metallurgist plays in the advancement of the different branches of engineering is overlooked. To say that the public does not know there is such a profession as metallurgical engineering seems to be a bold statement, but had there beep time a questionnaire could have proved this beyond doubt. Suppose a carefully-planned questionnaire had been sent to all high school students asking them, among other questions, to list the different branches of engineering, I believe that the several professions would have been listed in this manner: (1) Electrical engineering; (2) mechanical; (3) civil, and (4)' mining. One in each hundred might have listed metallurgy as an engineering profession. Even the Society for the Promotion of Engineering Education in its Bulletin No. 10-"Investigation of Engineering Education" lists Civil, Mining, Mechanical, Electrical, and Chemical, leaving out Metallurgical Engineering.

Jan 1, 1930

By Constantine Michalopoulos, Roger C. Van Tassel

Commercial demand for gold in the United States is important. It has a large impact on the total world commercial and overall non-monetary demand. Given the present free market price and our need to import gold, it has a substantial adverse effect upon our international payments position. But, according to most recent estimates, the United States demand is perhaps no more than 20% of the world as a whole. In 1971, United States consumption was estimated at 215.6 tons out of a total of 1,412.1 tons 1. This figure is very close to the 16% figure developed by Consolidated Gold Fields as the average for the years 1968-1970.2 Surveys of both production and use of gold on a world-wide basis are not new. With the bulk of gold production in only a few countries, it has been possible to develop fairly reliable series on gold output. Estimates have been developed on the known reserves of gold and probable output at various prices.3 On the demand side, figures have been somewhat less complete and reliable. The Bank for International Settlements and the Director of the United States Mint have regularly published estimates of commercial use in major industrial countries. The IMF has issued an increasingly comprehensive survey in its Annual Reports. The IMF has attempted to cover all nations-not restricting its efforts to major industrial nations-and has tried to estimate both gold taken for commercial uses (Estimated Industrial and Artistic Use) and for private hoarding. Their method is to begin with data on free world output plus any net sales by the Soviet Union, subtract any additions to world monetary stocks (or add to available supply for any net reductions in world monetary stocks), subtract estimates for commercial demand and have left as a residual an estimate for private hoarding. The method is straightforward and simple but the quality of the data is suspect. Industry sources tend to believe the figures as biased on the low side because of a persistent tendency to underreport gold movements.4

Jan 3, 1974

By Louise B. Freeman

Kentucky for the first time in its oil history passed the 10 million barrel mark. Of the total 10,019,641 bbl., 8,262,516 bbl. were produced in Western Kentucky, and Union County surpassed all others, with 4,056,142 bbl., or 40 percent of all the production for the state. There were 930 wells known to have been drilled during the year; 510 in Western Kentucky and 221 in the gas-producing area of Eastern Kentucky.

Jan 1, 1946

By J. L. Gillson

Andre Hubaux: In the writer's opinion, more stress should be put on field and microscope observations, as J. L. Gillson does. His discovery of relics of big labra-dorite feldspars from the Marcy anorthosite in all the other rocks is proof enough that previous field observations have been inadequate. The writer's field experience with anorthositie massifs is limited to the Egersund-Sogndal district in southern Norway; however, this is a very large and well exposed area. It seems to have so many points in common with the Adirondack region that a detailed comparison should be beneficial. This comparison was not possible 20 years ago, owing to the scarcity of geological data, at least for Norway. Both regions are now far better known—the Norway district because of the work of Professors Bugge and Barth 33-35 and especially because of the extensive field and microscopic research of P. Michot,30-35 who introduced me in the field to the problems of that region. In a particular unit of the Egersund district, a sodi-fication of the plagioclase, very similar to what Gillson calls "andesinization," has taken place. 12' The percentage of anorthite in the plagioclase has dropped from 42 to 43 pct in the original norite down to 27 pct, but never below that level. This metasomatical transformation is a part of a whole series of processes of mig-matitization which have produced, above the level of granitization, concentrations of Mg, Fe, and Ti and among them, patches and parallel bands of ilmenite and magnetite. Thus both regions present somewhat comparable features and the theories to explain them have several points in common. However, as there seem to be differences between some American conceptions and the views commonly accepted at the University of Liege, I would like to make some comments about J. L. Gill-son's article. The author speaks of the garnet as being an anti-stress mineral. However, garnet may be found in schists, where its helicitic texture, when present, demonstrates its formation during differential movement. Furthermore, the whole concept of stress and anti-

Jan 1, 1959

By AIME AIME

FEW men are better known in fuel engineering circles in the Middle West than the present Chairman of the Coal Division of the A.I.M.E. - Julian Elnathan Tobey. Now vice-president in charge of engineering of Appalachian Coals Inc., of Cincinnati, he has served that pioneer regional marketing agency since Aug. 1, 1934, when he became manager of its engineering department. His duties have included field promotion work in the interest of use of the agency's coals from eastern Kentucky and Tennessee, south western Virginia, and southern West Virginia in new plants of all types. He has been especially interested in certain industries which have shown an alarming tendency to change to natural gas or hydroelectric power; also in the development and practical application of small stokers and other mechanical equipment.

Jan 1, 1941

By H. E. Exner

This article is a critical review of the influence of surface preparation on crack formation at Vickers indentations in the test used by Palmqvist3-7 to evaluate the toughness of cemented carbides. Experimental results are presented which clearly show that grinding introduces compressive surface stresses into the cobalt phase and thus reduces the crack length. The deformed surface layer is removed by polishing and a stress pattern is approached corresponding to that in the bulk material. Cracks of maximum length are characteristic of this stress state. Deformation stresses can be removed by annealing above 800°C. On the basis of these results , sample preparation for the crack length test can be simplified, the accuracy of measurement is improved, and a simple and significani parameter is found to describe crack resistance of cemented carbides. FOLLOWING suggestions by Ammann and Hinniiber,1'2 Palmqvist3-7 developed a method for testing the toughness of cemented carbides using as a measure the sum of crack lengths at the four corners of a Vickers hardness indentation. This method has several advantages over the bend test commonly used in carbide technology: a) specially formed samples are unnecessary; b) sufficient information can be obtained from one sample; c) the scatter is relatively small; d) the range of actual values for commercial cutting alloys is wide. Thus, this test is both cheaper and more precise than the bend test. Nevertheless, Palmqvist's method is not widely used, mainly for two reasons: a) The relationship between crack length and the technological properties of the material (wear and shock resistance) is not clear. b) The crack length is strongly dependent on surface treatment. It is necessary, therefore, that surface preparation be very precise and reproducible, conditions usually hard to obtain. While any other simple mechanical test has this first drawback, the second became crucial in the application of the crack length method as a practical test. The reasons that this drawback could not be eliminated are, in our opinion, misleading and inconsistent interpretations of the influence of surface preparation on the crack length given in literature. In the following, after a short review of previous experimental results the interpretations given by different authors,4?'-11 cf. Table I, are discussed critically and a consistent explanation is presented on the basis of which improvements of the method of crack length testing are proposed. 1) PREVIOUS EXPERIMENTAL RESULTS In his first attempt to use the cracks at Vickers impressions as a quantitative measure of the toughness of cemented carbides, palmqvist3 calculated the work necessary to initiate cracks by the formula: Sk =k.Pk. [I] where k = numerical constant = 6.49, Sk = critical work to initiate cracks (gf cm), Pk = critical load (load necessary to initiate cracks) HV = Vickers hardness (kp per sq mm). The difficulties involved in experimental determination of the critical load were overcome by the observation that a linear relation holds between the applied load and the sum of the crack lengths at the four corners of the indentation. This linear function, given by Eq. [2] below, was confirmed by Dawihl and Alt-meyer9and by our experiments, see Fig. 1: I = a1.P +a2 [2] where 1 = sum of the crack lengths at a Vickers indentation, P = applied load, al, a2 = parameters dependent on the toughness of the alloy and the surface preparation. The critical load, Pk, is now given by a2, which can be obtained by extrapolating the load vs crack length line to zero crack length, see Fig. 1. This simple relationship, Eq. [2], led Palmqvist1,7 to a parameter which was more reproducible and easier to obtain experimentally than the critical work: the work, S300, put into the sample to produce an average crack length of 300 µm per indentation. This parameter is calculated using the formula: where the load, P3oo, giving a crack length of 300 µm, can be taken from the load-crack length plot, Fig. 1,

Jan 1, 1970

By T. H. Aldrich

(Chattanooga Meeting, October, 1908.) Tars paper is intended only to give a preliminary account of experiments made, and conclusions reached, concerning the treatment of certain refractory low-grade gold-ores, the profitable reduction of which may furnish a useful guide to the solution of similar mining and metallurgical problems, not only in the gold-bearing belt of the Southern United States, but perhaps in other regions also. It must be regarded as simply a ?report of progress," preceding a more elaborate and conclusive report of regular practice. The mines of the Hillabee Gold Mining Co. are located upon what is generally known locally as Hog Mountain, on the northern edge of Tallapoosa county, Ala., about 15 miles from Goodwater and 14 miles from Alexander City, stations on the Central of Georgia Railway. Gold has been known since 1839 to exist on this property, where it was discovered in that year by a man named Johnston. The property was worked for placer-gold by the old miners, and there are now the remains of four attempts to operate it by stamp-mill and plate-amalgamation. The present owners purchased it in 1896, and since that time they have experimented at frequent intervals, in order to devise a process that would satisfactorily recover the gold. In 1903 regular operations were begun. Geologically, the mountain consists of an intrusion of what has been pronounced true granite in altered sedimentary slates. The cooling of the granite produced shrinkage-cracks, which have become veins. There is considerable question as to the period of the slate formation; but it is undoubtedly, in my opinion, of Carboniferous age. The veins, about 50 in number, strike N. 60° to 80° E.; dip approximately 65° from the horizontal; vary from a few inches to 25 ft. (being in gen-

Nov 1, 1908

By AIME AIME

MICA is perhaps our No. 1. strategic mineral problem because of its large requirements in a variety of equipment for use in the military services, and because the principal source of this material has heretofore been British India, a source now threatened partly because of distance and lack of ships. [Block mica and bauxite were added to the "most critical" list published by the W.P.B. on Nov. 6.] No satisfactory substitute has yet been found for most of the uses of mica, which largely involve electrical insulation. Brazil is now our nearest and best major source of this material. No splitting plants have yet been established there but in 1941 we imported about a million pounds of block mica from that country and in 1942 that quantity will be considerably exceeded. In Brazil, mica is found almost exclusively in the pegmatite dikes along the mountain range bordering the eastern part of Minas Gerais. A belt, roughly 180 miles long by 100 miles wide, extends from Theophilo Ottoni to Carangolo. The principal mica-mining districts in this belt are the Governador Valladares area to the north and the Espera Feliz district to the south. The dikes are usually 10 to 50 meters wide and a mile or two long and intrude the old metamorphic schist formation. They are weathered and easily mined.

Jan 1, 1942

By Luis Toron, Salvador Cortes-Obregon

THE Oaxaca coal fields, shown in Fig. 1, are located in the Alta Mixteca region in the states of Oaxaca, Puebla, and Guerrero. Known out crops are scattered over 3125 square miles. It is probable that further exploration will reveal a more extensive area of deposits. The region is of great importance to Mexico, as at present the only sources of coal are the fields near the U. S. border. Steel mills are also located in the North, and finished products must travel 600 to 800 miles to the area of consumption in central Mexico. The Oaxaca coal, only 120 miles south of Mexico, D.F., lies close to several iron ore deposits. If this coal can be used in steel production is will be possible for the Mexican steel industry to reach new dimensions, commensurate with the growing industry of the central region. Coal can be utilized in thermoelectric plants in this area, which lacks not only petroleum and natural gas but also electric power. It can be used as domestic fuel, replacing charcoal and firewood.

Jan 5, 1954

By N. L. Britton

About two years ago Dr. Newberry referred to me for study a considerable collection of fossil plants sent him by Dr. Arthur F. Wendt, engineer of the silver mines " El Cerro Rico de Potosi" in Bolivia. As I had been interested in working up the extensive accumulations of existing plants made by Dr. H. H. Rusby in the Bolivian Andes further north, and in assisting Dr. Rusby in the study of those now being collected by Mr. Miguel Bang in other parts of that country, I was glad of an opportunity of ascertaining something of the Tertiary flora of the region. I was unable to take up the subject at that time, but have since been able to conclude the investigation, and the results are here presented. At a time when the mineral resources of the Southern States are attracting such widespread interest and attention, I have thought it appropriate to give a short general description of the iron-ore deposits of a territory concerning which little is as yet known and nothing published, so far as I am aware. The data used here are due to the preliminary examinations of the North Carolina Geological Survey, on which work I was engaged during the past summer, and my acknowledgments are due to Prof. J. A. Holmes, State Geologist, and Messrs. Harris, Ashe, and Lewis, of the survey, for their co-operation in the work; also to Messrs. A. S. McCreath and C. B. White for analyses which they Kindly furnished. Other analyses were made by Mr. Charles Baskerville, assistant chemist to the survey, and this may be understood where the name of the chemist is not mentioned. All samples for analysis were dried at 212' F. The accompanying map has been prepared from the revised sheets of the United States Geological Survey by Mr. H. L. Harris, and will be referred to throughout this paper. Ashe county lies in the extreme northwestern part of North Carolina, bordering on Tennessee and Virginia; it is drained principally by the north and south forks of New river and their tributaries, and is therefore on the eastern edge of the great Mississippi drainagebasin. The country is exceedingly rugged and mountainous, having an average elevation of about 2900 feet above sea-level. Jefferson, the county seat, near the center of the county, is 45 miles nearly due south from the Norfolk and Western R.R. at Marion, Va., and 30 miles northwest from the Richmond and Danville R.R. at Wilkesboro, N. C. Geologically the ore-deposits described in this paper are situated in the area of the crystalline rocks, consisting chiefly of gneiss, hornblende-schist, and micaceous schists.

Jan 1, 1893

By F. Julius Fohs

Centrally located with relation to the largest iron- and steel-producing districts of the United States, the fluorspar-deposits of Kentucky possess increasing interest and importance. As typical of the numerous fluorspar-mines of Kentucky and Illinois, I have selected for description the Memphis, because it and others of its immediate group exhibit the conditions characteristic of all. I. The Memphis MiNe. This mine lies 5 miles NW. of Marion, in Crittenden county, Kentucky, a station on the Chicago and Nashville division of .the Illinois Central R. R. For the first mile and a half out of Marion we see only Birdsville or Middle Chester sandstones of Mississippian age. Then we cross a fault of about 850 ft. displacement, and the Ste. Genevieve oolite sets in. Beyond the fault, oolite is the predominant rock, except that the hills to the north have a capping of Cypress or lowest Chester sandstone, 80 ft. below which is an outcrop of from 6 to 10 ft. of Ste. Genevieve (Rosiclare) sandstone. Occasional sink-holes are noticed, and as the mines are approached evidence of faulting is again seen. A line of .crude head-frames and open-cut dumps, extending for more than a quarter of a mile, marks the Klondike vein. The open-cuts are from 15 to 20 ft. deep, and in most of them, from the surface down, was found the reddish gravel which is really fluorspar—some of it white or purple and crystal-clear (if the red clay is washed off), and some carrying iron and silica, and stained by waters from the decaying limestone walls. In one of these cuts, at a depth of 20 ft., white and purplish honey-combed fluorspar was found, in which the larger cavities are due to the leaching of limestone and calcite, and the minute ones to the leaching of zinc-hlende.

Jan 1, 1910

By Hugh Marriott

MANGANESE and its ores have been recently dealt with in comprehensive papers to the Iron and Steel Institute by Sir Robert Hadfield, and in a series of papers read before the A. I. M. E. at the Cleveland meeting. I have taken the opportunity of adding this mineral, to my records of the "World's Mineral Production and Consumption," as recently pub-lished in the Economist ?. The tables bring out the following significant facts: The world's production has increased by 10 per cent since 1913. India's production has increased by 3 per cent since 1.913, the supply from this source now being 31.1 per cent of the world's output. Russia is now producing at about half its pre-war rate and yields 19 per cent of the world's production. West Africa supplies 12.5 per cent of the world's total output. Brazil's present output is 2.5 times that of the pre-war period, being 11.3 per cent of the world's output.

Jan 9, 1927

By J. L. Snoek

[ ] DISCUSSION J. L, SNOEK*-Stress-induced preferential diffusion in cubic body centered metals in the annealed state provides us with a powerful tool for determining the mobility of interstitially solved atoms as well as their location in the lattice and the exact nature of the distortion brought about in the lattice by their presence. Calculations given by D. Polder31 show that the distortion of the lattice, besides being proportional to the applied stress P, is also proportional to [VC, RT + xVCo] where T, V and Co are the temperature, molar volume of the solvent and molar concentration of the solute respectively and x is a constant describing the mutual interaction energy of the dissolved particles. This calculation obviously is no longer valid if x is negative and the abso¬lute value of xVCo surpasses that of RT. The lattice may then be expected to become tetragonal spontaneously. Such a spontaneous tetragonality seems to have been observed by W. Klemm and L, Grimm for the case of oxygen solved in vanadium.32 Measurements of the internal friction in cold worked iron containing carbon or nitrogen should provide us with information on the mobility as well as the preferential location of these particles in the iron lattice in the cold worked state. The work by T'ing-Sui Kê is a valuable contribution to this problem, The data obtained by T'ing Sui Kê and myself on cold worked samples of iron seem to indicate that carbon and nitrogen in these samples are found either in the normal (1/2 , 0, 0) interstices or in a new preferential position created by the cold working. The latter positions in my opinion can hardly by anything else but the edges of the dislocations. The observed larger distances of diffusion might be explained by assuming that the carbon atoms when freed from a certain dislocation by thermal agitation must diffuse over several atom distances before being caught in another dislocation. The theory however needs working out and no doubt will be much more complicated than the one valid for the annealed state. T'ING-SUI KÊ (author's reply)-It is highly encouraging to read the written discussion given by Dr, Snoek who initiated the theory of stress-induced preferential diffusion in cubic body centered metals in the annealed state, Since the presentation of this paper, the author has done more experimental work on this subject which seems to be able to settle several of the points raised by Dr. Snoek. It has been found that such stress-induced preferential diffusion occurs also in the solid solutions of carbon,33 oxygen,34 and nitrogen35 in tantalum which has a body centered cubic structure. Analysis of the shape of the observed internal friction. peaks indicates that the inter-

Jan 1, 1948

By Hollis L. Caswell

The present status of integrated circuits utilizing. superconductive switching. elements is reviewed with special attention given to fabrication techniques, methods for interconnecting completed circuits, and refrigeration requirements. Cryoelectronics has been largely an "inte- grated-circuit" technology since its conception because the switching speed of superconductive devices is attractive only when these devices are fabricated with thin-film techniques. It is true that cryotron circuits can be constructed from wires of appropriate materials (as indeed was done by Dudley Buck 1 in his early investigations) but these circuits will switch in times characteristic of milliseconds whereas similar circuits fabricated by thin-film methods have potential switching times of nanoseconds. Furthermore, cryo-electronic devices such as the cryotron lend themselves readily to fabrication by thin-film techniques since these components may be made from polycrys-talline thin films and are relatively insensitive to the presence of impurities (as measured by semiconductor standards). Therefore, during the past decade considerable effort has been devoted to developing techniques for batch fabricating circuit arrays containing superconductive switching elements. Technology had developed to the point several years ago that fabrication of cryoelectronic arrays containing up to one hundred devices was rather straightforward. However, larger arrays containing between lo4 and 106 components which are required for commercial development of cryoelectronics still pose very severe yield problems. Thus in a sense cryoelectronics found itself in 1962 at the point semiconductor technology finds itself today; namely, individual devices and small groups of integrated devices could be fabricated with acceptable yield and the outlook for building larger integrated-circuit arrays was bright. Unfortunately, problems associated largely with yield have made fabrication of these larger arrays difficult. Unlike semiconductor technology, cryoelectronics had to solve the problems of large-scale integration before it could become economically attractive. This has proven to be a sizable burden to bear. Since several reviews exist on superconductivity,2 superconductive devices,3 and cryoelectronic technology, no attempt will be made in this paper to summarize these areas. Instead a few specific topics will be dealt with in more detail. First, a brief description is given of selected superconducting switching and storage devices with special attention to several metallurgical techniques which improve the performance of these devices. Second, techniques used to fabricate cryoelectronic devices are described with emphasis on problems affecting yield. Third, techniques for interconnecting a number of cryoelectronic planes are described. And last, refrigeration of cryoelectronic components is discussed briefly since the low operating temperature of superconductive devices is an important consideration in this technology. SUPERCONDUCTING STORAGE AND SWITCHING DEVICES The basic superconductive switching device is the thin-film cryotron. The geometry of this device is attractively simple, since it involves only the intersection of two lines that are electrically insulated from each other. The switching element (gate) and control element (control) of a crossed-film cryotron are arranged as illustrated in Fig. 1. The material for the gate is selected to permit the gate to be switched from the superconducting to the normal (resistive) state by the application of a control current. Tin, which has a critical temperature (T,) of 3.7°K, is commonly used for the gate and the cryotron is operated at a temperature just below T, (for example, 3.5°K). The control material (normally lead, with T, = 7.2°K) is chosen so that the control is never driven normal during circuit operation. To improve cryotron operation, a ground plane, also of lead, is placed under all of the circuitry to act as a diamagnetic shield and improve the current-density uniformity across the width of various thin-film elements. Normally, line widths vary from 0.005 to ^ 0.020 in. and film thicknesses from 300 to 10,000A, although new fabrication techniques make narrower lines feasible. In fabricating cryotrons it is important that the edges of the gate elements be geometrically sharp to avoid undesirable switching characteristics associated with a thinner edge region, Fig. 2. One technique which has been used extensively to form patterns consists of placing a physical mask containing the film pattern between the evaporation source and the substrate and depositing through the mask. Film strips formed in this manner possess a penumbra at the film edges due to shadowing of the evapor-ant under the mask. Several techniques have been proposed for minimizing effects due to this penumbra. One of the more promising metallurgical techniques

Jan 1, 1967

By P. E. Doherty, B. Chalmers

Subboundaries may be revealed in aluminum by the formation of pits on the surface during cooling from elevated temperatures. The pits do not form in the vicinity of high- or low-angle boundaries. They are attributed to the condensation of vacancies from a super saturation produced during coolirzg. Using the vacancy pit and Schulz X-ray techniques for observing low-angle boundaries, a study was made of the transition from the nearly perfect seed to the striated structuke characterist-ic of aluminum crystals grown from the melt. It was found that the individual striation boundaries develop by the coalescence of very small-angle boundaries, as well as by the addition of individual dislocations. Several mechanisms for the formation of striations are discussed. Evidence was found suggesting that a super-saturation of vacancies exists near a growing interface, and it is proposed that the resulting climb of existing dislocalions produces "half'-loops" at the interface, which combine to form the low-angle striation boundaries. LINEAGE, or "striation" boundaries, have been studied in detail by Teghtsoonian and Chalmers 1,2 in crystals of tin grown from the melt, and by Atwater and Chalmers3 in lead. They found that single crystals grown from the melt consist of regions which are separated by subboundaries that lie roughly parallel to the growth direction. A difference in orientation of 0.5 to 3 deg exists between the striated regions; the misorientation is such that the lattice of one region could be brought into coincidence with the lattice of its neighbor by a rotation about an axis approximately parallel to the direction of growth of the crystal. They observed an incubation distance for the formation of striations which increased with decreasing growth rate. They also found that in any crystal, the sum of all rotations of the lattice in one sense, in going from one striation to the next, is very nearly equal to the sum of all the rotations in the opposite sense. A striation boundary, which is a low-angle grain boundary, can be described as an array of dislocations. If it is assumed that suitable dislocations are introduced into the crystal during solidification, the formation of striation boundaries can be explained as a result of the migration of the disloca- tions into arrays. The formation of arrays is energetically favorable since the energy of an assembly of dislocations can be reduced by the interaction of the stress fields when a suitable array is formed. This investigation presents and interprets new information concerning the nature and origin of striation boundaries in aluminum. EXPERIMENTAL TECHNIQUE Single crystals of high-purity aluminum (Alcoa 99.992 pct) were prepared by horizontal growth from the melt.'' The specimens were subsequently electropolished in a solution of 5 parts methanol to 1 part perchloric acid kept between -10° and 0°C in a bath of dry ice and alcohol. The current density was approximately 6 amps per sq in. Doherty and Davis9 have shown that in aluminum sub-boundaries with misorientations of not less than several seconds of arc may be revealed by the vacancy pit technique. During cooling from elevated temperatures pits form on electropolished surfaces of aluminum crystals as a result of the condensation of vacancies.11 Pits do not form in the vicinity of small- or large-angle grain boundaries, presumably because such boundaries act as sinks for vacancies. Boundaries of misorientations down to 3 sec of arc are revealed as pit-free regions, see Fig. 1. The Schulz X-ray technique12 was used to determine the angular misorientations of subboundaries. In this method, white radiation from a micro-focus X-ray tube is used to produce an image of a fairly large area of a single crystal surface. Subboundaries cause splitting in the diffracted image, see Fig. 2. Misorientations down to about 15 sec of arc may be observed with this technique. OBSERVATIONS AND DISCUSSION Figure 1 shows a striated aluminum crystal grown at 10 cm per hr etched by the vacancy pit technique. An incubation distance of about 1 cm is observed before the initiation of striation boundaries. Fig. 2 is a Schulz X-ray photograph of a striated crystal similar to that shown in Fig. 1. A large area of the crystal was studied by means of a series of photographs. Fig. 2, which is a reflection from the (100) plane, included about the first 4 cm of crystal to freeze. There is an incubation distance of about 1 cm, and a distance of about 2 cm over which the angle of misorientation builds up to its final value of approximately one degree. Some twist component can be seen in Fig. 2 at the right side of the photograph. From Fig. 2 it can be seen that the sum of all rotations of the lattice in one

Jan 1, 1962

By W. Jolley

Decarburized iron and Fe-3.28 pct Ni alloys were impact and tension tested in the temperature range of ambient to 4°K. It was found that alloying with nickel improves the fracture properties of the ferrite matrix. The improvement in toughness of iron alloyed with nickel is attributed to the effect of the nickel addition on the temperature and strain rate dependence of the yield stress as well as on slip behavior. The Fe-Ni alloy exhibits wavy slip when strained at temperatures down to at least 50°K. This behavior contrasts with that of the unalloyed iron where a change It is a generally accepted fact that of the common alloying elements of steel only nickel and manganese improve both the room-temperature yield strength and the notch impact properties. It has been argued for a number of years that manganese refines the ferrite grain size, the pearlite spacing, and the grain boundary carbides in medium- and low-carbon steels and thereby increases resistance to brittle fracture.''' This hypothesis recently was confirmed for a 0.04 pct C iron containing manganese, but at the same time from wavy to planar slip occurs at about 120°K. The observed lower temperature and strain rate dependence of the lower yield stress in the Fe-Ni alloy as compared to the unalloyed iron may be attributed to this difference in slip behavior. In contrast to suggestions published previously, transmission electron microscopy showed that the uniform dislocation distributions and the lack of dislocation tangles which are produced by low-temperature straining of bcc materials cannot be attributed to the absence of cross slip at these temperatures. no increase in notch toughness was observed in a decarburized Fe-Mn alloy.3 It thus appears that manganese only increases the toughness of Fe-Mn-C alloys by refining grain boundary carbides and has no toughening effect in carbon-free iron. On the other hand, the mechanism whereby nickel improves toughness has not been established. Hodge et a1.4 have clearly shown that a 3.28 pct Ni addition lowers the impact transition temperature of 0.02 pct C steel approximately 35°C when the grain size is maintained constant. Recently, Wullaert and Tetelman6 stated that nickel refined the grain boundary carbides of an Fe-C alloy and consequently increased the toughness. They also observed the previously reporteda-'

Jan 1, 1969