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By L. C. Brown, S. K. Behera

The diffusion rate in Ag-Sb couples is sensitive to con~pressive load with the width of Ag3Sb, the only phase present in the diffusion zone, increasing with stress up to 800 psi and remaining constant above this. Kirkendall marker experiments show silver to diffuse much faster than antimony in Ag3Sb and incipient porosity may therefore develop at the Ag/Ag3Sb interfnce restricting the transfer of atoms from the silver into the diflusion zone. Application of compressive stress reduces the tendency for porosity to develop and so increases the growth rate. In a recent paper Brown et al.1 observed a significant increase in the thickness of Cu2Te in Cu-Te diffusion couples on application of a compressive stress as low as 20 psi. Similar stress effects have also been observed in the Fe-A1,2 Al-u,3 arid cu-sb4,5 systems. It has been suggested that the increase in growth rates of intermetallic phases in these systems is due to a decrease in the amount of Kirkendall porosity with applied stress. In the present paper, results are presented of the effect of compressive stress on diffusion in Ag-Sb, together with a detailed examination of the Kirkendall effect. The Ag-Sb phase diagram6 shows that antimony has a moderate degree of solid solubility in silver, 5.7 at. pct at 350°C, but that there is essentially no solubility of silver in antimony. There are two intermediate phases— (hcp7) from 8.8 to 15.7 at. pct Sb and Ag3Sb (orthorhombic8) from 21.8 to 25.9 at. pct Sb. EXPERIMENTAL Diffusion couples were prepared from fine silver of 99.95 pct purity and from antimony of 99.7 pct purity. Both the silver and antimony were produced in the form of discs 1/2 in. in diam by approximately $ in. thick, with surfaces ground flat to 3/0 emery paper. Diffusion anneals were carried out in the apparatus previously described.1 A compressive load was applied to the diffusion couple through a lever arm system, with a reproducibility estimated to be ±10 psi. All runs were carried out in a protective hydrogen atmosphere. Following the diffusion anneal specimens were sectioned and polished and the width of the diffusion zone was measured metallographically. Composition profiles were measured using an electrostatically focused electron probe with a spot size of 10 , counting on Sb L radiation. Corrections for matrix absorptiori and fluorescent enhancement9 were not required. S. K. BEHERA, formerly Graducate Student, Department of Metallurgy, University of British Columbia, is now Postdoctoral Fellow, Whiteshell Nuclear Laboratories, Atomic Energy of Canada Ltd., Pinawa, Manitoba. L. C. BROWN, Junior Member AIME, is Associate Professor, Department of Metallurgy, University of British Columbia, Vancouver, B.C., Canada. Manuscript submitted June 14, 1968. IMD RESULTS Fig. 1 shows an electron probe traverse of a typical diffusion zone. In all couples examined only one intermediate phase was observed and the composition of this phase, 23 wt pct Sb, was in good agreement with the composition of Ag3Sb, 23 to 28 wt pct Sb. The presence of this phase was confirmed by X-ray diffraction of filings taken from the diffusion zone. The probe traverses showed no detectable solid solubility in either the silver or the antimony although the phase diagram indicates that some antimony, up to 6.5 wt pct pct Sb, should be in solid solution in the silver. However the width of this portion of the diffusion zone would be expected to be very small in view of the low diffusion coefficient in the silver, 4 x 10-l6 sq cm per sec at 350°C, 10 compared with that in the Ag,Sb, estimated as 3 x 10-8 sq cm per sec in the present work, and this region would therefore not be expected to be seen in the probe traverse. Application of stress resulted in a significant increase in the width of the diffusion zone, Fig. 2. At 350°C, the thickness of Ag3Sb increased from 250 at 0 psi to 400 p at the limiting stress of 800 psi, indicating an apparent 150 pct increase in the diffusion coefficient. Similar behavior was also observed at 400°C, indicating that the stress effect is not characteristic of just one temperature. The growth of Ag3Sb at 350°C and at various stresses is shown in Fig. 3. In every case the growth rate was parabolic indicating diffusion control. The kinetic curves all passed through the origin showing that delayed nucleation of Ag3Sb was not responsible for the stress effect and that it was a real growth effect. A series of tests were carried out in which diffusion was allowed to take place at a lower stress following an initial high stress diffusion anneal. Speci-

Jan 1, 1969

By P. G. Shewmon, F. N. Rhines

THE determination of the self-diffusion coefficient of magnesium has been made possible recently by discovery1-1 of a radioactive isotope, Mg28 having a half-life of 21.3 hr,1 and subject to manufacture in useful quantity. In the present research this material was condensed from the vapor phase upon a surface of high purity magnesium. The progress of diffusion of the tracer atoms into polycrystalline magnesium was followed by machining layers and measuring the change in the intensity of radiation as a function of the distance of each layer from the surface. The self-diffusion coefficient was found to be 2.1 X 10-8 sq cm per sec at 627°C, 3.6 X 10-9 sq cm per sec at 551°C, and 4.4 X 10-10sq cm per sec at 468°C; the activation energy is about 32,000 cal per mol. Experimental Procedure Since there was no other published measurement of a diffusion velocity in any magnesium-base material, is was necessary to employ a number of new experimental techniques. The short half-life of Mg28 made it necessary to complete the entire experimental procedure within three or four days. This meant that the work had to be done where a cyclotron was readily accessible and that all operations, prior to the diffusion heat treatment, had to be so designed as to minimize their time requirements. Unusual problems were imposed also by the chemical reactivity of magnesium, its high vapor pressure, and the fact that no satisfactory method for elec-trodepositing magnesium on magnesium is presently available. Finally, the machining and handling of the easily air-borne radioactive-magnesium chips involved certain health hazards, resulting in the need for further experimental restrictions. Preparation of Mg28 The Mg28 was produced in the Carnegie Institute of Technology syncrocyclotron by the neutron spallation of chlorine.5 his involved bombarding a 2 gram crystal of high purity NaCl with a beam of 350 mev protons for a period of 2 hr, after which the crystal was dissolved in warm water and the Mg28 was concentrated and purified by chemical means (see Appendix). About 50 microcuries of Mg28 thus were obtained in the form of magnesium oxinate (8 hydroxyquin-olatc?), which was ignited in air to produce MgO. This in turn was reduced to magnesium metal vapor, by the method of Russell, Taylor, and Cooper," in the vacuum apparatus shown schematically in Fig. 1. Here the essential part is a tantalum ribbon, slightly dished to receive the MgO. The ribbon, pre- viously outgassed at high temperature, is heated to about 1700°C by passing an electric current through it, whereupon tantalum oxide is formed, magnesium vapor is released almost instantaneously, and condensed partly upon the diffusion sample. Diffusion-Sample Preparation: Hot-extruded magnesium rod, 21/32 in. round was used in making the diffusion specimens. The magnesium analyzed as follows: 0.004 pct Al, 0.027 pct Fe, 0.040 pct Mn, 0.0004 pct Cu, 0.0002 pct Ni, and less than 0.01 pct Ca, 0.0004 pct Pb, 0.0011 pct Si, 0.001 pct Sn, and 0.001 pct Zn. A brief study of the crystal texture of this material revealed a sharp fiber texture with the (001) plane roughly parallel to the extrusion axis. Cylindrical samples 1/2 in. long by 5/8 in. were machined from this rod, the end faces dressed on 3/0 emery, and lightly etched with 20 pct HC1 in water. These samples then were annealed for at least twice the intended time of diffusion, at the intended diffusion temperature, in order to stabilize the grain structure at about 1 mm average diameter. The annealing treatments were conducted in argon in the same apparatus and in the same manner as the subsequent diffusion treatments, which will be described presently. Thus, a strain-free plane surface was produced, but there remained a layer of MgO which had largely to be removed before the layer of Mg28 was deposited. Most of this layer was taken off by two light passes over 3/0 emery paper. The balance of the oxide and a thin layer of metal were then removed by etching 5 to 10 min in 4 pct nital (4 pct HNO3 and 96 pct ethyl alcohol) made with absolute alcohol. There followed immediately three quick rinses in: 1-49 1/2 pct methanol, 49 1/2 pct acetone, and 1 pct formic acid, 2-50 pct methanol and 50 pct acetone, and 3-pure benzene. This procedure is essentially that of Sturkey.7 The resulting surface, which was of almost elec-tropolished brightness, remained plane and was free of cold work. It could be kept clean by storing under benzene, or in a desiccator; short exposure

Jan 1, 1955

By E. C. Truesdale, R. K. Waring

THE Research Division of The New Jersey Zinc Company (of Pa.) has conducted, over a period of years, numerous tests of the reducibility of various zinc ores and the reactivity of various kinds of coal, using a number of different experimental methods. Most of these tests have involved the reduction of mixtures of ore and coal. In such cases the following simultaneous reactions are believed to be mainly responsible for the production of zinc, as was shown by Bodenstein1 some years ago: ZnO + CO = Zn + CO2[I] C + CO2 = 2CO[2]. Each of these reactions is dependent upon the other for the supply of CO and C02, respectively, and the over-all rate of formation of zinc vapor will be determined by the slower of these two reactions. An analogous pair of reactions sometimes of importance is: ZnO + H2 = Zn + H2O[3] C+ H2O=CO+H2[4] While it is possible to obtain an indication of the relative reducibility of various ores, or of a fine versus a coarse ore, by testing them with a given coal, and while coal reactivities may be measured in a corresponding manner, a more direct determination of relative reaction rates is possible by carrying out the desired reactions, such as I and 2, separately and under reproducible conditions. It is one purpose of this paper to present some of the results that have been obtained by the latter method. C. G. Maier2 discusses the relative rates of reactions I and 2 and concludes that while at relatively low temperatures reaction I is faster than reaction 2, this difference becomes less with increasing temperatures, although at smelting temperatures reaction I is still the faster. He also says (p. 48), "At temperatures . . . between 1100° and 1300°C the zinc oxide reduction reaction is intrinsically more rapid than its physical limitations; that is, it is limited by gas diffusion rates." In the course of numerous reactivity tests involving the separate use of reactions and I and 2, we have obtained data that show by direct experiment, we believe for the first time, the correctness of Maier's statements concerning these reactions. We also include data on the relative rate of reaction 3, involving reduction by hydrogen. Finally, some interesting results obtained by carrying out the reduction of a zinc ore-coal briquet in streaming atmospheres of nitrogen, carbon monoxide and hydrogen, respectively, are presented.*

Jan 1, 1941

By E. V. Potter, H. C. Lukens

THE volume of hydrogen released from electrolytic manganese at various temperatures and pressures was determined in a previous investigation1 as part of a study to determine the most practical procedure for removing the hydrogen from electrolytic manganese metal. No attempt was made to determine the absolute volume of gas in the metal at any temperature and pressure; the volume of gas released showed only the variation in solubility with temperature and pressure. The results were very similar to those obtained by Sieverts and Moritz.2 Both sets of data show a minimum solubility between 500° and 700°C., but they differ in certain respects; on cooling from 500°C., our results showed an increase in solubility of about 7 C.C. as compared with an increase of 34 C.C. per 100 grams shown by Sieverts. Furthermore, the transition temperatures, as indicated by sharp breaks in the solubility curves, did not agree well with Sieverts' data. This information was of secondary importance in the earlier investigations, and the solubility at low temperatures and the transition temperatures were subject to considerable error. There- fore, a subsequent investigation, reported in this paper, was made to measure the absolute solubility at temperatures from room temperature through the melting point and make more accurate observations of the transition temperatures. APPARATUS AND METHOD The apparatus and method were essentially the same as those described in the previous work,1 as shown in Fig, I. At high temperatures, the small tube containing the thermocouple in the sample container A frequently broke off, so for some of this work the thermocouple was placed outside the sample container and protected by a quartz tube of about the same wall thickness as the sample container. No significant difference was found in the transition temperatures obtained in the two ways. The automatic temperature controller was used in these tests in the regions where there was little change in solubility with temperature. In the neighborhood of the transition points a continuously variable autotransformer was used instead of the automatic controller, and the power input to the furnace was adjusted so that the temperature increased or decreased at a very slow, uniform rate through the transition range. This procedure was followed because the temperature oscillations produced by the controller were too great compared with the transition range, and the transition points determined under such conditions were less accurate. ABSOLUTE SOLUBILITY Procedure and Results The absolute solubility of hydrogen in manganese could be determined most

Jan 1, 1946

By C. E. Nelson

The purpose of this discussion is to outline briefly the practices commonly followed in this country for the melting and refining of magnesium and its alloys. The processes used for the various forms of primary magnesium, as far as there are differences in the physical shape or behavior, will be discussed. The refining of general fine scrap or secondary magnesium was presented in an earlier paper.1 Inasmuch as the use of fluxes is an essential part of all the melting and refining processes, the principal aim of this paper will be to deal with these in sufficient detail to point out their unique characteristics, in order to make their use more effective. Types oF Melting Practice All melting and refining processes for magnesium and its alloys require the use of fluxes. These fluxes have a magnesium chloride base and other halide salts or oxides are added to give a density or behavior exactly suited to the particular melting practice. The successful handling of magnesium depends upon the proper use of the correct fluxes. There are four general methods of melting, summarized in the following paragraphs and treated in more detail in the section on Melting and Refining. Open-pot Method The open-pot method makes use of No. 230 flux.2 The flux provides protection during melting and a molten pool of flux into which the solid magnesium melts. It is stirred through the molten metal bath and agglomerates oxide or similar foreign bodies; then on quiet standing separates away, leaving the refined metal ball floating in an encircling layer of molten flux. It forms only a thin fluid film over the surface of the molten metal, which may be ' parted for hand-ladling processes and tends to cover the metal again after the ladle is removed. A very light dusting of the pot surface with fresh flux immediately after the ladle is removed is usually desirable. The open-pot method is used generally in the following processes: (I) alloying and secondary smelting in the production of ingot, (2) in sand foundries for premelting and to a smaller extent for the production of small castings requiring hand ladling, (3) in permanent-mold founding for premelting and also direct ladling to castings, (4) for continuous methods of preparing metal in the production of billets or ingots from which wrought products are fabricated, (5) in general scrap recovery. Crucible Process The crucible process makes use of No. 310 flux, which has the property of being thinly fluid at the start, to provide protection and refining qualities, and then drying out or thickening after a time, leaving a protecting crust on the pot surface until the time of casting. At that time it can be readily skimmed off or held back, thus allowing the contents of the crucible to be poured out directly into castings without fear of flux contamination. This flux is not

Jan 1, 1944

By G. S. Jenkins

The statistics set forth by Professor Mitchell in a proceding paper very carefully brought out the points that indicate that a marked amount of consideration must be given to" the haulage problem to adapt it to local conditions as encountered. Professor Mitchell's paper showed a spread of from 10 tons per man to 50 tons per man on the production crews, which spread can be recognized as entirely too large when one considers that the product is being sold at a price within very close limits. While a portion of this spread may be explained by different methods in cost accounting as to what employees are applicable to the production crew, it cannot all be blamed on an accounting method. A good portion must be explained by the improper application of equipment to the needs incurred by the local conditions. It is in an endeavor to go into this phase that this paper is given. It will be necessary to qualify the points covered in order to keep the subject from becoming too wide in scope. Along this line, conditions will be only those involved in bituminous coal mine practices and only the haulage of coal that is loaded with mobile loading machines in seams 4 ft thick and better. Haulage Methods Employed The Consolidated Coal Co. (Illinois) has been operating on a modernized basis for about 20 yr. By modernized we mean the loading of coal with mobile loading equipment. In review of haulage methods, it must be remembered that the main line electric haulage locomotive has been in service for some 40 or jo years. To augment this main line haulage, the mule did a quite satisfactory job during hand-loading days, but was later replaced by the gathering locomotive, either battery or cable-reel operated. This type of haulage was the method in common use at the time the mechanical loading of coal became of major importance and the success or failure of loading machine installations may be largely accredited to haulage facilities in the early days; that is, in the period around 1930. The Consolidated Coal Co. had its struggle with this problem beginning in about 1927 or 1928. We were somewhat fortunate in that we were already using gathering locomotives powered by storage batteries at the time we introduced mechanical loading. This meant that we did not have to spend as much time training motormen and trip riders as many mines did that utilized only mules for their secondary haulage. This was all advantage, and our efforts could be focused on ways and means of providing adequate car service to the loading machine. Like most operations, we endeavored to gear the car service to the capacity of the machine, with a large crew endeavoring to load the maximum tonnage that the machine would handle. Toward that end our first move was to install switches

Jan 1, 1949

The beginning of Colorado's mining industry is linked on one side with that of the Appalachian districts and on the other side with that of California, because the first discoveries were made by pioneers when on their way from Georgia to California. In the summer of 1849 a party of seven Georgians were taking a herd of thoroughbred horses across the continent to the Pacific coast. They reached Camp Lyon, on the Arkansas river, in October, and, meeting James Dempsey, a Government guide, they were persuaded by him that it was too late to cross the mountains that season. His advice was accepted, and, moving northward, they established a winter camp at the junction of Cherry creek with the Platte, close to the site of the city of Denver. Upon a sand-bar, lining the south side of the river, they built two cabins. During the closing months of 1849 they prospected the alluvial banks of Cherry creek, but they made no attempt to penetrate into the mountain canyons, near them, westward, for fear of the Indians.* They found gold in several places along Cherry creek, and particularly at a spot 16 miles up the stream from their camp. From the feathers of the wild geese that they shot they obtained quills in which they placed their gold-dust. This party of Georgians consisted of Dr. L. J. Russell and his brother, Green Russell, also A. T. Lloyd, G. W. Kiker, and P. H. Clark. Early in 1850 they crossed the main range of the Rocky Mountains by the Bridger pass and went on to California. They mined near Downieville, and were successful. Occasionally mention was made by them of the gold

Jan 1, 1932

By G. W. Brownell, H. T. F. Lundberg, R. W. Pringle, K. I. Roulston

The rapid improvement of the airborne scintillometer and the perfection of its efficiency for counting low energy gamma radiation has made it possible to work out a technique to map in great detail the radiation pattern at the earth's surface. On such maps low radiation over certain areas appears to indicate the existence of oil accumulations, forming a pattern similar to that obtained by the geo-chemists. RADIOACTIVE analyses of samples from the surface of oil fields were carried out more than 10 years ago in Alberta by the alpha particle ioniza-tion chamber technique,' but large enough tracts could not be covered in these investigations to make possible any evaluation of the method as a means of oil exploration. Considerable interest has recently been revived, however, as a result of certain striking advances which have been made in the instrumentation available -for the measurement of radioactivity. It is the object of this paper to indicate the nature of these improvements in radiation technology and then to describe the attempts that have been made to interpret the radioactive patterns obtained in the course of airborne recordings with the new instruments. Since the survey can be carried out from the air and records can be accumulated over vast areas in a short time, the result may easily lend itself to statistical treatment. Areas have been surveyed in Alberta, British Columbia, Saskatchewan, Quebec, Texas, New Mexico, Nebraska, Colorado, Utah, and Montana. Producing fields in Alberta and West Texas have been flown over several times in different directions, Fig. 1. The operations were then extended into unknown territory and drill holes were put down on the anomalies which looked promising. The results from these drillings were encouraging and have given hopes for the development of an entirely new method of oil exploration. Any large scale method for the survey of radioactive anomalies must be based on the measurement of gamma rays, as beta and alpha rays have much too short a range to be of any significance. Thus the essential improvement which has made the present stage of this work attainable is the development of new highly sensitive detectors for gamma radiation. In the past the only detectors of any consequence that were available were the ionization chamber and the geiger counter, but both of these suffer from the defect that only a small proportion of the gamma rays passing through the counter are detected, possibly 0.1 to 0.2 pct. The recent development of the scintillation counter2,3 has completely transformed the situation and has had a considerable impact on many branches of nuclear technology. The detection of alpha particles in zinc sulphide screens by visual observation of the individual scintillations which these particles produce dates back to the early spinthariscope of Rutherford and Crookes, but the combined use of an appropriate scintillating phosphor and photomultiplier tube had to await the technical development of the latter many years later. With this development came the modern era of the scintillation counter and a knowledge of phosphors which have a large light output under the bombarding action of gamma radiation. Some of these phosphors are relatively dense and are capable of stopping a large proportion of the incident gamma radiation. As the sensitive region is the whole volume of the crystal, a very high detection efficiency, 50 pct or more, can be obtained for medium energy gamma rays. Scintillation counters for geological purposes were first developed in 19494-6 in an attempt to utilize this remarkable improvement in efficiency, which has the attractive consequence that only a small portion of the normal background of the counter is due to cosmic radiation. In 1949 tests were made in northern Saskatchewan by Lundberg Explorations Ltd. with portable scintillation counters which gave excellent results in the search for uranium and served to indicate unknown uranium deposits in areas previously closely surveyed with geiger counters. Portable scintillometers (registered in Canada) are now commercially available and in regular use,' and the adaptation of the instrument to radioactivity oil well logging has also been very successful.8 Initial attempts to measure radioactivity from aircraft with scintillation counters were made during this period in the same area and yielded most encouraging results. It would be appropriate to consider some specific requirements for airborne investigations. The essential problem to be met in the detection of any radioactive source is the necessity of obtaining a signal greater than the statistical fluctuations of the background counting rate for the instrument. It is possible to show that Nt>2k2 is the condition for detectability of a signal where N = average background counting rate for the detection. t = time constant of the counting rate meter, used to determine the average number of counts arriving in a certain predetermined time interval. N' = average source counting rate at the detector. k = N/N', and N>>N'. Sample values are given in Table I. Assume that the aircraft carrying the equipment is travelling at 120 mph, in which case it will cover 176 ft in 1 sec. Assume also, as a first approximation, that a point source target is in range when the air-

Jan 1, 1954

By J. H. Henderson, L. A. Wilson, R. L. Gergins, R. J. Wygal, D. W. Reed

This paper presents a method of predicting the production history of an underground combustion recovery process. A rigorous solution of the thermodynamics and hydrodynamics involved is beyond the scope of this report. However, a practical scheme to appraise combustion recovery performance has been Worked out. By prudent assumptions, regarding the attainment of steady-state conditions, a trial-and-error solution, which satisfies both material balance and three-phase relative permeability requirements has been evolved and tested. As a combustion zone moves through a formation the interstitial water, the water of combustion and a portion of the oil wil1 be vaporized. These vapors will move downstream to a cooler region of the formation where they will condense. Part of the remaining oil will be displaced by the imposed gas drive and what remains behind will be consumed as fuel. The fluids will distribute themselves downstrean? in a manner which will satisfy the three-phase relative permeability characteristics of the formation. Three distinct zones will exist ahead of the combustion zone: (I) a zone termed a water bank which contains three mobile phases, oil, water and gas; (2) a region containing two mobile phases, oil and gas, called the oil bank; and (3) a zone having the fluid saturution distribution which existed prior to combustion. The mobile water will impose a water flood on the oil in the region containing three flowing phases. The process can be visualized as a simultaneous water .flood and combustion-supported gas drive. It is possible to estimate the saturation distributions in the water bank and oil bank as well as the production history for any combustion temperuture if the porosity, three-phase relative permeability characteristics, oil viscosity and initial saturations are known. This has been done for injection pressures ranging from I to 100 atm, oil viscosities of 10 to 1,000 cp and porosities from 20 to 40 per cent. Several of these calculations have been checked in the laboratory, with the result indicating rather good agreement between the predicted and observed production histories. The analytical and experimental techniques are described and the comparison of predicted and observed performance presented. INTRODUCTION Considerable research by the oil industry during the past 10 years has been directed toward the thermal recovery of crude oil. Of all schemes considered, the one receiving the most attention is in situ combustion. This is a process in which part of the oil is actually burned within the reservoir rock. The uniqueness of the process lies in its potential. Theoretically, this potential generates from the following: (1) it may open the door to vast reserves previously not economically producible, (2) it may induce increased production rates where low rates are now realized and (3) it may give high over-all recovery efficiency. The general idea of the process has received considerable attention in the literature '-' and the following brief description is intended for orientation only. In situ combustion can be visualized by considering a linear system, one end of which represents the injection well and the other the producing well. The formation at the inlet end is raised to ignition temperature by placing a gas or electric heater at the face of the formation or by the ignition of thermite, charcoal or similar material. While heating, the water and part of the oil in the heated region is vaporized and moved out into the reservoir by the injection of gas containing oxygen. In addition, part of the oil is displaced as liquid by the imposed gas drive. The oil not displaced is modified to an immobile, coke-like material (hereafter referred to as coke) by the high temperatures existing immediately ahead of the combustion zone. This coke is used as fuel, and the combustion front advances through the formation at a temperature which is probably in excess of 800°F. As the combustion front advancek it will drive ahead all interstitial oil not rendered immobile and all interstitial water plus the water formed by the combustion of hydrogen. As a result the sand behind the combustion zone is freed of all oil and water. Although the general description of the process has been outlined in the literature, there has been no consideration of the behavior of the fluids moving downstream from the combustion front. It is the purpose of this paper to present a technique

By Henry Howe

THE brilliant and very original matter in Professor Jeffries' discussion ? should rank not only as an independent paper, but as a most important one. In particular, the explanation which it gives of the remarkable Sauveur phenomenon, over which so many of us have puzzled long and hard, is so clear, complete, and cogent as to go far toward establishing Professor Jeffries' hypothesis. The very features of Professor Sauveur's photographs which fit this hypothesis so exactly are reproduced in Chappell's photographs of steel coarsened under somewhat different conditions. 1 The ideas developed by these discoveries are so novel that conven- ience of language seems to call for new conventional terms for expressing them. In, what follows here I propose certain terms for this end, for criticism and improvement, and I attempt to generalize from Professor Jeffries' hypotheses. Generally speaking, a given set of grains which undergo no growth in the cold will, when the temperature is raised progressively, start to grow on reaching a certain temperature, and will continue growing at all higher temperatures. The "germinative" temperature is that at which growth begins, quite as the conditions which cause a seed to grow are "germinative." We have then. an inert temperature range below the germinative temperature, and a growth range above it, the germinative temperature being the limit between these two ranges. So, too, a germinant grain is one which is at its germinative temperature, and hence beginning to grow, while inert grains are those below their own germinative temperature, and the term "growing grains" includes those which are germinant and those which are above their germinative temperature. These last could be called "supergerminant" if the distinction should be needed.

Jan 12, 1916

By John H. Hollomon

In a recent paper,' a very early suggestion by Ludwik2 concerning the nature of the mechanical behavior of metals has becn reexamined and extended. In essence it was suggested that there exists, at least under certain conditions, a mechanical equation of state; that the stress required for flow depends upon the instantaneous values of the strain, strain rate, and temperature, and not upon their past values. It is proposed that under these circumstances thc stress does not depend upon past history of these variables, but is like the temperature of a gas that depends only upon the instantaneous values of the pressure and volume. This notion has not been applied to present-day studies of metals, though it is especially applicable to the study of creep. It is the purpose of this paper to analyze the significance and possible range of applicability of this idea and to determine how it influences the accepted ideas concerning creep. Stress-strain Relations It is wcll known that the stress-strain curves of metals are influenced by both train rate and temperature. For a fixed strain rate and temperature there is associated with each metal a stress-strain curve. If either the strain rate or temperature is changed a new stress-strain curve will be characteristic (Fig. I). A much more genera1 relation between the effects of these variables is possible, however. Consider the stress-strain curves of Fig. I determined at

Jan 1, 1947

By John H. Hollomon

In a recent paper,' a very early suggestion by Ludwik2 concerning the nature of the mechanical behavior of metals has becn reexamined and extended. In essence it was suggested that there exists, at least under certain conditions, a mechanical equation of state; that the stress required for flow depends upon the instantaneous values of the strain, strain rate, and temperature, and not upon their past values. It is proposed that under these circumstances thc stress does not depend upon past history of these variables, but is like the temperature of a gas that depends only upon the instantaneous values of the pressure and volume. This notion has not been applied to present-day studies of metals, though it is especially applicable to the study of creep. It is the purpose of this paper to analyze the significance and possible range of applicability of this idea and to determine how it influences the accepted ideas concerning creep. Stress-strain Relations It is wcll known that the stress-strain curves of metals are influenced by both train rate and temperature. For a fixed strain rate and temperature there is associated with each metal a stress-strain curve. If either the strain rate or temperature is changed a new stress-strain curve will be characteristic (Fig. I). A much more genera1 relation between the effects of these variables is possible, however. Consider the stress-strain curves of Fig. I determined at

Jan 1, 1947

By Arcy A., J. G. Davis, D&apos Shock

Results of a pilot operation in the Carlsbad Basin are discussed. After hydrafracing between wells, a block of potash was removed by solution techniques. The distance between frac wells was about 200 ft, the thickness of potash mineralization, 5 ft. By proper manipulation, a feed of concentrate brine was obtained. The ex-periment showed that the thin-bedded potash could be removed by the solution techniques. The details of well construction, method of operation, and removal rates are discussed. Continental Oil Co.'s laboratory research on the fundamentals of potash solution mining has been expanded by means of a series of field tests, and subjects such as well completion and hydraulic fracturing were added to the investigation. Both single-well and multi-well systems were studied in the field work. Discussion Background: The current paper discusses one field test in which potash was solution mined by a two-well system from a thin sylvinite zone. The potential economic value of solution mining evolves from (1) the use of drilled holes and solution techniques instead of excavated shafts and caverns and (2) the ability to mine both land and marine deposits through any type of overburden geology and below conventional mining depths. Recent interest has been focused on potash' and other soluble minerals, such as trona. Solution extraction minerals, such as copper and uranium, are also worthy of important consideration. In addition, many of the techniques are directly applicable to the construction of horizontal underground storage carverns in salt. There are two general approaches to potash solution mining. The first is to mine on a single-well basis, in which the same well bore is used for both injection and production. This method is slow, and the areal extent may be quite limited in other than very thick ore zones. The second, and the preferred approach, is to mine on a multi-well basis in which the solvent is circulated between wells. This technique, if applied in a manner which allows the ore zone to be mined from the bottom upward, results in nearly all the solution taking place from the cavern roof. Salt removal rates, therefore, are very much higher than from a single-well system.l Wells can be interconnected into a multi-well pattern by several means. One is to join single-well caverns in the lower part of an ore zone. Another is to use the hydraulic fracturing techniques developed in the oil fields.' We preferred the fracture approach because of its potential for creating the greatest area of salt exposure. Test Site Description: The field tests were conducted in New Mexico's Carlsbad Basin, where the potash deposits are flat and uniform over reasonable distances. Here, 12 potash zones are present in the massive Salado Salt section. The specific target was the Third Ore Zone which is about 4 ft thick at our location and about 1150 ft deep. The test pattern was designed in the shape of an equilateral triangle with a fourth well located in the center, 200 ft from each of the vertex wells. This configuration allowed the ore zone to be hydraulically fractured from the center well with good assurance that the fracture would intersect the bore of at least one outside well. Several multi-well test patterns would be available if the fracture connected all wells. Well Completion: Surface casing was set in the top of the Salado Salt at 600 ft to shut off water flows from the surface sands, and the salt section was drilled and diamond-cored to a point below the Third Ore Zone. A drilling fluid made of diesel oil with a small amount of emulsified water was used to drill and core the salt. This fluid was highly successful in preventing enlargement of the drilled hole and in promoting good core recovery. The three outside wells were completed by setting 51/2-in. casing at the base of a streak of anhydrite about 20 ft above the ore zone. Pipe was set high so that the intersection point of the fracture could be detected even if the fracture migrated above the ore zone as it progressed outward from the center well. The center well itself was completed by cementing 51/2-in. casing through the Third Ore Zone. Cement bond logs run on the center well have shown excellent bonding. Fracturing Practice: A mechanical tool was used to cut a notch through the casing and into the salt at a point about 1 ft below the ore zone in the center well. The purpose of this notch was to fix the point of fracture entry into the salt. The fracturing was done with water at injection rtaes as high as 30 bbl per min. The salt parted at 1450 psi; and it required only 5 min for the fracture to reach the well which was 200 ft to the south. It took about 5 min more to reach the other two wells. Caliper surveys were run to locate the point of fracture entry in the three outside wells. The fracture appears to have drifted downward slightly, entering the outside wells at the top of a streak of carnallite 8 or 9 ft below the ore zone. A cross section of the wells selected for the multi-well test is shown in Fig. 1. The figure includes KC1 values based on core analysis and the trace of the fracture plane between the wells.

Jan 1, 1971

By J. E. Hilliard, J. W. Cahn

In this paper it is suggested that the degree of contiguity (or contact) between adjacent grains be described by three parameters which can be rigorously determined from measurements on a random plane of polish. An expression is also derived for the number of contacts per unit volume and it is shown that this quantity can-not, in general, be estintated from measurements on a random plane. IN a recent contribution1 Gurland has proposed various parameters for describing the degree of contiguity (or contact) between grains of the same phase in an alloy. To relate these parameters to measurements on a random two-dimensional section, it was necessary in most cases to make some assumption about the form of the structure. Since Gurland was specifically interested in sintered carbide structures, he chose, quite reasonably, to assume that the grains were constant-size spheres and that all the intersections were flat areas of constant radius. Since, as we will show, the relationships between the parameters and the measurements are strongly dependent on the grain shape and size distribution, it is evident that these assump tions will not be satisfactory approximations for a

Jan 1, 1960

By C. G. Durdaller, W. H. Robinson, G. M. Pound

The nucleation rate of the a (pay) to 0 (white) tin transformation was measured as a function of temperature and a tin particle size using an X-ray diffraction technique. The powder specimens of a tin were essentially monodisperse and the small dinzension of the particles of these specimens was varied from 13 to 75 p. Several types of nucleation sites of differing potency were fbund to be operative in the nucleation process, but it could not be determined whether these sites were on the free surface of the tin particles or within the volume. Assuming that they were on the free surface, the average density of the most potent sites was calculated to be 2.5 to 5.3 x 10' sites per sq cnz through the application of a Poisson distribztion finction to the isothermal data. Analysis of the temperature dependence' of the rate constmts at a given fraction transformed suggests that the active sites are regions of higher free energy and not catalytic interfaces. Appreciable induction periods were observed at the lower temperatures of transformation. Experimental studies1 of solid-solid phase transformations have led to the belief that the new phase nucleates at structural imperfections. The purpose of the present work was to learn more about the mechanism of nucleation in solids and the nature of the singularities at which nucleation occurs. In this investigation nucleation rates in the isothermal transformation of gray to white tin were measured by an X-ray diffraction technique using essentially monodisperse powders of gray tin. This particular phase transformation was chosen for study because it presented fewer experimental difficulties than most others. The experimental temperature-control problems were minimal because the two phases coexist in equilibrium at 13.3"C, and measurable transformation rates occur at temperatures only slightly above room temperature. The growth rate of the P phase into the a2 is sufficiently fast to make the measured transformation rate equivalent to the nucleation rate, provided that the particle size of the samples is small enough; for the experimental temperatures used in this study, the particle diameter must be less than 100 p. EXPERIMENTAL TECHNIQUE The P tin used in this study was obtained from Capper Pass and Son Ltd., North Ferriby, Yorkshire, England, and was of 99.999 pct purity. It was transformedS to the a phase and ground into a fine powder in an agate mortar. This powder was separated by a Roller air classifier into seven fractions whose dimensions, as determined by microscopic measurement of many thousands of particles, are given in Table I and whose distribution of size within each fraction is given in Figs. 1 and 2. The shape of the particles was roughly that of an oblate spheroid,

Jan 1, 1964

By Kenneth L. Cook

THE five serpentine masses exposed within the northern half of Riley County, Fig. 1, constitute a major part of the few exposures of igneous rock in Kansas.' Although not many subsurface data are available for this part of Riley County,2 six deep wellsV indicate that the basement complex lies between 2500 and 3000 ft below the earth's surface. A northwestward-trending ridge in the present basement surface, which extends across the northern half of Riley County, is indicated on Mettner's contour map.' The serpentine masses lie in a region that was active during Pennsylvanian and Permian time along two main tectonic trends, which may, in part at least, have developed contemporaneously." One trend is northeasterly, as evidenced by the Nemaha anticline, the Abilene anticline, the Voshell anticline, and many other smaller northeastward-trending folds. The other trend is northwesterly, as evidenced by the central Kansas uplift, the Salina basin syncline, and smaller northwestward-trending folds. The area of the Abilene anticline was actively deformed during much of this time, and the present surface rocks, for the most part Permian in age, show many normal faults." The Bala and Leonardville intrusions lie within a mile of the axis of the Abilene anticline, Fig. 1, as mapped by Wallace Lee;' the Randolph No. 1 and Randolph No. 2 intrusions lie within about 5 miles of the axis; and the Stockdale intrusion lies within about 8 miles of the axis. The igneous rocks have intruded horizontal or gently dipping limestones and shales that are late Permian in age.V he period of intrusion, according to Moore and Landes, was probably Cretaceous.' At present a detailed description of the petrography is available for only the Bala intrusion. Moore and Haynes' describe the rock at Bala as a green, serpentinized, porphyritic, peridotite breccia containing inclusions of shale. The ground mass consists chiefly of serpentine and calcite with considerable chromite (5 to 10 pct) and some magnetite. The phenocrysts consist principally of altered olivine with some altered augite and biotite. Although probably different in petrographic details, all the serpentine masses are somewhat similar in that 1) they consist of a dark green, fine-grained ground mass of igneous rock containing many xeno-liths composed of fragments of the neighboring sedimentary rock; 2) they tend to form small mounds on the landscape, thus indicating their greater resistance to weathering and erosion; and 3) they are magnetic. Previous Magnetic Survey of the Bala Intrusion: To the writer's knowledge, only the Bala intrusion had been surveyed with a magnetometer prior to the magnetic surveys discussed in this paper. Dreyer8 interprets the intrusion as a vertical, eastward-plunging dike, on the basis of the results of his magnetic survey, Fig. 1, with a vertical magnetom-

Jan 1, 1956

By J. F. Myers, S. E. Sharp

The safety data presented in this paper are based upon replies to a Questionnaire sent out to representative mining companics. The authors feel that it is a fair cross section of the milling industry, in that the 17 companies, of the United States and Canada, reporting on 22 mills, are scattered from the Hudson Bay to the Mexican border and from coast to coast. These data concern the accident records of the various plants from 1939 to 1944, inclusive and the six years are divided into two periods. The first period (1939, 1940 and 1941) represents something of a normal operating condition. The second period (1942, 1943 and 1944) represents the period of time that was most affected by war conditions. During the second period there was a high labor turnover, inexperienced workers were numerous, women replaced men in many kinds of work, a labor shortage existed more or less throughout the industry, and supervision was pushed for peak production. All of the companies reporting compiled their accident experiences for these six years in accordance with the standards set up by the American Standards Association (New York, N. Y.), consequently the tabu lated data presented herein are comparable. The authors of this paper feel that the industry as a whole is greatly indebted to the personnel of the companies that furnished these data, which make this study possible for presentation. This survey covers a total exposure of 74,528,880 man-hours, with 105,471 man-days of lost time from 870 accidents. Safety Records In Table I, the safety record is shown of the various mills reporting. The severity rate is usually conceded to be the most vital statistical figure in safety parlance, therefore the participating companies are listed in order of their severity rate for the combined six-year period, under size of organizatiori. The table also shows the frequency rate as well as the frequency-severity ratio (F/S). As noted in Table I, most of the companies suffered an increase in both severity and frequency rates during the second period; only six of the 22 enjoyed an improvement. From correspondence with the various plants, it seems that a few had very little labor shortage or turnover, and these were not greatly affected. A few plants, anticipating the situation, strengthened their training facilities and actually were able to show a better experience during the second period. This gives great credence to the value of organized training in any safety program. The frequency-severity ratio (F/S) shown in the last column of Table I offers

Jan 1, 1947

By S. E. Sharp, J. F. Myers

The safety data presented in this paper are based upon replies to a Questionnaire sent out to representative mining companics. The authors feel that it is a fair cross section of the milling industry, in that the 17 companies, of the United States and Canada, reporting on 22 mills, are scattered from the Hudson Bay to the Mexican border and from coast to coast. These data concern the accident records of the various plants from 1939 to 1944, inclusive and the six years are divided into two periods. The first period (1939, 1940 and 1941) represents something of a normal operating condition. The second period (1942, 1943 and 1944) represents the period of time that was most affected by war conditions. During the second period there was a high labor turnover, inexperienced workers were numerous, women replaced men in many kinds of work, a labor shortage existed more or less throughout the industry, and supervision was pushed for peak production. All of the companies reporting compiled their accident experiences for these six years in accordance with the standards set up by the American Standards Association (New York, N. Y.), consequently the tabu lated data presented herein are comparable. The authors of this paper feel that the industry as a whole is greatly indebted to the personnel of the companies that furnished these data, which make this study possible for presentation. This survey covers a total exposure of 74,528,880 man-hours, with 105,471 man-days of lost time from 870 accidents. Safety Records In Table I, the safety record is shown of the various mills reporting. The severity rate is usually conceded to be the most vital statistical figure in safety parlance, therefore the participating companies are listed in order of their severity rate for the combined six-year period, under size of organizatiori. The table also shows the frequency rate as well as the frequency-severity ratio (F/S). As noted in Table I, most of the companies suffered an increase in both severity and frequency rates during the second period; only six of the 22 enjoyed an improvement. From correspondence with the various plants, it seems that a few had very little labor shortage or turnover, and these were not greatly affected. A few plants, anticipating the situation, strengthened their training facilities and actually were able to show a better experience during the second period. This gives great credence to the value of organized training in any safety program. The frequency-severity ratio (F/S) shown in the last column of Table I offers

Jan 1, 1947

By E. H. Rose

THE present symposium on flotation machines provides a unique opportunity for group reappraisal of standard or habitual viewpoints. A symposium is by definition a trading post for observations that might prove complementary when put together, thus leading to useful thoughts that might not have been evident from the original observations individually. The present paper, pertaining to power consumption in flotation, is deliberately an experiment of that kind. Data were solicited from the operating superintendents of several of the major flotation plants on this continent. The information received, covering a total of 14 separate operations in seven plants, has been collated in terms of power intensity; that is, the total power input per cubic foot of cell volume. This departs somewhat from the conventional expression of power per ton of ore treated, though the latter figure is also given for the plants concerned. Because of wartime restrictions, particularly in Canada, identifying names of plants and machines are withheld. Not as a firm conclusion, but as a tender for symposium discussion, the following points are made: I. That flotation is a power operation in much the same sense as ball milling. 2. That contact time is the complement of power intensity and may be decreased as the latter is increased. 3. That a decrease in flotation power per ton of ore can result from an increase in power intensity. ANALOGY WITH GRINDING In grinding, it has become axiomatic that the more the power put into a given operation, the greater the work performance. The analogous view is now proposed that the effectiveness of any flotation operation will be related to the mechanical energy usefully applied to that operation. Under this view, each increment of properly directed input energy should give either an increase in unit tonnage or an improvement in the metallurgical separation (concentrate grade or tailing grade), until either the theoretical limit imposed by mineral constitution or surface condition is reached, or until further increments of power become uneconomic under the law of diminishing returns. Thus, as in grinding, there are two forms of output that greater power input or improved utilization of power can produce. As for the law of diminishing returns, lower unit cost of power through improved generating efficiency in the past decade has pushed the limit back. Over and above this, however, there is strong indication in the operationg data herein presented that higher power intensity results in an actual economy of over-all power consumption. Like crushing and grinding, flotation accomplishes a rupture of the forces of molecular attraction, by taking particles from the common environment and placing them in the two separate environments of

Jan 1, 1944

By Walter R. Hibbard, Ming-Kao Yen

VARIOUS rationalizations of preferred orientations in cold worked polycrystalline metals have been based on the operation of at least two,1 three,2 five,4 an indefinite number,5 and all,6 slip systems of the type occurring in single crystals. Pickus and Mathewson3 suggested that the cold rolling texture in face-centered cubic metals could be rationalized on the basis of two or more operating slip directions symmetrically disposed about the direction of flow in such a manner that the resolved shear stress factor is equal for all operating slip systems and lattice rotations cancel each other. The importance of the direction of flow, † the necessity for the operation of slip systems capable of producing the required, changes in external dimensions, the maintenance of a common surface between adjacent grains and a symmetrical arrangement of the operating slip systems in order to produce an end orientation which is stable under additional deformation lead to the following rationalization of textures based on the type of slip systems operative in single crystals. The rationalization is intended to explain why certain orientations are suitable for deformational flow without a change in orientation and thus are stable end orientations or ideal texture orientations. It does not attempt to explain how the grains of a randomly oriented polycrystalline aggregate will reach this orientation. The rationalization is based on the following four postulates: I. The ideal textures for polycrystalline aggregates are the result of reorientations of individual crystals toward the same stable end orientation at which no further reorientation will occur even during additional deformation. Since, in simple slip, - the relative orientations of the stress axis and the active slip system determine the change in orientation during slip, it is considered that the orientation of the stress axis with respect to the ideal texture determines what slip systems must be active to retain the stable end orientation. Therefore the stable end orientation should be a symmetrical one around the stress axis with respect to the active slip systems such that lattice rotations resulting from slip will cancel each other and prevent a resultant change in orientation. (Rotational symmetry only-not translation, inversion, nor others-is considered here.) Thus a metal under a pure stress should develop a texture consisting of one or more of the crystallographically symmetrical directions, <100>, <110> or <111> for cubic metals or <0001>, <1010> or <1120> for hexagonal dose-packed metals, parallel to the stress axis. 2. Since the active slip direction is the direction of glide during simple slip and thus the direction of maximum shear movement, in the ideal texture the active slip

Jan 1, 1948