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J. L. JONES,* Pittsburgh, Pa.-If a nickel anode is cast under commer-cial conditions, will it contain nickel oxide? Will the nickel oxide affect the rate of corrosion in a double sulfate solution; or will the nickel oxide dissolve in a double sulfate solution? I would also like to ask whether a 98 per cent. pure nickel anode will corrode as fast as a 96 per cent. nickel anode; whether electrolytic nickel will corrode less rapidly than nickel containing a small amount of carbon; and whether the materials some-times used in coating molds for casting nickel anodes will affect the rate of corrosion of the anode? In other words, whether an electrically non conducting coating is likely to be present that will prevent the nickel anode from corroding rapidly. JOHN F. THOMPSON.-The nickel oxide will not dissolve in the double sulfate solution, as far as we know. We do not make the ordinary nickel anode of commerce, but we supply nickel to the nickel anode makers. Those makers almost invariably buy a high-carbon nickel shot, ranging around 0.45 per cent. carbon. In their process, they even further, car-burize it so as to get nickel that will melt easily and be fluid enough to fill the mold, so that the ordinary cast anode on the market is unquestion-ably oxide free. The only time that such an anode will have oxide will be through an error in melting. Some cupola makers of anodes have had trouble with oxidation, but as a rule the anodes are thoroughly carburized; so much so that they probably carry a couple of per cent. of carbon of which around. 1.6 per cent. is graphite.

Jan 12, 1919

By T. P. Floridis

It was deemed desirable to obtain an understanding of the vacuum desulfurization process. McKechnie1 has reported that the sulfur content of nickel- and cobalt-base alloys is reduced in vacuo. Keverian and Taylor2 have observed that vacuum melting causes desulfurization of iron-carbon-silicon alloys. Garnyk and samarin3 have desulfurized transformer steel by vacuum treatment. Experiments were conducted in order to investigate the desulfurization of liquid iron under reduced pressures, and to establish the effect of some alloying elements, and various crucible materials. A vacuum-induction furnace of 50-lb capacity was used. The charge was Armco iron. Silicon was added as 90 pct ferrosilicon, carbon as electrode graphite, and aluminum as high-purity aluminum metal. Magnesia and silica crucibles were used, their inside diameters were 5 1/2 and 5 3/8 in., respectively. The temperature was measured with an optical pyrometer and it was held at 1600 1 15°C. Samples were withdrawn with quartz tubes of 6 mm ID, without disturbing the furnace atmosphere. Pressures were measured with an alphatron gage. The experimental results are shown in Fig. 1. They indicate that: 1) Sulfur can be removed from liquid iron alloys by vacuum treatment; 2) The desulfurization is enhanced by the presence of silicon, carbon, and aluminum, all these elements increase the activity of sulfur dissolved in liquid iron;4 3) The pronounced effect of silicon indicates that probably a volatile silicon sulfide is formed, Alcock and Richardson5 have observed a similar phenomenon; 4) The same rate of desulfurization was obtained when the metal was contained in either magnesia or silica crucibles. Dr. J. Keverian has contributed many discussions and recommendations. M. S. Sutliff has helped in conducting the heats. The permission of General Electric Co. for this publication is gratefully acknowledged.

Jan 1, 1960

By A. S. Yue

It was deemed desirable to obtain an understanding of the vacuum desulfurization process. McKechnie1 has reported that the sulfur content of nickel- and cobalt-base alloys is reduced in vacuo. Keverian and Taylor2 have observed that vacuum melting causes desulfurization of iron-carbon-silicon alloys. Garnyk and samarin3 have desulfurized transformer steel by vacuum treatment. Experiments were conducted in order to investigate the desulfurization of liquid iron under reduced pressures, and to establish the effect of some alloying elements, and various crucible materials. A vacuum-induction furnace of 50-lb capacity was used. The charge was Armco iron. Silicon was added as 90 pct ferrosilicon, carbon as electrode graphite, and aluminum as high-purity aluminum metal. Magnesia and silica crucibles were used, their inside diameters were 5 1/2 and 5 3/8 in., respectively. The temperature was measured with an optical pyrometer and it was held at 1600 1 15°C. Samples were withdrawn with quartz tubes of 6 mm ID, without disturbing the furnace atmosphere. Pressures were measured with an alphatron gage. The experimental results are shown in Fig. 1. They indicate that: 1) Sulfur can be removed from liquid iron alloys by vacuum treatment; 2) The desulfurization is enhanced by the presence of silicon, carbon, and aluminum, all these elements increase the activity of sulfur dissolved in liquid iron;4 3) The pronounced effect of silicon indicates that probably a volatile silicon sulfide is formed, Alcock and Richardson5 have observed a similar phenomenon; 4) The same rate of desulfurization was obtained when the metal was contained in either magnesia or silica crucibles. Dr. J. Keverian has contributed many discussions and recommendations. M. S. Sutliff has helped in conducting the heats. The permission of General Electric Co. for this publication is gratefully acknowledged.

Jan 1, 1960

By W. B. Clarke

It is the purpose of this paper to discuss briefly some of the recent developmellts in connection with the use of electrical apparatus for the mining of coal. For several years electricity has been employed extensively for the distribution of power, primarily for the operation of mine-locomotives and chain coal-cutters, and secondarily for motors driving pumps, ventilating-fans, rope-haulage, conveyors, crushers, auger-drills, coke-oven larries, etc. The severe and peculiar conditions which attend the development and distribution of power for the operation of coalmining machinery constitute a field to which the electricmotor seems to be especially adapted. The underground use of steam-engines, to any great extent, is impracticable for obvious reasons. The much higher efficiency of the electrical system is a potent argument in its favor as compared with compressed air, which, under ordinary circumstances, should only be employed for the operation of rock-drills and coal" punchers." The conditions in many mines prohibit the under-cutting of coal with a chain-machine; and the compressed-air " puncher," with its very low efficiency, is extensively employed. There have been no recent important improvements in the design and construction of the chain-machine, although, of course, minor changes are continually being made. More time and attention are being paid now than ever before to the details of mining-machinery, with the idea of eliminating the weaknesses which have been developed, and especially of facilitating repairs and renewals. Electric mine-locomotives are very extensively employecl for the haulage of coal on the main entries and the branchheadings; but in the majority of coal-mines the cars are still

Jan 1, 1904

By P. Niessen, S. J. Bercovici

RECENTLY Aust et al.&apos; proposed a model of non-equilibrium grain boundary segregation based on a vacancy gradient induced uphill diffusion process of solute to grain boundaries. According to their proposal, solute atoms which are attracted to vacancies would, during the cooling of a sample, migrate with vacancies toward grain boundaries (vacancy sinks) and thereby enhance the solute concentration in boundary regions. For solute atoms which are not attracted to vacancies no such boundary solute enrichment would be expected. These concepts were given experimental support by boundary and bulk mi-crohardness measurements of various thermally treated dilute zinc and lead alloys and also doped aluminum oxide. The underlying assumption in their work was that solute enrichment in boundary regions is indicated by higher microhardness values. From thermodynamic considerations1&apos;2 it appears that the solid-liquid solute distribution coefficient (K), defined as the concentration of solute in the solid to the concentration of solute in the liquid at equilibrium, indicates whether attractive or repulsive forces exist between vacancies and solute atoms. K < 1 indicates a solute-vacancy attractions, K > 1 indicates no, or a repulsive, vacancy-solute interaction. This note is to report on observations of different grain boundary etching phenomena in high purity zinc alloys. These phenomena appear to depend on whether a K < 1 or K > 1 solute is present. In experiments designed to measure directly the solute enrichment in grain boundary regions, samples of zone refined zinc with 0.1 at. pct solute additions were cooled from 380°C at a rate of 3°C per min. A surface layer of approximately 50 was then removed from the samples by chemical polishing. The samples&apos; surfaces were then protected by a chromating treatment such that in a subsequent etch only grain boundary regions were dissolved. The dissolved regions were approximately semicircular troughs, 10 µ in width. The grain boundaries were usually in the middle, i.e., at the bottom, of this trough. For zinc containing the K < 1 solutes cadmium and aluminum, the grain boundary was always indicated by a ridge as shown in Fig. 1. For pure zinc, and zinc containing the K > 1 solutes copper and gold, a groove at the bottom of the trough indicated the boundary position, Fig. 2., To test if these different grain boundary etching behaviors were possibly connected with the segregation process discussed above, the Zn-Cd alloy was again heated to 380°C and quenched into brine. After surface protection and etching it was found that this specimen no longer exhibited the grain boundary ridges but rather grain boundary grooves as shown in Fig. 2. It would appear, therefore, that the boundary ridge is a consequence of a process occurring during the slow cooling of the samples. From absorption spectrophotometric analysis it was found that for slowly cooled samples containing K < 1 solutes, the solute/zinc ratios of the material from the boundary trough were consistently considerably higher than the solute/zinc ratios of the bulk alloys. This boundary region solute enrichment was not observed in quenched samples. It is concluded therefore, that the boundary ridge shown in Fig. 1 is directly or indirectly connected with nonequilibrium solute segregation.

Jan 1, 1970

By T. K. Perkins, L. R. Kern, R. E. Wyant

Many factors influence the results of hydraulic fracturing to stimulate well productivity. Most of these factors have been studied and their effects discussed in the literature. However, the movement of sand through the crack during fracturing has received little consideration. Exactly where the sand goes in the fracture, how it gets there, and how this might influence results have not been studied, judging from published reports. To get an answer to some of these questions we have studied sand movement through a simulated crack segment in the laboratory. Although the work is preliminary, we have answered some questions about sand movement in a semiquantitative sense. We are reporting our results at this time in the hope of stimulating interest and further study in this important aspect of fracturing. LABORATORY EXPERIMENTS Fig. 1 is a schematic diagram of equipment used in this study. A segment of a vertical crack 0.25-in. wide was formed between two Plexiglas plates, and movement of sand in fluid through the crack was observed under various conditions. Sand and fluid were injected into the crack at constant rates. The top and bottom of the crack were closed so that the fluid flowed horizontally. Because of gravity most of the sand settled to the bottom before moving very far through the crack. If the fluid velocity exceeded a certain critical value, then all the sand injected was washed on through the crack even though it had settled to the bottom. When the fluid velocity was less than this value when sand injection was started, most of the sand which settled in the crack remained in place until enough of the area open to fluid flow was blocked by the settled sand to increase the fluid velocity to the critical value.. At this point all injected sand moved on through the crack even though it settled to the lower portion of the moving fluid section. All sand previously settled remained in place. When fluid velocity was increased at this paint by increasing fluid injection rate (without also increasing sand injection rate), some of the previously settled sand was washed out until enough area was open to flow that the velocity dropped to the critical value. Conversely, when the fluid velocity was decreased by decreasing the fluid injection rate (without changing the rate of sand injection), additional sand would settle until the critical velocity was again attained. In short, the critical velocity is an equilibrium value which the system will automatically seek, if possible. The equilibrium (or critical) velocity was measured under several conditions. The results of these measurements are shown in Pig. 2 where the equilibrium velocity is shown as a function of the amount of sand injected per minute. The points falling in the shaded band shown in Fig. 2 were obtained with water. The higher viscosities were obtained by adding CMC (carboxymethylcellu-lose). Data indicate that the equilibrium velocity is not very sensitive to sand size or transport fluid viscosity, or to sand injection rate (except at very low rates). Points connected by the solid CUrve in Fig. 2 were obtained with water and 20- to 40-mesh steel shot. The equilibrium velocity is apparently fairly sensitive to difference in density between particle and fluid. Only one run was made with a gelled fluid and that was gelled water at zero sand injection rate as shown in Fig. 2. (Measurements of equilibrium velocity at zero sand injection rate were made by filling the crack

By D. J. Reed

Concord coal mine near Bessemer, Ala., built, owned, and operated by Tennessee Coal & Iron Div., U. S. Steel Corp., produces only a metallurgical grade for use as coke in blast furnaces of the division at the Fairfield and Ensley works. Capacity of the operation is approximately 800 tph, half of which is delivered to the coke and coal chemical plant at Fairfield after beneficiation to metallurgical grade coal. The remaining portion of the mine run is rock and refuse removed during preparation. Concord mine coal is hoisted to the surface coal preparation plant by an underground slope conveyor. The slope conveyor is 2449 ft long and has a lift of 729 ft. At time of installation the Concord mine slope conveyor was the largest single conveyor unit ever made with respect to belt horsepower and total lift. After several years it became necessary to determine the cause of slope conveyor cover wear.

Nov 1, 1956

By Robert W. Fullerton, Donald T. King

INTRODUCTION AND THEORY by Robert W. Fullerton In coal preparation plants, as in any industrial operation where raw materials are handled, nuisance problems arising from the generation of dust are inevitable. Devices for the control or collection of dust are there- fore essential components of the plant process equipment. The general term "aerosol" is applied to small particles suspended in a gaseous medium, usually air, whose velocity under the force of gravity is small enough that the particles remain suspended for a reasonable length of time. Aerosols can be classified as dust, smokes, fumes, mists or fogs. Dust includes particles originally formed by pulverization of materials by such processes as crushing, grinding, drilling, blasting and abrasion. Smoke includes particles formed from the burning of organic materials. Fumes are particles formed by processes such as condensation and sublimation, usually at high temperatures. Mists or fogs are particles formed by the condensation of water or other vapors on some nuclei. The size of aerosol particles is generally designated in units of microns, there being 1000 microns to a millimeter and 25,400 microns to an inch. Particles of about 10 microns or above are visible to the naked eye. Table 14-1 shows size characteristics of the general classifications of particles discussed above and includes typical examples of particles commonly en- countered. Table 14-1 also shows the relationship between micron size and standard screen mesh sizes. Smoke and fume are usually in the range of 0.01 to one micron, dusts are in the range of one to 400 microns, mists are in the range of 0.1 to 100 microns, and fogs are in the range of one to 100 microns. For purposes of dust control, particles greater than 10 or 20 microns in size are considered large, particles one to 10 microns are considered fine and particles below one micron are ultrafine. Sources of Dust Because coal is relatively friable, the mining and subsequent handling operations break part of the coal into dust that can be readily carried by currents of air. In a coal preparation plant mechanical handling operations such as unloading, transferring from one belt to another, screening, cleaning, and crushing in a dry state result in the generation and release of varying amounts of additional dust. The dust problem, of course, is much less serious in plants employing entirely wet processing. In addition to dust from handling operations, thermal drying of the fine coal product frequently presents another dust collection problem. Most coal driers are

Jan 1, 1968

By C. E. Meissner

THE need for a practical method of deciding upon new alloy steel analyses to widen its markets was the problem facing the Chrome Steel Works at the beginning of 1927. In addition to determining the physical properties of the alloys under consideration, it was necessary to test their value in service. Small melts of steel in a crucible, from which test specimens could be made, were insufficient to determine more than physical properties, therefore actual castings and ingots had to be made before the products could be placed in service. Furthermore, to save further experimental work, it was desirable that these heats should be made on a "pilot" basis; that is, actually duplicating regular open-hearth furnace practice. Therefore a one-ton (2000-lb.) acid open-hearth furnace was built. FURNACE DESIGN There are no special features in the design of this furnace. Standard acid open-hearth practice is followed, with the reproportioning of the dimensions necessitated by its small size; notably, a considerably increased length in proportion to width in order to get proper flame propagation. After the first heat was made it was found that the checkers were insufficient. The checker chambers were increased in size and the checker openings were made much smaller. The furnace was started late in March, 1927, and made 65 heats. Experimental work was then stopped until the data accumulated could be worked up and summarized. The run was resumed in November and the furnace is still operating, having made at this writing 60 additional heats. For the last series of runs, there was some rebuilding of both the furnace itself and the checkers. Slag pockets were added. Fig. 1 shows details of construction; Fig. 2, the, general appearance. All designing was done by the operating and engineering staff. Construction materials were those available around the plant. The reversing valve is a standard butterfly type taken from an old furnace.

Jan 1, 1928

By H. C. Theuerer

EVEN the highest purity silicon available for semiconductor use contains significant amounts of donors and acceptors, usually aluminum, phosphorus, and boron. Aluminum and phosphorus can be removed from silicon by adaptations of the zone refining techniques&apos; widely used with germanium. Removal of boron, however, has been a difficult problem. The approximate distribution coefficient for boron in silicon is 0.8, so that while zone refining is possible, it is not very effective in any reasonable number of passes. It has been found, however, that boron can be effectively removed from silicon by treatment of a liquid zone with hydrogen and water vapor. Starting with 40 ohm-cm, n-type silicon, use of zone refining coupled with hydrogen

Jan 1, 1957

By Charles M. Cooley

DURING the last week in April, cards were sent out from New York to Institute members affiliated with the Mining, Geology, and Geophysics Div. The cards requested recipients to indicate their main technical interest, within the division, i.e., mining, or geology, or geophysics. The reason for the cards is simple. Within the Institute more than 8000 have expressed either primary or secondary interest in this division. However, there is no way to determine the technical association stimulating this interest.

Jan 6, 1953

By Frederic Dewey

BONE-ASH cupels have been used from time immemorial to absorb litharge, and accompanying oxides; in assaying. Doubtless, also, from the earliest days cupels have been most unjustly blamed for much poor assaying. It has long been known that the precious metals go with the litharge into the cupel. This occasions a loss of precious metals and reduces the results of the assay. There have been many investigations of cupels and the most diverse views have been expressed, the extremes being the statements of Lodge 1 that every cupel has some effect upon the loss in assaying telluride ores and of the Campredons2 that coarse and fine and hard and soft cupels all give the same loss of silver when cupelling the same weights. The truth lies between these statements and much nearer the latter. In a vast majority of cases the influence of the cupel is not dominant and is outweighed by other conditions, particularly the temperature of the cupelling bead. At the Spokane meeting of the Institute I presented a paper on the Assay and Valuation of Gold Bullion,3 which recorded the results of many hundreds of assays made in the Mint service under everyday commercial conditions, which of necessity differ from scientific conditions. In following this matter up, for the purpose of increasing the accuracy of our commercial methods of bullion assays, the question of the absorption of gold by the cupel was found to be a most important one and was taken up for investigation. In a lesser degree, the silver absorption is important and interesting, but at present it appears to be far more complicated and, while many figures showing silver absorption may be found through this paper, much further investigation is required to put the subject upon a satisfactory basis.

Jan 11, 1917

By F. P. Dewey

Bone-ash cupels have been used from time immemorial to absorb litharge, and accompanying oxides, in assaying. Doubtless, also, from the earliest days cupels have been most unjustly blamed for much poor assaying. It has long been known that the precious metals go with the litharge into the cupel. This occasions a loss of precious metals and reduces the results of the assay. There have been many investigations of cupels and the most diverse views have been expressed, the extremes being the statements of Lodge1 that every cupel has some effect upon the loss in assaying telluride ores and of the Campredons2 that coarse and fine and hard and soft cupels all give the same loss of silver when cupelling the same weights. The truth lies between these statements and much nearer the latter. In a vast majority of cases the influence of the cupel is not dominant and is outweighed by other conditions, particularly the temperature of the cupelling bead. At the Spokane meeting of the Institute I presented a paper on the Assay and Valuation of Gold Bullion,3 which recorded the results of many hundreds of assays made in the Mint service under everyday commercial conditions, which of necessity differ from scientific conditions. In following this matter up, for the purpose of increasing the accuracy of our commercial methods of bullion assays, the question of the absorption of gold by the cupel was found to be a most important one and was taken up for investigation. In a lesser degree, the silver absorption is important and interesting, but at resent it appears to be far more complicated and, while many figures showing silver absorption may be found through this paper, much further investigation is required to put the subject upon a satisfactory basis.

Jan 1, 1918

By H. A. Wheeler

That lead and zinc deposits are the result of prolonged,, slow deposition is the idea of most students of ore deposits, and in many cases, where the ore-bearing solutions have been very weak or the precipitating conditions have been very feeble, the ore accumulations have undoubtedly taken a long period of time. As these two vital conditions have been subject to great variations in the different mining camps, the following example is highly interesting in showing that deposition can be very rapid under favorable conditions, geologically speaking, and also extremely recent. In fact, the writer is inclined to regard most, if not all, of the Mississippi Valley deposits of lead and zinc as probably being very young, at least not older than Tertiary, if not Quarternary, in age. The extensive Joplin lead and zinc district, in southwestern Missouri, which is about 60 years old and has numerous mines that were abandoned from 1 to 50 years ago, shows that the lead and zinc today are in an active condition of solution and redeposition, although these two metals occur in the predominant form of sulfides. The mine waters from the older and more or less abandoned portions of the district are frequently so acid, mainly from the oxidation of associated pyrite, as to necessitate the use of wooden pipes and pumps. The first boom in the Oklahoma zinc fields, which is the southwestern extension of the Joplin district, occurred when ore was accidentally struck in drilling a water well. Among the mines then opened up was the Mission mine, at Lincolnville, Ottawa County, Okla. This mine was opened in 1903 in lean "sheet ground," or a flat blanket formation of chert carrying disseminated zinc blende, or "jack," and galena. Theore-body was very free from iron pyrites and the concentrates were very high grade, the "mineral," or lead concentrates, assayed 80 to 85 per cent. lead and the jack, or sphalerite, assayed 60 to 65 per cent. zinc. The orebody was very shallow, occurring at a depth of 76 to 95 ft. (22 to 28 m.) and very wet, requiring three or four pumps to handle the water. The mine was operated until 1914, when it was closed by litigation and immediately filled with water. The second Oklahoma boom, five years ago, opened up the large, active camps of Picher, Tar River, and Century, which are located 2 to 5 mi. west of Lincolnville. They are considerably deeper, being farther down on the westwardly dipping monocline that emanates from the Ozark

Jan 1, 1920

By Henry Kreisinger

IN evaluating coals as steaming fuel on the basis of chemical and physical properties of the coals, the only properties that can be used are those for which the methods of determination are well established and standardized, and those that affect all methods of burning the coals in the same way. The discussion is written from the standpoint of the coal consumer. The production of steam is the largest field for the use of coal. It includes stations for generating electric power, central heating plants, industrial power plants where steam is used for power generation, factory processes and heating. The field also includes steam locomotives. Small house-heating boilers are not included in this field because such small boilers generally burn specially prepared domestic fuel. The plants using the steam coal are equipped to burn the coal when fired by one of the three general methods: namely, hand, stoker, and pulverized coal. The hand firing is now restricted to small plants and to locomotives. Central stations and larger industrial plants use either stoker or pulverized-coal firing. Some locomotives also use stokers. Pulverized-coal firing has been tried in locomotives but so far its adapta-tion to this use has been handicapped by practical difficulties. The coals used for steaming purposes are generally of the bituminous and semibituminous classes, with volatile matter ranging from 15 to 35 per cent. Coals belonging to these classes are produced in many parts of the United States and form by far the largest part of the total coal production of the country. The value of any coal as fuel for steaming purposes depends on the following factors

Jan 1, 1935

By Anders Carlson

NOTABLE advances have been made in the evaluation of oil-reservoir rocks from information furnished by core analysis. Among the physical data employed, per-meability is of primary importance. It may be assumed that the permeability of a core sample, considered as a property inherent to the nature of the porous medium only, is not markedly altered by the coring opera-tion, therefore some degree of accuracy is justified in the laboratory determination of permeability constants by means of homo-geneous flow media. To provide that such relatively simple determinations be sus-ceptible to duplication and consistent inter-pretation should prove advantageous in the prediction of subsurface flow conditions involving nonhomogeneous fluids. The air permeameter seems to fill most satisfactorily the need for rapid and fairly accurate determinations. Instruments that are similar in design and operation have come into general use. However, this has not resulted in an encouraging uniformity in the results obtained. Recognizing the value of reducing measured values to a common quantitative standard, the authors have sought to determine possible reasons for undue discrepancies and means for their elimination. This paper will be specifically concerned with three factors, which appear to be of some importance in the establishment of consistent permeability values: (I) design and operation of the permeameter, (2) preparation and mounting of the sample, (3) type of flow created in the sample.

Jan 1, 1940

By D. W. Fuerstenau

A detailed study of the residence time distribution in an industrial balling circuit is presented. Using fired recycle pellets as a tracer impulse in each experiment, material was found to pass through the drum under plug flow conditions with a mean residence time of about 20 seconds. The time for a single pass through the entire circuit is about 60 seconds. Approximately three passes are required for fresh feed to report as product. Segregation of the tracer pellets in the system, according to their diameter, was observed and reasons for this are suggested. These results should be of potential use in the modeling and control of ball balling circuits in the iron ore industry.

Jan 1, 1985

By John J. Gilman

BECAUSE of their layerlike structure, zinc crystals exhibit strong anisotropies for almost all physical and chemical properties. This should, and indeed does, greatly influence the plasticity of zinc for various crystal orientations. At low temperatures, the investigator of this plastic anisotropy is plagued by the great variety of deformation modes that operate. However, at high temperatures (250° to 419°C) only two deformation modes predominate: basal (0001) and prismatic (1010) glide. Furthermore, since strain hardening is virtually absent at high temperatures, the plasticity for these two modes of deformation can be very simply described by means of two equations of state. It is the purpose of this paper to describe the experimental behavior of basal and prismatic glide in zinc crystals, and to interpret this behavior in terms of other physical properties (in particular, the thermal expansion coefficients and the elastic constants) using the theory of dislocations. Fig. 1 defines the two planes of the zinc structure that will be discussed. Glide occurs very readily on the basal planes at all temperatures, and there is a very large literature on this subject. Much of the literature has been reviewed by Schmid and Boas;&apos; it will not be reviewed here. Kolesnikovl was the first to show that if basal glide is circumvented by stressing a zinc crystal parallel to the basal planes (giving zero shear-stress on the basal planes) then, at temperatures above about 320°C, glide on the first-order prism planes occurs. His results have recently been confirmed by Cahn, Bear, and Bell." These previous workers have established the existence and crystallographic elements of prismatic glide; the present paper is concerned with the stress, strain rate, and temperature relations of prismatic glide as contrasted with basal glide. Experimental Methods The crystals were square ones, 6x6 mm, that had been grown in precision Pyrex tubes by a method that is described in detail elsewhere.&apos; Most of the crystals were 99.999+ pct Zn (New Jersey Zinc Co. CP grade). Some were alloyed with 0.1 -+-0.005 atomic pct Cd, and chemical analysis showed that almost all of the added cadmium persisted through the crystal-growing process. For measurements of nonbasal glide, crystals were oriented with their basal planes parallel to both the rod axis and one of the flat faces of the square cross section. However, the orientation of the close-packed directions [1210] with respect to the rod-axis was variable. For basal glide measurements, the angle between the basal plane and the specimen axis was 35". The orientations were measured by the Gren-inger back-reflection X-ray method. The problem of finding a suitable method of gripping the crystals was the most serious experimental obstacle that arose. Because of the large plastic anisotropy of zinc, the usual gripping methods were unsatisfactory. Some methods that were tried were: high melting-point solder, making heads on the ends by locally melting a crystal, and electroplating nickel on the ends to form enlarged portions. For all these methods, the regions of the grips were weaker than the crystals themselves. Finally, two methods were decided upon: bend tests and direct machining of tensile specimens. In the bend tests, specimens were loaded as simple beams so that gripping was not a problem. The beams were 1 in. long and the axis of bending was parallel to the hexagonal axis of the crystals. For the crystals that were machined into tensile specimens, brass bars with slots in them were used to support the crystals, and thereby minimize the distortions due to machining. The crystals were glued into the brass bars with plastic cement which was later dissolved away with acetone. See Fig. 2, left. No clamps were used near the crystals and the machining was done using a milling machine with a fly-cutter. The tool bit was very sharply pointed to minimize burnishing. The feed was less than 1 mil per cut. The depth of cut was 2 mil for roughing cuts, and % mil for the finishing cuts. This machining method produced surface layers of tiny recrys-tallized grains only 2 to 3 mil deep, and the bodies of the crystals were not measurably disturbed. After the crystals had been machined and removed from the brass holders, they were chemically polished until about 5 mil had been removed from all their surfaces. The polishing reagent consisted of equal parts of concentrated HNO,, 30 pct H3O and ethyl alcohol; it is described in detail elsewhere." A typical crystal is shown in Fig. 2, right. The I-shaped faces are normal to the hexagonal axis of the crystal; otherwise the projections at the ends would simply shear off when the crystal was loaded. The cross section in the 2?-in. gage length is 0.215x0.115 in. It was found that the polished

Jan 1, 1957

By Bernhard Blumenthal

A melting process was developed by which high purity electrolytic uranium crystals can be converted into sound ingots without serious contamination. Careful preparation of the crystals, melting in a high vacuum, and directional solidification led to a metal of better than 99.993 wt pct purity. The metallographic examination showed a substantially clean metal with only residual amounts of a second phase which responded to heat treatment. The density of high purity uranium is 19.05 g per cu cm. FOR the study of the fundamental properties of uranium and its alloys, a base metal of high purity is needed, and an investigation was started at Argonne several years ago to examine various methods of preparing high purity uranium. Early success was achieved by the fused salt electrolysis process in preparing high purity metal in crystal form,&apos; and the problem became that of melting the crystals into ingots without contamination. The electrolytic crystals contained a few ppm of heavy metals, less than 15 ppm C, and large quantities of potassium and lithium in the form of trapped fused salt electrolyte. On melting in vacuo in magnesia or urania crucibles, the metal picked up considerable quantities of carbon and some iron, copper, and silicon but lost most of the potassium and lithium. It was not metallographically clean, and much research work was necessary to determine the optimum melting conditions for minimum contamination. This work has resulted in the development of a melting procedure by which sound ingots can be prepared with only a limited contamination by carbon. In the section entitled "Melting of the Electrolytic Metal," the equipment and processes that have been developed for melting the electrolytic crystals are described in detail. The "Metallography" section is devoted to the metallography of high purity uranium, and the section "Density of High Purity Uranium" contains the first property measurement on high purity uranium—a density determination. Melting of the Electrolytic Metal Apparatus—Melting and Vacuum Equipment: Uranium may be melted in either resistance or induction-type electric furnaces. Resistance heating was found to be preferable to induction heating for melting down the electrolytic crystals, for several reasons: Although induction heating permits fast heating, this advantage cannot be utilized when crucibles with limited thermal shock resistance are used. Temperature control of induction-heated melts is poor, and the stirring effect increases the rate of contamination of the melt from the crucible, slag, or the furnace atmosphere; liquation and controlled solidification are difficult to carry out. Because of these objections, resistance heating was chosen. A 10 kw Globar resistance furnace of low heat capacity permitted uniform heating of a uranium charge to its melting point in 45 min. The furnace was insulated with a removable aluminum shield so that, after melting and removal of the shield, the furnace could be quickly cooled to room temperature. The furnace was equipped with an apparatus for directional solidification; see Fig. la. The crucible was suspended in the center of the furnace; and when the melting was complete, the crucible was slowly lowered into the cold end of the furnace tube. Solidification took place upward from the bottom; and when the rate of lowering was small, a sound ingot free from sink holes and shrinkage cavities was produced. To remove the large quantities of gas contained in the electrolytic crystals, melting in a high vacuum is mandatory. While, from the standpoint of contamination, melting in a highly purified argon atmosphere appeared feasible, lithium and potassium removal proved less efficient under such conditions. Also, a vacuum-melted ingot has a cleaner surface than one melted in an inert atmosphere. The vacuum system must be of very high pumping speed and leak tight so that a vacuum of less than 2x10-7 mm Hg is attainable when the system is pumped down cold. The system must have a high pumping speed, so that the pressure maximum which may rise to 1x10-4 mm during heating can be quickly reduced

Jan 1, 1956

By C. Norman Cochran

The pllnse diagvam for the NaF-AlF3 system was used to calcutate an ionic model for the NaF-AlF3 system. Assuming an ideal solution,a series of simultaneous equations expressing equilibria be-tween solid and liquid phases at the euleclic, perilec-tic, and melting points were solved for the activities of the ionic species, the dissociation constants, and the entropies and heats of fusion. The calculations suggest the existence of A13F1415 ions in addition to the F-1+AlF6-3 , and AlF4-4 ions previously proposed by others. The calculaled valnes give better agreement with vapor pressures than the previous model without Al3Fl14-5. Additional possible vefinements of the model are proposed. CRYOSCOPIC1 investigations and density data2 for the NaF-A1F3 system have previously been used to study the dissociation mechanism of Na3A1F6 and to derive equilibrium constants for its dissociation to NaF and NaAlF,. Depending primarily on the heat of fusion assumed for cryolite, the dissociation constants ranged between 0.02 and 0.18 from cryoscopic studies, and from 0.09 at 1273°K to 0.16 at 1363°K from density data. In most cases the values were unable to reproduce satisfactorily the experimental liquidus lines very far on the A1F3 side of the Na3A1Fe composition. This suggested the existence of at least one other ionized compound in the melt besides NaA1F4 in the Na3A1F6-A1F3 side of the system. This is assumed to be liquid Na&13F14 (chiolite), which is already established as a stable solid in phase studies of this system. MODEL FOR THE MELT The melt is assumed to be an ideal solution with ion activities equal to anion fractions. The only cation in the model is sodium so that Temkin and simple anionic activities are identical. Although the compounds are completely ionized to Na&apos; and the respective anion in the melt, molecular rather than ionic notation is used throughout this work. The Na3A1Fe is assumed to dissociate to NaA1F4 and NaF as in the former model, and Na&13F14 to dissociate to Na3A1Fe and NaA1F4. Other valid dissociation equilibria can be written involving these four compounds, but all of these can be obtained by combinations of the two described dissociation reactions and, thus, are automatically considered in these calculations. The model allows for no free AlF3 so that compositions for NAIF3 > 0.5 (mole fraction A1F3 on the NaF-A1F3 basis) cannot be treated. The question of the existence of free AlF3 in the melt will be discussed again later. The constants in the model were evaluated from points along the entire known liquidus line of the NaF-A1F3 system. Previous work employed only the liquidus line or densi- ties near the Na3A1F, composition. The liquidus line compositions used in the solution of the model are from unpublished work by Mr. P. A. Foster, Jr., for compositions between the Na3A1F6 melting point and the Na&13F14-A1F3 eutectic, and from the published works of Grjotheim,1 Phillips,3 and Foster4 for the remainder of the system. The relationships used in solving for the desired dissociation constants and heats and entropies of fusion are listed in Table I, and the points along the liquidus line at which each apply are indicated to the right of the relationships. The mole fractions of each of the separate species in the melt are symbolized by N. Relationships [I] and [2] are the respective dissocia-ation constants, Kl and K2, of Na3AIF6 and Na5A13F14 for this model. For simplicity, these constants will be assumed to be independent of temperature. Relationship [3] follows from the assumption of the ideal solution. The expression relating the values of N to the experimental values of NAIf3, is given in Relationship (41. Relationships [5], [6], and [7] each state the equilibrium between a compound in the melt and its pure solid phase for the portion of the liquidus lines where it precipitates. The heats of melting, AH,, and entropies of melting, AS,, used in [5], [6], and [7] are assumed to be independent of temperature. The compositions and temperatures of all five invariant points (two melting points, two eutectics, and one peritectic) along the liquidus lines from NAIF3 = 0 to NAIF3 = 0.5 were employed in the solution. The eutectic and peritectic compositions were particularly useful because each of these is involved in one more equation than other points along the liquidus lines and thus reduces the number of points required to solve for the constants. Also, their use assures that the inflection points in the derived liquidus line will correspond exactly with those on the experimental liquidus line. The total number of equations is 5k1 — 1, where n is the number of experimental composition points used. The number of unknowns is 4n + 5 (4n- 3 values of N, 3 values each of AH, and AS,, and 2 values of K). Thus, six points must be used in the solution to obtain an equal number of equations and unknowns. The one additional required experimental composition was taken on the liquidus line between the Na3A1Fe melting point and the Na3A1F6-Na5A13F14 peritectic. Previous work indicated this was a difficult portion of the curve to fit. The temperature used for the point was 1161°K, the same as for the NaF-Na3A1Fe eutectic. This choice of temperature gave two points with identical NNa3AIF6 values which simplifies the algebraic solution. The second point at this temperature is denoted 1161°&apos;K. PROCEDURE FOR SOLUTION OF EQUATIONS Values were assumed for NNa,AIF and NNaF at the NaF-Na3A1F6 eutectic at 1161°k. By an iterative procedure, the corresponding values for NNa5A13F14 and NNaAlF4 at 1161°K were determined from 131 and 141. A value was assumed for NNaAlF4 at 1161°&apos;K and

Jan 1, 1968