Search Documents

Jan 1, 1890

By C. J. Rosa, W. C. Hagel

An attempt is made to determine the diffusion coefficients of oxygen ions in hypostoichiometric zirconium oxide. A phenomenological theory is developed for three-phase, unidirectional volume diffusion of a gaseous species from a planar source. Knowledge about oxygen diffusion in a and ß zirconium and experimentally measured rates of movements of interfaces permit the evaluation of oxygen ion diffusivi-ties in ZrO2-x. The results conform to the relationship: sq cm per sec, for the temperature range of 875" to 1050° C. DIFFUSION coefficients of oxygen ions in stoichio-metric oxides have been studied by many investigators. The obtained results not only supplement the knowledge about the lattice-defect structures of oxides and conduction mechanisms but also provide information of technological importance. Rate processes such as oxide sintering, high-temperature creep deformation, and oxidation of metals and their alloys are directly dependent on diffusion phenomena. Unfortunately, diffusion coefficients obtained from studies on stoichio-metric oxides cannot be treated without restraints when applied to oxidation kinetics, if precise evaluations of oxidation rates are desired. Oxides formed on metals are usually nonstoichiometric and exhibit nonuniform distribution of either cation or anion vacancies across their thicknesses. Debuigne and Lehr1 extended Danckwerts'2 mathematical analyses and furnished a semitheoretical treatment for evaluating oxygen diffusion coefficients in zirconium oxide in terms of weight gain measurements during oxidation of zirconium in the temperature range 400° to 850°C. Their calculations are based on theoretical partitioning3 of the total amount of oxygen between a zirconium and its oxide phase. An inherent discrepancy appears to continue throughout their calculations. The amount of oxygen confined to the oxide phase should be corrected by multiplying the calculated oxide thickness by the inverse of Pilling-Bedworth ratio, if expansion of zirconium dioxide is taken into account. The purpose of the present investigation is to provide a new semitheoretical treatment for evaluating diffusion coefficients of moving species in hypostoichiometric oxide. The analyses are relevant to unidirectional volume diffusion. Although the presented method is quite general, its applicability will be discussed in terms of kinetic measurements from oxidation of zirconium at temperatures above the a/ß transition, for reasons stated in the later part of this paper. EXPERIMENTAL Pure, 99.93 wt pct, zirconium samples of approximately 2 by 1 by 0.35 cm were exposed to oxygen for various times at four temperature levels: 875°, 950°, 1000°, and 1050°C. High-purity, better than 99.9 vol pct oxygen was passed through a cold trap and columns containing anhydrous CaSO4 to remove residual water vapor. Before exposing to oxygen at a pressure of 500 Torr, specimens were subjected to wet abrasion on 200- through 600-grit Sic papers and polished with 1—p diamond dust. Prior to oxidizing, all zirconium samples were vacuum-annealed at 10-6 mm Hg for about 15 min at the test temperature. The temperature variation across the uniform heat zone was ±2°C from the preset value. Final polishing, for phase thicknesses measurements, was performed by using 8- and 1-p diamond dust and followed by vibrator polishing with 0.05-µ ? Al2O3 solution. Measurements of phase thicknesses were made by projection on a metallographic viewing screen. Conventional powder X-ray analyses for the oxide were employed. RESULTS Fig. 1 is an example of the cross section of oxidized zirconium. Designations of phases given below this figure are the same as those used in the three-phase diffusion system represented by Fig. 5 in the following section. Zirconium oxidized for longer exposure times showed two types of oxides: white oxide at the surface and an underlaying layer of gray oxide. X-ray powder patterns of these oxides at room tern-

Jan 1, 1969

By A. P. Miller, T. S. Washburn

Improved procedure in the manufacture of rail steel has come as the rail user demanded better wearing qualities combined with greater unit weight. With each weight increase per lineal yard has come greater difficulty in making a product that would successfully withstand all tests that modern rails must meet. With these facts in mind, and with a sincere desire to produce a rail whose service in track would be satisfactory in all respects, the steelmaker was quick to realize that all of the factors entering into his process would have to be more closely controlled. Control of rail-steel slags was recognized as one of the most important of many interdepending factors. The object of slag control is to hold the slag compositions within a range that gives the best results with respect to economy of production, uniformity of analysis, and quality of the finished rails. The most important component of the slag from the standpoint of these production and quality factors is the ferrous oxide content. This component is a good indicator of the basicity and oxidizing power of the slag, and these largely govern the effect of the slag on the steel. Consequently, the

Jan 1, 1935

By Frank T. Wheby

The cost of tunneling is highly sensitive to the rock characteristics through which the tunnel is to be driven. These characteristics affect in a major way the rates at which tunnels and shafts can be driven and the degree to which the openings must be supported to maintain them in a permanent stable condition. Tunnel and shaft design and cost criteria have been computerized, permitting estimates of tunnel-shaft systems to be made directly from inputs of rock mechanics characteristics and other data. Curves of quantities of steel, rock bolts, and other rock support items as related to tunnel size and rock quality designation are presented. An illustrative example of the use of the program in calculating the cost of a hypothetical tunnel system is included.

Jan 1, 1971

By David T. Day

In the summer of 1898, a demand suddenly arose for commercial quantities of the element osmium. At least half a ton was wanted for the manufacture of a new incandescent light. This led the writer to examine localities where platinum had been reported, in order to determine whether osmiridium mas contained in the crude platinum. With the co-operation of the concern most interested, the Welsbach Light Company, and in company with its President, Col. William E. Barrows, I visited most of the leading American localities where platinum has been obtained. I also wrote to every available placer-mine in the West for samples of the heaviest sands, in order to test them for platinum. The results of this inquiry are given in the present paper. Distribution. The notices of the occurrence of platinum in this country given in scientific journals include two interesting observa tions in the East. One concerns a nugget described by Peter Collier of Washington, D. C.,* and said to have been found on land adjacent to the village of Plattsburgh, N. Y., which weighed 104.4 grammes, and contained sufficient chromite to reduce the specific gravity from 17.35 for the heaviest portion to

Jan 1, 1901

By A. P. Miller, T. S. Washburn

Improved procedure in the manufacture of rail steel has come as the rail user demanded better wearing qualities combined with greater unit weight. With each weight increase per lineal yard has come greater difficulty in making a product that would successfully withstand all tests that modern rails must meet. With these facts in mind, and with a sincere desire to produce a rail whose service in track would be satisfactory in all respects, the steelmaker was quick to realize that all of the factors entering into his process would have to be more closely controlled. Control of rail-steel slags was recognized as one of the most important of many interdepending factors. The object of slag control is to hold the slag compositions within a range that gives the best results with respect to economy of production, uniformity of analysis, and quality of the finished rails. The most important component of the slag from the standpoint of these production and quality factors is the ferrous oxide content. This component is a good indicator of the basicity and oxidizing power of the slag, and these largely govern the effect of the slag on the steel. Consequently, the

Jan 1, 1935

As already said Pattin's map and the later one of Evans' showed coal in several places in Ohio as early as 1750, and possibly 1748; the reference on the latter map was' to an exposure near Bolivar, in Tuscarawas County, as well as along the Hocking River. So far. as now known, it 'was not mined in either place until 1810. George Croghan, in descending the Ohio with his party in 1765, mentions an "Alum Hill" which they saw near the present site of Pomeroy, probably an exposure of saline deposits, but does not mention coal. As settlement north of the Ohio River was prohibited until 1787, no coal was mined until long after that date. In 1785 a survey of seven ranges in the Ohio country was made, the line running west from a point on the north bank of 'the Ohio River, due north of the western termination of the southern boundary of Pennsylvania. The surveyors noted, "from hence to Stoney Brook between two very steep and high Ridges; it is eight yards wide, its bottom is of Slate and Sand Stone, and in many parts of it are large pieces of excellent Coal washed by, the Rains from the Neighboring Hills."' This was the present Yellow Creek, and the coal was from some of the lower measures. The Scioto Company published a pamphlet in French in 1787, to promote the sale of their lands and emigration to them, in which was said,

Jan 1, 1942

By O. E. Kiessling

THE Committee-on Production Control, at its meeting held during the last annual session in February, 1930, evidenced great interest in problems of stabilization affecting all mineral industries. . No immediate program of activity for the Committee as a- unit was decided on, however,, and efforts during the past pear have consisted lirgely of further stressing the economic aspects of mineral production and of the action by committee members, :.serving in their individual capacities, in sponsoring constructive changes, in specific, industries. Of greatest interest to the general subject of production control in 1930 was the very definite advance toward better coordination of demand and supply in the petroleum industry. Furthermore, since opinion both within and without the oil industry now favors a constructive program, and with a gradual change in legal precedents, it seems not unreasonable to expect greater progress in the near future.

Jan 1, 1931

By G. V. Raymor, James T. Waber, I. Rex Harris

The lattice parameters of a series of fcc alloys of cerium and thorium were measured at 93 " and 298OK. Lattice parameters were also estimated for 171OK. Substantial deviations, y, from Vegard's law were observed. Although y was negative at the two higher temperatures, it was positive and large at the lowest temperature. A variety of models, which have been proposed in the past, were considered, and the calculated values of y were compared with the observed values. The best agreement was achieved with values computed with Friedel's equation. THE purpose of this investigation was to determine the effect of temperature on the lattice parameter and on deviations from Vegard's law of Ce-Th alloys. A large negative deviation from Vegard's law was first observed independently by Weiner, Freeth, and Raynor' and Van vucht2 in the room-temperature lattice parameters of Ce-Th alloys that form a continuous series of solid solutions. This observation was confirmed by Evans and Raynor. The allotropy of unalloyed cerium was reviewed recently by Gschneidner, Elliott, and McDonald. In two subsequent papers,5" these authors reported the influence of various alloying additions on the y= transformation, which occurs below room temperature. Although other rare earths tend to stabilize the double-hexagonal phase, thorium, plutonium, and scandium as solutes tend to stabilize the normal fcc phase. With addition of sufficient thorium as a solute, there is evidence that the formation of is suppressed and it becomes possible to pass continuously with decreasing temperature from the room-temperature phase to the fcc a phase. Thus there is a closed loop which is similar in many ways to the y loop well-known in ferrous alloys. A closed field also occurs in the pressure-temperature "equilibrium" diagram of unalloyed cerium. Because of interest in the effect of thorium additions and their influence on the a and phases, lattice-parameter measurements were made at low temperatures on the fcc phase for a series of alloys ranging from 10 to 90 at. pct Th. The results obtained at three temperatures are shown in Fig. 1. Evans and Raynors analyzed the deviations from Vegard's law in Ce-Th alloys in terms of changes in the occupancy of the 4f electron level in cerium,

Jan 1, 1964

By A. Goldberg, T. E. Tietz, J. E. Dorn

Introduction The concept that the flow stress for plastic deformation of metals in the work hardening range is a function of the instantaneous values of the strain, strain rate and test temperature was promulgated by Ludwick' many years ago. This thought has been more or less a guiding principle throughout the immediate period of development and growth of mechanical metallurgy. It has been tacitly assumed or knowingly applied to many investigations on the plastic behavior of metals. Spurred by the theoretical interest and practical importance of the plastic behavior of metals, many investigators have attempted to determine empirical, semi-empirical, and theoretical equations2-l8 relating the flow stress with the strain, strain rate, and temperature. Although the applications of such equations have been extensive, the experimental verification of the existence of a mechanical equation of state is weak. Furthermore, some of the available evidence on plastic flow appears to suggest that no simple functional relation between stress, strain-rate, strain and temperature can exist. The mechanical equation of state demands that Where a = true stress = loadlinstantaneous area e = true strain _ Instantaneous gauge length ~ initial gauge length i = true strain rate T = temperature This formulation implies that da is an exact differential. Therefore the flow stress (a) is a function of the instantaneous values of the strain (c) the strain rate (i) and the temperature (T), independent of the previous mechanical or thermal history. Having reached a certain strain, strain rate, and temperature, by any path whatsoever, a definite and fixed value of the flow stress should be obtained. One check on the validity of the mechanical equation of state is easily obtained. Consider the following three tests on the stress-strain curve at constant temperature: A. Strain at rate :I B. Strain at rate it C. Strain at rate 11 to el and continue test at &. A graphical representation of possible results of such tests are shown in Fig I. If, for strains greater than el, test (C) data coincide exactly with the data from test (B), as shown in Fig ra, a limited verification of the mechanical equation of state is obtained for the range of strain rates from il to iz. But if the data from test (C) differ from those of (g) beyond strain t\ where the strain rate is changed from il to k2, the mechanical equation of state is not

Jan 1, 1949

By M. H. Richman, E. S. Meieran

An analytical method is presented which enables the electron diffraction patterns from a twinned region to be indexed. The method has only been applied to (112) twins in bcc lattices, but can easily be adapted to other types of twinned lattices. Calculations of all twin spots, including those superimposed on matrix spots, is made possible by this method. SINCE the advent of transmission electron microscopy, the analysis of selected-area electron diffraction patterns has become very important in the interpretation of electron micrographs. Frequently, as in the case of some martensites, twinned areas are observed and give rise to complex diffraction patterns, which so far can be analyzed only for the simplest orientations of the thin foil specimen with respect to the electron beam. In order to simplify the analysis of twin patterns of more complex orientations, an analytical method was devised which is capable of predicting the positions of all reflections from both matrix and twin regions for all possible foil orientations. Although the method has only been applied to the case of bcc metals twinned about a (112) plane, it is equally applicable to other Bravais lattices. This method has been successfully applied to selected-area electron diffraction patterns of Fe-Ni and Fe-Ni-C martensites and drawn tungsten wire. PROCEDURE Imagine the reciprocal lattice corresponding to a bcc material, with each point hkl representing the crystallographic plane (hkl). Since the extinction conditions require that for this lattice, only reflections where h + k + 1 = even integer are allowed, the three dimensional reciprocal lattice is actually fcc. Since in real space twinned regions and matrix regions are mirrored across a (112) plane, the twinned reciprocal lattice is derived from the matrix reciprocal lattice by a rotation of 180 deg about a (112) direction. While it is possible to calculate how a point hkl will shift under a twinning transformation to a new point htktlt using only the reciprocal lattice based on the orthonormal vectors [100], [010], and [001], the calculations are greatly simplified if a new orthonormal coordinate system containing the twin axis is introduced. The twinning operation then becomes a simple rotation of 180 deg about a principal coordinate axis (in this case the twinning axis), and a retransformation back to the original reciprocal space will give the position htktIt of the twinned reflection.

Jan 1, 1963

By Raimo Matikainen

Sublevel stoping has been used in Finland since the 1930's and today more than ten under- ground mines have adopted it as their main stoping method (Fig. I). Approximately 80% of the total underground tonnage is mined by sub- level stoping (Table 1) The first mines to introduce the sublevel stoping method in Finland were limestone mines. The development of sublevel stoping was very slow up to the mid 1960's when the switch to trackless mining started and the increase of mechanization lead to higher capacity and productivity. The method itself has been almost the same since the 1950's when long hole drilling was introduced. According to a future prognosis sublevel caving will give way to sub- level stoping; on the other hand, open pit mining will at the same time grow rapidly with some new mineral orebodies, which will he brought into production. Most Finnish orebodies are, however, only marginal ores and they could not support mining with more expensive methods than open pit mining or sublevel stoping. The future of sublevel stoping seems relatively bright. GEOLOGICAL AND ROCK MECHANICAL BACKGROUND The rock mechanical conditions in Finland are in general relatively good and the rocks firm. The compressive strength is normally 40 - 150 Mpa and modulus of elasticity 40 - 200 Gpa. Low values are common in altered and fractured rocks and near the ore contact Rock stress measurements have been carried out already for 20 years for mine design and monitoring purposes. The results of these measurements show that relatively high horizontal stresses seem to be common (Fig. 2).

Jan 1, 1981

Professor Jenney has performed a notable service in presenting this summary of the steadily increasing body of observation on the presence of carbon in rocks of all kinds and its probable influence upon ore-deposition, and in formulating a mode of comparing directly the relative resistance of minerals to oxidation, as well as their reducing-power, and the protective action which minerals having higher reducing-powers exert in preventing the oxidation of associated minerals which possess relatively lower affinities for oxygen. I have had an opportunity of observing a vein which falls within the scope of his interesting discussion. The vein at Ku Shau Tzu, Mongolia, lies directly across a contact of limestone and overlying bituminous shales. Probably it occupies a compression-fissure. The shale has been reduced to such a condition of' non-coherence that much of it can be crushed in the hand, producing a handful of angular fragments resembling beech-nuts in shape and size. In the limestone the metals are principally in argentiferous galena with some pyrite and blende; but the latter two are very subordinate in quantity to the galena. In short, it is an every-day lead-vein in limestone, with siliceous limestone gangue. It is one of those veins in which the ore is not continuous, but consists of a band in the country-rock in which seams of lead sulphide begin at one wall and cross in a bent form, increasing in thickness, to the other wall, where they thin out and end. This may indicate torsional stress, but the shape of the lenses points to some other action. They often ran nearly parallel to the hanging-wall for a considerable distance and crossed the vein on a moderate angle, but turned sharply along the vein on approaching the foot-wall. The intermediate rock contains nodules, bunches and specks of ore, and the lenses vary exceedingly in size, shape and position in the vein.

Jan 1, 1903

By Walter S. Weeks

THE process of cooling air by allowing it to expand and do work in an engine is well known, but the theory of obtaining cold air by free expansion without the aid of an engine operating with cutoff has been little discussed. Case 1 If compressed air is allowed to expand to the atmospheric pressure through an orifice in an sir line that is supplied by a running compressor, no cooling results except the negligible one due to the Joule-Thompson effect, which will not be considered in this discussion. The effect of moisture will also be neglected. Symbols P1 Absolute pressure in pipe line, lb. per sq. ft. P3 Atmospheric pressure, lb. per sq. ft. V1 Volume occupied by 1 lb. air in pipe. V3 Volume occupied by 1 lb. air at P3. Cv Specific heat of air at constant volume, B.t.u. per lb. per deg. F. Cp Specific heat at constant pressure, B.t.u. per lb. per deg. F. T1 Absolute temperature of air in pipe, deg. F. T3 Absolute temperature of air outside after expansion and mixing and coming to rest. J Mechanical equivalent of heat (778 ft. lb.) R Gas constant for air, ft-lb. per deg. F. = 53.3. Formulas Consider 1 lb. of air moving out of a pipe. The air behind it does work on it to the extent of P1V1 ft-lb. This work is really done by the thrust of the piston of the compressor and does not come from any energy that exists in the air in the pipe. The pound of air contains

Jan 1, 1937

By William E. Ford, Edward Salisbury Dana

The aluminate, ferrates, etc., allied chemically to the borates, have been already intro- duced among the oxides. They include the species of the Spinel Group, pp. 418-423, also Chrysoberyl, p. 423, etc. SUSSEXITE. In fibrous seams or veins. H. = 3. G. = 3.42. Luster silky to pearly. Color white with a tinge of pink or yellow. Translucent. Index, 1.59.

Jan 1, 1922

Discussion of the paper of J. K. FURST, presented at the Pittsburgh meeting, October, 1914, and printed in" Bulletin No. 94, October, 1914, pp. 2493 to 2514. W..McA. JOHNSON, New York, N. Y.-On discussing this paper I am open to the criticism of "bringing coals to Newcastle," as I, a zinc man, am bringing new ideas on steel to Pittsburgh. But still the view of an outsider can be valuable to the insider. Any multistage process, where each apparatus operates on its particular part of the work at a high efficiency, constitutes an advance in the state of art. But in multiplicity there can be complication and ensuing loss and inefficiency. The duplex steel process is not the pronounced success which was predicted for it by its adherents, for several of such plants have reverted to plain open-hearth methods. If we regard broadly refining processes, such as the Bessemer, open-hearth, puddling, copper refining, lead cupelling, nickel refining, we find that in general refining processes are intermittent and 'concentration processes are continuous. (This generalization I believe to be original with me; it was communicated to Dr. E. F. Roeber, editor, and appeared as an editorial in Metallurgical and Chemical Engineering, March, 1905.) Where we desire primarily quality in a metallurgical operation we must put a batch of metal in the furnace, work on it until we get it to the required purity, test it, and take it out; whereas, if we desire primarily quantity we shove ore into a furnace and smelt it as fast as possible, allowing conditions to make a non-uniform product provided only we get tonnage. From general commercial principles, I believe that the weak point of the duplex process is that the operation is not a money maker unless the plant is kept at. 90 to 95 per cent. of its rated capacity, or unless the Bessemerizing is done so often that it is practically continuous. For in some manner the operation should be made continuous and the control on the tonnage should be commercially flexible. The commercial rigidity of having to control purity exactly increases operating costs without a corresponding gain. Conversely, the chief reason for failure of "steel from ore direct" is that it makes a final operation continuous, which should be naturally intermittent.

Jan 4, 1915

By P. D. Merica

ALUMINUM and its alloys have been the subject of much investigation, during recent years, in the course of which the principal features of the constitution of most of the binary alloy systems with aluminum have been determined. Except in the case of a few metals-silicon, bismuth, cadmium, lead, zinc, and tin-an aluminum-rich compound is formed in each binary system, which forms a eutectic with the aluminum or its solid solution with this compound. Thus such compounds as FeAl3, CuAl2, Mg4Al3, and NiAl3 are formed, which are found in aluminum-rich alloys of their respective series as eutectics with the aluminum solid solution. These compounds are, in all cases, hard and brittle and their presence affects profoundly the physical properties of the alloys in which they occur. Within the zinc-aluminum system a compound, Al2Zn3, is formed that decomposes at lower temperatures. Silicon and tin each form a simple eutectiferous series with aluminum; bismuth, lead, and cadmium are only partly miscible in the liquid state with it. The extent of the solubility in aluminum, in solid solution, of these compounds or of the elements themselves, in the case of those series

Jan 7, 1919

By H. DeWitt Smith

THE disastrous effect of two major wars on foreign economic health is giving American capital opportunities which might have not otherwise developed. At a time when discovery of major orebodies in the United States awaits fuller application of new geophysical tools and technical methods, U. S. investors must seek other fields where investment may be put to work. The unsettling effects of war have made it almost impossible for foreign nationals to develop mineral wealth, permitting Americans to enter at a time when U. S. mining, with a few exceptions, is in the process of expanding known orebodies and developing only a few new ones. Available capital, however, is not the only pre- requisite for entering the foreign mineral development field. The capital must be able to work in favorable economic atmosphere, a condition not easily satisfied in a world constantly in a state of political and social flux. In many countries, the political theory changes as often as the wind direction in March. Thus, the political stability of the form of government is of prime importance to the investor. In addition, a balanced budget and a moderate tax structure are important. Because in making foreign investment it is inevitable that one will have dealings with government officials, it is basic that they must be of high integrity. In countries filling the requirements, it will usually be found that the economic initiative of the individual is respected. Newmont Mining Corp.'s three major investments in the last 15 years have been in Canada and the

Jan 1, 1952

By Scott Turner

OUR Institute, in its annual Directory, states the following: The purpose of each Technical Committee is to further the development of the special mineral industries in its field, chiefly through obtaining and discussing papers suitable for publication by the Institute. The proper field of the new Health and Safety in Mines Committee is judged to include the entire mining industry, and involves the multitude of health and safety problems arising in all kinds of mining operations. The mining industry in the United States has made much progress during recent years in reducing accidents. This advance has been widespread, and has been especially notable in the mining of iron ore. Yet the statistics of the U. S. Bureau of Mines, when compared with figures of the National Safety Council for other industries, show that mining still has a higher personal mishap rate than any other major industry in this country. In addition, studies of dollars-and-cents cost of casualty occurrences indicate that an important part of our mining cost, held by various authorities to be as much as 10 per cent of the total, is due to accidents.

Jan 1, 1933

By H. H. Klepfer, K. J. Gill, P. Chiotti

SOME observations relative to the U-Zn system have been made by other investigators. Chipman1 and Carter2 have reported the preparation of several U-Zn alloys and point out that these alloys are generally difficult to prepare. Chipman1 reported evidence for a high melting compound at about 90 atomic pct Zn and the possible existence of a eutec-tic between the compound and uranium. Raynor," in a theoretical discussion of the alloying properties of uranium, included zinc among the elements predicted to have little or no solubility in a, p, or y uranium. In the present investigation, thermal analyses, X-ray, metallographic, and vapor-pressure data were obtained to determine the phase boundaries. The relatively high zinc pressure over most of the alloys at temperatures of 900 °C and above proved troublesome and special techniques had to be employed in preparing suitable alloys. Materials and Preparation of Alloys The metals employed in this investigation were Ames Laboratory biscuit uranium containing less than 500 ppm total impurities and Bunker Hill slab zinc or Baker Analyzed reagent granulated zinc, both with a purity of 99.99+ pct. Due to the high vapor pressure of zinc and the high reactivity of both uranium and zinc with oxygen at only moderately high temperatures, alloys were prepared in closed containers which had either been evacuated or evacuated and filled with helium. High purity magnesia, magnesia containing 10 pct calcium fluoride, and tantalum proved to be suitable crucible materials. Tw-o different procedures, described below, were used to prepare alloys, the latter being the most satisfactory. The metals, uranium turnings and granulated zinc, were cleaned with dilute nitric acid, rinsed, dried, and placed immediately in a helium-fill'ed dry box. The two metals were placed' in a 10 mil Ta crucible. The charge was enclosed in the tantalum crucible by welding on a preformed tantalum cap. This assembly was enclosed inside a stainless steel (AISI 309) bomb. The bomb was made by welding a piece of stainless steel plate on each end of a stainless steel pipe. All these operations were carried out in a helium atmosphere. These assemblies were heated in a muffle furnace at temperatures between 1100" and 1200°C for 10 to 15 min or held as long as 15 to 20 hr in the 950" to 1000°C temperature range before quenching. Spectrographic and chemical analyses showed no tantalum pickup by the alloys, indicating no reaction between the alloys and the crucibles. However, some of these crucibles failed, probably due to imperfections in the welds of the stainless steel or tantalum crucibles. The second and most satisfactory method was to prepare the alloys by powder metallurgy techniques. The procedure was to press degreased and acid-etched uranium turnings with granulated zinc into 20 g compacts under 20,000-psi pressure. The compacts were placed in MgO crucibles, and sealed in evacuated Vycor or fused silica tubes. The alloys were then heated as long as two weeks at about 550°C in a muffle furnace. The pressed compacts were observed to expand by several volume percent during heating and it was necessary to make allowances for this expansion in order to avoid breaking the crucible and Vycor tube. This method was found very satisfactory for preparing alloys which were suitable for thermal analysis or vapor pressure studies. Experimental Methods and Results The phase diagram for the U-Zn system at 1 atrn pressure, shown in Fig. 1, is based primarily on vapor pressure measurements and on thermal analysis taken at temperatures below 950°C. Fig. 2 shows the U-Zn diagram at 5 atrn pressure, constructed on the basis of thermal analysis of alloys in sealed containers up to 1150°C and on the basis of metallographic, X-ray, and analytical data. The alloys sealed under vacuum were actually under their own vapor pressure and those sealed in an atmosphere of helium were under an additional pressure due to the helium. At temperatures up to 1100°C the zinc pressure is 5 atrn or less for these alloys; consequently the maximum pressure over the alloys sealed under a helium atmosphere was 10 atrn or less at temperatures up to 1100°C. Changes in pressure of this order of magnitude do not appreciably alter the position of most solid-solid or liquid-solid phase boundaries. In constructing the phase diagram for a pressure of 5 atm, the effect of pressure on all phase boundaries except those for liquid-vapor or solid-vapor regions was considered negligible.

Jan 1, 1958