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By A Guinier

RECIPITATION in alloys is undoubtedly one of the most essential phase transformations in metallurgy and, besides, it is a phenomenon of great interest to physicists. It seems then that it can be chosen as a topic for an Annual IMD Lecture. Of course, the subject is a very wide one and I shall discuss here only a very restricted part of it. I should like to show why it is now considered that there is, at the beginning of the process, a stage distinct from the real precipitation, which is the pre-precipitation. We shall be chiefly interested in the atomic structure of the metal in this preprecipi-tation stage. Numerous reviews on this subject have been published recently.', ' The latest was given by H. K. Hardyh t the last meeting of the Institute of Metals in London. One of the most complete articles has been written by the late Dr. Geisler." I should like, at the beginning of this lecture, to pay a tribute to the memory of our friend Arthur Geisler. Some of the ideas which will be developed here are different from those advocated by him. But everybody knows the considerable progress in experiment and in theory which we owe to him and, personally, I deeply feel how fruitful have been the long discussions which we have had during many years. Experimental Basis of the Precipitation Problems Let us recall the essential facts pertaining to the problem of the precipitation. The starting point and the final one are well known. The initial stage is the supersaturated solid solution before quenching. The dissolved atoms replace some of the atoms of the solvent at the points of a definite lattice. It is generally considered that the distribution of the atoms is completely random, and that the lattice distortions are relatively weak. These assumptions are only an approximation. It has now beenproven", that, in some cases, the dissolved atoms have a tendency to segregate to form very small nuclei. These fluctuations of composition are greater than the normal statistical fluctuations in a purely random alloy. We shall see the role played by these nuclei later. The final state is obtained by a very long annealing at such a temperature that an equilibrium is reached in a reasonable time. The alloy is then composed of a matrix which is a saturated solid solution, much poorer than the initial one. Imbedded

Jan 1, 1957

By J. H. Bain, D. C. Haigh, L. C. Parsons

Jan 1, 1964

By E. C. Olsen

This paper describes the unusual hazardous conditions encountered in mining thick, inclined coal beds under heavy cover in Carbon County, Utah. This description includes heavy roof conditions, sloughing ribs, steep pitches, and severe bouncing experience. Emphasis is placed on the top bench system of mining and development in the top half of a 16-ft seam, under the roof rock, which is bolted, and the recovery of the bottom coal on retreat; success of bolted roof and ribs; and shuttle car haulage on pitches up to 25%. The use of protective cages for operators of face equipment, the guarding of belt conveyor systems to prevent injury associated with deliberate entry, and the positive lockout of electrical equipment is described and illustrated. Most coal mining areas of the Western United States are characterized either by thick beds, steep pitches or heavy cover. Individually, each of these may present inherent safety hazards that in- fluence mining. When all are met at one location, the combined effect is to make the safe operation of the mining property a challenge to management. These combined conditions are met in the coal mines of the Columbia-Geneva Steel Div. of the United States Steel Corp., in southeastern Utah. This coal bed measures up to 16 ft in thickness, the pitch is as much as 25% and mining is under a cover approaching 3000 ft. The Sunnyside coal bed is found in the Book Cliff Mountains, a great escarpment extending from west of Castle Gate, Utah, some 180 miles to Grand Junction, Colo. West of Green River, Utah, the Book Cliffs swing sharply to the north because of the domelike uplift of the San Rafael Swell to the southwest. It is in this northerly extension of the Book Cliffs that the Sunnyside coal in the Blackhawk Formation of the Mesa Verde Group, Upper Cretaceous Age is found. The strata are transected by numerous faults with from a few inches to as much as a hundred feet of displacement. All of these faults have had some effect on the mining operation, either in roof control or, in the case of major faulting, the pattern of mine development. MINING PRACTICES Mining has generally been confined to the Lower Sunnyside Seam which measures from 7 to 16 ft in

Jan 1, 1963

By R. F. Nielsen, R. G. Bentsen

Jan 1, 1966

By Frank Rieber

THE study of earthquakes long ago developed the fact that by studying the travel times of the various groups of waves from the same earthquake, as received on seismographs at varying distances, major discontinuities in the earth's crust could be reasonably well defined. Using this original discovery, and adapting the mathematical methods originally devised in seismology for determining the depth below the surface at which such discontinuities occur, other investigators were able to develop a new branch of seismology which promises to be extremely useful in extending the boundaries of our information on local conditions below the earth's surface. As an outstanding example of the applications of this work, we have the so-called "seismograph" exploration of the Gulf Coastal region, which has resulted in the discovery of a large number of salt domes, from many of which oil fields may be developed. The original seismological investigations, from which different major discontinuities in the earth's crust were deduced, as well as these later successful experiments in locating salt-dome structures, involve relatively simple problems. In each case we are dealing with surface materials in which elastic waves will be propagated with a fairly definite velocity. Under this material we have something quite different, in which the elastic waves will be propagated with a much higher velocity. The transition from one medium to the other is likewise relatively abrupt. For example, in the Gulf Coastal region the sedimentary formations have a velocity of 6000 or 7000 ft. per sec., while the velocity of elastic waves in the cap rock of a salt dome may exceed 15,000 ft. per sec. Under such conditions, delineation of the formation is a relatively simple matter, and, furthermore, there is very little opportunity for ambiguous results.

Jan 1, 1928

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 Frank E. Woolley, Robert D. Pehlke

Jan 1, 1965

By Robert B. Fulton

The use of industrial minerals by the chemical industry as raw materials for manufacturing and in processing spans a wide assortment of minerals. This chapter aims to supplement rather than duplicate the commodity chapters. Its objective, to describe the uses of industrial minerals in the manufacture of chemicals, is attained by considering minerals used by the chemical industry in terms of the chemical element required and by giving particular emphasis to market factors. The mineral aspect, which is covered in the commodity chapters, is subordinated and attention is focused on the chemical and market aspects. Condensing this broad subject into a few pages permits treating only the most important elements derived from industrial minerals. The elements derived from petroleum, hydrogen and carbon, which quantitatively dominate as raw materials for the chemical industry, are omitted, as are the metallic elements and the minerals covered in other "use" chapters such as phosphorous, potash, and nitrogen for fertilizers and titanium dioxide for pigments. After eliminating on this basis, our definition leaves six elements of major importance: boron, bromine, chlorine, fluorine, sodium, and sulfur. These elements are treated individually under separate headings. Salt brines have particular importance as raw material sources for the chemical industry as shown in Table 1 "Salt Brine Derivatives" (Anon., 1967), which charts the chemical compounds derived from four types of brines: (1) Owens Lake type brines which are sources of boron and sodium compounds; (2) Midland type brines from which bromine, iodine, and chlorides of calcium, magnesium, potassium, and sodium are derived; (3) Searles Lake type yielding boron, bromine, lithium, magnesium, potassium, and sodium compounds; and (4) Silver Peak type produced mainly for lithium. Table 2 (Jones, 1973) affords an overview of the chief industrial minerals, the chemical products derived from them, and end uses of the products.

Jan 1, 1975

By A. E. Anderson, H. J. Hilll

Laboratory data for 155 field muds and 77 .shales have been used to develop correlations to estimate the net streaming potential component of the SP. Analysis of these data and comparison with field tests show that streaming potential corrections must be made to obtain an accurate estimate of the electrochemical potential for use in the determinntion of formation water resi-iiviy. The self-potential curve is related to formation water resistivity, and considerable effort within the oil industry has been directed toward clarifying this relationship. The Schlumbergers and Leonardon1,2 recognized that two types of potentials, electrochemical and electro-kinetic, resulted in the net potential variation in the borehole. Most of the later papers have dealt with the electrochemical component and its controlling parameters. The investigations of Wyllie,2" Salisch' and Moore5 provide the most extensive sources of data on streaming potentials across mud cakes. These authors observed streaming potentials of sufficient magnitude to be of critical importance in SP interpretation, if it is assumed that streaming potentials develop only opposite permeable beds. Streaming potentials across shales have been reported by Schenck and by Gondouin, et al.7 Since SP magnitude is the difference in potential opposite shale and sand beds, these authors suggested that the net streaming potential component may be negligible. The present investigation was initiated to evaluate empirically some of the parameters controlling the magnitude of the net borehole streaming potential and to determine whether useful relations between mud properties and net streaming potential could be established. Field muds were used in this investigation. These muds were characterized by the amount and type of chemical treatment utilized for five days before Sampling. Filter loss, mud resistivity, mud density and filtrate resistivity were determined for each mud with conventional methods and apparatus. Mud filtrate pH was estimated with Hydrion pH paper for the appropriate range. Streaming PotentIals Across MuD Cakes Commercial calomel-saturated KC1 electrodes are subject to potential changes attributed to contamination of the very small fiber-tip bridge by particles of clay from the drilling mud.3 To minimize this difficulty, a large diameter bridge (Fig. 1) was constructed with saturated KC1-agar gel and a filter disc of microporous porcelain. Experiments showed that streaming potentials across this bridge are less than 0.2 mv at pressure dif-

By R. J. Colony

DEPOSITS of iron are widely scattered in the folded Cretaceous rocks and the associated igneous intrusives of Puerto Rico. Most of them are too small for commercial development, but a few have aroused some scientific and economic interest, among them the large body of residua] limonite at the west end of the island near Mayaguez1-6 (Fig. 1) and the mixed hematite and magnetite deposit on the southern slopes of the Sierra de Cayey, about four miles north of Arroyo.7-9 Neither of these orebodies has been developed, nor have investigations of the widely distributed deposits of magnetite, which include all the remaining occurrences of iron deserving of economic consideration, proceeded beyond the exploratory stage. With the possible exception of the mixed deposit near Arroyo, the magnetite is directly associated with andesitic and dioritic intrusives, which invade the Cretaceous rock section, and the bulk of it, occurring in calcareous sediments, is clearly of contact-replacement origin. The small deposit on Rio Portugues, north of Ponce, is found in a limestone band near its contact with an andesite dike.10,11 Two deposits of unde-

Jan 1, 1935

By W. J. Kroll

Jan 1, 1960

By R. L. Caldwell, E. E. Glenn, L. J. Norton, A. J. D. Straus, S. V. Holcomb, J. Zemanek

A new and unique logging tool, called the Borehole Televiewer (BHTV), has been developed to inspect boreholes and to evaluate formations. Even though geologists and engineers have had only about 3 years' experience with the BHTV, the thinking of many of them has been radically influenced by the fascinating and revealing "log-picture" recorded with the tool. The BHTV fills a need for a logging tool that can produce a direct and descriptive record of the physical properties of the borehole environment. Although primarily developed to evaluate fractured reservoirs, the BHTV has been used successfully to solve a variety of problems related to formation evaluation and borehole inspection. Geologists and petroleum engineers have been confounded for many years by the problems of locating and evaluating fractures. Interpretation of the usual resistivity, acoustic or radioactivity logs, as well as the analysis of cores, for evaluation of fractured reservoirs is extremely difficult and often not definitive. This is understandable since analysis of cores from fractured formations has reported variously: (a) low porosity, (b) no effective permeability, (c) lack of any matrix oil saturation and (d) oil stains on fracture planes as the only indications of potential production.14 In recent years acoustic amplitude logs have been introduced and used with varying degrees of success to locate fractures.8'9'11"13 Conventional amplitude logs at best give only qualitative answers where quantitative ones are desired. The logs reveal nothing of the orientation of the fractures. In addition to these logs, various types of cameras, television, and rubber impression packers have been used for borehole inspection. (See Appendix.) The BHTV logging tool supplies both the quantitative and the orientation answers about fractures. The borehole can be filled with any homogeneous, gas-free liquid such as fresh water, saturated brine, crude oil or drilling muds. This tool takes an "acoustic picture" of the borehole wall. The resulting log is a representation of the borehole wall as if it were split vertically and laid flat. The log is oriented with respect to magnetic north. Any physical changes in the borehole wall are seen as changes in picture intensity. In this way, fractures, deformation or pits are reflected on the log. Tool Description The fundamental parts of the BHTV are shown in Fig. 1. A piezoelectric transducer probes the borehole wall with bursts of acoustic energy. A flux-gate magnetometer senses the earth's magnetic field and provides the means for determining the orientation of the log. A motor rotates the transducer and mag-

Jan 1, 1970

By Charles H. Jacoby

The solution mining of evaporites has a history of approximately 5,000 years. The insitu leaching of metalliferous ore will have many of the same characteristic problems which have confronted industry for years in the production of evaporite minerals. Basically we will be converting the less soluble forms of valuable metals into their more soluble salts and producing these in much the same manner as, for example, sodium chloride. There are a number of problems which we are faced with that are more complex and complicated and, therefore, will require a higher degree of sophistication than previously employed. One of our most important undertakings will be the clearcut definition of the problems involved. While a great deal of expertise can be drawn from the solution mining of evaporites and the oil industry, problems peculiar to the hydrometallurgical field will need to be solved. One of these is the introduction of permeability into an impermeable rock so as to expose the sought after values of metals which by volume are infinitesimal when compared with sodium chloride, potash or other type water soluble mineralization. After establishing this permeability which will be miniscule when compared to a solution cavity, there will be the maintenance of this permeability. In general, salt deposits are of a somewhat uniform chemical composition and thus their chemistry was relatively simple. Each metalliferous ore body is somewhat unique in its chemistry and will need to be treated accordingly.

Jan 1, 1974

By R. C. Earlougher

Jan 1, 1970

By A. J. Terrones

THE classical papers on contact metasomatic deposits by Lindgren on the Clifton-Morenci district,' by Barrell on Marysville, Mont.,' and by Gold-schmitt on the Oslo district, Norway,' laid the foundation for understanding of the importance of separating the metamorphic process from the subsequent metasomatic stage. Knopf' made a big step forward by recognizing that sulfide ore minerals are invariably younger than silicates and by further stressing the importance of structural control" in ore finding. Some years later Harrison Schmitt" fought the idea that contact metasomatic deposits are erratic, irregular, bunchy, economically marginal, and of small size, concluding that these descriptions have little factual basis. He emphasized the importance of detail mapping and careful geological study as fundamental requirements for a better understanding of these deposits. This article presents a comparative description of the structural features at the Magistral, Antamina, Morococha, Vilca, Ferrobamba, Katanga (Quibio), Tintaya, and Huarca contact deposits (Fig. 1). Further, it will describe how these structural features controlled the emplacement of the intrusives, their shape, distribution of metamorphic and metasomatic halos, and sulfide deposition in post-skarn structural channelways. Finally, the modifications introduced by a superimposed hydrothermal stage recognized at some localities will be discussed. Primary exploration and careful sampling of recognized structural targets were instrumental in outlining the copper ore potential at the Antamina and Tintaya districts, thus proving the benefits and reward of careful geological examinations in this type of deposit. The Magistral District: This district lies in the Province of Pallasca, Department of Ancash, in northern Peru, at 8o 16' S and 77" 47' W. High to medium grade copper orebodies in garnetite, bordering a quartz monzonite stock, are exposed at the bottom of a glaciated valley in the western slope of the Andes at 4250 m (14,000 ft)* elevation.

Jan 1, 1959

By A. Roberts

This paper reviews progress in equipment design and in the techniques applied to mine lighting in Great Britain. The incidence of the disease miner's nystagmus, which was a major source of concern only a few years ago, has now diminished, largely owing to improvements in standards of lighting in mines. The reorganisation of the coal mining industry, involving increasing mech-anisation, together with new safety legislation, has brought about the widespread use of mains electric lighting underground. An account is given of some of the results of research to determine the lighting conditions needed for compliance with the compulsory legal requirement of "sufficient and suitable" general lighting at specific localities in British mines. Some details are given of the techniques applied and the results of recent research in the problem of glare from miners' cap lamps. Of the various factors in the working environment of the miner, it is true to say that lighting is seldom given attention comparable with that devoted to other factors, such as dust, heat and humidity, or atmospheric gas content. No doubt one reason for this lies in the ability of the human eye to adapt itself to low brightness levels. Be that as it may, the fact is that at the turn of the 20th century the miner's working light improved little throughout the centuries during which mining technology has developed. Indeed, in coal mines which encounter a methane explosion hazard, flame safety lamps, with a luminous intensity less than one candle power, were virtually the sole means of lighting during almost the whole of the 19th century. The 20th century has witnessed a substantial improvement in lighting techniques underground in coal and metalliferous mining. In Great Britain the general pattern has been one of standards periodically raised by the implementation of Statutory Regulations imposed under successive hlines Acts, but it is fair to add that the more progressive mining companies usually anticipated the Statutory Regulations, which when they have been put into effect have served to turn into general practice what was already being done at the better mines. In earlier years, official requirements were limited to the specification of approved lamp designs, with stipulated minimum values of luminous intensity and light output, but more recently the necessity of satisfactory maintenance of standards during service has been recognized, and the current regulations not only require that a maintenance organisation should exist, but also specify a maximum permissible depreciation below initial approval standards.'

Jan 1, 1961

By J. M. Toguri, K. Grjotheim

It is known 1,2 that the equilibrium between titanium metal, TiCl2 , and TiCl3, in a solvent of molten metal chlorides, is influenced both by the total amount of dissolved titanium and by the type of solvent. Assuming that the trivalent titanium forms the complex ion Ti111 Cl4, the equilibrium reaction may be expressed by the following equation, (Me) TiIII cl4+ 1/2 Ti = 3/2 TiII cl2+ (Me) Cl The ideal ionic equilibrium constant for this reaction is, Where the N's are the molar ionic fractions in the equilibrium melt, and (Me) the different types of cations present in the equilibrium mixture. The following thermodynamic relation is derived between Kand the concentration of cations in the equilibrium melt, mix The N"S are the equivalent ionic fractions, and so forth are constants corresponding to the standard changes in free energy for reactions in melts where only the cation indicated is present, and f (y1) is a function of the activity coefficients in the equilibrium mixture. When this term vanishes, a simplified linear relationship between In Kideal and the concentration is obtained. The simplified relationship has been applied with satisfactory results to the experimental data of Mellgren and pie,' and Kreye and Kellogg.2 MANY existing methods for the production of light metals involve the reduction of their respective metal halides in the presence of salt melts composed of alkali or alkaline earth chlorides. In such a solution phase, the light-metal halide may undergo stepwise reduction from a higher, to a lower valence, and finally to a zero valent state. In this connection, the disproportionation equilibrium is of great interest. In the case where the higher valence is three and the lower valence is two, the disproportionation equilibrium may be written as follows, 3 Me11 = 2 Me111 + Me [I] If this equilibrium occurs in a salt melt containing a large excess of alkali chlorides, a typical ionic melt is obtained. It is then possible to formulate the cation equilibrium: 2 Me+h' + Me = 3 Me++ [II] Reaction [11] is analogous to a cation exchange reaction. It has been shown thermodynamically that the equilibrium constant for such a reaction in 2

Jan 1, 1960

By R. Costantini

The author discusses the promising future of the use of pipelines for transportation of ore slurries over long distances, citing existing installations. Various criteria and factors affecting the use and size of pipelines are considered. Among the factors influencing the use of pipelines are particle size, specific gravity, abrasiveness, minimum velocities, and pumping considerations. Long-distance transportation of solids by hydraulic pipelines holds the promise of great economic benefits. Today within the confines of most mineral processing plants, the moving of solids about in slurry form by pipeline is commonplace, since the method offers great advantages when conditions are suitable. Yet, this method is surprisingly slow in being adopted on a broad scale for transportation of solids over long distances (arbitrarily the term will be applied to one over five miles long). This is especially surprising in view of the successful realization in this country within the last five years of two daring ventures in long-distance solids pipelines. A 72-mile long, 6-in. diam pipeline of the American Gilsonite Co. has been satisfactorily transporting 700 tpd of gilsonite from the mine at Bonanza, Utah, to the processing plant at Grand Junction, Colo., since April 1957. The 108-mile long 10-in. diam pipeline of the Pittsburgh Consolidation Coal Co. has been transporting about 4000 tpd of finely crushed coal from the mine at Cadiz, Ohio, to the Eastlake power plant of the Cleveland Electric Illuminating Co. on Lake Erie since January 1958. However, besides two projects in the operations of The Anaconda Co. there have been hardly any other significant solids pipeline developments in the minerals industry during the last three years. The two projects are the 14-mile long, 6-in. diam copper concentrate gravity pipeline at Anaconda's El Salvador project in Chile which has been transporting about 800 tpd since January 1959. The second is a 16-in. diam tailings pipeline at the Anaconda Reduction Works, Anaconda, Mont., designed to transport about 20,000 tpd of deslimed flotation tailings for dam building. This pipeline, which is currently undergoing tryout tests and which will be about seven miles in length, will have a maximum of three 20-in. rubber-lined centrifugal pumps in series at the starting point, each developing a maximum of 100 ft of head, to supplement gravity. It is the writer's opinion that the major reason for the hesitation in considering pipeline operations is confusion due to an inadequate understanding of the basic physical principles affecting the slurry flow process by many engineers in the industry. This in turn begets an attitude of fear and trepidation instead of confidence on the part of many management executives, which leads to a minimizing of the advantages and exaggeration of difficulties when considering the possibility of a long-distance solids pipeline. The promotion of better understanding and consequently the promotion of greater confidence in the potentials of long-distance solids pipelines when conditions are suitable is thus the main purpose of this article. To this end, after considering several examples of the possibilities for solids pipelines in the minerals field, the relative significance of the major factors affecting pulp flow, and some major aspects of slurry pumping will be discussed on a general qualitative level. Then a brief outline of the semi-empirical quantitative methods developed to date for estimating slurry flow behavior will be presented. SOME POSSIBILITIES To give an idea of the magnitude of the possible economic benefits, it should be interesting to mention briefly some of the projects currently under consideration and to suggest some likely future possibilities. At Anaconda's El Salvador Project in Chile (Fig. 1) it is eventually planned to extend the existing 14-mile pipeline by another 60 miles to bring the copper concentrates down to the coast of the Pacific Ocean. Preliminary tests indicate that the projected 6-in. pipeline will be able to transport approximately 2000 tpd of concentrates at a pulp density of 40 to

Jan 1, 1961

By F. D. Richardson

STAFF: Editor, Gerhard Derge Carnegie lnstitute of Technology Schenley Park Pittsburgh, Pa. 15213 Editorial Assistant, M. A. Redmerski Production Editor, Otto T. Johnson THE METALLURGICAL SOCIETY: Jack H. Scoff, President; Richard C. Cole, Past-President; Harold 0. Emerick, President-Elect; Ralph L. Hennebach, Treasurer; Robert W. Shearman, Secretary; Donald A. Parks, Assistant Secretary; Leslie S. Wilcoxson, Assistant Secretary. PUBLICATIONS COMMITTEE OF THE METALLURGICAL SOCIETY: R. E. Lund, Chairman; T. E. Dancy, H. O. Emerick, P. R. Gouwens, R. E. Grace, J. H. Jackson, H. H. Johnson, A. E. Lee, Jr., R. R. Nosh, R. D. Pehlke, and Paul Queneau. Review and selection of manuscripts is under the supervision of the following Publications Committees: Extroctive Metallurgy Division: R. E. Grace, Choirmon; G. M. Bell, D. W. Bridges, J. M. Cigon, G. W. Heoly, T. A. Henrie, R. D. (Holli-doy, C. E. O'Neill, C. S. Somis, A. W. Schlech-ten, and Charles Shull. Iron and Steel Division: R. D. Pehlke, Choirmon; T. P. Floridis, Arnulf Muon, G. R. St. Pierre, E. T. Turkdogan, L. H.Von Vlock, and J. M. Uys. lnstitute of Metals Division: H. H. Johnson, Jr., Chairman; J. B. Clark, Vice Choirmon; M. R. Achter, G. F. Bolling. J. O. Brittoin, G. P. Conard, II, R. S. Davis, L. A. Girifolco, G. T. Hohn, J. P. Hirth, L. Himmel, G.T.horn, George Krauss, J. D. Livingston, R. D. Manning, H. M. Otte, S. V. Rodcliffe, R. E. Reed-Hill, H. C. Rogers, E. ScaIa, O. Sherby, M. T. Simnad, G. R. Speich, E. A. Steigerwald, R. A. Swolin, W. A. Tiller, W. R. Upthegrove, J. B. Wagner, Jr., Derek Wolton, H. W. Weart, W. W. Webb, and D. Published seven times yearly in February, March, April, June, August, October, and December by the American lnstitute of Mining, Metallurgical, and Petroleum Engineers, Inc., 345 East 47th Street New York, N. Y. 10017. Telephone PLAZA 2 -6800. Subscription $30 per year for non-AtME members m United States and North, South, and Central America; $32, foreign; $7.50 for AlME members Single copies, $6.00, single copier foreign, $6.50. The AiME is not responsible for any statement made or opinion expressed in its publications . . . Copyright 1964 by the American Institute of Mining, Metallurgical, and Petroleum Engineers, Inc. . . . Registered cable address, AiME New York Indexed in Engineering Index, Industrial Arts Index, and Chemical Abstracts. Second dost postaas poid ot New York, N. Y.,ond Ann Arbor, Mich. Volume 230, Number 6.

Jan 1, 1964

By L. F. Pease, J. H. Brophy

A phase diagram for the Ta-Zr system is presented. The system is of the minimum-melting point type with the 0-zirconium phase decomposing monotectoidally at 785°C and 95.5 at. pct Zr. The minimum solidus temperature is 1875°C and the temperature of the top of the monotectoid loop is 1775°C. Techniques employed included X-ray diffraction and fluorescmce, electron microprobe analyses, diffusion couples, metallography, and melting-point measurements. Errors due to interstitial solutes and in melting observations are particularly common in this system, and their occurrence is discussed. SEVERAL versions of the Ta-Zr phase diagram have been reported in the literature.lm7 Williams et al.' report a diagram of the minimum-melting point type with a monotectoid reaction at 800°C and 12 wt pct Ta. The minimum in the solidus occurs at 1820°C and 25 wt pct Ta, while the top of the monotectoid gap is located at 1780°C and 80 wt pct Ta. The experimental techniques employed were metallography, electrical resistance variation with temperature, dilatometry, X-ray diffraction, and direct observation of melting by the technique of Pirani and ~lterthum.' Experience in the Nb-Zr phase diagram has shown that small changes in the interstitial content can cause large shifts in the positions of the phase boundaries. Small amounts of inter -stitials can cause similar changes in the Ta-Zr system and may be responsible for the wide variations in the phase diagrams previously reported.'-' The authors15 have found that alloys containing 0.75 wt pct 0 and 1.0 wt pct Ni with tantalum contents from 19 to 85 at. pct often contain a lamellar or cellular precipitate after annealing above 1400°C. This precipitate is very similar to that reported by pollack,12 Ralls," and Donlevy17 for the Ni-Zr system. In the present investigation, a wider variety of experimental techniques and improved alloy purity were applied to the resolution of errors in diagrams for this system as they now appear in the literature. New results have been obtained in the areas of alloy homogeneity and purity. Errors in the common techniques of direct melting observation in binary alloys have been demonstrated. In the commercially important high-tantalum region, the more accurate metallographic method of solidus determination has been employed. EXPERIMENTAL PROCEDURE Nominal analyses of the materials employed are given in Table I. The zirconium was low hafnium reactor grade iodide crystal bar, and the tantalum was in the form of high-purity sheet. Powders were impossible to use because of gas content. Alloys were melted on a water-cooled copper hearth, with a thoriated tungsten-tipped nonconsumable electrode in 2/3 atm of Zr "gettered" argon. Alloys were

Jan 1, 1963