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By WILLIAM BOWIE

IN most human endeavors a knowledge of the terrain is essential to the effective carrying out of projects, but no line of work is more dependent on maps than theoretical and applied geology. Maps of a kind do exist for all of the area of the United States, but most of them are crude affairs and of little use in engineering, planning, and scientific research. Topographic mapping in the United States was initiated on a national scale by the U. S. Geological Survey and the organizations that were merged in its creation to make base maps for geologists. Their work could not be effectively done then and cannot be effectively done now without maps that accurately delineate the earth's surface. The distribution of the rock masses that contain valuable mineral bodies, or that by their intrusion brought them into existence, is the first step in a study of the mineral resources of the nation. This work requires three-dimensional maps, that is, topographic maps on which the land forms are shown by contours.

Jan 1, 1938

By F. J. Escandon V.

The Plomosas stratiform lead and zinc deposits are located in northeastern Chihuahua in a sequence of folded Paleozoic and Jurassic rocks. They consist mainly of channel or blanket-like bodies of ellipsoidal cross section restricted to a 60-in-thick shaly limestone and a 30-m-thick marble horizon of La Casita formation, with some reemplacement veins and shoots within the Plomosas formation. The mineralogy consists of iron-poor sphalerite, galena with a small silver content, and pyrite, in a gangue of calcite, barite, and minor quartz. The ore bodies present a lateral zoning with zinc-lead ratios increasing to the northwest. Vertical zoning shows marked changes in zinc-lead ratios and in the width and tenor of the ore which cannot be related to sedimentary or diagenetic features. Transgressive mineralization and some small fissure veins and breccia pipes also point to an epigenetic origin. Sulfur isotope analysis and geochemical data indicate hydrothermal solutions. Texture of the ores in the Mina Vieja marble is coarse, but in the Cuesta shale it is banded along bedding. The low iron and silver content of the sphalerite and galena and the weak hydrothermal alteration (only marbleization) of the wall rock suggest a telethermal stage of the solutions. There is no evidence of a possible intrusive rock mineralization.

Jan 1, 1976

By John Suman

DURING the past few years the taking of cores in drilling with rotary equipment has been perfected to a remarkable degree in the Gulf Coast fields of Texas and Louisiana. Taking of cores is becoming quite a common thing, especially in the newer fields, and drillers are becoming expert in this work. The writer has seen cores 5 to 8 ft. long taken with great ease in wells as deep as 4500 ft. Coring is doing much to remove the prejudice which so many petroleum engineers seem to have against .the use of rotary drilling equipment for exploratory work. Some operators .are now claiming that when used with a reasonable amount of coring the rotary system is even more satis-factory than cable tools for exploring in certain territory. A case has recently been pointed out in the South Electra field of North Texas, where producing oil sands, passed over by cable-tool drillers, are being brought in with rotary equipment. It seems that in this particular territory the sands are rather thin. Cable-tool drilling was carried on for the most part in a wet hole and the red mud encountered in drilling caved into the hole very badly, so that the cuttings showed mostly red mud and the driller, thinking that the sand did not amount to anything, carried his water string through the sand. The later .operators, drilling into the sand with rotary equipment and coring it, found that it was well worth testing.

Jan 10, 1922

By Jay N. Fairbanks, Richard G. Robinson

This paper discusses a computer program and related formulas for fire fighting responses by coal mine personnel. The computer will interpret the mine air analysis, print reports, and provide relevant graphs allowing quick and accurate responses to coal mine fires.

Jan 1, 1983

By C. W. Davis

THE name fuller's earth, which was derived from its early use in "fulling" or removing grease from woolen goods, is a term that is generally considered to designate mineral matter, containing hydrous aluminum silicates of the clay group, which has a high capacity for removing colors from oils, whether of animal, vegetable, or mineral origin. Fuller's earths are usually dried and may be "tempered" by heating or may be treated with water or reagents to improve their efficiency. For our purpose the term "acid-treated earths" will include those products from the partial decomposition of mineral water -by acid which are equal to or more efficient than an untreated fuller's earth from Quincy, Fla., when used in bleaching mineral oil by the "contact" process. In general, the contact process for treating oils consists of heating and agitating a mixture of oil and finely divided adsorbent, the latter being subsequently removed by filtration. The term "adsorbent" is used because, although there has been a great deal of controversy over the mechanism of removal of impurities from oils by mineral matter, there is no doubt that adsorption, which involves the surface of the solid, plays a major part.1 The properties that make fuller's earth useful in the treatment of petroleum products by "percolation" and in the purification of edible oils by the contact process have long been studied, but the comparatively recent adaptation of the contact process to the bleaching of petroleum products has made desirable the further investigation of fuller's earth and other, adsorbent earths.

Jan 1, 1929

By LUIS EAIYLNN SALAS

IF the ordinary wet method be attempted for silver-bullion containing tin, much trouble is experienced, varying with the amount of tin present. Even with a percentage as low as 0.05, the end-point is masked by a persistent turbidity, while with amounts ranging from 0.5 per cent. upward, the determination of the exact end-point is impossible, owing to the finely divided or colloidal metastannic acid resisting all efforts to cause it to settle, or to give a clear supernatant liquid. The object of the following experiments was to seek a remedy for these difficulties, and to find the conditions whereby the Gay Lussac method might be applied directly to these bullions. Material containing tin is met with frequently in bullion from Mexico or Bolivia; and tin is carried (sometimes in large quantities) in jewelers' sweeps. 1. A bullion was prepared containing Ag, 74; Cu, 25; and Sn, 1 per cent. A weighed amount was treated by the humid assay-method as if it were an ordinary bullion free from tin. Ten cc. of HNO3 (1.21) was added, and the bottle was heated until all traces of red fumes had been expelled. Before heating, the solutions were moderately turbid; and after heating, the turbidity greatly increased. One hundred cc. of normal NaCl solution was added and the bottle was shaken vigorously at intervals during 30 min. The turbidity persisted. The bottle was allowed to stand over

Mar 1, 1912

By Donald D. Smythe

This paper describes briefly the topography and geology of the region where the mica-bearing pegmatites are found and discusses prospecting, the quality of the mica, its preparation, and evaluation of the deposits. Muscovite mica occurs in a number of widely separated localities in Brazil, but production has come largely from deposits in the southeastern and eastern part of the State of Minas Gerais (Fig. I). There the deposits form a discontinuous zone, which starts at a point go km. north of the city of Rio de Janeiro and extends north for some 500 km., roughly parallel to the coast. A maximum width of 180 km. is reached along the Rio Doce. To the west in Minas Gerais, and extending east into the states of Espirito Santo and Rio de Janeiro, the mica zone proper is fringed by areas in which there are scattered occurrences of mica-bearing pegmatites. A few of these outlying deposits have produced commercial mica, but most of them are unimportant. To the southwest, in the State of Sao Paulo, there are a number of mines, which at one time produced a very considerable amount of sheet mica, largely as a byproduct of kaolin mining. These deposits, and a few others lying between them and the main productive areas to the northeast, appear to be the southwestern continuation of the strong Minas Gerais mica zone. In the vicinity of Conquista, just north of the Minas Gerais boundary in the State of Bahia, and still farther north, near Jacobina, there are several known mica deposits. Their location indicates that they may be the northern continuation of the main mica zone. The major part of Brazilian mica production has come from four areas within the mica zone proper; from north to south, Governador Valadares, Raul Soares, Espera Feliz, and Muriaé.. The first is go km. from north to south and reaches a maximum width of 180 km. The Raul Soares area extends 135 km. from northeast to southwest, and in places is 80 km. wide. The Espera Feliz area is 100 km. from north to south, and reaches a width of 35 km. The Muriai. area extends 150 km. from northeast to southwest and its width reaches 40 kilometers. Between the known productive areas, and in the areas directly to the southwest and to the north of them, little mica has been produced. These gaps, as well as certain irregularities in the outline of the mica zone itself, are to be ascribed either to lack of prospecting or to conditions preventing the discovery of mica, rather than to its nonexistence. Elsewhere in Brazil mica has been reported from eastern Goiaz, Ceará, Pernambuco, Rio Grande do Sul, Matto Grosso, and Amazonas. Production from these sources is negligible at present. Because of the inferior quality of the mica from the more accessible of these localities, and the operational difficulties occasioned by the remoteness of others, it is improbable that they will become important producers for some time to come.

Jan 1, 1948

By Donald D. Smythe

This paper describes briefly the topography and geology of the region where the mica-bearing pegmatites are found and discusses prospecting, the quality of the mica, its preparation, and evaluation of the deposits. Muscovite mica occurs in a number of widely separated localities in Brazil, but production has come largely from deposits in the southeastern and eastern part of the State of Minas Gerais (Fig. I). There the deposits form a discontinuous zone, which starts at a point go km. north of the city of Rio de Janeiro and extends north for some 500 km., roughly parallel to the coast. A maximum width of 180 km. is reached along the Rio Doce. To the west in Minas Gerais, and extending east into the states of Espirito Santo and Rio de Janeiro, the mica zone proper is fringed by areas in which there are scattered occurrences of mica-bearing pegmatites. A few of these outlying deposits have produced commercial mica, but most of them are unimportant. To the southwest, in the State of Sao Paulo, there are a number of mines, which at one time produced a very considerable amount of sheet mica, largely as a byproduct of kaolin mining. These deposits, and a few others lying between them and the main productive areas to the northeast, appear to be the southwestern continuation of the strong Minas Gerais mica zone. In the vicinity of Conquista, just north of the Minas Gerais boundary in the State of Bahia, and still farther north, near Jacobina, there are several known mica deposits. Their location indicates that they may be the northern continuation of the main mica zone. The major part of Brazilian mica production has come from four areas within the mica zone proper; from north to south, Governador Valadares, Raul Soares, Espera Feliz, and Muriaé.. The first is go km. from north to south and reaches a maximum width of 180 km. The Raul Soares area extends 135 km. from northeast to southwest, and in places is 80 km. wide. The Espera Feliz area is 100 km. from north to south, and reaches a width of 35 km. The Muriai. area extends 150 km. from northeast to southwest and its width reaches 40 kilometers. Between the known productive areas, and in the areas directly to the southwest and to the north of them, little mica has been produced. These gaps, as well as certain irregularities in the outline of the mica zone itself, are to be ascribed either to lack of prospecting or to conditions preventing the discovery of mica, rather than to its nonexistence. Elsewhere in Brazil mica has been reported from eastern Goiaz, Ceará, Pernambuco, Rio Grande do Sul, Matto Grosso, and Amazonas. Production from these sources is negligible at present. Because of the inferior quality of the mica from the more accessible of these localities, and the operational difficulties occasioned by the remoteness of others, it is improbable that they will become important producers for some time to come.

Jan 1, 1948

By Ellsworth Daggett

THE system of pitwork used with the Cornish pumping engine, and which, for want of a better name, we may call the Cornish system of pitwork, consists essentially of a series of plunger-pumps, situated one below the other, in a shaft or incline, the plungers being operated by a rod called the pitman or pump-rod, which must, therefore, extend from the motor at the surface to the lowest pump. The subject will be best understood by reference to Fig. 1, in which k may be taken as typical of the ordinary plunger-pump, in which S is the suction pipe, u, the lower valve situated in the H piece T; v, the upper valve situated in the valve-box O; I, the mounting-pipe or column through which the water is carried to the surface; L, the plunger-barrel, and P, the plunger working through the stuffing-box, and actuated by the branch rod r, which is attached to the main pump-rod, R. The action of the pump is as follows : On the ascent of the plunger, acting now by suction, the water flows from the reservoir through the valve u, into the barrel, L. On the descent of the plunger, the water is forced up through the valve, v, which acts merely as a check valve, into the pipe, I, through which it is, at each successive down-stroke of the plunger, forced upward until it reaches the next reservoir, from which it is taken by another similar pump, and so on until it reaches the surface or drain-tunnel. The pump is obviously only single-acting, i. e., it acts only during one-half of its entire stroke. The weight of water raised during the up-stroke of the plunger is equal to the weight of a column of water whose base is the area of the plunger and whose height is the mean distance between the plunger-face and the surface of water in the lower reservoir, a distance not usually exceeding 12 or 15 feet, and which obviously cannot under the most favorable circumstances, exceed 25 or 30 feet. The water forced up during the down-stroke is equal to the weight of a column of water whose base equals the area of the plunger and whose height equals the length of the mounting column above the mean position of the plunger-face, say from 150 to 300 feet. Almost all of the useful work, therefore, is done on the de-

Jan 1, 1879

By P. V. Brough, K. B. Gillaspie

DECISION to build a mill at the Bayard property was made in May 1942. Western-Knapp Engineering Co., of San Francisco, assisted by engineers of U. S. Smelting, handled the design and construction. Much of the milling equipment was moved from the Company's mill at Goldroad, Ariz. Wartime restrictions necessitated wood construction and paper sheathing except for structures adjacent to the Bullfrog shaft. Construction started in September 1942 and milling in March 1943. Bayard ores are processed in a single-ection mill. About half of the ore treated during the past year was hoisted through the Bullfrog shaft and the rest was trucked from other shafts. Coarse storage includes four bins, two of 120 tons each for Bullfrog ores and two of 85 to 120 tons each, served by a truck ramp. The low capacity figure refers to

Jan 1, 1948

By Gordon E. Agar, David M. Hopstock

This paper describes the procedures and results of a series of experiments conducted to determine the depressing effect of sodium, calcium and magnesium ions on the amine flotation of quartz. It also presents an analysis of the experimental results by the electrical double layer theory. The flotation of quartz with primary amines has been practiced on a large scale in the phosphate industry for many years. Some glass sand —and recently iron ore — has also been treated by this flotation technique. These applications have been highly successful and demonstrate that a complete mastery of all the details of an operation is not needed to achieve an economic success. There are times, though, when it becomes important to recognize, both qualitatively and quantitatively, the effects of some previously ignored variables. The effects of cations on the amine flotation process, particularly those ions that contribute to water hardness and abound in sea water, are a case in point. In conjunction with the development of a cationic flotation reagent for separating quartz from apatite, it became necessary to quantify the influence of calcium and magnesium on the separation. In order to strengthen and broaden current understanding of the flotation process, the results were interpreted by means of the electrical double layer theory. THEORETICAL BACKGROUND Assume that, given the same equipment, procedure, and time, the recovery of quartz by amine flotation is a function of only the adsorption density of aminium ions in the Stern layer, i.e., that for any given adsorption density there exists only one recovery percentage. By the Stern-Grahame treatment of the electrical double layer,'-' for any ionic species in a solution in equilibrium with quartz,

Jan 1, 1969

This consolidated index covers all publications of the Institute for the years 1926 through 1935. The following list indicates subjects of volumes and gives numbers or abbreviations used to designate them. TRANSACTIONS VOLUME *G26. Petroleum Development and Technology in 1925 (Published in 1926). *G26. Petroleum Development and Technology in 1926. *E27. Institute of Metals Proceedings. 73. Nonferrous Metallurgy, Milling and Concentration, Nonmetallic Minerals, Institute of Metals and Iron and Steel. [ ]

Jan 1, 1936

By T. Koulomzine

The theory of the Askania magnetometer, as well as a complete discussion of all factors influencing magnetometer readings, is very ably described by J. Wallace Joyce. We will assume that the reader is thoroughly familiar with this theory and we will use whenever possible the same notations for the physical values involved in the theory. On the other hand, we believe that the principal formulas of the magnetometer can be deduced much more easily by the use of differential calculus than by the methods employed by Joyce. Consequently, we are presenting herewith a resume of the theory of the vertical magnetometer in order to determine the correct formula of the temperature coefficient which we propose to compensate.

Jan 1, 1949

By Charles Albert Ashburner

The coal-fields of the United States have been variously classified as to their geographical positions. In 1887 I proposed slight changes to the classification generally used, for more convenient description of our coal-fields in my report on the statistical history of coal in the States during 1886 for the United States Geological Survey. This new classification seems to meet all practical requirements and has been generally adopted. The coal-areas are grouped in two divisions—the anthracite division and the bituminous division. The anthracite division, in a commercial sense, may be said to include the anthracite districts of Pennsylvania alone, although small amounts of anthracite are mined in Colorado and have been

Jan 1, 1890

By C. W. Davis

THE name fuller's earth, which was derived from its early use in "fulling" or removing grease from woolen goods, is a term that is generally considered to designate mineral matter, containing hydrous aluminum silicates of the clay group, which has a high capacity for removing colors from oils, whether of animal, vegetable, or mineral origin. Fuller's earths are usually dried and may be "tempered" by heating or may be treated with water or reagents to improve their efficiency. For our purpose the term "acid-treated earths" will include those products from the partial decomposition of mineral water by acid which are equal to or more efficient than an untreated fuller's earth from Quincy, Fla., when used in bleaching mineral oil by the "contact" process. In general, the contact process for treating oils consists of heating and agitating a mixture of oil and finely divided adsorbent, the latter being subsequently removed by filtration. The term "adsorbent" is used because, although there has been a great deal of controversy over the mechanism of removal of impurities from oils by mineral matter, there is no doubt that adsorption, which involves the surface of the solid, plays a major part.1 The properties that make fuller's earth useful in the treatment of petroleum products by "percolation" and in the purification of edible oils by the contact process have long been studied, but the comparatively recent adaptation of the contact process to the bleaching of petroleum products has made desirable the further investigation of fuller's earth and other adsorbent earths.

Jan 1, 1929

By W. M. Albrecht, W. D. Klopp, R. I. Jaffee, B. G. Koehl

Kinetic studies were made of the reactions of tantalum with oxygen, nitrogen, and air at 400o to 1500°C. The tantalum-oxygen reaction is linear from 500° to 1250°C. The tantalum-nitrogen reaction follows a cubic rate law at 400° to 700°C and a parabolic rate law at 800" to 1475°C. The reaction behavior in air is initially parabolic followed by a transition to linear behavior. In the search for high-temperature materials, considerable interest is being shown in the refractory metal, tantalum. It is the third highest melting metal with a melting point of 2996°C. Also, tantalum has excellent ductility, making it one of the most workable refractory metals. In considering high-temperature applications of tantalum, the oxidation kinetics of the metal must be known. Such information also serves as a basis for the development of corrosion resistant tantalum-base alloys. Therefore, this study was made to investigate the reaction of tantalum with air, nitrogen, and oxygen. LITERATURE Several oxides of tantalum have been reported. The pentoxide, Taz05, is the only oxide of tantalum whose identity has been established. A high-temperature modification, aTa2Os, has been reported by several investigators.1-4 A low-temperature phase, ßTa2O5, undergoes an allotropic transformation at 1320o to 1350oC. 5-8 Four other oxides of tantalum have been reported. The oxides TaO2, TaO, and Ta4O have been reported by schonberg.9 A suboxide Ta2O, was observed by Wasilewski 6. However, the presence of oxides lower than Ta2O5 is questioned by Lagergren and Magneli.7 In oxidation studies, vermilyeal0 and Peterson, et al.,12 reported one possible phase intermediate between Ta and Ta2O5. Only Ta2O5 was formed in the tantalum air reaction, as reported by Michae1.l3 Several studies have been made on the kinetics of the tantalum-oxygen reaction. vermilyeal4 investigated the range 50° to 300°C and found that the rate of growth of a thin adherent oxide film could be described by the Cabrera-Mott theory. Gulbransen and Andrew15,18 studied the reaction kinetics of tantalum in oxygen pressure of 1/10 atm at 250° to 450°C. At all temperatures the reaction followed the parabolic rate law for periods up to two hours. The oxidation behavior in the range 500" to 1000°C was found to be linear at oxygen pressures of 0.2 to 600 psi according to Peterson. et al.l1 At very low pressures (1 x 10-3 to 2 X lo-' mm of Hg) Gebhardt and seghezzi17 reported linear oxidation at 800° to 1500°C. The reaction of tantalum with air is similar to the reaction with oxygen. Studies have been made by Waber, et a1.,12 and Michae1.l3 Two nitrides of tantalum, TaN and Ta2N are known. Their structures have been determined by Brauer and Zapp 18,19 The tantalum-nitrogen reaction kinetics have been investigated by Gulbransen and Andrews. 15, 16 The reaction follows the parabolic rate law at 500° to 850°C at a nitrogen pressure of 1/10 ,atm. At the same temperature, the tantalum-nitrogen reaction is much slower than the tantalum-oxygen reaction. EXPERIMENTAL TECHNIQUES Material— The material used in this study was high-purity, electron-beam-melted tantalum obtained from the Temescal Metallurgical Corp. The hardness of the as received ingot was 76 Vhn. The analysis of the material is given in Table I. Methods—Cylindrical specimens of tantalum approximately 0.9 cm in diam and 0.5 cm in length

Jan 1, 1962

By JOHN JERMAIN

In my opinion, the explanation of the fuel-requirements involving the conception of heat available and necessary above a critical temperature, as advanced by Johnson 1 and elaborated by Howe, Raymond and others,2 affords a theoretically correct basis for such an accounting. It is the purpose of this paper to set forth a first crude attempt to construct a formula which shall show quantitatively the relation between the various factors affecting fuel-economy, and afford a means of comparing the enormous amount of data on the fuel-consumption of various blast-furnaces, at various times and under various conditions of operation. I have also applied this formula to a large number. of individual cases, and have, by its means, compared the furnace-practice of several important iron-making districts. II. DERIVATION OF FORMULA FOR FUEL-REQUIREMENTS. The general expression for the fuel-requirements of the blast-furnace, which I believe to be theoretically correct as to form, is as follows Carbon per ton of iron = Heat per ton of iron necessary in hearth above Tc./Heat per pound of carbon available in hearth above Tc. XFactor of rate of driving. +Carbon dissolved by CO2 of flux. +Carbon dissolved incidental to reduction of ore. + Carbon dissolved in pig-iron. (NOTE.-Tc = critical temperature.) Since, according to Johnson's theory, fuel-economy is usually limited by heat available and necessary in the hearth, rather than by the total heat supplied and necessary, we may write Carbon needed in hearth = Hn/Ha in which Hn is the heat per ton of iron necessary in the hearth above some critical temperature, and Ha is the heat per pound of carbon available in the hearth above this same critical tem¬perature. 1 Trans., xxxvi., 454 (1906). 2 Trans, xxxvi., 792 to 798 (1906) ; Trans, xxxvii., 216 to 237 (1907).

May 1, 1911

By J. M. GLEDHILL

(Washington Meeting, May, 1905.) A Discussion of Mr. J. M. Gledhill's paper, read by title at the Lake Superior meeting, but presented first at the New Yolk meeting of the Iron and Steel Institute (October, 1904), and here published under a mutual agreement. Between the two Institutes. Discussion. MR. E: WINDSOR RICHARDS, Past-President, said that at a recent meeting of the Institution of Mechanical Engineers a paper was read on tool steel, and he called the attention of the members to the high-speed tool steel at the Bethlehem Works. They would have the pleasure of seeing those wonderful works and would see 60, 70, 80 and 100 tons oil lathe with half-a-dozen of these high-speed tools running. PROP. H. M. HOWE (Columbia University) said that they all looked upon these high-speed tool steels as of very great importance, particularly to the machine shop. One point occurred to hire : Had it really been shown that Swedish steel is necessary, or better than equally pure steel that is not Swedish; and is cemented steel really necessary, and is there any advantage in using that, rather than equally pure open-hearth steel'! It might be well if the author could indicate the kind of evidence on which lie bases his assertion that it is necessary to have cemented Swedish steel. Many were hoping for the development of high-speed steels from elements which exist in great quantities, such as silicon, manganese and chromium, rather than from rarer metals like molybdenum, vanadium and tungsten, the supply of which is likely to be soon exhausted. If the high-cutting speed was to last more than a generation, it. seemed to him that they would have to draw upon the common ele¬ments and not upon the rare ones. MR. Tom WESTGARTH (Middlesbrough) said he fully appreci¬ated what had been said about the advantages of using high-speed steel, because great benefit had been derived from the

Mar 1, 1905

By G. R. Speich, L. Zwell, H. A. Wriedt

HORNBOGEN1 has recently shown that it is possible to measure the degree of segregation accompanying cellular precipitation in ferritic Fe-Zn alloys by measuring the lattice parameter of the ferrite phase within the cell. In extending this work to study a wider range of composition and to evaluate the free-energy change accompanying the growth of the cells, the lattice parameter and the boundary of the a! phase in Fe-Zn alloys were redetermined to check the earlier work of Schramm.2 This appeared to be necessary since the Fe-Zn diagram has been drastically revised since the work of Schramm. Stadelmaier and Bridgers3 have recently shown that, contrary to prior belief: the y iron field is closed and the a phase boundary extends to an a + T + L peritectic at 782°C where peritectic a contains 42 at, pet Zn. The phase T in equilibrium with the a solid solution has a composition near Fe3Zn10 and a cubic 081 type structure.' The alloys were prepared by two different methods. In the first method carbonyl iron powder (400 mesh, 99.8 pet pure) and high-purity zinc powder (200 mesh, 99.99 pet pure) were mixed in a ball mill and then pressed in a die at 40,000 psi pressure to make compacts with a diameter of 5/8 in. and a thickness of l/4 in. These were sealed in evacuated quartz capsules, gradually heated to 1100°C over a period of 1 week (3 days at 600°C) 3 days at 800°C, 1 day at (1100°C), and then quenched in iced brine. For the alloys containing 23.4 and 30.1 at. pet Zn, the final homogenization anneals were performed at 1000" and 850°C) respectively, to prevent melting. In the second method, alloys were prepared by saturating high-purity iron millings (0.001 in. thick, 99.9 pet pure) in zinc vapor. For each alloy the impregnation was conducted at a fixed vapor pressure of zinc and a fixed temperature between 750' and 800°C. When saturated, the millings were quenched in water. The compositions of the alloys prepared by both methods are shown in Table I. The lattice parameters of the ferritic solid solutions were determined by comparing the 26 values of their 310, peaks (using Co Ka) or of their 211 , peaks (using Cr Ka) with those of corresponding peaks for high-purity a iron. The 20 values were measured at room temperature with an X-ray dif-fractometer (G.E.-XRD5). By using a fiducial value of 2.8664Å for the lattice parameter of pure a iron at 25oC,5 the lattice parameters of the zinc-bearing

Jan 1, 1964

By Harry C. Gatos, Frank J. Bachner, Mario D. Banus

The portion of the Nb-Sn phase diagram between 75 and 79 at. pct Nb at temperatures near the liquidus has been investigated by melting alloys of known composition and examining the microstmc-tzlres resulting when these melts were quenched. The Nb-Sn samples were contained in magnesia sleeves, and were mounted in a high-pressure apparatus. It was shown that Nb3Sn me1ts by a peri-tectic decomposition and that the composition of the compound Nb3Sn at the peritectic horizontal lies between 77 and 78 at. pct Nb. Analysis of the phases present in the samples was accomplished by anodic staining techniques and an electron-microbeam analyzer. DURING the past several years a great deal of work has been devoted to the Nb-Sn system, and the bulk of this work has been primarily concerned with the intermetallic phase Nb3Sn. However, the melting characteristics of Nb3Sn have not been investigated because of the difficulty in maintaining known compositions due to tin losses by vaporization, and the added difficulty of containing Nb-Sn alloys without sample-container reaction at the high temperatures involved. This paper reports on the development of a technique for containing Nb-Sn alloys under pressure high enough to prevent tin losses at temperatures in excess of the liquidus. Using this technique, melts of known composition were made and a phase diagram near the liquidus is proposed based on the microstructures resulting when these melts were quenched. EXPERIMENTAL The Nb-Sn alloys weighing 0.7 g each were prepared in the form of cylinders. Niobium powder, -200, +325 mesh, and tin shavings with a minute amount of tin powder for a binder were mixed in the desired proportions and cold-pressed at 50,000 psi in a 0.150-in. die. This cylinder was then enclosed as shown in Fig. 1, and the entire arrangement mounted in a 2.6-in. pyrophyllite tetrahedron.' The desired temperatures (-2500°C) presented several problems in high-pressure container materials. Boron nitride, the usual sample holder, was found to react with niobium to form the nitride. However, MgO cans and plugs machined from refractory rods did not melt nor react with the sample. Thick tantalum contact disks were used to carry the large currents (~450 amps) to the graphite heater, since tantalum did not melt and had enough strength to prevent extrusion of the sample. It was further observed that the graphite heater and tantalum disks could not be in direct contact with the pyrophyllite because it melts and decomposes at these temperatures to kyanite and coesite (SiO2),2 the former reacting with graphite and the latter with tantalum to form the silicide. The use of a MgO outer sleeve

Jan 1, 1965