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By Sam F. Carter

FOR some time melters and metallurgists have recognized the fact that steels may be made to identical compositions as ordinarily analyzed, but with considerable variations in physical properties. Good melting practice signifies a combination of furnace operations that will produce steel with consistently good physical properties after proper consideration of cost, production efficiency, and chemical control. In acid practice, these operations may be classified fundamentally as: (I) the oxidizing boil, (2) recarburization and deoxidation, (3) slag adjustment, and (4) final deoxidation. These operations affect the properties of the steel through variations in the minute quantities of several microscopic, submicroscopic, and dissolved constituents, which are out of reach of ordinary analyses but are very influential upon the crystallographic slippage and the molecular cohesion of the structure. One of these constituents is the FeO left in solution in the steel. Herty has shown that steels high in dissolved FeO have decreased ductility and impact and increased hardness and electrical resistance. There is also much evidence that FeO in solution affects carbon solubility and diffusion, and consequently abnormality and carburizing behavior.

Jan 1, 1947

Mr. Brown : .That part of the Standard Company's plant which has been added since the publication of Mr. Leggett's paper, and is described in mine, renders the single-phase, alternating system, which Mr. Hale has called " unelastic," much more elastic than it had been. The original plant at Bodie was substantially the same as the Telluride plant mentioned in his paper. The machines came from the same shops, and were practically the same; but while the Telluride Company has changed completely to a polyphase system, the Standard Company has retained its original plant, but has belted on a directcurrent generator at the receiving end, thereby converting the water-power into electricity, electricity into power, the power into electricity, and finally again electricity into power for use in the mines. This is a roundabout course, to be sure, but it shows that there are possibilities even in the out-of-date single-phase system. The only point perhaps, that deserves particular notice with respect to the hoist is the fact that the rheostat, or starting-resistance, was not built originally

Jan 1, 1897

By Howard Willey

MINING operations of the Charcas unit at present are limited to the Tiro General mine at Charcas, in the State of San Luis Potosi, Mexico. The Tiro General mine was first operated during the Spanish occupation of Mexico for rich silver ores in an oxidized zone along the outcrop of the principal vein. In depth the ore is a complex sulfide with widely varying proportions of sphalerite, argentiferous galena and chalcopyrite; and until recent years, it was economically impossible to carry on mining otherwise than irregularly in sections of the veins richest in galena and chalcopyrite. The advent of selective flotation brought the orebody as a whole within the field of economic interest, and a flotation mill of 650 metric tons daily capacity was constructed in the year 1925. The mining of partly worked-out sections of the mine, as well as the very heavy ground in most of the stopes opened in virgin ore, presented an unusually difficult problem. This -paper describes the so-called "filled top slice" stoping method finally adopted as the standard system.

Jan 1, 1930

By Robert H. Richards, Richard W. Lodge

A great deal of speculation, as well as actual experiment, has been devoted to ascertaining the changes in the materials (luring their descent in an iron blast-furnace, affecting (1) the chemical constitution, (2) the mechanical condition, and (3) the arrangement of the materials. With a view to throw some light upon the third question, we constructed a model and tried experiments which are here described. Our model is a vertical section of a furnace, with the lines of the Edgar Thomson furnace D of 1885 for the use of which we arc indebted to Mr. Gayley. The model is 40 inches high, and made to scale (1/2 inch equals 1 foot), and the horizontal section of the space through which the charge falls at any point in the descent is 11/2 in. x d, d being the diameter of the furnace at that place. We are unable to say just where the idea of making this model came from ; perhaps, partly from The Principles of the Manufacture of Iron, and Steel, 1884, I. Lowthian Bell, p. 124 ; partly, also, from

Jan 1, 1888

By G. M. Ritcey

Sulphuric acid leaching has been up to the present, the most popular of the leaching routes. Oxide ores are usually leached with sulphuric acid directly by dump leaching, as practiced at the Bagdad or Bluebird Mines in Arizona, or by vat leaching as done at Inspiration Mining in Arizona. Upgrading of the low-grade oxide ores by dump leaching followed by cementation of the copper from solution by scrap iron has been replaced by the leaching-solvent extraction-electrowinning route which results in a high purity product at the mill site at reduced production costs compared to previous practice. High-grade oxide ores, vat leached with H2SO4, can contain, for example, 25 g Cu/l and 25 g H2S04/,l, or higher concentrations of both, and are presently fed directly to electrorefining plants. Advantages of coupling solvent extraction-electrowinning with the low cost dump leaching instead of using cementation, are as follows (1): a) the production of high purity electrolytic copper rather than cement copper;

Jan 1, 1978

By Hsun Hu

C. G. Dunn (Geneva1 Electvic Reseavclz Labo,vatory)-Dr. Hu16 has obtained a number of rolling and annealing texture results that partly agree with those of Dunn17 and Dunn and Kohl8 for experiments of a similar nature. I would like to discuss some of the points of agreement as well as some of disagreement and then present some unpublished data as a contribution to the work on textures. Firstly, there is agreement on the components produced during a 70 pct cold-rolling reduction of a (110) [001 ] single crystal; there is agreement on the forma- tion of a (110) [001] recrystallization texture provided recrystallization occurs at 800°C or higher; and there is agreement on the formation of (120) [001] components provided recrystallization occurs below 600°C. There is some disagreement on the low-temperature recrystallization since I also obtained a substantial amount of a (110) [001] component while the author obtained only (120) [001] components. I also discussed the differences between low- and high-temperature recrystallization (which included further annealing changes in the samples on long

Jan 1, 1962

By Richard D. Hagni

Mississippi Valley-type ore deposits contain significant quantities of minor elements, which are present partly in the form of separate mineral phases and partly in solid solution in the major sulfide phases for which these deposits are exploited. These elements, as separate phases, are: copper, mainly in chalcopyrite and enargite; cobalt and nickel, chiefly in thiospinels and bravoite; rare earth elements associated with certain fluorites; and native gold. Many economically important minor elements occur in solid solution in sphalerite, including silver, cadmium, iron, germanium, gallium, indium, thallium, cobalt, nickel, and mercury. Significant amounts of silver and antimony, and perhaps very small amounts of gold, are present in solid solution in galena. Chalcopyrite may contain small amounts of silver, molybdenum, bismuth, cadmium, cobalt, and nickel. Marcasite and pyrite may contain silver, thallium, cobalt, and nickel. Although some of the minor elements contained in the Mississippi Valley-type deposits are currently recovered at the smelters and refineries, many are lost in tailings, sludges, and slags; consequently, important quantities of these elements are potentially recoverable as non-conventional resources.

Jan 1, 1983

By G. A. Alers, J. H. Bechtold, R. W. Armstrong

The plastic flow of .molybdenum was studied in compression at temperatures below the ductile-to-brittle transition in tension. It was found that molybdenum is ductile in compression at all temperatures down to —196°C. The yield strength continues to increase with decreased test temperature below the tensile ductile-to-brittle transition temperature range. Difficulty was encountered in correlating the experimental data obtained with existing theories of plastic flow. THE body-centered-cubic metals as a group show a rapid and very large increase in yield strength with decreasing test temperature.' It is of fundamental importance to the understanding of the mechanism of plastic flow that this general characteristic be examined carefully. Unfortunately, brittle fracture in low-temperature tensile tests prohibits the measurement of flow properties at very low temperatures. By using compression tests, fracture can be suppressed and the plastic flow of the bcc metals can be studied far below their tensile ductile-to-brittle transition temperatures. Molybdenum was chosen for this experiment and plastic-flow data were obtained down to —196°C.

Jan 1, 1959

By Robert Glass Cleland

THE CONNECTING link between Phelps Dodge and the copper mines at Bisbee and Morenci was a Canadian-born mining engineer and metallurgist named James Douglas. Judged by almost any standard, Douglas was an extraordinary man. Like John Muir of the California red- woods, he had in his blood "the heather and bog juices of Scotland," and the rugged virtues of a singularly great race. His father, for whom he was named, was a graduate of Edinburgh University, a member of the Royal College of Surgeons in London, and a man of rash and adventurous spirit. Extremely catholic in his intellectual interests and attainments, he was unusually skilled in his profession, certain-sometimes to the point of disastrous stubbornness--of his own judgments and decisions, careless of life or fortune where duty or moral issues were involved, and always deeply moved by the sufferings and misfortunes of his fellow men. The career of the senior Douglas included a curious medley of novel and adventurous experiences-prolonged hunger and cold while acting as surgeon on a Greenland

Jan 1, 1952

By N. F. Neumann, A. W. Schlechten

Metal chlorides were formed by reacting metal oxides and calcium chloride; the effect of additions to the reaction mixture was studied. It was found that by use of proper additions, metal chlorides could be prepared from mixtures that were not reactive under ordinary conditions. ManY recent metallurgical developments involve the use of chlorine or chlorides as primary reagents; good examples are found in the production of ductile zirconium and titanium by reduction of their chlorides with magnesium. Various methods of preparing metal chlorides are used and many others have been proposed. Some chlorides are formed by the direct combination of a metal or alloy with chlorine. Other processes react chlorine and metallic oxides; carbon or other reducing agents are usually employed to reduce the metal oxides and so promote chlorination. Metallic chlorides have also been produced by the exchange of chlorine between metal oxides and a chloride, such as sodium chloride. This type of reaction was the basis for the old process of chloride roasting in which metal ores were roasted in the presence of salt. Soluble chlorides thus formed

Jan 1, 1959

By Robert Glass Cleland

FROM the time of its organization down to 1917, a period of more than eighty years, Phelps, Dodge & Co. was seldom involved in what could be called a major labor difficulty. Behind this remarkable record lay both a philosophy and its practical application. The philosophy was an attitude toward society called the Golden Rule. That philosophy had been a living principle in the lives of the founders of the company, Anson Phelps, Daniel James, and William E. Dodge. Their successors, William E. Dodge, Jr., and Daniel Willis James, accepted the same philosophy. Dr. James Douglas governed his life by it. All of these men and their families had given tangible expression to that conviction in benefactions of great magnitude and variety-churches, hospitals, educational institutions, libraries, missionary undertakings, and other organizations for human betterment, such as the Young Men's and Young Women's Christian Associations, and the development of model communities about their mills and factories. According to the best standards of their generation, they had sought to improve the condition of labor,

Jan 1, 1952

By G. H. Shefelbine

DISCOVERED during the time of the Spaniards, the Namiquipa silver-lead-zinc mines in Chihuahua, Mexico, remained idle until 1916, when mining claims were first denounced. About 1922 a Japanese company, the Santo Domingo Mining Co., was formed to mine the oxide silver ore. The company built a 75-tpd cyanide plant and mined in the area for a number of years. Because of an error in surveying in one of the company's mines situated in another district, mining was carried over into a claim owned by General Marcel Caraveo, at that time governor of Chihuahua. Santo Domingo Mining Co. lost the resulting lawsuit and consequently had no capital to continue operating at Namiquipa. Later, Ray Brown and Eugenio Caballero formed a company to operate the mine, shipping crude ore to the American Smelting and Refining Co. smelter at Avalos, Chihuahua. The cyanide plant was changed to flotation with a capacity of 75 tons per 24 hr. In 1936 the property was again closed owing to labor trouble, a drop in the price of silver, and increased water in the mine.

Jan 10, 1957

By S. F. Emmons

The first paper which appears in the published Transactions of our Institute is that read by our respected Secretary at its first meeting in Wilkes-Barre in May, 1871. It is entitled " The Geographical Distribution of Mining Districts in the United States," and presents a brief but masterly review of what was known of the distribution of our deposits of useful minerals, particularly the metals, not only from a geographical but from a geological stand-point. At the request of Dr. Raymond I agreed, somewhat hastily, perhaps, to write for this occasion a brief sketch of the geological distribution of the deposits of the useful metals in this country, in the light of the increased knowledge of the present day. In the time given no personal investigation was possible, and as it was therefore out of the question to attempt to make anything that could be considered an original contribution to the history of our ore-deposits, I have been obliged to limit myself to an examination of such pub-

Jan 1, 1894

By Albert Zima

ACCORDING to recently published statistics, it is predicted that as much oil must be produced during the next 16 years as has been produced during the past 75, in order to satisfy the high rate of consumption of petroleum products. During 1934, over 17,000 oil wells were completed in the United States, and it is expected that over 20,000 additional wells will be drilled during the current year. Were it not for the remarkable progress made during recent years in the improvement of drilling technique and in the development of equipment used in the production phase of the oil industry, it is doubtful whether sufficient oil could be produced to meet present requirements. A few years ago, wells seldom were deeper than 3500 to 4000 ft., owing to the limitations of the drilling methods and equipment employed. Today, however, through the application of scientific drilling methods and the adaptation of modern equipment and improved materials, many wells range from 6000 to 8000 ft, in depth, and a few recent completions exceed 10,000 feet.

Jan 1, 1935

By John E. Willson, Ben L. Seegmiller

A portable electronic instrument was designed and constructed to detect unknown stress magnitudes in rocks. The principle used to detect stress is based on the propagation velocity method. This method allows the stress in a rock subjected to a load of unknown magnitude to be determined, provided that the wave velocity-stress relationship for similar rock is known. This is accomplished by measuring the travel time of longitudinal mechanical waves passing between two points a set distance apart in a rock. The velocity of the wave is calculated and the stress determined from the wave velocity-stress relationship. If the sending and receiving transducer spacing is constant, a time vs. stress relationship rather than the velocity-stress relationship may be used. The method is nondestructive and tests can be made without drilling or otherwise disturbing the rocks. The first studies undertaken in the United States to determine stress in rocks using propagation velocity techniques were reported by Obert1,2 in 1939 and 1940. The Soviet Union first reported using propagation methods to study rock pressures in 1951.8 Success of the method led to the development of a pulse-type ultrasonic seismoscope4 in 1953. Using this instrument, Ivanov and Betaneli5,6 in 1963 succeeded in devising and testing under field conditions a method of investigating coal pillar stresses. In 1967 Osipova7 reported results of similar studies in the Nakhichevan salt mines. In France, Tincelin8 has used the propagation velocity method to study the stress distribution in iron ore pillars. Uhlmann9 has investigated stresses in salt and potash pillars in Germany, using velocity techniques. Determination of uniaxial stress by propagation velocity methods is limited to rocks which have readily detectable wave velocity-stress variations. The present stress detection instrument is restricted in application to rocks which have a velocity change under stress of at least 300 fps. Examples of rocks which meet this requirement are sandstones, coal, and possibly some limestones. Testing of this instrument was limited to a laboratory study and the results may or may not be indicative of what would be found in a field test. A program of field experiments to study the feasibility of using this instrument to determine mine pillar and tunnel stresses is in progress. Instrument Design The instrument has two main components: A probe and a control-display unit. The probe is a hand-held device to which two identical rodlike transducers are rigidly mounted. Coaxial cable connects the probe to the control-display unit which is mounted in an enclosed carrying case measuring 7 % x 9 x 13 in. The instrument is designed so it may be carried and operated by one man. Weight of the probe and enclosed control-display unit is approximately 20.1b. The probe consists of two transducers identical in construction. One transducer is used to convert electronic pulses to mechanical waves and transmit these waves into a rock. The other detects the transmitted waves in the rock and converts them back into electronic signals. The basic element in both transducers is a piezoelectric crystal. The crystal is a disk made of lead titanate zirconate and has a natural resonant frequency of 400 kHz ±1% in the thickness mode. A schematic of one of the two identical transducing elements is shown in [Fig. 1.] A spacing of 6 in. between sending and receiving transducers has been found to be most satisfactory. The control-display unit consists of a pulse generator and a 1-in. oscilloscope. Various electronic devices are used for the power supply, amplification, and calibration. The amplitude of the square wave from the pulse generator can be continuously varied between 0 and +20 vdc. Pulse width can be set at 1, 2, 3, or 4 µsec. The repetition rate of the pulse can have the following values: 50, 75, 100, 150, 200, 250, 300, 400, 500, 750, and 1000 Hz. The oscilloscope delay system allows the travel time of the longitudinal wave passing through a rock to be measured to an accuracy ±0.1 µsec in the range from 0 to 995 µsec. Fig. 2 is a schematic of the various electronic sections in the control-display unit. Laboratory Testing The first step in using the instrument is to develop a velocity-stress or a time-stress curve for the par-

Jan 1, 1972

By Arnulf Muan, R. W. Taylor

Activities of iron in Fe-Pt alloys have been dctermined by equilibrating mixtures of platinum metal and iron oxide at known oxygen Pressures in a thermobalance at 1300°C. Conzpositions and iron activities of the oxide phase at equilibrium are known from previous work, and compositions of the Fe-Pt alloy phase formed at equilibrium were detcvt?zined from the observed weight changes of the samples. The activity curve obtained shows a strow negative deviation from Raoult's law. THE present investigation was undertaken as part of a research program dealing with phase equilibrium relations existing among the oxides of iron and titanium at 1300°C. At low oxygen pressures of the gas phase in equilibrium with these oxides, the iron activity of the system is high, and considerable alloying of iron with the platinum used as a container material takes place. Thermodynamic data for Fe-Pt alloys at 1300°C are needed in order to evaluate quantitatively the extent of such reactions. Larson and chipmanlhave determined activities of iron in Fe-Pt alloys at 1550°C by equilibrating platinum metal with CaO-iron oxide-SiOzmelts in which the iron activities were known. Compositions of the resulting Fe-Pt alloys were determined by chemical analysis. Mundiath and Gerassimov2 have studied thermodynamic properties of Fe-Pt alloys by electromotive force measurements in the temperature range 550" to 1000°C. The experimental method used in the present investigation is a slight modification of that used by Grube and Ratsch3 in studies of NiCr-alloys. 1) EXPERIMENTAL METHOD 1) General. Mixtures of platinum metal and iron oxide were equilibrated at 1300°C in atmospheres of known oxygzn przssures, and the course of the reactions was followed by measuring the weight changes of the mixtures. The principles involved in the derivation of composition-activity relations from these measurements are illustrated by the composition triangle for the system Fe-FeZO3-Pt shown in Fig. 1. Take as an example a mixture of FeZO3 (hematite) and platinum such that the total composition is represented by point T. If this mixture is heated to 1300c in air (poz = 0.21 atm) and the oxygen pressure is then reduced gradually, the oxygen content of the oxide phase decreases and increasing amounts of iron enter the metal phase. As the oxide phase and the metal phase for all practical purposes are insoluble in each other, their compositions are represented by points moving toward Fe along the joins Fe-Fe,03 and Fe-Pt, respectively. The total composition of the mixture during this process also changes, but only with respect to oxygen content, because the vapor pressures of iron and platinum are negligible at 1300°C. Hence the change in total composition is described by a straight line (constant Fe/Pt ratio) radiating from the 0 apex of the composition triangle Fe-Pt-0, of which the triangle in Fig. 1 is a part. Only one such line ("oxygen reaction line", T-T",) is shown in Fig. 1. The total composition of the alloy-iron oxide mixture at any instant must, in addition, be located on the straight line (conjugation line) connecting the two points representing the compositions of the two coexisting phases. It therefore follows that the total composition of the mixture at any instant is represented by the point of intersection between the conjugation line and the oxygen reaction line. An example of the situation prevailing at a chosen oxygen pressure, po2, is shown in Fig. 1 by points a' (alloy composition), b' (oxide composition) and T' (total composition). Point b' is known from the work of Darken and Gurry,4 and point T' is experimentally determined by the observed weight change of the mixture (distance T-T). Hence, point a', the composition of the alloy, is determined from the above data as the intersection between the join Pt-Fe and the extension of the straight line bl-7'. The activity of iron in the alloy at equilibrium is identical to that of the iron oxide phase, if the same

Jan 1, 1962

By N. J. Grant, D. S. Bloom

N recent reports, Sully' and Beck and coworkers' I have advanced hypotheses concerning the formation of the phase. Both of these hypotheses are based on Pauling's theories of the electronic configuration of the elements of the first transition group. Sully considered that the number of electrons which can be absorbed in filling electron "holes" is the factor which determines whether or not the structure can form. Beck suggested that the presence of a certain concentration of electron "holes" is the controlling value. It can be shown that a similar criterion can be developed without making reference to Pauling's theories. Table I shows the elements of the first transition group and the incidence of the a structure in the binary systems of these elements according to the data presently available. Also appended is the number of electrons considered to exist in the 3d-4s levels of these elements. If the atomic percentages for the phase are listed as shown in Table 11, and if the number of electrons in the 3d-4s levels per atom is calculated for the a boundary values, the results are as shown in the last column. It can be seen that the numerical values are all in the vicinity of 7 electrons per atom. This is true also for the ternary Cr-Mo-Ni IT phase, which occurs in a system in which none of the binary compositions are known to develop the phase. In the Fe-Mo binary, the high temperature a phase, which occurs at a composition of 50 atomic pct of each element, also yields a ,;1 e of 7 electrons per atom. From inspection of Tables I and 11, it develops that any series of sequential numbers which is assigned to the elements under consideration will result in the numbers pertaining to a compositions grouping themselves around one specific number. It does not follow, however, that this random number necessarily has physical significance. Such a point has already been discussed by Hume-Rothery." One interesting point develops from this study, however, and that is the position of manganese with reference to the other elements and to the phase. In the system used here, the formation of phase is associated approximately with the value of 7 electrons per atom, which is also the number of electrons per atom that manganese has. Manganese, it will be recalled, exists in three different crystal forms, none of which are the usual, simpler metallic forms; on the other hand, elements just to the left of manganese (in Table I) generally have lower coordination-number structures (body-centered cubic) than do elements to the right of manganese (face-centered cubic). The contribution to a complex crystal structure by the interalloying of elements from opposite sides of manganese is significant in that the a phase is formed in binary systems including one element from each side of manganese, with manganese capable of participating with both sides. It is indeed an interesting coincidence that manganese, with 7 electrons per atom, solidifies in complex crystal forms, and that when alloys of the transition elements are made which have seven 3d-4s electrons per atom, they, too, tend to assume a complex crystal form. From the above, it might be deduced that the study of the a phase might be advanced by a critical examination of the element manganese and how its structure is affected by small additions of elements which change the 3d-4s electrons per atom number. The role of atom size would also be of interest in formation. References ' A. H. Sully: The Sigma Phase in Binary Alloys of the Transition Elements. Journal Inst. Metals (1951) 80, Part 4, p. 173. 2 S. Rideout, W. D. Manly, E. L. Kamen, B. S. Lement, and P. A. Beck: Intermediate Phases in Ternary Alloy Systems of Transition Elements. Trans. AIME (1951) 191, p. 872; Journal of Metals (October 1951). "W. Hume-Rothery, H. M. Irving, and R. J. P. Williams: The Valencies of the Transition Elements in the Metallic State. Proc. Royal Soc. (September 1951) 208A. p. 431.

Jan 1, 1954

By D. S. Bloom

RECENTLY a report has been published on an investigation of the MO-RU system by E. Raub.' In this report it is stated that below approximately 1200°C the system consists of two terminal solid-solution phases and the intervening two-phase field; at 1200°C and above, an intermetallic compound labeled Mo,Ru, makes an appearance. Along with some other little known systems in which it was considered possible for a u phase to form, the Mo-Ru system had been under investigation in this laboratory. Since molybdenum and ruthenium have very high melting points and also since ruthenium is expensive, the investigation was confined to X-ray diffraction by sintered powder compacts. The compositions which were studied were (in atomic percentages): 75 Mo-25 Ru, 67 Mo-33 Ru, 50 Mo-50 Ru, and 25 Mo-75 Ru. All compacts were made from the pure powders, and no chemical analyses were attempted. Each compact weighed about 5 g. All annealing was done in evacuated Vycor capsules, and even though the capsules completely collapsed at 1250°C, they still admitted no air. The results of this investigation in general corroborate the work of Raub. Up to 1150°C the two terminal solutions and the intervening two-phase field were found, and at 1200°C and above an intermetallic compound was found. However, the composition limits of the compound were estimated to lie close to 70 atomic pct Mo rather than 62.5 atomic pct Mo as Raub had reported. At least the X-ray diffraction results indicated that the 75 atomic pct Mo specimen consisted of the molybdenum solid solution plus the compound, while the 67 atomic pct Mo specimen consisted of the ruthenium solid solution plus the compound and the equiatomic composition contained only very little of the compound. The most interesting observation, however, was that the diffraction pattern of the compound was similar to that of the well known u phases, except that unusually large lattice constants were indicated. The d-values, or interplanar spacings, of the diffraction lines (as produced by filtered copper KCX radiation) of the compound are given in Table I, as determined from specimens annealed at 1250°C for 9 hr and then quenched in water. Also shown are the lines of the Mn-Mo u phase as given by Decker, Waterstrat, and Kasper,' the lines of the Fe-Mo a as given by Goldschmidt," and the lines of the Mo-Ru phase multiplied by constants in order to make comparison with the Mn-Mo and Fe-Mo patterns easier. These results indicate that the compound in the Mo-Ru system is apparently isomorphous with the other o- compounds. The rather large lattice constants of the Mo-Ru a phase are acceptable in view of the comparatively large size of the constituent atoms. The data in Table I for the Mo-Ru compound check quite well with those given by Raub, not shown here, though there are some discrepancies between the two sets of data in the estimated intensities of a few lines. Although very little is known at present about this u phase, there are some things which may be pointed out, mainly in comparison with other better known u phases. Even though molybdenum and ruthenium are in the same columns in the Table of Elements as chromium and iron, respectively, the Mo-Ru u phase contains much more molybdenum than ruthenium, while the Cr-Fe u phase centers around or very nearly around the equiatomic composition; furthermore, the Mo-Ru u is stable only above approximately 1200°C, but the Cr-Fe u is stable only below about 825 °C. With respect to its being unstable below 1200°C, the Mo-Ru u is similar to the other binary molybdenum u phases in the Co-Mo and Fe-Mo systems. Similar to the latter two systems, the Mo-Ru u apparently exists over a rather narrow composition range, whereas the Cr-Fe u at lower temperatures is stable over a much wider composition range. The Mo-Ru u thus is closer to the other molybdenum u phases than to the Cr-Fe cr phase. The most striking feature of the Mo-Ru u phase, however, is the absence of any of the transition elements of the First Long Period.

Jan 1, 1956

By A. Phillips, D. H. Killpatrick, V. Kerlins

The tensile failure of two dispersion-strengthened Ni-20 Cr alloys was studied and compared to the fracture of a similar alloy with no dispersoid. The fracture characteristics were studied using electron fruc-tography and transmission electron microscopy. In all three cases, the mode of failure was found to be microvoid coalescence. The failure in the dispersion-strengthened alloys was found to have initiated at the particles. The size of the dimples in the fracto-graphs was found to be related to the spacing of the particles, but not to the total elongation before failure. The elongation before failure was found to be related only to the amount of dispersed phase. These results are compared to those predicted by a theoretical model of ductile failure. THE continually increasing strength requirements for creep-resistant materials capable of long life at service temperatures above 1600"F (875"C) have developed considerable interest in dispersion-strengthened nickel-base alloys. The high yield strength of these alloys results from the presence of a dispersion of fine particles of thoria which act to impede the normal motion of dislocations. Many theories have been presented to explain the role of the dispersion in the strengthening of these alloys. A good review of these theories is presented by Ansell.' The ultimate strength of such alloys is not only related to mechanisms raising the yield strength, but also to the amount of work-hardening which occurs. This work-hardening is determined by the work-hardening rate and the amount of plastic strain before failure. Since fracture limits the amount of plastic strain, a study was undertaken to gain a better understanding of the fracture mechanisms in these alloys. Electron fractography and transmission electron microscopy were used to study the fracture characteristics in two dispersion-strengthened alloys and one similar alloy containing no dispersoid. These results are related to the tensile properties of the dispersion-strengthened alloys at room temperature and at 2000°F (1095°C). The results are also related to a theory for ductile fracture. 1) PROCEDURE Standard tensile specimens were made from 0.020-in. (0.051-cm) sheets of three different Ni-Cr alloys. The alloys had nominal compositions of Ni-20Cr, Ni-20Cr-2Th0,, and Ni-2OCr-4Th0,. All alloys were supplied in an annealed condition. The specimens were fractured in tension at room temperature to determine the effect of the dispersed thoria on the fracture appearance. The tensile properties were determined from the average of a minimum of three ten- sile specimens for each condition tested. The fracture surface of all of the alloys was examined by electron microscopy using standard two-stage plastic-carbon replica techniques. Thin foils of the dispersion-strengthened alloys were used to investigate the size and spacings of the dispersion particles, and to investigate sections of the 2 pct thoria alloy taken from areas of the specimen adjacent to the fracture surface. The thin foils were mechanically ground to 0.010 in. (0.025 cm) and then chemically polished to approximately 0.001 in. (0.003 cm) in a solution of 29 g of ferric chloride and 10 ml hydrochloric acid in a liter of water. The polishing solution was maintained at 150"F (65°C) during the thinning operation. The final thinning of the foil was done electrolytically using a solution of 700 ml ethanol, 100 ml 2-butoxy eth-anol, 120 ml distilled water, and 78 ml perchloric acid (70 pct). The potential was maintained at 15 v and the bath temperature at -20°~ (-29°C) during the thinning operation. The final thickness of the foil was approximately l000A as determined from the width of twins boundaries observed in many of the foils. 2) RESULTS AND DISCUSSION The electron fractographs of the fracture surfaces of the alloys are shown in Figs. 1, 2, and 3. The normal interpretation of this type of fractographz is that, as a result of the difference between elastic and plastic properties of the matrix and the particles or other inhomogeneities in the alloy, microvoids are formed

Jan 1, 1969

By Arnulf Muan, D. P. Masse

PHASE relations in the system CoO-SiO2 have been determined as a basis for further investigations of thermodynamic properties of olivine solid solutions involving Co2SiO4 as a component. Previous data on the system CoO-SiO2 are incomplete or uncertain. Biltz and Lemke1 determined the melting point of cobalt orthosilicate as 1345°C , but Asanti and Kohlmeyer2 have later found a considerably higher temperature, 1420°C. The latter authors also studied melting relations of one mixture on the CO side and two mixtures on the SiO2 side of the orthosilicate composition and sketched a tentative phase diagram for a limited composition range of the system. However, no phase identification was carried out, and the authors left unanswered the question of the possible existence of a stable meta-silicate phase. Greig3 showed that a 90 wt pct SiO2-10 wt pct Co mixture at 1725°C consists of two immiscible liquid phases. The quenching technique was used in the present investigation. Mixtures of high-purity cobalt oxide ("Fisher Certified") and dehydrated silicic acid ("Baker Analyzed") were equilibrated in air atmosphere. The samples were then quenched to room temperature and the phases present were identified by microscopic and X-ray examination. The samples were kept in small envelopes made from thin (0.0004 in.) platinum foil. Thermodynamic data which have become available recently for Pt-Co alloys4 were used to check that the losses of COO from the oxide samples by alloying of cobalt with platinum in the present investigation were too small to change significantly the compositions of the oxide material during the equilibration. A vertical tube furnace with an 80 pct Pt 20 pct Rh resistance winding was used in runs up to 1510°C. Temperatures in these runs were measured with a Pt vs 90 pct Pt 10 pct Rh thermocouple calibrated against the melting point of diopside (CaMgSi2O6, 1391.5?C). The given temperatures as measured by this technique are estimated to be accurate to *5°C. Quench runs at temperatures above 1650°C were made with a modified Roberts and Morey5 strip furnace, using strip resistors composed of a 60 pct Pt-40 pct Rh alloy. Temperatures were measured with an optical pyrometer which was calibrated against the liquidus temperature of a mixture composed of 10 wt pct CaO, 90 wt pct SiO2 (1707°C). The temperatures measured with this technique have an estimated accuracy of +15°C. The results are shown graphically in Fig. 1. Only one intermediate phase, the orthosilicate Co2SiO4 with olivine-type structure, is stable in addition to the end members cobalt oxide and silica. The melting point of the orthosilicate was found to be 1415" ± 5°C. The metastilicate CoSiO3 is not stable at the temperatures of the present investigation. The two eutectic points in the system CoO-SiO2 where COO plus olivine, and olivine plus silica, coexist with liquid were found to be 72 wt pct COO and 1407°C and 63 wt pct COO and 1381°C, respectively. The melting point of cobalt oxide in air was taken as 1745?C, based on the previous data of Aukrust and Muan.6 Within limits of error (+ 5?C), identical eutectic temperatures to those determined in air were found when two representative mixtures were equilibrated at 1 atm O2 pressure and in an atmosphere of 84 vol pct CO2, 16 vol pct H2. This suggests that changes in oxidation state of cobalt in the condensed phases are not significant as far as their effect on the phase relations are concerned. This inference was substantiated by failure to detect7 any "excess oxygen" (i.e., oxygen in excess of that contained in Co2SiO4) in a sample of orthosilicate composition equilibrated in air 10°C above the liquidus temperature and subsequently quenched to room temperature. This work was carried out as part of a research program sponsored by the U.S. Atomic Energy Commission under Contract No. AT(30-1)-2781.

Jan 1, 1965