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By M. Gell, G. R. Leveran

The high- and low-cycle fatigue properties of the nickel-base superalloy, Mar-MBOO, in columnar-grained and single-crystal forms were determined at room temperature. It was found that the fatigue lives of these materials were greatly affected by the size of preexisting cracks in MC-type carbides contained in the micro structure. Most of the data falls on two curves given by: (zN)'/A€= K, where Nf is the number of cycles to failure, Af is the total strain range, and K is a function of carbide size. No difference was observed in the fatigue behavior of the columnar-grained and single-crystal materials for the same MC carbide size. Matrix slip and crack initiation occurred at precracked MC carbides and, to a lesser extent, at micropores. Fatigue crack propagation was mainly in the Stage I mode, i.e., on cry stallo graPhic slip planes. The Stage I fracture in these materials was unusual in that distinct features were observed on the fracture surfaces. In high-cycle fatigue, these features resembled those commonly observed on the cleavage fracture surfaces of bcc and hcp materials. Yet, in this study, the cracks propagated slowly in a cyclic manner. In low-cycle fatigue, the Stage I facets contained equiaxed dimples, similar to those observed on the tensile fracture surfaces of ductile materials. These observations indicate that both local normal and shear stresses are involved in these Stage I fractures. A model is proposed to explain these results based on the weakening of the cohesive energy of the active slip planes by reversed shear deformation and the fracture of the bonds across the weakened planes by the local normal stress. RECENT developments in casting technology have produced cast nickel-base superalloys in columnar -grained and single-crystal forms.1'2 The tensile and creep properties of the nickel-base superalloy, Mar-M200, cast in these forms have been shown to be superior to the corresponding properties of the conventionally cast polycrystalline material.lp2 This improvement in properties results, in part, from the elimination of grain boundaries in the single crystals and the alignment of the grain boundaries parallel to the stress axis in the columnar-grained castings. As part of a program to evaluate the fatigue properties of nickel-base superalloys cast in single-crystal and columnar-grained forms, a study has been made of the cyclic deformation and fracture of Mar-M2OO at room temperature. M. fiFl I .hininr Mpmher AIMF ic ^pninr Rocoarrh Accn^iata anH I) EXPERIMENTAL PROCEDURE The composition range of Mar-Ma00 in weight percent is: 8 to 10 Cr, 9 to 11 Co, 11.5 to 13.5 W, 0.75 to 1.25 Cb, 1.75 to 2.25 Ti, 4.75 to 5.25 Al, 0.01 to 0.02 B, 0.03 to 0.08 Zr, 0.07 to 0.12 C, bal. Ni. All of the castings met the above specifications. The castings were solutionized for 1 to 4 hr at 2250°F followed by aging at 1600°F for 32 hr which resulted in a 0.2 pct offset yield stress of 150,000 psi at room temperature. The microstructure of the material consisted of cuboidal, coherent particles of ordered, fcc Ni3(A1,Ti) (commonly designated y'), approximately 0.3 p on edge, distributed in an fcc y solid-solution matrix. MC carbides together with shrinkage and gas micropores were also distributed throughout the materials. The MC carbides and micropores were located preferentially in the interdendritic interstices, as well as in the grain boundaries in the columnar-grained castings. The (100) direction of all the single crystals and the common (100) axis of the grains in the columnar materials were aligned within about 5 deg of the specimen axis. Fatigue testing was carried out in the high-cycle (HCF) and low-cycle (LCF) fatigue regions, with the major difference being gross yielding of the specimen occurred during the first cycle in the LCF region. This division also corresponded with the more usual one in which the life of a specimen in LCF is less than lo4 cycles and that in HCF is greater than lo4 cycles. The designs of the high-cycle fatigue and low-cycle fatigue specimens are shown in Figs. l(a) and (c), respectively. The gage sections of both HCF and LCF specimens were electropolished prior to testing. The HCF specimens were tested in an MTS, closed-loop, hydraulic fatigue machine at 10 cps in air. The specimens were cycled between a tensile stress of 5000 psi and a maximum tensile stress which ranged from 35,000 to 125,000 psi, Fig. l(b). The LCF specimens were cycled under strain control from zero to a maximum tensile strain, Fig. l(d), in a Wiedemann-Baldwin testing machine. The experimental procedure has been described elsewhere.3'4 Both HCF and LCF tests were interrupted periodically in order to replicate the development of slip and cracking at the specimen surface. This was accomplished by placing plastic replicating tape around the gage section of the specimen while the specimen was in the mahine. The size of the MC carbides for all specimens was measured on a polished longitudinal section through the gage section after fatigue testing. The method of measurement consisted of carefully scanning the entire polished section in order to locate the largest MC carbides. Photographs were then taken of the six longest carbides oriented approximately normal to the

Jan 1, 1969

By E. B. Hughes, F. G. Norris

Oxidation is characteristic of all processes for making steel from pig iron. This thought has been aptly expressed by H. W. Graham13 in the recent Howe Memorial Lecture, "The process of steel-making consists of using iron oxide to reduce the carbon content of the pig iron to the desired level." Direct oxidation refers to the reaction that results from introducing oxygen either alone or mixed with other gases directly into the steel bath. In working a heat, oxygen in some form is added to the steel to remove the undesirable constituents as oxides. There are two general methods of supplying this oxygen to the open hearth bath. The method in which the oxygen is added as a compound such as Con or iron ore is designated an indirect method because the steel bath must first decompose the compound to attain oxygen in a usable form. The other method in which oxygen is added to the bath in the elemental or gaseous form, more or less diluted by other gases such as nitrogen, is a direct method because no decomposition is necessary before the oxygen reacts with iron to form FeO which is dissolved in the bath in a usable form. Bubble formation (at least of a macroscopic size) presents no problem in case of direct oxidation because the reacting agent (oxygen) is in the form of bubbles when entering the metal. Regardless of whether oxygen is intro- duced into the bath directly or indirectly, several reactions proceed concurrently. In the presence of the bath of molten iron, FeO is formed either by oxidation of iron by oxygen or reduction of oxides by iron. This FeO dissolved in the molten iron is the source of oxygen for the oxidation of manganese, carbon, silicon, and phosphorus if these are present. The oxidation of carbon from steel is the controlling steelmaking reaction. The introduction of oxygen into the bath, its reaction in the elimination of impurities, and its control by the use of de-oxidizing additions have been subjects of importance since steel was first made by the bessemer process. Direct oxidation is, in a sense, an application of the bessemer principle to the open hearth process. Graham13 states: "The use of oxygen or air jets introduced into the metal bath is essentially an effort to approach in the open hearth the turbulence, rapid interface reaction, and high production rate per hour that exists in the bessemer process." The general subject, "Oxygen in Steel-making," was given new life by the studies of Herty and associates starting about1925. The current interest in elemental oxygen is intimately related to the large scale production of oxygen developed during the war period. Some of the first applications were made during the early summer of 1946 at the Steel Co. of Canada using oxygen with the fuel. Such a use is of considerable interest and importance in contributing to faster heats but is not the subject of the present discussion which deals entirely with the introduction of elemental oxygen directly into the open hearth bath.

Jan 1, 1949

By E. B. Hughes, F. G. Norris

Oxidation is characteristic of all processes for making steel from pig iron. This thought has been aptly expressed by H. W. Graham13 in the recent Howe Memorial Lecture, "The process of steel-making consists of using iron oxide to reduce the carbon content of the pig iron to the desired level." Direct oxidation refers to the reaction that results from introducing oxygen either alone or mixed with other gases directly into the steel bath. In working a heat, oxygen in some form is added to the steel to remove the undesirable constituents as oxides. There are two general methods of supplying this oxygen to the open hearth bath. The method in which the oxygen is added as a compound such as Con or iron ore is designated an indirect method because the steel bath must first decompose the compound to attain oxygen in a usable form. The other method in which oxygen is added to the bath in the elemental or gaseous form, more or less diluted by other gases such as nitrogen, is a direct method because no decomposition is necessary before the oxygen reacts with iron to form FeO which is dissolved in the bath in a usable form. Bubble formation (at least of a macroscopic size) presents no problem in case of direct oxidation because the reacting agent (oxygen) is in the form of bubbles when entering the metal. Regardless of whether oxygen is intro- duced into the bath directly or indirectly, several reactions proceed concurrently. In the presence of the bath of molten iron, FeO is formed either by oxidation of iron by oxygen or reduction of oxides by iron. This FeO dissolved in the molten iron is the source of oxygen for the oxidation of manganese, carbon, silicon, and phosphorus if these are present. The oxidation of carbon from steel is the controlling steelmaking reaction. The introduction of oxygen into the bath, its reaction in the elimination of impurities, and its control by the use of de-oxidizing additions have been subjects of importance since steel was first made by the bessemer process. Direct oxidation is, in a sense, an application of the bessemer principle to the open hearth process. Graham13 states: "The use of oxygen or air jets introduced into the metal bath is essentially an effort to approach in the open hearth the turbulence, rapid interface reaction, and high production rate per hour that exists in the bessemer process." The general subject, "Oxygen in Steel-making," was given new life by the studies of Herty and associates starting about1925. The current interest in elemental oxygen is intimately related to the large scale production of oxygen developed during the war period. Some of the first applications were made during the early summer of 1946 at the Steel Co. of Canada using oxygen with the fuel. Such a use is of considerable interest and importance in contributing to faster heats but is not the subject of the present discussion which deals entirely with the introduction of elemental oxygen directly into the open hearth bath.

Jan 1, 1949

By ARTHUR S. DWIGH

Discussion of the paper of W. W. NORTON, presented at the Salt Lake meeting, August, 1914, and printed in Bulletin No. 92, August., 1914, pp. 1993 to 1999. ARTHUR S. DWIGHT, New York, N. Y.-Mr. Norton's chief argument is directed against the idea that the D. & L. sinter is any better material for the blast furnace than the H. & H. product. He supports this by citing two experimental furnace runs. Reducibility.-To discuss a furnace record like that quoted by Mr. Norton for the five days' run in August, 1912, is manifestly difficult for an outsider, but a possible explanation for the poor reduction on Furnace No. 5, smelting D. & L. sinter, may lie in the fact that both sets of furnaces carried the same fuel charges. Other things being equal, if 11 ½ per cent. coke was right for the furnaces smelting H. & H. product, it Was too much for the furnace smelting D. & L. product, as I shall endeavor to show later, and incipient overfire, accompanied by higher leads in slag and matte, was induced. It may sound like a paradox to say that excessive fuel sometimes produces poor reduction, but it is a sad fact. In certain plants where practically the entire charge to the blast furnaces receives a preliminary treatment by being sintered on the D. & L. machines the peculiarities of this problem have had to be very carefully studied, for serious metallurgical difficulties presented themselves when the change was first made to D. & L. sinter in large quantities. Some of these plants had blast pots before they had D. & L. machines, and many opportunities were afforded for comparative study of this very point. There is reason to believe that, clue to the long period of blowing and the higher temperatures developed in the pots from greater mass action, the iron in the H. & H. product is present chiefly as Fe203, perhaps in the form of ferrites, while in the D. & L. product the iron is present as FeO. The fuel charge in the blast furnace must be so proportioned as to exactly meet the chemical and thermic requirements of reduction and melting. If ally of these functions have been performed before the material enters the furnace, a corresponding allowance should be made or the fuel balance will be disturbed and bad work will result. One of the functions of the coke is to reduce enough metallic Fe for the matte requirements, leaving the remainder of the iron as FeO to go into the slag. In smelting almost any other material than D. & L. sinter the iron must-be reduced from the higher oxides, Fe203 or Fe304, to the protoxide, FeO, before a true comparative basis is reached. Experience has shown that with about one-half D. & L. sinter on the charge the coke should-be cut about 10 per cent. This theoretical benefit is borne out by the practical blast-furnace results on a large scale in numerous plants. In fact, wherever this very important factor is ignored the evil symptoms of excessive fuel will be indicated,

Jan 11, 1914

C. W. Kempton, Oro Blanco, Ariz.: In his interesting paper, Mr. Ingalls refers to reports of tin-deposits near Sain Alto, Zacatecas, Mexico. During 1891 I made some personal examinations of these deposits. They are, for the most part, located from 10 to 30 miles west of the town, in the Sierra del Fraile.

Jan 1, 1896

By H. K. Work, H. B. Emerick

IN the past year the steel industry underwent an abrupt conversion from a war tempo to a highly competitive peacetime schedule. It is still too early to gain a comprehensive picture as to which of the measures in production metallurgy, that made the war effort so successful, will remain in the postwar production of steel, but many of them undoubtedly will fill an important place after the war. Considerable speculation has developed regarding the disposition of the war-born production facilities of the steel industry. These include new open-hearth and electric furnaces, as well as vast numbers of auxiliary, supplementary, and balancing units that increased and speeded up production beyond the normal capacities of existing melting furnaces and finishing mills. Although these facilities were installed primarily to help meet war requirements, consideration was also given, in planning, to their possible peacetime use. The new equipment is generally modern and efficient, and it seems reasonable to suppose that strategically located units will gradually be absorbed by various steel companies to supplement their own facilities, or to replace in kind, obsolete and inefficient equipment now ready to be scrapped. Some, however,

Jan 1, 1946

By A. J. Mortlock

Cobalt and nickel have been diffused at tracer concentrations in gold at several temperatures in the range from approximately 700° to 950°C. The diffusion penetration profiles were determined by a serial sectioning technique in which the gold is first anodized and then the anodic layer is dissolved in acid. In this ulay sections as thin as 250A could be removed reproduci-bly. In all cases, the region close to the specimen surface was characterized by irregular behavior in the sense that the logarithm of concentration was not linear in the square of the penetration distance. In sotne cases, there zuas an indication of the operation of very slow dijfusion in this region, while in others the apparent diffusion coejj'icient was negative. Possible reasons for this anomalous behavior are briefly discussed. In recent years it has been found that the region close to the surface of a metal can sometimes exhibit anomalously slow diffusion characteristics relative to the interior of the metal. One of the best examples of this fact is the work of Styris and omizuka,' who showed that the apparent diffusion coefficient for zinc in the region withi: about 1 p of the free surface of copper was about ,,,, that at deeper penetrations. This result is particularly interesting, because it is free from the possibly complicating effects of low solubility of the diffusing tracer in the solvent metal. In the case of diffusion under conditions of low solubilitjr, interpretaticn of the results in terms of lattice diffusion is difficult because of the enhanced short-circuiting produced by segregation to dislocations.2'3 Measurements by Duhl et 1. suggest that cobalt diffusing in gold may also show a near-surface effect of this type. Once again the solubility is high, so that this result could be of great interest. However, the technique used for analyzing the diffusion penetration zones by Duhl, viz. the counting of residual gamma activity in the specimen following sectioning, appears to have indicated a near-surface effect in a parallel experiment on the self-diffusion of gold reported at the same time. The latter result is known to be spurious, since Kidson5 has demonstrated that self-diffusion in gold does not show this effect. Duhl et 01. also reported some measurements on the diffusion of nickel in gold, but failed to give any data for the near-surface region. As the solubility of nickel in gold is high, such data would also be of special interest. We, therefore, decided to conduct another set of experiments on the diffusion of nickel and cobalt in gold, using a sectioning technique that allows the individual sections to be assayed for solute content and thus gives direct determinations of penetration profiles. Also, by sectioning with an anodizing/stripping tech- nique, very thin layers can be removed and the region close to the surface studied in detail. MATERIALS The gold specimens were supplied as single crystal disks $ in. in diam by a in. high by Monocrystals Co. of Cleveland, Ohio. The gold itself was of spectro-scopic purity, i.e., better than 99.99 pct pure. METHOD Specimen Preparation. One flat end face of each gold crystal was spark planed with a Servomet spark erosion machine set for minimum spark energy. Following this treatment the crystals were preannealed for 2 to 4 days at temperatures of either 400" or 700°C. The three crystals preannealed at 700°C showed signs of recrystallization. The spark-planed end face of each crystal was then coated with the appropriate amount of 63i or 60 radioactive tracer. This deposit was laid down in a simple plating bath containing the as-supplied solution of the radioactive isotope as well as sufficient ammonium oxalate to saturate the solution. Some ammonium oxalate remained undissolved on the floor of the bath for this purpose. During plating further additions of ammonium oxalate were sometimes required to allow the plating to continue satisfactorily, perhaps due to passivation of the undissolved oxalate already present. The thickness of the deposited layer was determined by comparison of the apparent surface activity of the plated specimen with that of a similar specimen having a weighable deposit of the isotope on its end face. Correction for self-absorption of the radiation was made in this calculation. Annealing. The deposited crystals were annealed in a hydrogen atmosphere in sealed silica tubes. During this heat treatment they were supported, active face down, on optically flat silica plates. The temperature was measured with calibrated Pt vs Pt-10 pct Rh thermocouples, and the tabulated values can be taken to be correct to Z°C. All the crystals showed evidence of recrystallization following these heat treatments, suggesting that initially they may not have been good single crystals or had suffered strain during delivery. Concentration Profile Analysis. After annealing, the crystals were sectioned by the anodizing-stripping technique.6 The anodizing involved suspension of the specimen with its cylindrical axis horiz6ntal by a gold wire in a 200-ml beaker containing 1 M Hg304. A cathode in the form of a strip of gold sheet, 2 in. wide and positioned to be in contact with the curved side of the beaker, completely encircled the specimen. An anodizing current of 30 ma, corresponding to a current density of 5 ma per sq cm on the surface of the specimen, was passed for times ranging from 5 to 150 min depending on the thickness of gold to be removed; the solution was stirred continuously during this process. Following this treatment, the specimen

Jan 1, 1969

PRESIDENT WILLIAM L. SAUNDERS,1 NEW YORK, N. Y. PAST PRESIDENTS CHARLES F. RAND,1 NEW York , N. Y. BENJAMIN B. THAYER,2 . NEW YORK, N. Y. FIRST VICE-PRESIDENT PHILIP N. MOORE,1 ST. Louis, Mo. TREASURER GEORGE C. STONE,1 NEW YORK, N.Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, NEW York, N. Y.

Jan 4, 1915

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

Jan 1, 1903

By W. W. Eckles

This paper is presented as a suniniary report of the use of well gas composition correlations obtained from mass spectrometer recordings as a means of identification and determination of reservoir continuity. Conventional methods for detecting composition differences are en-pensive, elaborate, and difficult to obtain. This excludes the use of extensive composition data for most applications. During recent years the mass spec-trometer has come into general use as an analytical tool in petroleum refineries. The use of mass spectrometer composition patterns ir~ characterizing or "finger-printing" the produced gas from a reservoir, presents a novel method for correlatitlg gas samples from well to well. The mass spectrometer provides a trace similar to an electric log. having peaks which represent the abuntlnnce of certaitz hydrocarbons in the well gas sample. Without going further into the detailed analysis the idea has been advanced that these traces or patterns could be used as a means of identifying a particular natural gas. This theory has proven to be essentially correct. The mass spectrometer pattern method is simple and cheap as COi?7pared to other standard methods. It greatly facilitates the solution of reservoir and geological problems in which correlation of well gas Com-positions is a factor. Specific field applications have been made. This paper concerns the results obtained in 465 individual gas analyses from 35 fields and 77 res- ervoirs. In a number of cases it has been found that such data have been extremely valuable in the determination of reservoir continuity. In at least one case, the method was a valuable contribution in tracing a reservoir from sand to sand in a coinplex fnulted field involving n11rnerous gas reservoirs. Field applications are presented to illustrate the possibilities of the method at the present stage of developnient and to stimulate the ernployrnent of this new approach by geologists and petroleum engineers in the industry. INTRODUCTION Identification of producing horizons and the determination of reservoir continuity are often a problem in those areas where dome structures and highly faulted sands are encountered. To complicate the picture further, there may be numerous sands, one on top of the other which dip and diverge in different directions. Even though it may be possible to develop some solutions to the preceding problems on the basis of the geological and reservoir data on hand. it is readily recognized that substantiating data based on independent methods would he extremely valuable. It has been found through field studies that correiation of well gas composition can be used to advantage in the geological and engineering study of a complex reservoir identification problem. METHOD FOR COMPARISON AND CORRELATION OF WELL GAS SAMPLES Since a large number of well gas samples are required in a gas identification or reservoir con- tinuity problem, it is necessary that a method of analysis be employed which can detect differences in composition readily and inexpensively. Although detection would be possible by means of low temperature fractional distillation (POD) analpsis, the method requires a relatively large sample and is comparatively slow and expensive to run. The mass spectrometer affords an inexpensive and precise analysis of small well gas samples taken at the surface which are about 1/300 as large as a POD sample. These samples can be obtained by regular field personnei and shipped to the spectrometer for analysis. It is, therefore, a practical approach to the problem. A typical record from the mass spectrometer is illustrated in Fig. I. The peaks on the record represent the abundance of ions produced from the different hydrocarbon molecules making up the gas sam-ple. In well gas comparisons only five peaks are employed, since the other peaks are formed from the same gas molecules and furnish no additional information. The five peaks used represent the abundance of methane, propane, ethane, butane and heavier, and oxygen. They are referred to respectively as the 16, 29, 30, 43, and 32 peaks. The oxygen peak is used to correct for air content in

Jan 1, 1958

BUFFALO J R Atkinson, Chairman (Hamilton, Ont, Canada) H R Morlock, Secretary CHICAGO H Erler, Chairman (Gary, Ind ) M E Nickel, Vice-Chairman A M Kroner, Secretary-Treasurer CLEVELAND C W Cravens, Chairman (Cleveland) E J Sobey, Vice-Chairman E Kondas, Secretary Leo Svete, Treasurer DETROIT M Groat, Chairman (Ecorse, Mich ) H W Clark, Secretary

Jan 1, 1957

By L. A. Geoffrion, R. H. Perkins, J. C. Biery

Densities of cerium metal and several lour-melting binary cerium alloys were measured over the range 25° to 800°C. A rolumeter, using NaK as working fluid, was used to obtain the data. The cerium, Ce-Co, Ce-Ni, and Ce-Cu alloys all exhibited an increase in density on melting, while a Ce-Mn alloy expanded on melting. FOR the proper design of a nuclear reactor, the change in density of the fuel with temperature must be known. This is especially important in a system utilizing molten fuel, such as LAMPRE (Los Alamos Molten Plutonium Reactor Experiment), since a relatively large change in density usually occurs during the solid-liquid transition. The fuel for LAMPRE is a Pu-2.5 wt pct Fe alloy with a melting temperature of 410°C. However, limitations in reactor design with this fuel have led to consideration of other plutonium-containing alloys for use in future generations of this type of reactor. Several ternary alloys containing plutonium and cerium as two components have satisfactorily low melting points. The system that at the present time appears to be most acceptable is Pu-Ce-Co; it exhibits little change in melting temperature with wide variation in plutonium concentration. Other alloys that have received some consideration contain nickel, copper, and manganese as the third constituent. The proposed fuel alloys are difficult to handle experimentally in the 25" to 800°C temperature range since they oxidize readily, react with many solvents, and contain a poisonous fissionable material. In addition, in this temperature range the alloys pass through the solid-liquid transition. Several techniques are available for measuring the densities and volume coefficients of expansion of solids or liquids. However, the only apparatus that appears suitable for measuring expansion coefficients over this temperature range and through the phase transition is a volumeter. In a volumeter, the indicating medium must be essentially inert to and insoluble in the material being studied. It must also possess a low vapor pressure over the operating temperature range, and its coefficient of expansion must be accurately known. One material that is satisfactory in nearly all of these respects is the alloy Na-78 wt pct K, which melts at -10°C and has a vapor pressure of 860 mm Hg at 800°C. This relatively high vapor pressure at 800°C requires an overpressure of an inert gas to prevent boiling. While a volumeter is capable of determining accurately the volume coefficients of expansion of materials, it cannot be used for absolute density measurements. Therefore, a density determination at a known temperature must be coupled with the volumeter measurements to give all the desired data. The weight-loss technique using immersion in bromobenzene at room temperature proved to be satisfactory. The preliminary work that was done on this experimental program involved developing and calibrating the equipment, and measuring the densities and volume coefficients of expansion of cerium and some low-melting binary cerium alloys. The complications that are caused with the introduction of plutonium into the system were avoided until the equipment was proved to be satisfactory and until experience was gained in its operation. It is this first phase of the experimental work that is described in this report. DESCRIPTION OF EQUIPMENT AND OPERATING PROCEDURE The NaK volumeter is shown schematically in Fig. 1. Basically, the equipment consists of two weld-sealed stainless-steel containers of nearly identical volume. One container holds a tantalum crucible and the specimen being measured; the other contains a tantalum crucible and a tantalum specimen used as a control reference material. To avoid temperature gradients, the bombs are located in a copper block inside the furnace. Stainless-steel capillaries of equal length and volume connect each stainless-steel container to a glass viewing capillary. The stainless-steel containers, stainless-steel capillaries, and a portion of the glass capillaries are filled with NaK (22 wt pct Na-78 wt pct K). The NaK/gas interface in the glass capillary is viewed with a cathetometer which is accurate to *0.5 mm. The cathetometer readings are used to calculate the volume changes of the samples during a run. This volumeter is basically the same as that described by F. Knight in Plutonium 1960. 2 However, changes in equipment design and operating procedure were made to eliminate some major operating difficulties. These changes are summarized below. 1) In filling the manometer with NaK, gas was frequently entrained in the system. Evacuation of the system before filling failed to eliminate the en-

Jan 1, 1965

PRESIDENT. CHARLES F. RAND,1 NEW YORK, N. Y. PAST PRESIDENTS. CHARLES KIRCHHOFF,1 NEW YORK, N. Y. JAMES F. KEMP,2 NEW YORK, N. Y. FIRST VICE-PRESIDENT. BENJAMIN B. THAYER,1 NEW YORK, N. Y. TREASURER. GEORGE C. STONE,1 NEW YORK, N. Y. SECRETARY EMERITUS. ROSSITER W. RAYMOND NEW YORK, N. Y.

Jan 5, 1913

By Archer E. Wheeler

IN the copper industry, the year 1942 was one of striving for larger tonnage and increased production. The demands of the war program placed copper high in the list of strategic metals and the Government encouraged production by offering a premium of 5c. per pound for copper output in excess of the 1941 quotas. This had the effect of increasing the tempo of existing operations and also of initiating a number of projects which will eventually result in production from sources not hitherto exploited. No radically new methods of copper reduction were reported.

Jan 1, 1943

By George A. Hill

WE of the oil industry, devoted to freedom of initiative, free competitive enter- prise, and free American institutions, applaud, with one voice, affirmation by the President of the national will and purpose to preserve and to protect, against all aggressors, "our American way of life with our individual and national freedom." We subscribe utterly and completely to this guiding declaration and seek its further definition as applied to the oil industry. Fortunately for all, the policy of the Government, after adequate study and deliberation, has been given precise definition. The National Defense Advisory Commission, with its patriotic, highly qualified, and distinguished personnel, has unanimously agreed to and adopted twelve general principles governing national defense contracts and also fair labor standard requirements. The President of the

Jan 1, 1940

By Philip Morse

THE Australian lead-smelting plants began to use charges carrying high zinc percentages somewhat earlier than was common with American plants. When lead smelting first started in Australia the immense deposits of oxidized lead at Broken Hill were available but later these oxidized ores became exhausted and were replaced by sulfides. This was before the days of flotation and these sulfides when concentrated carried about 1 per cent. of zinc to 6 per cent. of lead. The works of the Sulphide Corpn. at Cockle Creek was perhaps the pioneer in high-zinc slags but the Port Pirie plant of the Proprietary Co. was a close and very able second and has continued the work to the present time. The Cockle Creek lead furnaces remained in operation until shortly after the war when most of the Broken Hill companies combined and took over the Port Pirie plant to treat their concentrates. As it was the practice both at Cockle Creek and Port Pirie to carry 20 per cent. or more of lead on the charge, it was found that under these conditions of large amounts of zinc in the charge, good roasting was absolutely necessary and matte production was unwise. The Huntington-Heberlein system of roasting was introduced and later the Dwight & Lloyd process. In this way, by roasting the sulfide portions of the charge as thoroughly as possible and making no matte, a method of smelting was developed where the slag over long periods carried as high as 20 per cent. ZnO without serious furnace troubles, and slags carrying even up to 33 per cent. ZnO have been reported. The zinc slags were not very different in appearance from the ordinary slags produced in American practice except that they gave off more smoke and fume on tapping. The slag usually ran hot and freely, coming from the tap in a full stream. Normally there was little crust on the sides' of the furnace and the tuyeres gave no trouble though they were always rather dark.

Jan 1, 1929

By H. A. Wriedt

A method of calculating activities in binary systems having miscibility gaps is described. The method, which applies only to the phase in which the gap occurs, is exact when the function defined by the equation varies linearly with composition. Analytical and numerical solutions (as a function of the conjugate phase compositions) are presented for two coefficients A and B from which the thermodynamic activities can be calculated. Deviations from Henry's law, calculable by the method presented, are shown graphically for the particula~ case of the component i at the edge of the miscibility gap more remote .from pure component i. For symmetrical gaps, the deviation from Henry's law at this gap edge becomes smaller as the gap becomes wider, The interrelation of gap location, the direction of departures from Henry's law and the occurrence of maxima and minzma in these departures is discussed in some detail. Values for a and for activity calculated from phase diagrams show fair to excellent agreement with corresponding experimental values in the Al-Zn and CaO-SiO2 systems. WHEN structurally similar phases, B and 6, lie at the sides of a two-phase region in a constitution diagram, it can be assumed that, stably or metast-ably, they will become completely miscible at a higher temperature. The B and 6 phases are particular composition ranges of a single B6 phase region with a miscibility gap. Below, as above, the critical solution temperature, the free energy of formation of the 06 phase is a continuous function of composition through the range of the miscibility gap. It is the purpose of this paper to use this continuous free-energy function in order to develop a simple method for computing the thermodynamic activities in the B6 solution of a binary system. To make these calculations it is assumed that the function ai, familiar from Gibbs-Duhem integrations and defined by the equation

Jan 1, 1962

By O. E., Kiessling

THE better control of production was made the topic for a special program of the annual meeting of the Institute last February. In the discussion at that meeting it was brought out that in many branches of the mineral industry (as in other industries), there was faulty industrial coordination. Those who were best informed by reason of their intimate connection with coal, copper, oil, iron, lead and zinc, and almost all other of the essential minerals pointed to a condition of chronic over-capacity, to the dissipating use of irreplaceable minerals, to an unstabilized price structure, and to over-stimulatecl production and the destruction of some mineral resources over and above what is thought to be the needs of prudent cur- rent consumption. The discussion went far enough to point out the existence of various problems, and the question then raised was "what can be done by way of self-coordination of industry?" by "production control from within?" or in other words, "how can the mineral industry protect its resources against waste and at the same time protect both the producer and consumer against loss from prices that are too low or too high?"

Jan 1, 1928

By Charles L. Mantell, P. P. Napolitano

High-purity tellurium oJ semiconductor grade may be prepared by a combination of electrowinning from tellurium oxide, electrorefining and controlled atmosphere melting, as detailed in the paper. SEMICONDUCTOR devices such as transistors and rectifiers depend upon extremely pure forms of silicon, germanium, and selenium. Although tellurium is chemically related to these elements, it has not been studied as a semiconductor because commercial forms are too impure. Highly purified tellurium would be an interesting starting point for a study of its solid-state characteristics. Tellurium shows a greater electrical conductivity in the direction of the helices or chains forming the crystals than at right angles to the chains, and thus is a semiconductor. Unlike selenium, the conductivity is only slightly increased by exposure to light. Impurities such as Ag, Cu, Au, Fe, Sn, As, Sb, Bi, Br, and I provide accepters and make extrinsic tellurium of the P type. So far, however, no elements have been found which, when introduced, would act as donors. Small amounts of tellurium dioxide enormously increase the thermoelectric power. Many extremely pure metals have been made by electrolytic refining or electrowinning procedures. Tellurium forms compounds in a number of valences, as indicated in Table I. The physical properties given in Table II do not show any unusual conditions which would interfere with the formation of elec- trodes, or the deposition of the metal on a cathode. Tellurium dioxide could be obtained in relatively high purities of 98 pct TeO2 or better at reasonable prices. Tellurium dioxide is soluble in caustic to form tellurites, which are conductive, ionizable, and from which tellurium metal may be deposited at a cathode. Preliminary solubility tests to saturation of tellurium dioxide in approximately 10 pct sodium hydroxide gave the results of Table III. The temperature range is a practical one for electroplating. Electrochemical test facilities were set up and these met the operating conditions of Table IV. For a determination of purity of deposits, there was available a Jarrell Ash Co. quantitative emission

Jan 1, 1964

The meeting of the Institute of Metals Division was held in Phila-delphia from Sept. 30 to Oct. 2, inclusive. On Monday evening preceding the meeting, a dinner was held at the Ritz-Carlton Hotel at which many of the former officers of the Division and of the present officers and execu-tive committee were present. The subject of a membership committee was discussed and a motion to appoint such a committee with powers to go over the membership list for the selection of divisional members and to institute plans for additional members was passed. Mr. H. E. Howe and Dr. Johnston of the National Research Council attended the meeting and presented their plans for an Alloys Research Association. Many opinions were voiced as to the practicability of such a scheme and Mr. Howe expressed himself in appreciation of the cooperative thought and efforts given him. On Tuesday morning the Institute of Metals Division joined sessions with the American Foundrymen's Association and listened to the opening addresses. In the afternoon a boat ride was taken on the Delaware River, visiting the plants of the Cramp Ship and Engine Building Co. and the shipyard of the Emergency Fleet Corpn. at Hog Island. The launching of the boat christened "Afoundria" at 5 p.m. was witnessed by members of the party. The opening technical session was held on Tuesday evening at the Ritz-Carlton Hotel at 8 o'clock. The next session was held at the Ritz-Carlton at 10 o'clock on Wednesday morning and the final session at the same time and place on Thursday morning. The sessions were well attended and the discussion was good. The highly technical nature of some of the papers on the program was of special note. Taken as a whole the meeting was one of the most successful ever held. The follow-ing papers were presented:

Jan 11, 1919