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By Milton E. Wadsworth, J. Brent Hiskey

Galvanic interaction between particulate chalcopyrite (CuFeS2) and copper results in the rapid conversion of chalcopyrite to chalcocite. The effects of temperature, surface area, concentration of sulfuric acid and agitation were systematically evaluated. The kinetics were found to be controlled by a steady-state current flow controlled by the effective anodic and cathodic surface areas involved in the galvanic couple. The experimental activation energy was 11.5 and stoichiometric data and reaction products have been characterized. The overall kinetic system has been evaluated based upon an electrochemical model.

Jan 1, 1974

By R. B. Schluter, M. M. Fine

A process for winning copper from pelletized chalcocite concentrate without matte smelting and converting is under development at the Twin Cities Metallurgy Research Center of the U.S. Bureau of Mines. The new procedure includes a two-stage fluid-bed treatment in which the pelletized concentrate with 33% Cu and 7% S is first desulfurized to about 0.5% S in an oxidizing atmosphere, and then metallized by reduction with hydrogen. The reduced product is melted with flux to separate metallic copper from the gangue. The metal must be refined to remove residual sulfur and iron. The pelletizing of the fine concentrate into mini-pellets prior to fluid-bed treatment is an important feature of the process, because it permits shorter reaction time, decreases dusting, and facilitates subsequent processing.

Jan 1, 1972

By ir. H. Eraly

The allocation of miners to teams, and of teams to production faces, is complicated by the high degree of absenteism of miners in Belgium. Therefore, the exact knowledge of who is actually present at the beginning of a shift and of the exact skills of those present, enables the foremen and mine captains to constitute their teams before all men go down into the mine in the most effective way possible. This paper describes the system of attendance recording and of displays which the foremen use to constitute their teams and/or to interrogate the personnel data base in order to do so. It shows how the foremen dialogue with the computer, to change the function of a miner within a team, to another team, or the function of a team as a whole. The implementation of the system, data bases, and data communication equipment and procedures, is described. The benefits obtained are presented for each level of the company: foremen and team supervisors, engineers, mine management.

Jan 1, 1977

By N. A. D. Parlee, E. M. Sacris

OXYGEN solubility in liquid silver has been well studied.1-6 It has been established that the solubility follows Sieverts' law reasonably well5'6 up to po2

Jan 1, 1968

[PRESIDENT ASD DIRECTOR LOUIS S. CATES 3 .New York, N. Y. PAST PRESIDENT AND DIRECTOR CHESTER A. FULTON1 .Baltimore, Md. HARVET S. MUDD 2I Los Angeles, Calif.]

Jan 1, 1946

By W. C. Coons, E. H. Rennhack, R. A. Perkins

THE constitution of Ti-N alloys containing up to 17.5 wt pct N has been investigated by Palty, Margolin, and Nielsen.1 Their results, which confirmed earlier work

Jan 1, 1969

By Basil Prescott

A thorough knowledge of the peculiarities of this type of orebody is necessary in sampling these limestone replacement deposits. Oxidized ores are often overestimated because of error in determining specific gravity and actual cross-section of the orebody, and sulfide ores are often underestimated because it is difficult to scatter the samples so that they will accurately represent the area under consideration. This paper describes various methods of sampling and cites factors that enter into the estimation of these deposits. IN THE science of evolution of the species, there is a law which, simply stated, avers that the history of the individual repeats the history of the race. Similarly, if unassisted by the experience of others, each successful engineer would perfect and develop his methods and technique from the rough grab sample up to the carefully taken, recorded and studied samples and observations which now determine and decide the expenditure of the large sums required for modern mining. Hence real progress results from the interchange of experience, as in that way the entire experience of the profession can be made available to every engineer. The literature of this subject is already voluminous, but some progress has been made in the gathering of data and in their compilation or presentation.

Jan 3, 1924

By F. P. Dewey

The subject of this paper does not embrace the consideration of ways and means for the increase of analytical accuracy, or the question what could or should be attained in that direction. I desire simply to call attention to the degree of accuracy exhibited in actual every-day practice. In estimating this, little weight will be given to the evidence afforded by the agreement of duplicate or multiple determinations by the same chemist; for I am convinced that such agreement is a delusion and a snare. Nor will special importance be attached to the agreement of two or even three analyses in special cases, or to the agreement between two methods practiced by the same analyst. I propose to compare the results obtained by several chemists, working upon the same sample and by various methods, in order to exhibit, as I have said, the actual condition of practice. The available material for illustrating this phase of the question is unfortunately scanty; but something has been done; and I hope, by calling attention to some of the work in this line, to stimulate further work in the same direction by inducing others to prepare suitable samples and submit them to various chemists who are competent and willing to make the necessary determinations, and fully describe the methods they employ. I draw most of my illustrations from the Transactions of the Institute, the Proceedings of the Association of Official Agricultural Chemists, and from personal experience. Manganese in Steel.—In May, 1881, Mr. William Kent presented a paper to the Institute entitled " Manganese Deter-

Jan 1, 1897

By Jackson M. Langton

Substantial evidence supports the theory that high-angle faults and overthrusts in the Morenci-Metcalf region were initially caused by a Late Precambrian-Early Paleozoic stress field. These faults were reactivated in Late Paleozoic-Early Mesozoic time which completed the structural framework prior to the Laramide Orogeny. Excluding an interruption by diabase dikes and sills, Paleocene-Eocene magmas invaded the pre-existing structures and became progressively more sialic in composition and nearer to the surface with each subsequent injection. The last sialic intrusion was highly explosive, rendering the country rocks more permeable for hypogene and supergene activity. Widespread dilation, instigated by uplift and subsequent magma intrusion, caused extension to the northwest and southeast. A major locus of hypo gene alteration and mineralization appears to be centered around the south and southeast periphery of the youngest granite porphyry stock. A potassic, sulfide-deficient core is telescoped by a pyritic, phyllic zone which in turn is enveloped by widespread propylitic alteration.

Jan 1, 1974

By Frank C. Smith

The following article covers the history of a metallurgical campaign, commenced in March, 1905, at the mines of the Socorro Bold Co., in the so-called desert region of Yuma county, Arizona. The results obtained were simply a function of necessity, as will be seen from the description of the local economic conditions and the character of the ores treated. The mines and mill of the Socorro Gold Co. are located near the small village of Harrisburg, about 60 miles from Congress Junction, Ariz., which, at the time this work was undertaken, was the nearest railroad station, and from which all supplies were brought by wagon through the desert, at a cost varying from $10 to $15 per ton in addition to the railroad freights. Wood, the only available fuel, cost $7 per cord. Water for all purposes was pumped to the plant from a well in the valley about 4 miles away. Under the Arizona law, a working-shift is 8 hr. Wages were $6 per day for foremen and mill-men, $4 per day for blacksmiths and engineers, $3.50 per day for miners, and $3 per day for shovelers and trammers. The ore consisted of quartz, in which, above the 250-ft. level, the iron-minerale were largely oxidized and some free gold was visible; below that level few traces of oxidation occurred, and pyrite constituted the principal mineralizer in the quartz, together with occasional pockets of galena and a few eccentric specks of covellite. The 20-stamp mill was equipped with plates for amalgamation, and three Standard tables for concentration. The tails from the tables mere elevated by a centrifugal pump to a launder, by which they were conveyed to a 60-ton cyanide-mill for further treatment. The cyanide-mill was erected at so great a distance from the stamp-mill that a separate crew of workers and a separate power-plant were necessary. No arrangement had been made for the treatment of the concen-

Jan 1, 1907

By Henry M. Howe

This paper gives the results of an investigation of the beha vior of the argentiferous cobalt-nickel arsenides of Temiskam-ing, Ontario, in roasting, made in the metallurgical laboratories of the School of Mines of Columbia University in the City of New York. The ore was kindly given by the owners of the La Rose and Trethewey properties at Cobalt, Ontario, and Mr E. J. Hall, Tutor in Assaying in Columbia University, has helped us much. I. Object of the Investigation. The object of the investigation was to learn: 1. The temperature at which the arsenic is most rapidly expelled ; 2. The thoroughness with which it is expelled by prolonged roasting at this temperature; 3. The effect of adding charcoal (a) near the end of the roast and (b) at. the beginning of the roast. II. Nature of the ORe. The important ores mined in the Temiskaming deposits are: native silver—with small amounts of dyscrasite (Ag,Sb), ar-gentite (Ag,S), pyrargyrite (Ag,SbS,)—smaltite (CoAs,), chlo-anthite (NiAs,) and niccolite (NiAs). Mispickel (FeAsS) and cobaltite (CoAsS) also occur in smaller quantities. The average composition of the ore shipped from this district for the first six months of 1905 was: silver, from 4.1 to 4.8 per cent.; cobalt, from 6.9 to 8.2 per cent.; nickel, from 3 to 4.7 per cent.; and arsenic, from 30.9 to 34.6 per cent. The ore which we treated consists chiefly of smaltite. In our 1aboratory-work

Jan 1, 1908

By E. Buehler, H. J. Levinstein

The temperature ranges in which the three inter-metallic phases in the Nb-Sn system form have been determined and the composition and structure of two of the three phases has been established. The kinetics of the formation of Nb3Sn in cored wire samples has been studied in the temperature range of 800° to 1050°C. From 800°to 950°C the rate of formation increases by four orders of magnitude. The rate-controlling step for the formation process in this temperature range appears to be the diffilsion of tin through NbSn. At higher temperatu~es a change occurs in the mechanism of the formation process such that up to a temperature of 1050°C the rate of formation of Nb3Sn does not increase above the rate observed at 950°C. For temperatures helow 950°C the current-carrying capacity of the wire increases with increased percent reaction reaching a maximum value when the formation process is 90 to 95 pct complete. The maximum current-carrying capacity obtainable in this temperature range is independent of the temperature. Above 950°C tlze current-carrying capacity obtainable in the wire decreases with increasing temperature of formation. A model is proposed which accounts for the ohserved behavior. RECENTLY, Buehler et a1.l reported the results of an investigation of the process variables which influence the superconducting properties of Nb3Sn-cored wire. These results indicated that at least four variables affect the properties of the manufactured wire. These include composition, particle size of the starting powder mix, temperature of heat treatment, and time of heat treatment. In order to understand completely the role of these variables, it is necessary to have an accurate knowledge of the phase equilibria in the Nb-Sn system. At the present time, phase-equilibrium diagrams for the Nb-Sn system have been published by a number of investigators.2-5 The diagrams differ as to the number of phases present, the composition of the phases, and the temperature range of stability of the phases. The present investigation was undertaken in order to resolve these differences. Since the investigation of Buehler et al. demon- strated that the length of time at the temperature of heat treatment affected the superconducting properties of Nb3Sn, it is apparent that it is necessary to understand the kinetics of the formation process as well as the equilibrium conditions before a complete understanding of the system is possible. As a result, the kinetics of formation of the various phases in the system were also studied in this investigation. EXPEFUMENTAL PROCEDURE Diffusion couples and sintered powdered compacts were employed in the phase-diagram investigation. The diffusion couples were made by filling 1/8-in.-ID monel-sheathed niobium tubes with tin. The monel sheath was employed to facilitate drawing.' The tubes were then drawn to a tin-core diameter of 32 mils. Samples approximately 3 in. long were then cut from the drawn composite. The tin was drilled out of the ends to a depth of 1/4 in. and niobium-wire plugs were inserted into the ends and peened over. The monel was removed by etching in concentrated nitric acid, after which the samples were sealed in evacuated quartz bulbs and heat-treated in a resistance-wound tube furnace. The samples were quenched into ice water upon removal from the furnace. The diffusion couple samples were examined metallographically employing a chemical etching solution consisting of 10 ml of saturated chromic acid per g of NaF. In addition, two anodizing solutions were used for phase-identification purposes. The first was the picklesimer7 solution; the second consisted of equal parts by volume of 30 pct H2O2 and concentrated NH4OH to which 1 g of NaF was added per 25 ml of solution. The anodizing conditions for the second solution were 2 v and 100 ma with a tin cathode. The powdered compacts were made by pressing previously mixed powders of 99.9 pct pure Sn and 99.6 pct pure Nb supplied by the United Mineral Co. into cylinders 3/8 in. in diameter by 1/2 in. long. The cylinders were then sealed in quartz tubes and heat-treated in the same manner as the diffusion couples. The samples were examined metallographically and by X-ray diffraction techniques. Since it was desirable to be able to correlate the kinetic data with current-carrying capacity, the type of specimen chosen for this part of the investigation had to be a compromise between the optimum system for studying kinetics and one which was suitable for making current-carrying capacity

Jan 1, 1964

By Shiou-Chuan Sun

THIS paper presents the design and operation of a frothmeter capable of measuring the frothing characteristics of pine oils and other frothing reagents. The experimental data show that the froth-ability of pine oil is governed by: 1—rate of aeration, 2—time of aeration, 3—height of liquid column, 4—chemical composition of pine oil, 5—pH value of solution, 6—temperature of solution, and 7—concentration of pine oil in solution. The effect of mineral particles on the behavior of froth also was studied, and the results can be found in a separate paper.' The results also show that the relative froth-abilities of pine oils in the frothmeter generally correlate with those in actual flotation, provided that other factors are kept constant. In addition to pine oils, the other well-established flotation frothers were tested, and the results are included. In this paper, compressed air frothing is the frothing process performed by means of purified compressed air, whereas sucked air frothing is the frothing process accomplished by purified air sucked into the glass cylinder by a vacuum system. The term vacuum frothing denotes that froth was formed by degassing of the air-saturated liquid under a closed vacuum system. Apparatus The frothmeter, shown in Fig. 1, is capable of re-producibly measuring the volume and persistence of froth as well as the volume of air bubbles entrapped in the liquid and is capable of being used for compressed air frothing, sucked air frothing, and vacuum frothing. Fig. la shows that for compressed air frothing, the apparatus consists of an airflow regulating system, 1-3; a purifying and drying system, 4-8; a standardized flowmeter to measure the rate of airflow from zero to 500 cc per sec, 9; and a graduated glass cylinder, 13; equipped with an air regulating stopcock, 10; an air chamber, 11; and a fritted glass disk to produce froth, 12. The fritted glass disk, 5 cm in diam and 0.3 cm thick, has an average pore diameter of 85 to 145 microns. The pyrex glass cylinder has a uniform ID of 5.588 cm and an effective height of 63 cm. The inside cross-sectional area of the glass cylinder was calculated to be 24.53 sq cm, or 3.8 sq in. For sucked air frothing, Fig. lb shows that the apparatus for compressed air frothing is used again, with the following modifications: 1—compressed air and its regulating system, 1-3, are eliminated; and 2—a vacuum system, 16, equipped with a vapor trap, 15, and a vacuum manometer, 17, is added. The vacuum system can be either a water aspirator or a laboratory vacuum pump. Any desired rate of airflow can be drawn into the glass cylinder, 13, by adjusting the opening of the air regulating stopcock, 10. The sucked air stream is cleaned by the purifying and drying system, 4-8, before entering the glass cylinder, 13. When this setup is used for vacuum frothing, the air regulating stopcock is closed. The frothmeter has been used for almost 3 years and has proved to give reproducible results, as illustrated in Table I. With a magnifying glass and suitable illumination, the frothmeter also can be used to study the attachment of air bubbles to coarse mineral particles.' Experimental Procedures Except where otherwise stated, the data presented were established by means of the compressed air method. The volume and persistence of froth were recorded respectively at the end of 4 and 6 min of aeration at a constant rate of airflow of 29.3 cc per sec, which is equivalent to 71.6 cc per sq cm per min, or 462.6 cc per sq in. per min. The aqueous solution for each test, containing 1000 cc of distilled water and 19.2 ± 0.5 mg frothing reagent, was adjusted to a pH of 6.9 0.2. The volume of froth is expressed as cubic centimeter per square centimeter and is equivalent to the height of the froth column (the distance between the bottom and the meniscus of the froth). The volume of froth was obtained by multiplying the height of froth by the cross-sectional area of the glass cylinder, 24.53 sq cm. Before each test, the glass cylinder, 13, was cleaned thoroughly with jets of tap water, ethyl alcohol, tap water, cleaning solution, tap water, and finally distilled water. The cylinder with stopcock,

Jan 1, 1953

By G. L. Chierici

Starting from Muskat's theory of water and gas coning, maximum permissible oil production rates without water and/or free-gas production have been determined, in a broad range of reservoir and well parameters, using the potentiometric model technique. The main assumptions made are as follows: (1) the reservoir rock is homogeneeous (either isotropic or anisotropic); (2) the volume of the aquifer underlying the oil zone is very small, so that it does not contribute to reservoir energy; and (3) the gas cap expands at a very low rate, so that it can be assumed to be in quasi-static conditions. The results obtained are presented in the form of diagrams which can be used for solving two types of problems: (1) given the reservoir and fluids characteristics, as well as the position and length of the perforated interval, determine the maximum oil production rate without water and/or free-gas production; and (2) given the reservoir and fluids characteristics only, determine the position and length of the perforated interval which optimize the maximum permissible oil production rate, without water and/or free-gas production. INTRODUCTION In oil reservoirs where the oil-bearing formation is underlain by an aquifer which does not participate in the production mechanism, water-coning is a limiting factor to the flow rates of producing wells. Production rates are usually kept to a value that will prevent the water from entering the wells. The entry of water into a well lowers its productivity by increasing the weigbt of the fluid column; moreover, the separation of water from the effluent, at the surface, may constitute a very difficult problem in cases of heavy viscous oils. A similar situation is encountered in oil reservoirs with a gas cap overlying the oil-saturated zone; here a downward gas cone is induced by the flow of oil towards the producing wells. Production rates must be low enough to prevent the gas from being produced; producing gas from the gas cap would be a waste of energy. Of course, water-coning and gas-coning phenomena can occur at the same time in the same reservoir if the oil-producing formation is both overlain by a gas zone and underlain by a water zone. Due to its relevant practical importance, the mechanism of coning was studied by many people.2,3,5-8 Defining the conditions for getting the maximum water-free and/or gas-free oil production rate is a difficult problem, often encountered under one of the following aspects: 1. Predict the maximum flow rate that can be assigned to a completed well without the simultaneous production of water and/or free-gas. 2. Define the optimum length and position of the interval to be perforated in a well, in order to obtain the maximum water and gas-free production rate. A systematic study of these problems was made by means of the electrical analog technique. The results of this study are presented here, under the form of a set of curves providing solutions for the above stated problems. These curves are valid only for homogeneous forrnations, either isotropic or anisotropic. Should the formation be non-homogeneous (by horizontal or vertical variation of permeability, shale diaphragms, fractures, etc.), a specific potentiometric study would be required for each specific case. Especially when shale diaphragms of some radial extension are present, the critical rates observed are much larger than would be expected from the diagrams. STATEMENT OF THE PROBLEM In the present study the aquifer is supposed to be of such limited volume that it does not contribute to the energy of the reservoir. Moreover, the gas cap is supposed to expand at such a low rate that the potential gradient in the gas cap is negligible. Under static conditions water-oil and gas-oil interfaces (T1 and T2) are both horizontal. When the reservoir production starts, below each well these interfaces take a cone-like shape (Fig. 1) having as an axis the axis of the well. This shape results from the equilibrium between potential gradients in the oil zone and gravitational forces due to density differences between oil and water and between oil and gas. Assuming the oil-bearing formation to be homogeneous and the oil to be incompressible, the analysis of the problem (see Appendix) shows that the oil-water and gas-oil interfaces are stable only if the oil production rate of the well is not higher than the following values.

Jan 1, 1965

By Shiou-Chuan Sun

THIS paper presents the design and operation of a frothmeter capable of measuring the frothing characteristics of pine oils and other frothing reagents. The experimental data show that the froth-ability of pine oil is governed by: 1—rate of aeration, 2—time of aeration, 3—height of liquid column, 4—chemical composition of pine oil, 5—pH value of solution, 6—temperature of solution, and 7—concentration of pine oil in solution. The effect of mineral particles on the behavior of froth also was studied, and the results can be found in a separate paper.' The results also show that the relative froth-abilities of pine oils in the frothmeter generally correlate with those in actual flotation, provided that other factors are kept constant. In addition to pine oils, the other well-established flotation frothers were tested, and the results are included. In this paper, compressed air frothing is the frothing process performed by means of purified compressed air, whereas sucked air frothing is the frothing process accomplished by purified air sucked into the glass cylinder by a vacuum system. The term vacuum frothing denotes that froth was formed by degassing of the air-saturated liquid under a closed vacuum system. Apparatus The frothmeter, shown in Fig. 1, is capable of re-producibly measuring the volume and persistence of froth as well as the volume of air bubbles entrapped in the liquid and is capable of being used for compressed air frothing, sucked air frothing, and vacuum frothing. Fig. la shows that for compressed air frothing, the apparatus consists of an airflow regulating system, 1-3; a purifying and drying system, 4-8; a standardized flowmeter to measure the rate of airflow from zero to 500 cc per sec, 9; and a graduated glass cylinder, 13; equipped with an air regulating stopcock, 10; an air chamber, 11; and a fritted glass disk to produce froth, 12. The fritted glass disk, 5 cm in diam and 0.3 cm thick, has an average pore diameter of 85 to 145 microns. The pyrex glass cylinder has a uniform ID of 5.588 cm and an effective height of 63 cm. The inside cross-sectional area of the glass cylinder was calculated to be 24.53 sq cm, or 3.8 sq in. For sucked air frothing, Fig. lb shows that the apparatus for compressed air frothing is used again, with the following modifications: 1—compressed air and its regulating system, 1-3, are eliminated; and 2—a vacuum system, 16, equipped with a vapor trap, 15, and a vacuum manometer, 17, is added. The vacuum system can be either a water aspirator or a laboratory vacuum pump. Any desired rate of airflow can be drawn into the glass cylinder, 13, by adjusting the opening of the air regulating stopcock, 10. The sucked air stream is cleaned by the purifying and drying system, 4-8, before entering the glass cylinder, 13. When this setup is used for vacuum frothing, the air regulating stopcock is closed. The frothmeter has been used for almost 3 years and has proved to give reproducible results, as illustrated in Table I. With a magnifying glass and suitable illumination, the frothmeter also can be used to study the attachment of air bubbles to coarse mineral particles.' Experimental Procedures Except where otherwise stated, the data presented were established by means of the compressed air method. The volume and persistence of froth were recorded respectively at the end of 4 and 6 min of aeration at a constant rate of airflow of 29.3 cc per sec, which is equivalent to 71.6 cc per sq cm per min, or 462.6 cc per sq in. per min. The aqueous solution for each test, containing 1000 cc of distilled water and 19.2 ± 0.5 mg frothing reagent, was adjusted to a pH of 6.9 0.2. The volume of froth is expressed as cubic centimeter per square centimeter and is equivalent to the height of the froth column (the distance between the bottom and the meniscus of the froth). The volume of froth was obtained by multiplying the height of froth by the cross-sectional area of the glass cylinder, 24.53 sq cm. Before each test, the glass cylinder, 13, was cleaned thoroughly with jets of tap water, ethyl alcohol, tap water, cleaning solution, tap water, and finally distilled water. The cylinder with stopcock,

Jan 1, 1953

By R. M. Waterstrat

The phases occurring in the V-Mn system were studied by means of X-yay diffraction and metallo-paphic techniques, using are-melted alloy specimens annealed in the temperature range 800° to 1150°C and quenched. The bcc solid solution extends at 1250°C all the way from vanadium to 6-manganese. Below 1050°C the a-phase is formed, and the terminal a-manganese phase is stabilized up to about 900°C by vanadium in solid solution. IN the only previous general survey of the V-Mn system Cornelius, Bungardt and Schiedtl reported the existence of three intermediate phases corresponding to the approximate compositions VMn,, VMn, and V5Mn. The phase VMn8 has recently been identified as a o phase2 but the alloy VMn was found to have a bcc structure2 corresponding apparently to the vanadium solid solution rather than to the large cubic unit cell reported by Cornelius et al. 1 Subsequent work by Rostoker and Yamamoto3 has shown that the vanadium-base bcc solid solution extends to at least 15 pct Mn at 900°C. An alloy corresponding to the composition VMn, was examined by Elliott,4 who reported that the as-cast sample as well as samples annealed at 1200o and 1300°C had bcc structures, but that annealing at 1000°, 800") and 600°C produced two phases. One of these phases was apparently the bcc solid solution and the other resembled the o phase structure. Hellawell and Hume-Rothery5 established the phase relationships in manganese-rich alloys above 1000°C, and showed that the o phase in this system is replaced by the 6 Mn (bcc) solid solution at temperatures above 1050°C. These results suggest that a continuous bcc solid solution may exist above 1050°C between vanadium and 6 Mn. The present investigation was undertaken in order to develop more complete information in regard to this system. EXPERIMENTAL METHODS The alloys used in the present work were prepared by arc-melting electrolytic manganese having a minimum purity of 99.9 pct and vanadium lumps with a purity of 99.7 pct. The major impurities present in these metals were carbon, nitrogen, and oxygen and this would account for the small percentage of nonmetallic inclusions observed metal-lographically. The arc-melting was at first performed under a helium atmosphere and it was necessary to keep the melting times as short as possible in order to minimize the loss of manganese by vaporization. It was later found that the evaporation of manganese was considerably reduced when the melting was done under argon atmosphere. The final composition of each alloy was calculated by assuming that the total weight loss during melting was due to evaporation of manganese. Compositions which were calculated in this manner agreed reasonably well with the results of chemical analysis, as shown in Table I. Spectrographic analysis revealed the presence of contamination by tungsten, but in no case was the percentage of tungsten greater then 0.4 at. pct. The specimens were in each case broken in half and the fractured section was examined visually and microscopically for evidence of inhomogeneity. Each specimen was homogenized at temperatures near l100°C, as shown in Table I. After this treatment most specimens consisted of large columnar grains of the bcc vanadium solid solution. The etchant used in most of the metallographic work consisted of 20 pct nitric acid, 20 pct hydro-flouric acid, and 60 pct glycerine. It was found that this etchant would clearly delineate the phases present in these alloys although it does not produce any striking contrast between the phases. For certain manganese-rich alloys, a 1 pct aqueous solution of nitric acid was used. This etchant gave a brown color to the a-manganese phase, whereas the o phase was virtually unattacked and appeared very light as shown in Fig. 1. The etchants used by Cornelius et a1.l were found to produce spurious effects in some of these alloys. In particular, the vanadium-rich alloys etched in hot sulfuric acid often appeared to consist of two phases when both X-ray diffraction and etching with the glycerine-acid mixture indicated the presence of single phase bcc solid solution. A few percent of what appears to be an oxide or nitride phase was found at the grain boundaries and in the interior of the grains, especially in the vanadium-rich alloys. All alloys were annealed in sealed silica tubes containing 1 atm of pure argon and these tubes were then quenched in cold water. Although some manganese loss occurred during annealing, the loss seemed to be confined to the surface of the speci-

Jan 1, 1962

By I. S. Levy, J. L. Brimhall, B. Mastel

Specimens of' Hastelloy X-280, a low-cobalt version of the solid-solution- hardened nickel-base alloy Hastelloy X, were given a series of thermomechanical treatttzents. They were then Lensile-tested at room temperature and 1350°F. The Microstructures of the specimens tested at 1350°F were studied by electron Microscopy. Microscopy showed that dislocation tangling, caused by the cold working, mas still in evidence after aging-for 24 hr to temperatures as high as 1550oF. (Cr, Mo)23 C6, (Fe, Mo)6 C'. as well us an unidentifiable phase precipitale due to the combination of the thermomechanical treatments and subsequent tensile strain. The room -temperature and 1350°F tensile properties show a general increase ill strength and decreccse in ductility with increusing cold-work level. This is due to the dislocation taangling-. PerLurbatiot~s to this general trend occur- due to solid-solution weakening at the higher cold-work levels as a direct result of the preciplitation reactions. THE requirements for corrosion resistance and high-temperature strength place nickel-base alloys among the more promising materials for advanced nuclear reactor applications. However, when these alloys are irradiated at service temperatures, they generally suffer severe embrittlement'" and reduction in rupture life.3 Certain experimental treatments resulted in improvements in the tensile and stress-rupture properties of Hastelloy X-280, a solution-hardened nickel-base alloy.' To provide a basis for understanding these improvements, unirradiated tensile specimens were examined by electron microscopy. The results are reported in this paper. EXPERIMENTAL DETAILS Material. Hastelloy X-280, a low-cobalt version of Hastelloy X, is a member of the solution-hardened class of nickel-base alloys. The Hastelloy X-280 was obtained from 4- and 1-in: thick plates in the mill -annealed condition. Table I gives the chemical composition of the material as reported by the National Spectrographic Laboratories. ~x~erimental Treatments. Plates of suitable size, 12 by 3 by 1 in., or by + in., were cut under a water jet from the stock material and examined ultrasonic -ally for homogeneity of grain size and absence of voids. The acceptable plates were solution-treated at 2150°Ffor 1 hr and air-cooled. These plates were then reduced in thickness by cold rolling 0, 10, 15: or 20 pct along the original rolling direction. The plates were machined into buttonhead tensile specimens with a gage diameter of 0.125 in., with a gage length of 1.125 in., and with their tensile axes parallel to the rolling direction. The specimens were examined for quality of finish with a penetrant dye, ultra son ically checked for voids, and finally given a dimensional tolerance check with an optical comparator. The acceptable specimens were aged for 24 hr at either 1000" or 1500 F and air-cooled. These specimens were then held at 540°F in a water loop for approximately 18 days to qualify as controls for similar specimens irradiated under the same conditions of time, temperature, water chemistry, and flow rate. Table U summarizes the treatments. These treatments were investigated to establish whether prior precipitation and stabilization of carbide phases at strain sites within the matrix could reduce the amount of carbides available for precipitation at grain boundaries during service. Tensile-Test Conditions. Specimens were tested to fracture at room temperature or 1350 F in air on an Instron tensile-testing machine at a crosshead speed of 0.05 in. per min. The time for the furnace to reach equilibrium at 1350°F was approximately 30 min; soak time prior to testing was 15 min; and test duration was approximately 5 min.

Jan 1, 1968

1. List of Manuscripts Seen in America 2. List of Manuscripts Seen in England 3. List of Maps Examined 4. List of Newspapers Examined 5. General Bibliography - Numbered Reference List

Jan 1, 1942

By F. D. Rosi, C. H. Mathews

THE plastic properties of face-centered cubic metals below room temperature present a field of investigation which has not been extensively ex-plored. The work by Schmid and Boas1 has demonstrated the importance of temperature upon such properties as strain hardening and critical resolved shear stress. The work by Yamaguchi2 upon the shear stress as related to the number of slip bands accentuates the necessity for further experiments of a similar nature. The approach to a mechanical equation of state from the standpoint of thermal fluctuations and activation energies by Becker3 and more recently by Kauzmann4 further emphasizes the need for a quantitative and more comprehensive analysis of the dependence of fundamental plastic properties on temperature. The purpose of the present work was to investigate specifically: (1) The gross shape of the stress-strain curves at several temperatures, (2) the change in the critical shear stress as a function of temperature, and (3) the number and appearance of slip bands as a function of strain and temperature. Preparation of Specimens Single-crystal specimens of 99.996+ pct alumi-num, 1/2 in. in diam and 5 to 6 in. in length, were made by the Bridgman method of gradual solidification from the liquid state. The crystallographic orientation of the single crystals was determined from back-reflection, Laue X-ray photograms ac-cording to the method described by Greninger.6 In most specimens the Laue photograms showed double diffraction spots indicative of the lineage structure type of imperfection, discussed in great detail by Buerger.7 The angular spread of these spots was never observed to exceed 2". Most of the crystals were radiographed to insure against microporosity. In preparing the metal surface for optical microscopy, the following sequence of operations gave good results: The as-cast crystals were turned down in a lathe, 0.001 in. per cut, to obtain a 2.5 in. gauge length. The cold-worked layer resulting from this operation was removed chemically by etching with Tucker's reagent. Then the specimen was polished mechanically through 2/0 metallographic emery paper, after which it was etched again to remove the cold-worked layer resulting from the mechanical treatment. A 48-hr anneal at 580°C ±10°C followed so as to insure an essentially stress-free single crystal. After the annealing treatment, the specimen was electrolytically polished in a 2:l solution of methyl alcohol and concentrated nitric acid. With a current density of 10 amp per sq dm (decimeter) the time required to obtain a satisfactory surface varied from 10 to 12 min. The polish-ing was carried out for short periods of 2 min to avoid rapid deterioration of the solution as well as to enable the rotation of the specimen 180" for uniformity of polish. It was necessary to place the solution in a bath of dry ice in view of its explosive nature at room temperature. Etching of the electrolytically polished surface was accomplished by using the fuming etch-pit method recommended by Lacombe and Beaujard8 for high-purity aluminum. Method for Tensile Testing A modification of the loading equipment devised by Miller9 was used. In this apparatus, the specimen was suspended from a chain and gimbal arrangement (for axial loading) in a heavy steel framework connected at the bottom to a balanced 6:1 lever and bucket system. Loading of the specimen was accomplished by allowing sand to flow from a reservoir into the bucket suspended from the longer end of the lever-arm at a rate of approximately 3 lb per min. Strain measurements were made using the Baldwin SR-4, bonded, resistance-wire, strain gauge and an SR-4 portable strain indicator (type K), which permits a reading accuracy of 2 microinches per inch. For low-temperature study, the gauge was calibrated by measuring the elastic modulus of an annealed stainless steel rod, which is known to be independent of temperature."

Jan 1, 1951

By Robert Glass Cleland

[MINING DIVISION GENERAL WESTERN ADMINISTRATION Harrison M. Lavender, Vice-President and General Manager Charles R. Kuzell, Assistant General Manager Walter C. Lawson, Assistant to Vice-president and Genera1 Manager]

Jan 1, 1952