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By P. S. Kotval, O. H. Nestor

Stacking fault energy measurements of nickel-base alloys have been mainly confined to binary and ternary systems. In this paper, the stacking fault energy has been measured by the rolling texture method in a series of ten alloys which comprise successive additions of Cr, Mo, Fe, and C to pure nickel, eventually resulting in an alloy of the composition of Hastelloy alloy X. The alloys studied here are single-phase, solid solutions with the exception of two alloys in which some undissolved particles of "primary" carbide have been retained. It is found that successive additions of chromium, molybdenum, and iron all lower the stacking fault energy, with iron having only a minor effect. The stacking fault energy is found to increase when carbon is added in solid solution. The results from the rolling texture measurements are correlated with thin foil observations of dislocation substructures in these alloys. In a recent paper' it was pointed out that the dislocation substructure of various superalloy matrices could be classified into three broad categories based on 'high', 'medium', and 'low' stacking fault energy. It has also been demonstrated2 that the dislocation substructure in each of these categories has a well defined role in the nucleation of strengthening precipitates which is different from the role played by the dislocation substructure in other categories. Thus, it becomes desirable to understand the influence of various solute elements on the stacking fault energy and hence on the dislocation substructure of the matrix, before any further development of superalloys by mi-crostructural predesign can be undertaken. Recently, Beeston and France have studied the influence of increasing solute additions on the stacking fault energy of a series of binary nickel-base alloys relevant to the Nimonic series using the rolling texture method, and have then estimated the effect of a given alloy addition in five commercial Nimonic alloys. However, comparison with stacking fault energy data from other investigations''5 suggests that the influence of a given solute element in a nickel-base binary system is not necessarily the same in a ternary or more complex superalloy system. Accordingly, the present work was undertaken to study the effect of successive addition of solute elements to pure nickel, the final composition being the nominal composition of Hastelloy X. The rolling texture method of stacking fault energy measurement was used since it can be used for the whole range of stacking fault energy values and does not have the disadvantage of, say, the Node method which is only applicable to low values of stacking fault energy. In addition, the rolling texture method provides a means of determining the stacking fault energy which is statistically more significant than that provided by other methods. EXPERIMENTAL TECHNIQUES Button heats of alloys of the compositions shown in Table I were prepared. Each button was remelted not less than four times. After a slight deformation (approximately 5 pct) all alloys were homogenized at 2200°F except alloys, H . I, and J. Alloys H and I were solution heat treated at 2150°F and alloy J at 2282OF. The buttons were cold worked by rolling, using "end-to-end" passes and intermediate anneals at the homogenization temperatures mentioned above. After each annealing treatment the samples were rapidly water quenched to avoid any precipitation. In alloys F and I, however, a few particles of "primary" carbides were retained even after the homogenization treatments at the temperatures mentioned above. Part of the solution heat treated material was cold worked to 0.04-in.-thick sheet and the penultimate reduction was -50 pct of deformation as recommended by Dillamore et al. All annealing was carried out in vacuo within sealed quartz capsules. Some of the material from each alloy was rolled down further to 0.004 in. strip for thin foil transmission electron microscopy specimens. Specimens of this strip were annealed at the homogenization temperature for 1 hr and then strained 7 pct by rolling at room temperature. Thin foils were prepared from the strip specimens by the 'window" technique using an Ethanol-Perchloric acid electrolyte at 32°F and a voltage of 22 v. Stainless steel cathodes were employed. All transmission electron microscopy was performed in a JEM-7 electron microscope using an accelerating voltage of 100 kv. Specimens from the 0.04 in. sheet which had been rolled -60 pct in the final pass were electropolished to remove the surface layers to a depth of approximately 0.002 in. Rolling texture pole figures for all the alloys were determined using a Schulz ring and nickel filtered CuKa radiation at 50 kv and 20 ma. The texture parameter Io/(lo + I,,) (where Io is the

Jan 1, 1970

By R. F. Yap, N. Arbiter, C. C. Harris

A fully-instrumented driving mechanism has been constructed to study the power, aerating and solid suspension characteristics of several laboratory flotation machines. Machines operating over normal flotation speed ranges give substantially constant power numbers in liquid systems indicating that they operate close to fully baffled turbulent flow conditions. Owing to lack of geometrical scaling, power numbers for different sizes of cells of the same make are different. Even larger differences occur between cells of different manufacturers. For a given impeller, varying the tank size did not significantly affect the power consumption. Tank geometry and baffling has a slight effect on power consumption with shrouded impellers. For a given impeller speed, suspension height decreases while power increases with increasing mass of solids in suspension. While power consumption is hardly affected by particle size and clearance between the impeller and tank bottom, the suspension height significantly increases as clearance increases and as particle size decreases. Aeration was found to affect not only power but also the suspension characteristics of the machine. For closely sized particles, drastic sedimentation occurred when a critical value of the air flow number was exceeded. The critical air flow number decreased with increasing particle size. This effect was less marked with a wide particle size range. The self-aerating capacity of flotation machines increases with cell size at a given speed for the same impeller-shroud system, but decreases in the presence of frother and solids. Equations have been established for correlating all of the studied variables. Data taken from the literature were also correlated with these equations. The modern mechanical flotation machine has, over a period of 60 years, displaced other designs to become the dominant type. Once the correct chemical environmental conditions have been established, the major requirement, selective mineral-air adherence, is essentially a function of two operating variables — impeller speed and air rate. The special nature of this dependence is such that in the same apparatus, but under different operating conditions, adherence can be either prevented or destroyed. Another aspect of this observation is that flotation machines though differing in detail to a considerable extent can produce similar metallurgical results. It must be concluded that having determined the correct reagent levels, establishing the correct operating conditions are at least as important as machine design. Since about 1960, after 30 years of fairly stable circumstances, manufacturers have been developing new types of machines whose major feature is emphasis on pulp flow characteristics by virtue of new im-peller-stator designs. As far as can be ascertained, these new designs necessitate radical departures from accepted impeller speed-air rate values. Performance data are still awaited. Flotation machine development has been empirical, as is selection of operating conditions. The purpose of the work at Columbia University has been to elucidate the fundamentals of the subject so that the purely mechanical aspects of the flotation process can be understood in hydrodynamic terms.1-6 Hopefully, this might lead to intelligent selection of a particular machine and its operating conditions for a specific ore based on a minimum of testing, or even to new types of flotation machines. The present investigation is the most comprehensive to date.7,8 Earlier work, which was largely exploratory, has been repeated and extended and employes the most accurate measuring techniques available. Additionally, sufficient hydrodynamic data were obtained under flotation conditions to delineate the relevant operating ranges. Attention has been given to scaling in that several geometrically scaled tanks and impellers have been constructed and tested; it has been pointed out elsewhere that undistorted geometrical scaling rarely pertains in flotation machine design.5 This paper is divided into sections dealing with relevant combinations of the three phases: liquid, air and solid. Summaries of the literature have been given in previous publications2-4 and will not be repeated here. Recently, several reviews of mixing have appeared, which can be usefully referenced.9-11 It is of interest to note that flotation is not included

Jan 1, 1970

By Roland Blanchard

Recent discovery at Mount Isa of copper mineralization in commercial amount at a depth of 1000 ft., coinciding with downward termination of ore at about the same depth within the larger silver-lead-zinc lenses that have been the standby of Mount Isa's production to date, has been cited as an example in support of mineral zoning. A previous paper by the author and Graham Hall1 furnished a detailed description of the geology of the ore at Mount Isa as exposed up to that time, but necessarily dealt mainly with the silver-lead-zinc mineralization. Most of the geologic facts that constitute the first half of the present paper were set forth in the previous one in much greater detail, with full supporting evidence for the facts cited. The large amount of underground development (approximately 20 miles) and the extensive exploration carried out by diamond drilling (100,000 ft.) at Mount Isa, added to extensive microscope work conducted over a period of years, both by the company's staff and by others, had made possible the calculation within fairly close limits of mineralogical composition of the principal mineralized block of ground down to 1000-ft. depth, and had established closely the mineral succession, with reasons for deposition of the various minerals in the patterns now occupied by them. The geologic facts as outlined in the previous paper remain as stated; but because substantial development within the new copper ore body and further exploratory diamond drilling within the new silver-lead-zinc area (Racecourse) have taken place since that paper was written, statements and figures relating to those two areas in the present paper supersede those furnished in the previous one. The recent work likewise has established more clearly the paragenetic relationship between the chalco-pyrite and galena. Evidence confirming the relationship is furnished in the present paper. The facts of ore occurrence at Mount Isa show Accepted Zonal Succession Silver sulphantimonides Galena Sphalerite Tetrahedrite Arsenical sulphides Chalcopyrite Pyrrhotite Mount Isa Succession I In the main but prob- Silver sulphantimonides ably not wholly Tetrahedrite I contemporaneous Galena Pyrrhotite Sphalerite Arsenical sulphides They show further: (I) that instead of the silver-lead minerals yielding to increased zinc in depth, the zinc yields to increased silver-lead; (2) no dovetailing of the silver-lead-zinc sulphides into chalcopyrite takes place; (3) despite the large amount of pyrrhotite deposited in the district (estimated at upward of 100,000,000 tons), its deposition took place under moderately low temperature conditions; (4) no evidence has been found for increase in temperature of deposition, with depth, to deepest exploration in ore (1475 ft.). The anomalous condition at Mount Jsa, both as to the unorthodox mineral succession and the largely unorthodox patteru of mineral distribution, is explained in the present paper,

Jan 1, 1949

By Roland Blanchard

Recent discovery at Mount Isa of copper mineralization in commercial amount at a depth of 1000 ft., coinciding with downward termination of ore at about the same depth within the larger silver-lead-zinc lenses that have been the standby of Mount Isa's production to date, has been cited as an example in support of mineral zoning. A previous paper by the author and Graham Hall1 furnished a detailed description of the geology of the ore at Mount Isa as exposed up to that time, but necessarily dealt mainly with the silver-lead-zinc mineralization. Most of the geologic facts that constitute the first half of the present paper were set forth in the previous one in much greater detail, with full supporting evidence for the facts cited. The large amount of underground development (approximately 20 miles) and the extensive exploration carried out by diamond drilling (100,000 ft.) at Mount Isa, added to extensive microscope work conducted over a period of years, both by the company's staff and by others, had made possible the calculation within fairly close limits of mineralogical composition of the principal mineralized block of ground down to 1000-ft. depth, and had established closely the mineral succession, with reasons for deposition of the various minerals in the patterns now occupied by them. The geologic facts as outlined in the previous paper remain as stated; but because substantial development within the new copper ore body and further exploratory diamond drilling within the new silver-lead-zinc area (Racecourse) have taken place since that paper was written, statements and figures relating to those two areas in the present paper supersede those furnished in the previous one. The recent work likewise has established more clearly the paragenetic relationship between the chalco-pyrite and galena. Evidence confirming the relationship is furnished in the present paper. The facts of ore occurrence at Mount Isa show Accepted Zonal Succession Silver sulphantimonides Galena Sphalerite Tetrahedrite Arsenical sulphides Chalcopyrite Pyrrhotite Mount Isa Succession I In the main but prob- Silver sulphantimonides ably not wholly Tetrahedrite I contemporaneous Galena Pyrrhotite Sphalerite Arsenical sulphides They show further: (I) that instead of the silver-lead minerals yielding to increased zinc in depth, the zinc yields to increased silver-lead; (2) no dovetailing of the silver-lead-zinc sulphides into chalcopyrite takes place; (3) despite the large amount of pyrrhotite deposited in the district (estimated at upward of 100,000,000 tons), its deposition took place under moderately low temperature conditions; (4) no evidence has been found for increase in temperature of deposition, with depth, to deepest exploration in ore (1475 ft.). The anomalous condition at Mount Jsa, both as to the unorthodox mineral succession and the largely unorthodox patteru of mineral distribution, is explained in the present paper,

Jan 1, 1949

By Arthur L. Walker

In June, 1893, while I was with the Old Dominion Copper Co. at Globe, Ariz., I received an offer to take charge, as manager, of the Baltimore Electric? Refining Co. which had recently built a plant at Baltimore, Md., having a capacity of about 1200 tons of electrolytic copper per month, using the Hayden series system. This was a very large output, for in those days the plants were small and the art was in its infancy. At the beginning of 1893 there were 11 electrolytic refineries in the United States, most of them using the multiple system. The Hayden series system was used at Baltimore and Bridgeport and the Smith series system was in operation at the Electrolytic Copper Co. at Ansonia, COM., and at the Pennsylvania Salt Co. at Philadelphia. In the latter system the plates were placed in a horizontal position, but the operating difficulties were so numerous it was soon discarded. The total production of these 11 plants in 1892 was very small; I have not been able to discover reliable figures of production. There were about thirty electrolytic copper refineries in the world that year, according to Titus Ulke, and the entire production of these

Jan 1, 1932

Time as a Factor in the Making and Treating of Steel. By John Johnston. (Howe Lecture) (T.P. 1478) Influence of Chromium and Molybdenum on Structure, Hardness and Decarburization of 0.35 Per Cent Carbon Steel. By R. F. Miller and R. F. Campbell. (T.P. 1345) Mechanical Properties of Iron-manganese Alloys. By F, M. Walters, Jr., I. R. Kramer and B. M. Loring. (T.P. 1369) The Instability of Low-expansion Iron-nickel-cobalt Alloys. By I. R. Kramer and F. M. Walters, Jr. (T.P. 1370) The S-curve of a Chromium-nickel Steel. By B. M. Loring. (T.P. 1383) A Magnetic Determination of the A3 Transformation Point in Iron. By B. A. Rogers and K. 0. Stamm. (T.P. 1388) Rapid Tension Tests Using Two-load Method. By A. V. de Forest, C. W. MacGregor and A. R. Anderson. (T.P. 1393) Effects of Scrap in the Blast-furnace Burden. By C. L. T. Edwards. (T.P. 1270) Temperature Gradients through Composite Carbon Columns and their Application to Blastfurnace Linings. By F. J. Vosburgh and M. R. HatFIeld. (T.P. 1363) Correlations of Some Coke Properties with Blast-furnace Operation. By H. W. Johnson. (T.P. 1402) The Technical Cohesive Strength and Yield Strength of Metals. By D. J. McAdam, Jr. (T.P. 1414) Effects of Eight Complex Deoxidizers on Some 0.40 Per Cent Carbon Forging Steels. By George F. Comstock. (T.P. 1417) Significance of the Bessemer End Point. By H. T. Bowman. (T.P. 1428) Structural Diagrams of Nickel Irons and Steels. By J. T. EasE and N. B. Pilling. (T.P. 1432) Carbides in Low-chromium Steel. By Walter Crafts and C. M. OFFenhauer. (T.P. 1436) Hardenability Calculated from Chemical Composition. By M. A. Grossmann. (T.P. 1437) Recrystallization of Silicon Ferrite in Terms of Rate of Nucleation and Rate of Growth. By J. K. Stanley and R. F. Mehl. (T.P. 1438) The Solubility of Carbon as Graphite in Gamma Iron. By R. W. Gurry. (T.P. 1440) An Evaluation of the Factors Affecting Iron Oxide in the Open-hearth Bath. By J. E. Gould and H. J. Hand. (T.P. 1442) Precision in Creep Testing. By J. A. Fellows, Earnshaw Cook and Howard S. Avery. (T.P. 1443) Lattice Relationships in the Decomposition of Austenite to Pearlite, Bainite and Martensite. By G. V. Smith and R. F. Mehl. (T.P. 1459) Rate of Nucleation and Rate of Growth of Pearlite. By F. C. Hull, R. A. Colton and R. F. Mehl. (T.P. 1460) Weight Change as a Criterion of Extent of Decarburization or Carburization. By R. W. Gurry. (T.P. 1470) Observations in the Making and Use of Sulphite-treated Steels. By E. L, Ramsey and L. G. Graper. (T.P. 1476) Diffusion in Metal Accompanied by Phase Change. By L. S. Darken. (T.P. 1479) Engineering Properties of Heat-resistant Alloys. By Howard S. Avery, Earnshaw Cook and J. A. Fellows. (T.P. 1480) Distribution of Manganese and of Sulphur between Slag and Metal in the Open-hearth Furnace. By L. S. Darken and B. M. Larsen. (T.P. 1481)

Jan 1, 1942

Time as a Factor in the Making and Treating of Steel. By John Johnston. (Howe Lecture) (T.P. 1478) Influence of Chromium and Molybdenum on Structure, Hardness and Decarburization of 0.35 Per Cent Carbon Steel. By R. F. Miller and R. F. Campbell. (T.P. 1345) Mechanical Properties of Iron-manganese Alloys. By F, M. Walters, Jr., I. R. Kramer and B. M. Loring. (T.P. 1369) The Instability of Low-expansion Iron-nickel-cobalt Alloys. By I. R. Kramer and F. M. Walters, Jr. (T.P. 1370) The S-curve of a Chromium-nickel Steel. By B. M. Loring. (T.P. 1383) A Magnetic Determination of the A3 Transformation Point in Iron. By B. A. Rogers and K. 0. Stamm. (T.P. 1388) Rapid Tension Tests Using Two-load Method. By A. V. de Forest, C. W. MacGregor and A. R. Anderson. (T.P. 1393) Effects of Scrap in the Blast-furnace Burden. By C. L. T. Edwards. (T.P. 1270) Temperature Gradients through Composite Carbon Columns and their Application to Blastfurnace Linings. By F. J. Vosburgh and M. R. HatFIeld. (T.P. 1363) Correlations of Some Coke Properties with Blast-furnace Operation. By H. W. Johnson. (T.P. 1402) The Technical Cohesive Strength and Yield Strength of Metals. By D. J. McAdam, Jr. (T.P. 1414) Effects of Eight Complex Deoxidizers on Some 0.40 Per Cent Carbon Forging Steels. By George F. Comstock. (T.P. 1417) Significance of the Bessemer End Point. By H. T. Bowman. (T.P. 1428) Structural Diagrams of Nickel Irons and Steels. By J. T. EasE and N. B. Pilling. (T.P. 1432) Carbides in Low-chromium Steel. By Walter Crafts and C. M. OFFenhauer. (T.P. 1436) Hardenability Calculated from Chemical Composition. By M. A. Grossmann. (T.P. 1437) Recrystallization of Silicon Ferrite in Terms of Rate of Nucleation and Rate of Growth. By J. K. Stanley and R. F. Mehl. (T.P. 1438) The Solubility of Carbon as Graphite in Gamma Iron. By R. W. Gurry. (T.P. 1440) An Evaluation of the Factors Affecting Iron Oxide in the Open-hearth Bath. By J. E. Gould and H. J. Hand. (T.P. 1442) Precision in Creep Testing. By J. A. Fellows, Earnshaw Cook and Howard S. Avery. (T.P. 1443) Lattice Relationships in the Decomposition of Austenite to Pearlite, Bainite and Martensite. By G. V. Smith and R. F. Mehl. (T.P. 1459) Rate of Nucleation and Rate of Growth of Pearlite. By F. C. Hull, R. A. Colton and R. F. Mehl. (T.P. 1460) Weight Change as a Criterion of Extent of Decarburization or Carburization. By R. W. Gurry. (T.P. 1470) Observations in the Making and Use of Sulphite-treated Steels. By E. L, Ramsey and L. G. Graper. (T.P. 1476) Diffusion in Metal Accompanied by Phase Change. By L. S. Darken. (T.P. 1479) Engineering Properties of Heat-resistant Alloys. By Howard S. Avery, Earnshaw Cook and J. A. Fellows. (T.P. 1480) Distribution of Manganese and of Sulphur between Slag and Metal in the Open-hearth Furnace. By L. S. Darken and B. M. Larsen. (T.P. 1481)

Jan 1, 1942

By Arthur L. Crawford

PLAGER gold is perhaps the most difficult of the common mineral deposits to evaluate. Not only are the erratic pay streaks a source of never-ending uncertainty, but the spotty distribution of the gold in iso¬lated nuggets is a perpetual source of error and disappointment to the sampler. Experienced engineers have long realized this difficulty and have been wary in predicting assay values except in the most general terms, and then only after extensive and usually expensive sampling. During the past year I have had the opportunity of checking a number of gold placers, and from the results obtained I believe that the microscope may be employed to advantage in placer sampling.

Jan 1, 1933

By Paul M. Tyler

THE winning of metals from Nature has been advanced to a degree of efficiency that commands admiration even in this Machine Age. Economy of human effort underground, in surface plants, and in treatment works, and better means of performing all manner of operations have cut costs and im¬proved products to an extent that seems far beyond the wildest imagin¬ings of those that labored in the days of hand mining and muscular metallurgy. Principles and methods borrowed from other professions and sciences - mechanical engineering, chemistry, and physics-all have con¬tributed to the rapid development of ore production and treatment, but no small part of the achievements must be credited to the free exchange of ideas within the industry itself and mass attack upon problems of mutual concern. The esprit de corps or class consciousness that has contributed so effectively to the progress of the metal industries has been less apparent among nonmetallic mineral producers. As a class they have been handicapped by inadequate contact with the metal-mining fraternity as well as among themselves.

Jan 1, 1935

By Willard L. Hunter

Four solvent extraction systems were studied to determine their efficiency jor extraction and separation of tantalum and columbium. Aqueous feed solutions of varying HF-HCl concentrations and metal content were contacted with equal volumes of cyclohexanone, 3-methyl-2-butanone, and 2-pentanone and solutions of varying HF-H2S04 concentrations were contacted with equal volumes of 2-pentanone. One multistage continuous test was made in a polyethylene pulse column using cy clohexanone as the organic phase. In each system studied, columbium and tantalum purities in excess of 95 pct with respect to each other were obtained in single-stage tests at low acidities in the feed solution. Separation factors ranging from 1700 to 2400 were obtained when rising HF-HCl mixtures in the aqueous phase. Best results were obtained when a solution of HF-H2S04 was used as the aqueous phase and 2-pentanone as the organic phase. A separation factor in excess of 6000 was obtained in one stage with aqueous solution concentrations of 2 _N HF and 2N H2S0,. When acid concentrations were increaszd to 52 HF and 10 _N H2S0,, 99.9 pct of the tantalum and 98.2 pct of the columbium initially present in the feed solution were transferred to the organic phase. The separation of columnbium and tantalum obtainable by means of the solvent extraction systems presented in this paper was found to corn -pare favorably with other systems, including the HF-H2SO4-methyl isobutyl ketone system currently used by most producers for the extraction and separation of these metals. TANTALUM and columbium are always found together in minerals of commercial significance, although the proportion of the two metals in ores varies within broad limits. Columbium is estimated to be 13 times more abundant than tantalum. Five methods generally employed for the separat:ion of these metals are: 1) fractional crystallization (the Marignac process),2 2) solvent separation, 3) fractional distillation of their chlorides, 4) ion exchange, and 5) selective reduction. Of these methods, the one currently used by industry to the greatest extent is that of solvent separation. One of the early technical developments in solvent separation of tantalum from columbium was reported by the Bureau of Mines: the HF-HC1-methyl isobutyl ketone system; data were presented for both laboratory and pilot-plant experimentation.3 Of twenty-eight organic solvents tested for their ability to extract tantalum from an HF-HC1 solution of columbium and tantalum, 3-pentanone (diethyl ke-tone), cyclohexanone, 2-pentanone, and 3-methyl-2-butanone were chosen for further study. Data on the HF-HC1-diethyl ketone system has been published4 and data describing the use of cy clohexanone, 2-pentanone, and 3-methyl-2-butanone as the organic phase are included in this report. RAW MATERIAL The source of tantalum and columbium oxides for this study was ('Geomines" tin slag from the Manono Smelter, Cie Geomines, Gelges, S.A., Congo. In order to extract the valuable Ta-Cb content, the slags were carbided, chlorinated, and the sublimate from chlo-rination was hydrolized and washed free of chloride with water. The washed material was air-dried and stored in a stoppered container. Throughout the paper, "feed material" refers to this mixture of hydrated oxides which was employed because of its high solubility in aqueous solutions. Typical analysis of the hydrated oxides is shown in Table I. I) HF-HC1-CYCLOHEXANONE SYSTEM Batch Separation. Effect of Acid Concentration. To determine the effect of varying the acid concentration upon the transfer of tantalum and columbium, a series of tests was made in which approximately 2.5 g of feed material was added to 25 ml solutions of 2, 4, 6, 8, and 10 N HF and 0 through 5 N HC1. Tantalum pentoxide concentration of the solu%ons was approximately 21 g per liter and columbium pentoxide was 14 g per liter. These starting solutions were shaken with equal volumes of cyclohexanone in 100 ml polyethylene bottles for 30 min. The phases were carefully separated in 125 ml glass separatory funnels. The time of contact of the solutions with the separatory funnels was kept at a minimum to reduce silica contamination. The measured phases were separated into 400 ml polyethylene beakers and the metal contents of each were precipitated by addition of an excess of ammonium hydroxide. Precipitate from each phase was filtered on ashless filter paper, ignited at 800" to 1000°C for 45 min, weighed, and analyzed by X-ray fluorescence.5 Data tabulated in Table I1 and illustrated in Fig. 1, show that maximum separation of tantalum from columbium for each HF concentration was obtained with no HCl present. The purest tantalum product was obtained with some HCl present. The highest separation factor was obtained at 2 N HF and

Jan 1, 1970

By Arnulf Muan, Carlos Landolt

Equilibria involving Cu-Pt alloys, copper oxides, and atmospheres of known ox2gen pressures have been determined at 1000' and 1200 C. The data obtained have been used to calculate activity-composition relations in the alloys. A moderate negative deviation from ideality is found. At high copper concentrations, the results of the present study are in good agreement with those of previous investigators, whereas at low copper concentrations the activities obtained in this investigation are slightly higher than those reported previously. The present study is part of a research program dealing with the determination of phase relations and thermodynamic properties of copper-containing systems at high temperatures. The information available for such systems is very scanty, particularly for copper oxides and their combinations with other oxide components. Platinum is commonly used as a container in studies of oxide equilibria. To evaluate quantitatively the extent of reaction between the oxide and the container, a knowledge of activity-composition relations in Cu-Pt alloys is necessary. Such data are not available for Cu-Pt alloys in the temperature range of particular interest in the present research program, and particularly for alloys low in copper. Studies of various aspects of the systems Cu-Pt and Cu-0 have been reported in previous literature. The system Cu-Pt is known1 to form a continuous solid-solution series above 812.C, whereas ordered phases are present in certain composition ranges at lower temperatures. Thermodynamic data for the system have been reviewed by Hultgren et al.,' who presented free energies of mixing at 65Oo C, mainly derived from electromotive force cell measurements by Weibke and Matthes.3 Enthalpies of mixing at 640°C have been obtained by Oriani and Murphy4 with liquid tin calorime-try. Their results differ considerably from those derived from the temperature dependence of the data of Weibke and Matthes. Thermodynamic data for the disordered alloys have been obtained by Assayag,5 and more recently by Schmahl and Minzl,6 by Myles and Darby,7 and by McCormack, Myers, and Saxer.8 The two latter sets of data7'' became available after the present study was completed. In the system Cu-0+ two oxides are stable at high temperatures, CuO and CuzO+ each having only minor deviations from stoichiometry. Equilibria in the liquidus temperature region of the system Cu2O-CuO have been studied by Roberts and systemsmyth,9'10CuzO-CuO by Vogel and ocher,I1 by Osterwald,12 and recently the the present authors.13 The system is of the eutectic type with a eutectic temperature of 1083.C The composition of the eutectic liquid corresponds to Xcu0 = °.44, and the oxygen pressure of the coexisting gas phase is Po2 = 0.55 atm.13 Equilibrium oxygen pressures for coexistence of solid CuO and solid Cu2O have been determined by Schmahl and Muller,l4 by Gadalla, Ford, and white,l5 by Bidwell,16 and recently by the present authors.13 There is reasonably good agreement among the various sets of data. Free energies of formation of Cu2O(s) from the elements have been derived by Tretyakov,17 by Bidwell,16 by Kiukkola and wagner,18 by Pal'guev and Neuimin," and by Steele and Alcock,20 There is particularly good agreement among the latter three1'-20 sets of data. THEORETICAL BASIS Consider a subsolidus isothermal section of the system Cu-Pt-0, as shown in Fig. 1. Two phase as-

Jan 1, 1970

By Harold Price

PRIOR to Sept. 1, 1928, there had never been constructed what might be termed a long pipe line with electric-welded field joints. Nevertheless, by Sept. 1, 1929, within the period of a year, more than 2500 miles of electric-welded lines have been completed. These lines vary in diameter from 6 to 20 in., and in length from 50 to 700 miles. Before Sept. 1, 1928, no such line had been constructed .longer than 50 miles, and only one of nearly that length, a 40-mile 7-in. gas line in Louisiana. This was in reality the first pipe line to use electric-welded field joints. During the past year the following lines have been electric-welded by the Welding Engineering Co. alone: Texas Pipe Line Co.-157 miles of 8-in. line from Corsicana, Texas, to San Augustine, Texas. (This was the first electric-welded oil line.) Texas Pipe Line Co.-80 miles of 8-in. from Lafors, Texas, to Childress, Texas. Texas Pipe Line Co.-39 miles of 10-in. from Monahans, Texas, to Jal, New Mexico. Texas Pipe Line Co.-50 miles of 6-in, from San Antonio, Texas, to San Marcus, Texas. Texas-Empire Pipe Line Co.-424 miles of 12-in. from Cushing, Okla. to Chicago, Illinois. In addition to the field welding mentioned above,1 250 miles of 12-in. line was electric-welded into double joints at the pipe mill at Indiana Harbor, Ind.

Jan 1, 1929

By C. B. Post, D. G. Schoffstall

A determinatioil of the hydrogen content of molten steel by means of the Vacuum-extraction method, as reported here, consists in first casting a sample of the bath in a bomb, so that the gases evolved during solidification are trapped for analysis. A portion of the cast steel sample is then prepared and heated at a temperature of 600" to 800°C. under high vacuum, and the gaser given off during this vacuum extraction (which are shown to be hydrogen), are collected and measured. Analysis of the gases evolved on solidification and the gases in the solid sample enables an accurate determination of hydrogen in the molten steel. Fig. I shows the bomb and accessories that have been found suitable for trapping the gases evolved on solidification. The bomb is made of scamless steel pipe, approximately 7 in. long by 136 in. i.d., and welded at the bottom. An ordinary pipe cap has a vacuuni-type metal stopcock threaded and brazed in its upper end. This pipe cap fits onto the bomb by means of machined threads. A flange is brazed to the pipe at the point where the cap starts to tighten up, and a rubber gasket is placed between the flange and cap. Heavy vacuum grease is used between the flange and gasket and the gasket and cap. The weight of the complete bomb and it? interval volume is known before the sample is cast. In practice, a sample of about 400 grams of steel is poured into the bomb, the funnel quickly swung out of the way, the bomb cap spun down the threads and tightened against the gasket, and the bomb set in a pail of water to keep the gasket and vacuum grease cool. It is estimated that at least 80 per cent 01 the gases evolved from the liquid sample during solidification are trapped in the bomb."

Jan 1, 1945

By Henry M. Howe

This paper is a discussion of the extremely valuable one of Mathewson and Phillips, The Recrystallization of Cold-Worked Alpha Brass on Annealing,1 which not only gives us a wealth of important data reached with great intelligence, but also shows both uncommon powers of imagination and a perfectly fair spirit. Let me try to analyze some of their results, and to enunciate some of the laws to which these results point. For brevity I refer to them as "The Authors." The page numbers in parentheses refer to their paper. 1. The Visible Aspects of Recrystallization.—Plastic deformation in a single direction, as in cold-rolling, draws the grains out in that direction, that is, inequiaxes them, without destroying their apparent individuality. Each grain seems to endure the drawing out without changing either its volume or its orientation materially, for the etching tint of each grain seems to be as uniform after as before the drawing out, save for the "etch bands,"2 shown in Figs. A to D of the Authors' Plate I. As the drawn-out metal is heated progressively, on reaching a certain "disintegration temperature" these old grains seem to break up, probably into submicroscopic fragments, and this apparent disintegration is followed by a coalescence of these fragments, so that their number decreases and their size increases, till they may become very much coarser than before the drawing out. Ruder3 coarsened the grains of silicon steel in this way till single grains reached an area of 50 cm. (7.75 sq. in.). The deformation itself probably breaks each grain up into many very small fragments, but the fact that each grain continues to have a uniform etching tint different from that of its neighbors indicates that these fragments retain the initial common orientation of the grain. The apparent disintegration which we observe, then, is rather an abandonment of community of orientation for individuality of orientation, by the fragments formed earlier during the deformation. Hence we

Jan 1, 1917

By A. English, M. J. Greaves

This paper is a discussion of pelletizing systems developed over the last 15 to 20 years for the agglomeration of fine iron ore concentrates. Five different pelletizing systems are now in commercial use in the U.S., and for the purposes of comparison, estimated operating costs and capital costs for the construction of four of them are included. Capacities of existing commercial plants are examined, together with the anticipated capabilities of plants presently being built or projected. In just 21 years, the art of pelletizing iron ore concentrates has reached maturity with mastery of the separation of finely divided concentrates from low-grade iron ores and their agglomeration into pellets containing about 65% iron. This accomplishment has firmly established an improved feed for the blast furnace, with resulting benefits in faster reduction of burdens and greater economy of operation. The present production capacity of pelletizing facilities in the U.S. is about 20 million tons annually, and it is expected to double by 1970. The rapid expansion of pelletizing in the U. S. has been closely observed in European countries, notably in Sweden and Germany, where pioneer agglomerating techniques were developed early in this century. PELLETIZING PLANTS AND PROCESSES Twelve commercial pelletizing plants are presently in operation in the U. S. and Canada. An equal number are in various stages of engineering and construction, and many others are being considered. The pelletizing systems currently employed include shaft furnaces, horizontal grates using three different airflow arrangements, and grate kilns. The capacity of pelletizing operations in North America is shown in Table I. All of these plants are integrated with the mine, the ore-crushing facilities and the concentrating plant and are equipped with storage and loading-out facilities for the product. Normally, a pelletizing plant is composed of a shuttle conveyor above the receiving bins; balling equipment; a heat-hardening system including the necessary auxiliaries such as furnaces, burners and controls, ducts, fans, meters and instrumentation; fines recovery equipment; and product handling equipment. Also included are the necessary auxiliaries and utilities such as boilers or power plant; oil unloading and storage facilities; coal unloading storage, grinding and distribution facilities; and bentonite or other additive storage and distribution equipment. Shaft Furnaces: Vertical shaft furnaces used in this country are limited to the treatment of natural magnetite concentrates containing minor quantities of residual fluxing elements. Fig. 1 shows a perspective view of the shaft furnace with balling, feeding and pellet-handling equipment. An elevation of a shaft furnace is shown in Fig. 2. A commercial shaft furnace unit is about 45 ft in height with a 6 x 14-ft rectangular cross section and has a nominal production rate of approximately 50 gross tons of pellets per hour. The upper portion of the furnace shaft is constructed of fire brick as protection from the high process temperatures involved. The lower portion of the shaft is lined with abrasion-resistant brick to withstand erosion from the fired pellets. Rectangular-shaped, refractory-lined and insulated combustion chambers are situated on each side of the shaft furnace. Oil or gas is burned to produce high temperature gases which are forced into the furnace through ports located near the top of the combustion chambers. The shaft furnaces operate at a pressure of approximately 6 psi. Pellets are fed into the top of the furnace by a pantographic feeder designed to produce the desired pellet stockline. The furnace is kept filled at all times and pellets are fed and discharged from the furnace at the same rate. In early development, 10 to 12 lb of solid fuel was incorporated in the pellets. However, the main source of process heat is now derived from the combustion chamber gases. In some instances no solid fuel is used. The pellet movement in the shaft furnace is counter-current to the flow of gases. Ambient air is introduced through louvers at the lower end of the furnace, at about 6 psi, cooling the fired pellets and supplementing the heat of the high temperature gases from the combustion chamber ports. The zone of maximum temperature, located above the ports of the combus-

Jan 1, 1963

By Arnulf Muan, R. E. Johnson

Equilibrium CO2 /CO ratios of a gas phase coexisting with selected oxide phase assemblages of the system CaO-"Fe0"-SiOz and vnetallic iron have been determined at 1080°C. The data obtained are used to calculate activity-conzposition relations for metasili-cute, orthosilicate, and CaO- "FeO" solid solutions, and to determine a new value for the free energy of formation of C&S&0,. The metasilicate solution is practically ideal, whereas large deviations from ideality exist in the othe,r two solid solutions. BECAUSE of the geochemical and metallurgical importance of the oxides CaO, "FeO", and SiOz, the system CaO-"FeO"-SiO2 has been the subject of several experimental studies during the past 30 years. Following the delineation of phase relations at liquidus temperatures by a group of investigators at the Geophysical Laboratory of the Carnegie Institution of Washington in 1933,1 Chipman and associates in the early forties2,3 determined activities of FeO in liquids of this system. Since that time, many attempts have been made to interpret the data of Chipman et al. in terms of the constitution of the silicate liquids and the interaction parameters among the various constituents of the system (see for instance papers by Richardson4 and by Flood and coworkers5). One of the assumptions made in some of these interpretations4 is that the binary silicate systems CaSiO3-FeSiO3 and CazSi04-Fe2SiO4 mix ideally in the solid state. The objective of the present study is to provide experimental data on activity-com position relations in solid solutions of the system CaO-"FeO"-SiO2. Such data will contribute toward an understanding of the thermodynamics of silicate solid-solution phases in general, and will serve specifically to confirm or refute some of the assumptions made in interpreting liquid slag behavior. PREVIOUS WORK Phase relations in the system CaO-"FeO"-SiO2 in contact with metallic iron were determined by Bowen, Schairer, and Posnjak,1 and additional phase-equilibrium data for this system have been presented by Allen and snow.' A reproduction of the most up-to-date phase diagram for this system is shown in Fig. 1.7'8 Of particular interest in the present investigation are the relations among the various crystalline phases slightly below the lowest solidus temperature in the system, as shown in Fig. 2. The present work will be concerned primarily with some of the composition

Jan 1, 1968

By John W. Weeton, Donald W. Petrasek

Relatively few metal-metal systems exist that would permit the creation of fiber-metal composites consisting of mutually insoluble constituents. It is anticipated that most high strength-to-weight ratio and high -temperature fiber composites ultimately to be produced will utilize high-strength fibers embedded in a highly alloyed matrix. An investigation was conducted to determine the effect of alloying on the tensile Properties and micro-structure of tungsten-fibey-reinforced composites. Composites were made of tungsten fibers infiltrated with copper binary alloys that contain elements of varying solubility in tungsten. Room-temperature tensile tests were made on the composites, and a metallographic study of the microstructure of the fiber-metal-matrix interfaces was conducted. It was shown that, as the depth of penetration of some alloying elements into the fiber increased, a decrease in both tensile strength and ductility of the composite results. A notch effect, due to the formation of a brittle alloy zone with the tungsten fiber, was observed and gave rise to greater reductions in tensile properties and ductility behavior than would be Predicted by a law-of-mixture relation alone. In recent years, investigators have considered combining fibrous materials with relatively weak binder materials. The interest in fiber-reinforced composites results from the fact that fibers or wires may be exceedingly strong and exhibit mechanical properties superior to those of the bulk materials from which they are derived. For example, tungsten wires drawn to less than 1 mil in diameter may have strengths of over 600,000 psi,' while steel wires ranging from 10 to 3 mils in diameter may have strengths of the order of 300,000 to over 600,000 psi.2 Both metallic and ceramic whiskers are known to have very high strengths. For example, iron whiskers have been shown to have strengths of 1.9 million psi3 and sapphire whiskers have been reported to have strengths of the order of 1.7 million psi.4 If all or part of the strengths of such fibers could be retained, subsequent to the incorporation of the fibers in an engineering material, a superior material could result. In previous work done at the Lewis Research Center, McDanels, Jech, and weeton5 demonstrated the feasibility of fabricating metal-fiber—metal-matrix composites that utilized the full strengths of the fiber and matrix materials. Tungsten fibers were combined with a copper matrix by a liquid-infiltration method such that the tungsten fibers were uniaxially oriented parallel to the tensile axis of the composite. A linear relation was established that related the tensile strength of the composite with the volume percent of the fibers. Mutually insoluble constituents were selected for the study so that the strength of the composite could be quantitatively related to the strength of the individual constituents. The fact that there are only a few metals that are mutually insoluble with tungsten, e.g., copper, silver, gold, and zinc, and that these either have low melting points, high vapor pressures, or poor oxidation resistance, makes it necessary to utilize other metals that are soluble in tungsten, where high-temperature applications are ultimately contemplated. It was anticipated that, for most practical fiber-reinforced composite materials, it would be necessary to use a fiber and metallic matrix that would have varying degrees of solubility for each other. A logical extension of the earlier work was thus felt to be a study that would determine the effects of elements that had mutual solubility with the tungsten. Numerous investigators have found that tungsten fibers may be damaged by thermal treatments or contamination of the surface of the fiber by alloying elements.6-10 On the other hand, surface treatments may improve the strength of such fibers."-" Relatively little work with composites containing tungsten fibers have been reported. The work of parikh14 has shown that kinked, short-length tungsten, steel, and molybdenum fibers could str'engthen such matrices as silver, gold, and copper. Some of the combinations of fibers and matrices studied by

Jan 1, 1964

By Lysle E. Shaffer

INCREASING attention has been given in the last decade to the possibilities of mine leasing in the West. The practice as described in this article does not refer to the leasing of entire properties for corporate operation. It is intended to deal rather with the advantages and problems incident to leasing portions of properties to individuals who themselves, individually or in groups, do the actual mining and transportation of the ore. These individuals are sometimes called "leasers" and sometimes called "tributors." The contracts under which they work set up an independent relationship of lessor and leaser, between themselves and the mineowner or operator. This relationship has many advantages to both sides over those created by the ordinary relationship of employer and employe. From the standpoint of the owners there is no liability on independent contractors for industrial injuries, social security taxes, unemployment taxes, or the manifold restrictions of the Federal Labor Relations and Wage Hour Acts and similar state acts where they exist. As the leaser's income depends on the quantity and quality of ore produced, there is a distinct incentive for maximum production of a good grade of ore. This in turn promotes careful mining of the areas under lease. Ordinarily in mining, labor cost is a high percentage of the total cost of operation. Under a leasing system, even if the leasers be allowed to retain half of the gross values that they produce, and the owner or operator gets half, in the case of marginal ore bodies this is ordinarily more than the lessor would realize if the property were worked by day labor. In some instances mineral deposits under a leasing system may become ore, whereas under a day-labor system they would

Jan 1, 1948

By P. Greenfield, P. A. Beck

RECENT work by J. Darby, Jr. in this laboratory has shown that the reported vanadium-rich limit of the s phase in the Co-V system at 1200°C is in error. The appearance of a second phase in s actually is restricted to alloys containing over 68 atomic pct V. The error in the original value is due apparently to a reaction that takes place along the numerous cracks in the s specimens between the alloy and the impurities present in the He + 8 pct H atmosphere in the annealing furnace. Such a reaction and the consequent appearance of a second phase can be suppressed if the alloys are sealed under vacuum in Vycor tubing. The new value of 68 atomic pct V for the vana-dium-rich limit of the s phase in the Co-V system effects slightly the s compositions calculated from average values of N, and N,. for various s phases. The standard deviation between experimental mean compositions and those calculated from the assumption that s is characterized by a constant number of 3d + 4s electrons per atom (N,), is slightly reduced from 9.1 to 8.8 pct. The maximum divergence for the V-Mn s phase is reduced from 15.5 to 14 atomic pct. The standard deviation calculated from constant electron vacancy numbers given by N.. = 4.66 (Mo + Cr + V) + 3.2 (Mn) + 2.2(Fe) + 1.71(Co) + 1.6(Ni) is now greatly reduced, as the maximum divergence for this correlation previously occurred in the V-Co system. This maximum divergence is reduced from 7.6 to 2.3 pct, and the standard deviation for all s- phases is reduced from 4.1 to only 2.9 pct. The correlation for electron vacancy numbers given by N. 5.66 (V when with Ni or Co) + 4.88 (V when with Mn or Fe) + 4.66 (Cr + Mn) + 3.3 (Mn) + 2.66 (Fe) + 1.71 (Co) + 0.61 (Ni) is made slightly worse, and the standard deviation increases from 2.8 to 3.9 pct. These changes, however, do not affect the conclusions of the paper.' The deviation between calculated and experimental s compositions is much less for either one of the electron vacancy correlations than for the correlation with the number of 3d + 4s electrons.

Jan 1, 1955

Jan 1, 1900