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By FORTUNATO PEREIRA

(San Francisco Meeting, October, 1911.) I. GENERAL DESCRIPTION. The Department of Narino (formerly included in the Department of Cauca) is a narrow band about 170 km. (100 miles) wide in the southern part of the Republic of Colombia, FIG. 1.-SKETCH-MAP OF THE SOUTHWESTERN PART OF COLOMBIA. near the boundary of Ecuador, as shown in the sketch-map, Fig. 1. Its capital is Pasto, a small city of 25,000 inhabitants; the principal towns are Túquerres, Cumbal, Ypiales, Barbacoas, and Tumaco. The port on the Pacific ocean is Tumaco, and traffic in the interior is carried partly on the Patia river (steam navigation to the fluvial port of Barbacoas), and afterwards overland over poor roads by human bearers or on mule-back.

Aug 1, 1912

By M. S. Rashid, C. J. Altstetter

Allotropic transformations in cerium have been studied by dilatometric, resistometric, X-ray diffraction, and metallographic techniques. The dilatometric study indicated that, on cooling below O°C, the high-temperature fcc phase, y, transforms partly to the hexagonal phase, ß, and, on further cooling, to the collapsed fcc phase, a. The amount of $ phase present at room temperature is increased by repeated cycling through the a-y transformation. It has been shown metallograPhically that the y-ß transformation has many characteristics of a martensitic transformation. In contrast to the y-ß transformation the ?-a transformation does not give the manifestation of a shear transformation. Small cellular ? domains of random shape and size collapse to a in a short time with no apparent coordination with neighboring domains. The considerable confusion in the literature over the existence of more than one high-temperature fcc phase is discussed. Two such phases have been reported in the literature and an attempt is made in this study to clarify the situation. Twelve fcc and two hcp structures have been shown to be easily reproduced or eliminated. It is proposed that the two "additional" allotropes reported in the literature and fourteen of the phases detected here are not allotropes of cerium but are due to contamination. CERIUM exists in several allotropic forms, but there is some disagreement over what the forms are. Furthermore, the conditions favoring the presence of a particular allotrope and the nature of the transformations from one form to another are uncertain. The objectives of this research were 1) to ascertain the allotropic forms of cerium, 2) to establish the conditions under which the allotropes exist, 3) to study the effects of annealing and thermal cycling on the allotropic transformations, and 4) to study the transformation mechanisms. Dilatometric, resistometric, metallographic, and X-ray diffraction techniques were employed. The form of cerium commonly found at room temperature is fcc and is designated ?. A complex hexagonal phase, 8, forms when y is cooled to slightly below room temperature. At still lower temperatures the y fcc structure transforms to an fcc form with a much smaller lattice parameter, termed a cerium. A bcc form, 6, which exists just below the melting point (800°C), will not be considered further in this work. There is a substantial body of experimental evidence (reviewed by Gschneidnerl) which favors the acceptance of these four allotropes, though some investigators have tried unsuccessfully to observe the ß hexagonal form.'-' There is disagreement, however, over the phase-transformation temperatures, due, in part, to broad hysteresis and overlapping of the transformations between the a, ß, and ? forms. The transformations are also sensitive to prior thermal and mechanical treatment. The differing purity of cerium used by different investigators is undoubtedly a factor. Cerium is difficult to separate from other elements and is quite reactive, igniting spontaneously when it is filed in air. The highest purity of cerium to date is reported to contain several hundred parts per million by weight of impurities, and early investigations were carried out on cerium containing several percent of impurities. There have been reports of more than one fcc allotrope at room temperature. Gschneidner, Elliott, and McDonald5 obtained diffraction patterns of an fcc phase with a lattice parameter about 1 pct less than that of the ? phase, instead of the y phase, on slowly cooling cerium filings from 23° to -198°C and warming them back to room temperature. However, when the sample was heated to 447°C and cooled to room temperature it consisted of only the ? phase. They have designated this new fcc phase "a-? intermediate", and say it is quite sensitive to impurities. After prolonged high-temperature treatment of a powder specimen, Weiner and Raynor2 obtained a diffraction pattern of an fcc phase of lattice parameter about 1 pct less than the ? phase. This they called the y' phase. It could not be reconverted to the y phase and is claimed to be different from the a-? intermediate phase.5,6 Dialer and Rothe3 reported two fcc phases* after cycling their powder specimens between room temperature and -192°C. Gschneidner, Elliott, and McDonald5 suggested that one of the fcc structures obtained by Dialer and Rothe was equivalent to their "a-? intermediate" phase. Table I presents some pertinent data on the proposed allotropes. For the ?(fcc)-ß(hexagonal) transformation

Jan 1, 1967

By C. P. Miller

In order to determine the usefulness of geochemical and biogeochemical prospecting for nickel, ten localities representing several types of nickel occurrences were selected as sites from which to collect plant and soil samples. This report covers the investigations in two of the areas. After a brief geologic description of the areas, the author presents details of the experimental tests and resulting data. Conclusions drawn from the studies led to several general guides for further prospecting. In a study of the usefulness of geochemical and biogeochemical prospecting for nickel made about three years ago, approximately ten localities, representing several different types of nickel occurrences, were sampled and about 1500 samples of plant and soil were collected. This report will cover briefly the data and results for two areas, and a summary of guides for prospecting. DESCRIPTION OF AREAS SAMPLED One locality is the Red Flats nickel prospect in Curry County, Ore., about six miles southeast of Goldbeach, and the other is the Little Rocky Creek prospect in Stillwater County, southcentral Montana, just southeast of the Benbow chromite mine. The Oregon area is a lateritic-type nickel deposit formed on a nickel-rich serpentinite peridotite complex, similar to the Josephine intrusion in southwestern Oregon. The Montana area is a nickel prospect in norite, peridotite, and related rocks of the Stillwater igneous complex. The Stillwater complex is a series of layered basic and ultrabasic rocks, with a layer of norite-gabbro at the base and a series of peridotites and gabbros above. The nickel in the Oregon deposit occurs in both the peridotite and the overlying soil. A deep lateritic soil is developed locally on the peridotite and serpentinite and constitutes the ore. The average nickel content of the lateritic soil is less than 1 pct, whereas the nickel content of the weathered peridotite is about 1 to 1.5 pct. The nickel occurs as garnierite (Mg, Fe, Ni, Mn)3 (OH)4 (SiA1)2O5 in the soil and in the olivine and pyroxene in the peridotite where it probably substitutes for Fe2+ or Mg2+ in the silicate lattices. Nickel is found in three distinct ways in the Still-water rocks: 1) it is in the olivine and pyroxene minerals in norite, harzburgite, etc.; 2) it occurs as widely disseminated grains of pentlandite-pyr-rhotite, which tend to be concentrated in the lower norite band; and 3) it occurs as discrete bodies of pentlandite-pyrrhotite and chalcopyrite which are localized in the norite zone, close to the contact with the underlying rocks. The nickel content of the norite is probably less than 1 pct, and the nickel content of the pods and lenses within the norite is about 1 pct. PROSPECTING APPROACH Although the areas are different geologically, the approach in prospecting them is fundamentally the same. The procedure is twofold: 1) a rapid reconnaissance survey to outline an area of high nickel content, and 2) a more detailed survey to outline zones of possible ore grade within the area of high nickel. The possible ore at Red Flats is concentrated in the lateritic soil, whereas at Little Rocky Creek it is in the sulfide pods. Both types are surrounded by an area of relatively high nickel content. CHEMICAL ANALYSIS Chemical analyses of nickel were made by a di-methylglyoxime colorimetric test, similar to the standard test for nickel, utilizing concentrated sul-furic acid for extraction. The lower limit of detection for nickel in soil by the method used was about 10 ppm and for nickel in plants about 5 ppm. The relative deviation was about 25 pct. SOIL PROSPECTING General Statements: A summary of the approximate average parts per million of nickel in soil, as compiled from the literature and from my study, is given in Table I. Selected references are given at the end of the paper. Few of the investigators reported the type of extraction or analysis, so the data given may not be strictly comparable to mine, which were made with a sulfuric acid extraction. Any nickel concentration greater than these average values might be considered anomalous, although each area must be studied in relation to the surrounding rocks. Method of Soil Sampling: The soil samples were taken in a zone from 1 in. to 1 ft below the humus layer, and within a 15-ft radius around a station.

Jan 1, 1961

By R. M. Brick

SEGREGATION can occur only in cast alloys that solidify over a range of temperatures with a difference in composition of liquid and solid phases within this range (ignoring monotectic systems and chemical reactions as in rimming. steels). Thus a pure binary eutectic alloy should show no segregation unless undercooling occurs for one of the solid constituents of the eutectic; e.g., chill-cast Al-12 per cent Si alloys. The phasial condition implicitly described above-solidification over a range of temperatures with a compositional difference between solid. and liquid-is found in nearly all solid solutions or combinations of solid solutions and eutectics. Metastable conditions of solidification of these types of alloys cause coring; i.e., a difference in composition between the center of a dendrite and its periphery. This composition gradient can be detected usually only by microscopic examination of etched structures; it is a "micro" effect. The gradient of more immediate industrial concern is that between the center of a cast section and the surface layers. This gross (macro) effect is usually determinable only by sampling of the casting at different points, with chemical analyses of each sample. If the compositional difference is of the same type as in coring, the first parts to freeze being enriched in higher-melting-point constituents, and vice versa, the effect is called normal segregation. When what is apparently the first part of the casting to solidify shows a higher concentration of low-melting-point constituents, the effect is called inverse segregation. These macro effects are quite separate from the micro effect, coring, yet the latter must be. described first because it is an essential part of the picture. CORING Solid Solution, Ni-Cu The nickel-copper phase diagram is reproduced in Fig. Ia, in which the solid lines represent the equilibrium liquidus 1, 3, 7 and solidus 2, 5, 8, and where the vertical 1, 4, 8 represents a 55 per cent Cu alloy. Upon moderately rapid solidification, the first dendritic axes of composition 2 (see Fig. 1b) start to form at a temperature somewhat under I. Solidification continues by growth of the dendritic nuclei, but at temperature 4 the increment solidifying is of composition 5. The rapidity of this crystal growth prevents diffusion of nickel and copper atoms from adjusting the composition of the entire dendrite at 5, which it would be under equilibrium conditions. The average composition of a specific dendrite, or the entire solid phase, at temperature 4 might be that indicated

Jan 1, 1944

NEW MEMBERS The following list comprises the names of those persons who became members during the period of Apr. 10, 1917, to May 10, 1917. ANDERSON, GEORGE K., JR., Supt., Iron Ore Mines, The Low Moor Iron Co. of Va., Longdale, Va. AVERY, DAVID, Met Collins House, Collins St., Melbourne, Vic., Australia. BATES WILLIAM T., Shift Foreman, American Zinc Co. of Tenn., Mascot, Tenn. BIRD, ELMER, Min. & Civil Engr P. O. Box 1483, Boise, Idaho. BLACKBURN, JOSEPH R., Vice-Pres. & Genl. Mgr., Austen Coal & Coke Co., Austen, Preston Co., W. Va. BOTSFORD, FRANK P., Asst. Genl. Supt., Eastern Mesaba, Pickands Mather & Co., Gilbert, St. Luis Co., Minn. BRADEN, SPRUILLE, Min. Engr., Andes Exploration Co. of Maine, Casilla 83-D, Santiago, Chile South America. BROWNE, DAVID G., Mill Designer, New Jersey Zinc Co., 55 Wall St., New York, N. Y. BRUDERLIN, EMIL J., Met. Engr., Ohio & Colorado Smelt. & Ref. Co., Salida, Colo. CAMPBELL, DONALD C., Min. Engr., Campbell Wells & Elmendorf, 114 James St., Seattle, Wash. CARRIGAN, J. J., Asst. Genl. Supt. of Mines, Anaconda Copper Min. Co., Butte, Mont.

Jan 6, 1917

By Arthur L. Christenson, Clarence E. Jackson

In the establishment of the relationship between weldability and hardenability, two methods have been employed in correcting for the grain growth produced in the heat-affected zone: first, the hardenability calculated from chemical composition* may be corrected to the grain size observed in an actual weld? or, second, a hardenability test may be made on the steel quenched from a temperature high enough to produce a grain size comparable to that found in the heat-affected zone.8 In order to obtain grain sizes in the end-quench hardenability bar comparable to those resulting in the base metal from the welding cycle, a quenching temperature of 2Ioo°F. has been used. In studies of the end-quench hardenability specimen quenched from 2Ioo°F. instead of from a lower temperature of I7OO°F., it is impor-TaiiT to ascertain The relative cooling rates for various distances along the bar. It is a question as to whether the cooling occurs at the same rate or whether there is any significant difference from the standard cooling-rate curve published by Jominy and confirmed by others.4,5 This paper reports experimental evidence concerning the effect of quenching temperature on the cooling rates in the end-quench hardenability test. The effect of quenching temperatures on cooling rates has been studied by a number of investigators.6'7 French has considered this effect from both theoretical and experimental aspects. In French's studies on complete quenching of spheres and rounds, an increase in the quenching temperature caused an increase in the cooling rate at 720°C. at the center of the specimen. The center cooling velocity also has been shown to be dependent upon the surface per unit volume for the type of specimens studied; the velocity of cooling increases with an increase in the surface per unit volume. Three methods of indicating the rapidity of cooling of a body of metal during a quenching operation have been propped: I. The time it takes for the metal to cool from the quenching temperature to a temperature halfway between the quenching temperature and the temperature of the quenching medium (half-temperature time): Grossmann, Asimow and Urban7 justify the use of this criterion by the fact that the half-temperature time includes the temperature and time of incubation as well as the zone of formation of pearlite and, further, the data so derived accord very closely with experimental values. 2. The time interval the metal remains in a given temperature range; for example,

Jan 1, 1944

By Arthur L. Christenson, Clarence E. Jackson

In the establishment of the relationship between weldability and hardenability, two methods have been employed in correcting for the grain growth produced in the heat-affected zone: first, the hardenability calculated from chemical composition* may be corrected to the grain size observed in an actual weld? or, second, a hardenability test may be made on the steel quenched from a temperature high enough to produce a grain size comparable to that found in the heat-affected zone.8 In order to obtain grain sizes in the end-quench hardenability bar comparable to those resulting in the base metal from the welding cycle, a quenching temperature of 2Ioo°F. has been used. In studies of the end-quench hardenability specimen quenched from 2Ioo°F. instead of from a lower temperature of I7OO°F., it is impor-TaiiT to ascertain The relative cooling rates for various distances along the bar. It is a question as to whether the cooling occurs at the same rate or whether there is any significant difference from the standard cooling-rate curve published by Jominy and confirmed by others.4,5 This paper reports experimental evidence concerning the effect of quenching temperature on the cooling rates in the end-quench hardenability test. The effect of quenching temperatures on cooling rates has been studied by a number of investigators.6'7 French has considered this effect from both theoretical and experimental aspects. In French's studies on complete quenching of spheres and rounds, an increase in the quenching temperature caused an increase in the cooling rate at 720°C. at the center of the specimen. The center cooling velocity also has been shown to be dependent upon the surface per unit volume for the type of specimens studied; the velocity of cooling increases with an increase in the surface per unit volume. Three methods of indicating the rapidity of cooling of a body of metal during a quenching operation have been propped: I. The time it takes for the metal to cool from the quenching temperature to a temperature halfway between the quenching temperature and the temperature of the quenching medium (half-temperature time): Grossmann, Asimow and Urban7 justify the use of this criterion by the fact that the half-temperature time includes the temperature and time of incubation as well as the zone of formation of pearlite and, further, the data so derived accord very closely with experimental values. 2. The time interval the metal remains in a given temperature range; for example,

Jan 1, 1944

By E. E. Schumacher

IN a laboratory devoted to the furtherance of the science of communication, the breadth and variety of the problems encountered are challenging to a metallurgist. In my own long association with the Bell Telephone Laboratories, our metallurgical group has dealt with a vast number of alloys, both ferrous and nonferrous, and with many materials in the border range of metallic properties., The objectives of our design engineers embrace every phase of telephony, and the properties they desire in metals are generally unusual, frequently unique, and often conflicting. Commercial alloys have not always been available with properties to meet a special requirement in the telephone plant, and many alloys have had, therefore, to be custom-made. Anyone who has had the opportunity to observe the results of tests of all types on numerous such alloys, both commercially and specially produced, or who has taken part in the development of an alloy of some necessary, but new or unusual combination of properties, could not fail to be impressed by the frequency with which a desired goal has been reached or adequately approached through the presence of decimal quantities of alloying elements. Nor could One fail to be struck by the occasions when, conversely, of a minute amount Of impurity element has rendered an alloy useful. It is no exaggeration to state that the content be- hind the decimal point often spells success or fail-ure, and the critical content is sometimes far to the right of the decimal point as I shall later illustrate. The great effects of small additions have long been recognized and have, in fact, been described by many investigators. The importance of the minute, however, cannot be overemphasized. Therefore, in this discussion, I propose to illustrate for you some of the startling instances, drawn primarily from our own experiences, wherein small, even vanishingly small, proportions of stranger elements in otherwise common aggregates have com-pletely changed the customary pattern of behavior. No one property has a monopoly as to being dis-proportionately affected by minor elements. Nearly all properties are affected, but there is time here to include only a selected few. I have chosen, there-fore, three of general interest: strength, magnetic, and electrical properties. I shall inquire into both the mechanisms and consequences of these disproportionate effects and try to share with you the fascination and challenge of this field. Strength Properties of Lead and Lead Alloys To illustrate the effect of the minute on strength properties I have selected lead and its alloys, with which we have worked extensively for many years. Lead has the advantages of being available in quantity in a state of high purity and of being fairly easy to melt and fabricate without contamination to any extent detectable by the spectrograph. It has the interesting disadvantages of recovery and recrystallization at room temperature. Whether I

Jan 1, 1951

By W. F. Chiao, R. B. Gordon

Tile sharp-yield point found in magnesium crystals in the solulion-treated and aged condition is studied by dislocation internal-friction experiments. The results show that the sharp yield is not file to the sudden release of pinned dislocations hut is movc likely due to the rapid multiplication of an initially small number of dislocations. Recovery or the dislocation internal friction after deformation is also studied. This yecovery results from the re-pinning of dislocations by a solute, presumably nitrogen, which moves with a relatively small activation energy. SHARP-yield points, when they occur, are a striking feature of the stress-strain curve generated during a tensile test. Although commonly associated with steel, sharp yielding has been found in a variety of metallic and nonmetallic crystalline materials. In particular, sharp-yield points have been found in zinc"' and cadmium3 containing nitrogen. With this background, Geiselman and Guy4 investigated the tensile properties of magnesium single crystals containing nitrogen to see if sharp yielding also occurs in this system. They found that sharp yields did indeed occur in solution-treated and aged specimens tested at elevated temperature but were not able to give conclusive proof that the sharp yield was caused by nitrogen, a yield drop being observed even in their purest crystals. Sharp-yield points have also been found in various polycrystalline magnesium alloys.7'8 In the study of the sharp-yield phenomenon it is desired to observe the behavior of dislocations in the earliest stages of the deformation process. Internal-friction experiments are useful for this purpose because dislocation damping is sensitive to the mobility of free-dislocation segments. At low strain amplitudes the damping, A, due to the the forced vibration of dislocation segments of average length L is ? =KAL4 [1] where A is the dislocation density and K, if the applied frequency is well below the resonant frequency of the dislocation segments? is a constant for the sample under observation.5 Dislocation damping, because of the fourth-power dependence on L, is particularly sensitive to the creation of free-dislocation segments during deformation. Since sharp yielding is associated with the sudden release of pinned-dislocation segments, marked changes in the dislocation damping are expected at the yield point.6 The use of the dislocation-damping observations to help elucidate the incompletely understood mechanism of yielding in magnesium is the primary objective of the experiments reported here. PROCEDURE Many investigations have shown that very marked and rapid changes occur in the dislocation damping of of a deformed material as soon as the straining is stopped.5 It was quite essential, then, for the purpose of this investigation, to make the damping measurements during the deformation of the samples. This can only be accomplished through the use of the ultrasonic-pulse method. In this method traveling sound-wave pulses are used and, in contrast to resonating-bar methods, only the sample ends are set in vibration. Thus, the sample can be gripped along its sides in the tensile-test machine without disturbing the damping measurements. In the pulse method, the decrease in the amplitude of a sound pulse is measured as it travels back and forth through the sample. If A is the amplitude after traversing a distance x and A. is the initial amplitude, A=Aoe-ax [2] and a is called the attenuation. It is commonly measured either in units of cm-I or as db per µ sec. The observed attenuation in a metal sample is due to a number of causes. These include scattering by grain boundaries and impurity particles, thermo-elastic damping, diffraction effects, stress-induced ordering of solute atoms, and dislocation damping. The total observed attenuation in a given sample usually cannot be resolved into these various components, but changes in a due solely to changes in dislocation damping can be accurately determined, provided the experiment is arranged so that all other sources of damping are held constant. It is desired to reduce the extraneous sources of attenuation to a minimum and for this reason the experiments are done on single crystals of high purity. Magnesium crystals offer the further advantage that, when properly oriented, only a single set of slip planes is active during deformation. Crystal Preparation. The method of sample preparation is similar to that of Geiselman and Guy.4 The starting material was high-purity, sublimed magnesium rod supplied by the Dow Chemical Co. Melting under Dow 310 flux was used to reduce the nitrogen content of the starting material: the fluxing was done under an argon atmosphere and the

Jan 1, 1965

By H. O. Hofman

PAGE I. Introductory,.......... 258 11. Condensed Account of Past and Present Plants,. .. 259 111. The Ores. Table I., Average Analyses,..... IV. Metallurgical Treatment—Roasting OF Ores,... The Allen-O'Hara Furnace,....... The Wethey Furnace,........272 The Pearee Turret-Furnaces,....... 273 The MacDougall Furnace,.......275 Original MacDougall,.......276 Herreshoff,......... Evans-Klepetko,........ General Results (Table II.),.......282 V. Smelting Ores in The Blast-Furnace,...,. Table 111. Examples of Montana Blast-Furnace Smelting,. 284 Table IV. Analyses of Coke and Coke-Ash,. .. . VI. Smelting Ores in the ReveRberatory Matting-Furnace,. 289 Table V. Percentage of Components of Charge,. .. 290 Table VI. Analyses of Flue-Dust and Briquettes,. .. Table VII. Examples of Montana Reverberatory-Smelting,. 292 Table VIII. Analyses of Coals,...... Table IX. Analyses of Producer-Coal and Ash,. .. Details of Practice,........297 VII. Converting Coppr-Matte,....... 302 Table X. Analyses of Materials of Converter-Linings,. . 306 Table XI. Montana Converters,......308 Yield of Metal..........308 VIII. Electrolytic Refining of Copper,..... Refining of Cathodes,........ 313 Table XII. Details of Electrolytic Refineries,. .. . Table XIII. Efficiency of Some Rocky Mountain Coals,. . 316 I. Introductory. In 1901,* this country produced 268,782 long tons of fine copper. Of this total, Montana is credited with 102,621 long tons, or 38.2 per cent.

Jan 1, 1904

By A. H. Larson, L. G. Twidwell

The influence which Au, Ag, Sb, Bi, Sn, and Cu have, both individually and collectively, on the activity coefficient of sulfur in liquid lead at 600"C zuas studied by circulating a H2S-Hz gas wlixture over a specific lead alloy until equilibrium was attained. Subsequently, the H2S concentration in the equilibrium gas mixture and sulfur concentration in the condensed phase were deterruined. The elements gold, silver, and antinzony (above 8 at. pct) increased the activity coefficient of sulfur. Bismuth had no apparent effect. Tin (above 3 at. pct) and copper decreased the coefficient. The influence of an individual element, i, on sulfur is best reported as the interaction parameter, riS, which is defined as The values o these first-order interaction zus are: ESzu = —55.0. These interaction parameters are used to predict the activity coefficient of sulfur in six fouv-component alloys and one seven-component alloy. Comparisons are made with direct experimental determinations. INTERACTIONS in dilute solution have been studied by many investigators. Most of the experimental work has been confined to solute-solvent interactions in simple binary systems and solute-solute interactions in ternary systems. Dealy and pehlke"~ have summarized the available literature on activity coefficients at infinite dilution in nonferrous binary alloys and have calculated from published data the values for interaction parameters in dilute nonferrous alloys. Interaction parameters are a convenient means of summarizing the effect of one solute species on another in a given solvent. Only a few investigators have studied interactions of the nonmetallic element sulfur in a metallic solvent. They are as follows: Rosenqvist,~ sulfur in silver; Rosenqvist and Cox,4 sulfur in steel; chipman, sulfur in alloy steels; Alcock and Richardson,% ulfur in copper alloys; Cheng and Alcock,' sulfur in iron, cobalt, and nickel; Cheng and ~lcock,' sulfur in lead and tin. The only reported work on the Pb-S system in the dilute-solution region is that of Cheng and Alcock.' Their investigation involved a study of the solubility of sulfur in liquid lead over the temperature range 500" to 680°C. The results may be summarized by the following relationship: S (dissolved in lead) + Pb(1) = PbS(s) log at. %S = -3388/T + 3.511 Experimentally, it was found that Henry's law was valid up to the solubility limit of sulfur in lead, i.e., at 600°C up to 0.43 pct. Their investigation did not include the study of sulfur in lead alloys. More accurate calculations could be made in smelting and refining systems if activity coefficients of solute species could be accurately predicted in complex solutions. One of the objectives of this study was to compare the experimental data with the values calculated from the equations derived from models for dilute solutions proposed by wagner9 and Alcock and Richardson. A temperature of 600°C was chosen as the experimental temperature to attain reasonable reaction rates and to minimize volatilization of the condensed phase. EXPERIMENTAL Materials. The Pb, Au, Ag, Sb, Bi, Sn, and Cu used for preparation of the alloys were American Smelting and Refining Co. research-grade materials. All were 99.999+ pct purity except the antimony and tin which were 99.99+ pct. The initial alloys prepared for this study consisted of twenty-one binary alloys, eleven ternary alloys, and one six-component alloy. The constituent elements were mixed for each desired alloy and were placed in a crucible machined from spectrographically pure graphite. The crucible was placed in a vycor tube which was evacuated with a vacuum pump and gettered by titanium sponge at 800°C for 8 to 12 hr. After the gettering was completed, the chamber containing the titanium was sealed and removed. The remaining sample chamber was placed in a tube furnace at 800°C for 2 hr and quenched in cold water. The final operation consisted of homogenization of the alloy for 1 to 2 weeks at a temperature just below the solidus for the individual system. The resulting master alloys were sectioned into small pieces and a random choice made for individual equilibrations. Cobalt sulfide (Cogs8) used to control the gas atmosphere in the circulation system was prepared by passing dried HzS for 24 hr over a Co-S mixture heated to 700°C in a tube furnace. This material was then mixed with cobalt metal to give a two-phase mixture which, when heated in hydrogen to a particular temperature, produced a desired H2S/H2 gas atmosphere in the circulation system. A Cu2S-Cu mixture also used in this study was prepared in a comparable manner. Apparatus for Equilibrium Measurements. The experimental technique of this study required apparatus

Jan 1, 1967

By C. A. Shook, W. H. W. Husband, D. B. Haas

Although previous studies l,2,3 have been made, no correlations for pressure drop have been proposed. This is probably because severe particle breakage occurred and pressure drops changed substantially with time. A quantitative statement of the relationship of pressure drop to the parameters of the system is desirable for lignite since, unlike higher rank coals, lignite slurries are thixotropic. The present investigation was undertaken to quantify the pipeline behavior and required continuous monitoring of pressure drop and size distribution.

Jan 2, 1979

By J. Chipman, J. B. Gero, T. B. Winkler

IN the basic open hearth process the reaction of manganese in the bath with iron oxide in the slag attains a condition very closely approximating true equilibrium, and the distribution of manganese between slag and metal during the refining period is determined by the factors which control this equilibrium condition. For this reason a number of investigators have studied this reaction both in the laboratory and under various conditions of furnace operation. The principle reaction and its equilibrium constant are: FeO (in slag) + Mn = MnO (in slag) + Fe (liq.) [1] (MnO) .= (FeO),[%Mn] The symbols in parentheses represent activities of the two oxides in the slag which, in the simple slags consisting almost wholly of the two oxides, may be assumed equal to the respective mol fractions. The symbol (FeO)r is used to denote the total iron oxide computed as FeO; or it is the sum of the mol fraction of FeO plus twice that of Fe2O3. Early attempts to obtain laboratory data on this reaction suffered from failure to appreciate the great speed of the reaction. When slag and metal are cooled slowly together, the equilibrium shifts with temperature and the final compositions correspond to equilibrium at the freezing point rather than at bath temperature. The early work of Oberhoffer and Schenck¹ and of Tammann and Oelsen² apparently suffered from this source of error. In most of the other published laboratory investigationsa. '.' this error was not present but other uncertainties have existed, notably dependence upon optical temperature measurements and exposure to atmospheric oxidation.

Jan 1, 1951

By H. W. Bell

There was considerable prospecting for new supplies of oil in Arkansas during the past year, regardless of the overproduction affecting the industry throughout the country. Justification for this new work was not lacking, as the local markets more than threatened to absorb a declining production. There were, however, no important new discoveries in the state during 1929. The McDonald area in sec. 2515, S.-18 W., threatened to expand into a major producing area. Oil showings had been encountered here in wells drilled by the McDonald Oil Corpn. as early as the fall of 1928. In July, 1929, an initial production of 1000 bbl. of 32" oil was obtained in McDonald Bros. B-3 Wilson, from a sand at 2780 to 2786 ft., which is about 80 ft. higher than the sand previously tested in the neighboring wells. This production declined rapidly. At the end of the year there were six producers making about 200 bbl. per day total. Seven dry holes have temporarily stopped development in that area. The showing of B-3 was sufficient to cause considerable leasing activity. The area lies several miles west of the Louann portion of the Smackover field. The discovery well went to 2873 ft. and found Glen Rose lime in bottom. The age of the producing sand is in doubt; it seems closely related to the Tokio sand. During 1929, several paying wells were brought in, as a northeastern extension to the Smackover Heavy area, in sec. 34 and 35-15-15, from the Nacatoch sand. Over 20 new wells were drilled and resulted in at least 1500 bbl. production. The down-dip or off-structure territory contiguous to the Smackover uplift was further tested at various locations with the usual results; that is, a showing of "salt water gas," which soon blew off and in some cases a slight showing of oil. These gas showings, found further down the dip than oil, are the results of the ability of water to take gas into solution at the rate of about 3 per cent. by volume at atmospheric pressure and proportionally larger quantities, if available, at higher pressures (measured on the absolute scale). During the year no off-structure wrinkles sufficient to trap conlmercial quantities of oil have been found outside of the other known fields of

Jan 1, 1930

By H. Bartholomew, L. Bernstein

Experirmental bonds of Ag-In SLID to gold, copper, nickel, Kovar, Dumet, nickel-plated molybdenum, ALL-Pt vrzetallizing on ceramic, and nickel-plated Mo-Ti metallizing on Al2O3 ceramic have been made and exalnined. Metallographic taper sections were made of all bonds for Phase identification. In addition, failuve temperatltres were determined for bonds heated undev shear load. Sowe bonds were subjected to electvon-probe microanalysis. The ternary SLID system Ag-In-Sn was similarly evaluated. Plwtonticrogaphs and electron-probe data are discussed and related to over-all phase diagrams , diffusion effects, and wetting properties of the liquid. The rates of diffusion andor compound formation of gold, silver, and copper in indium and In-Sn liquids are found to descend in that order, as measured by the relatzve thickness of phase layers in the interfaces of bonds made at 200to 400°C. It is concluded that the SLID process enables one to produce bonds which are stable at high temperatures, after having been fabricated at low temperatures, and meet most requirements for application in interconnection, silicon bonding, or hermetic sealing of electronic devices. In a previous publication by one of the authors, the theory and principle of SLID bonding in simple binary systems was discussed. SLID bonding can be defined as a joining process using a preform with a laminated structure: a low-melting material clad on a high-melting core. During the bonding cycle a metallurgical transformation occurs such that the resultant structure can withstand, without reliquefying, temperatures higher than those at which the bond was made. The phases present in the joint interface region are high-melting compounds or, if equilibrium is reached, solid solution. Properties will depend on the phases present, ultimately approaching those of the solid substrate core of the SLID preform. The high-temperature strength of bonds made in these systems was correlated to phase identification in the interfacial bond regions from metallographic cross sections and electron-probe X-ray microanalysis data. When complex electronic components are assembled, multiphase systems result at the interfaces of bond regions. In these ternary and higher-order systems very little diffusion and phase-diagram data is available with which to predict the nature of the interfacia1 region that will result from conventional fabrication processes and subsequent field use of the component. Clarke and Rhines did early work in the field using the Al-Mg-Zn system as a vehicle. Guy and co-workers studied a portion of the Cu-Zn-Ni system and some mathematical4 and general5 aspects of multiphase diffusion. irkald' and coworkerse recently studied diffusion in the Cu-Zn-Sn system. No diffusion studies have been made on ternary systems directly applicable to this investigation but some phase diagrams are available: g-u-n, u-i-n, and CU-i-n. I) DESCRIPTION AND EXPERIMENTAL PROCEDURE The elements Au, Ag, Cu, Ni, In, and Sn are found in alloy systems commonly used in fabricating and assembling electronic components. Reference to the appropriate phase diagrams9 and the previous publication will indicate that the binary systems of any of the two low-melting elements, indium and tin, with any one of the other four higher-melting elements are capable of producing SLID bonds. It is not unreasonable to assume that any ternary or higher-order alloy system containing at least one of the elements gold, silver, copper, or nickel and one or both of the elements indium and tin could be used to produce bonds which are stable at high temperatures, after having been fabricated at low temperatures. Indeed, the liquidus contours and isothermal sections of those phase diagrams available7 do so indicate. The parameters affecting the bond and the equipment used in evaluating the bond were described in an earlier paper.' The current investigation used the

Jan 1, 1967

By H. T. Green, R. M. Brick

True stress-strain data on alloys of pure iron with up to 2.4 pct Al were obtained in the temperature range +100° to —185°C. Alumi-num was found to reduce yield and flow stresses of iron at low temperatures but to have little or no effect on ductility. The effects of temperature and composition on strain hardening are discussed. SEVERAL independent studies of the behavior of high purity iron binary alloys at low temperatures are now in progress in attempts to evaluate systematically the variables affecting the low temperature brittleness of ferritic steels. This paper reports the results of one such investigation in which the tensile properties of aluminum and aluminum plus silicon ferrites were measured from 100" to —192°C. True stress-natural strain data have been obtained in order to evaluate as many as possible of the parameters which describe the behavior of the materials involved. In comparable studies at the National Physical Laboratory in England, iron and iron alloys of high purity have been produced' and tested at subat-mospheric temperatures.' True stress-natural strain curves were obtained there also. The purest iron contained 0.0025 pct C and 0.001 pct O and N. Even this, as normalized at 950°C following hot rolling, showed little ductility at -196°C. The grain size was ASTM No. 3, and the room-temperature yield strength was 17,800 psi (which seems too high for pure iron). Some of the NPL irons contained considerably more oxygen and demonstrated intergran-ular fracture at —196°C. The authors2 carefully differentiated between intergranular fractures associated with excessive oxygen content and transcrys-talline cleavage with little ductility encountered at —196°C in the purer material. The cleavage stress was half again as great as that associated with inter-granular fracture. Test Material, Preparation, and Procedures Of a number of Fe-A1 alloys produced, eight were considered to be sufficiently pure for testing. Partial chemical analyses (Table I), low observed yield points, and high ductilities indicate these alloys to be comparatively pure for vacuum-melted irons of sizable ingots, 5 Ib or more. To produce the binary Fe-A1 alloys, electrolytic iron was melted in air, cast into slabs, and rolled to strips 0.010 in. thick. These strips, joined into a continuous ribbon and wound into 2 1/2 in. diameter spools, were subjected for four weeks to a moving atmosphere of purified dry hydrogen in a stainless-steel tube at 1050" to 1150°C. Charges of these spools were melted in beryllia crucibles under good vacuums (1 micron), and aluminum (99.97 pct Al) was added to the melts. Compositions of these alloys are recorded in Table I. The ingots were hot forged and then cold rolled at least 65 pct to 3/8 in. rods which were vacuum annealed to the desired grain size, approximately ASTM No. 4, prior to machining into tensile test bars. All tensile specimens had gage sections 1 in. long, with a fillet of 1.5 in. radius to the shoulder. Gage diameters were 0.250 in, except for a few rods where additional cold work required use of a 0.200 in. gage section. After machining, 0.002 in. was removed from the gage diameter using 240, 400, and 600-grit metallo-graphic papers. The final polish with 600 grit left the fine scratches running in the longitudinal direction. By this means, surface metal strained during machining was removed. A few specimens heat treated after machining were similarly reduced 0.004 in. to remove any material affected chemically by the atmosphere during heat treatments, as is discussed in a later section. Tensile tests of the eight alloys at constant temperatures from +100° to —185°C were performed in apparatus which has been described." The essentials include a double-walled insulated metal vessel which contained the liquid heat-transfer medium surrounding the test specimen. A constant temperature was maintained by means of a pyrometer which regulated the pressure of dry air driving liquid air through a copper coil. Temperature variation was less than ±2°C during a specific test. For axial straining, two lengths of case-hardened chain, terminating in simple shackles, loaded the specimen through threaded grips. The lower grip bar passed through a hole in the bottom of the test vessel to which it was joined by a thin-walled

Jan 1, 1955

By J. B. Newkirk, A. H. Geisler

Certain of the permanent magnet alloys provide ideal systems for the study of the kinetics of the precipitation reaction and the correlation of structure with properties. One such system, Cu-Ni-Fe, was found by Bradley1,2 to exhibit a coherent transition state in the precipitation process analogous to that reported for Al-Cu alloys somewhat earlier.3 The attractiveness of some perrnanent magnet alloys for study lies in the fact that vertical sections of the ternary phase diagram in certain regions of composition (Fig I) have as their prototype the binary Ni-Au diagram. Alloys of this type decompose into products that have the same crystal lattice type but only slightly different lattice parameters. The advantages that such alloy systems oA&apos;er for study over the usual in which an intermetallic compound is formed are many: 1. Since the precipitate has the same crystal strutture as the matrix, complex atomic movements are not required to form the new lattice. 2. Similarly, complex orientation relationships are not involved for both the matrix and the precipitate would be ex. petted to have the same orientation. 3, Small &,registry of the decomposition products at equilibrium (in contrast with Cu-Ag alloys) is conducive to extensive coherent growth in the transient state and thus the transition lattice can be detected by the usual X ray diffraction methods. 4. Finally, the relative quantities of precipitate and depleted matrix can be varied from 0 to 100 pet* thus permitting wide freedom for the study of the effect of cornposition on coherent growth and properties. In the Cu-Ni-Fe alloys of appropriate composition, the face-centered cubic precipitate and also the depleted matrix when first formed are coherent with the parent matrix.1&apos;2 The two have the same <Jo parameter as the original matrix but they are both tetragonal; the precipitate has an axial ratio c/a < I while that of the depleted matrix is c/a > I. When coherency is lost they assume the normal face-centered cubic structure with the depleted matrix having a lattice parameter greater than the original matrix and that of the precipitate less. Such a mechanism would also be expected for CU-Ni-CO alloys because of the similarity in constitution but this had not been demonstrated. The Present investigation was conducted on a CU-Ni-CO alloy. The constitution diagram and magnetic properties of these alloys have been fairly well established, however, no previous determinations of mechanism of precipitation and no correlation of structure with properties had been made. Thus, an alloy of this system Was chosen for a comprehensive investiga-

Jan 1, 1949

By Francis B. Foley

Fundamentally, slag control in acid open-hearth steelmaking cannot be considered from any different viewpoint than can that in basic open-hearth melting. The same laws of mass action and distribution apply in both cases, so that while most, if not all, of the recent intensive study of slag-metal reactions have been carried on in basic furnaces the principles evolved are nevertheless applicable to acid open-hearth steelmaking and it is therefore not our intention to discuss the various possible chemical reactions in the slag and between slag and metal. The points we have to carry in mind, in considering acid melting practice, are the differences in the type of steels produced and the difference in the chemistry of both the steel and the slag. The acid furnace is used to produce, let us not say "quality" steel, for, after all, a "quality" steel for one purpose is not a "quality" steel for another, but steels that require acid melting practice to be of proper "quality." Steels that are required to have high physical properties in tests taken transversely from forgings are peculiarly the product of acid furnaces. In this class may be placed various ordnance materials, notably gun forgings and projectiles and large commercial forgings requiring high transverse ductility. Forgings requiring an extremely hard surface, polished and free from imperfections, are also typical acid-steel products. Of course, such forgings can be made of basic open-hearth steel, but not with the same assurance of success. At the start, the preparation of the slag in the acid and basic furnaces differs. Lime is charged in the beginning of a basic heat to form a slag, but in the acid furnace nothing is added for the special purpose of producing a slag when the heat is melted down. The result is that the acid furnace has much less volume of slag than the basic. The slag formed upon melting down is made up almost entirely of the oxides of elements contained in the metallic charge, notably oxides of iron, manganese and silicon, the amount of silica being augmented somewhat by erosion of the furnace lining. A typical acid open-hearth slag, when the bath is completely melted, will have an analysis about as follows: CaO, 3.40 per cent; SiO2, 51.9; Fe2O3, 1.25 ; FeO, 28.86; Al2o3, 1.82; MnO, 12.22. The high iron oxide content of the slag gives it a black appearance. The metal is high in carbon and some manganese and silicon will be present, depending on the amount in the original charge, the amount of

Jan 1, 1935

By Francis B. Foley

Fundamentally, slag control in acid open-hearth steelmaking cannot be considered from any different viewpoint than can that in basic open-hearth melting. The same laws of mass action and distribution apply in both cases, so that while most, if not all, of the recent intensive study of slag-metal reactions have been carried on in basic furnaces the principles evolved are nevertheless applicable to acid open-hearth steelmaking and it is therefore not our intention to discuss the various possible chemical reactions in the slag and between slag and metal. The points we have to carry in mind, in considering acid melting practice, are the differences in the type of steels produced and the difference in the chemistry of both the steel and the slag. The acid furnace is used to produce, let us not say "quality" steel, for, after all, a "quality" steel for one purpose is not a "quality" steel for another, but steels that require acid melting practice to be of proper "quality." Steels that are required to have high physical properties in tests taken transversely from forgings are peculiarly the product of acid furnaces. In this class may be placed various ordnance materials, notably gun forgings and projectiles and large commercial forgings requiring high transverse ductility. Forgings requiring an extremely hard surface, polished and free from imperfections, are also typical acid-steel products. Of course, such forgings can be made of basic open-hearth steel, but not with the same assurance of success. At the start, the preparation of the slag in the acid and basic furnaces differs. Lime is charged in the beginning of a basic heat to form a slag, but in the acid furnace nothing is added for the special purpose of producing a slag when the heat is melted down. The result is that the acid furnace has much less volume of slag than the basic. The slag formed upon melting down is made up almost entirely of the oxides of elements contained in the metallic charge, notably oxides of iron, manganese and silicon, the amount of silica being augmented somewhat by erosion of the furnace lining. A typical acid open-hearth slag, when the bath is completely melted, will have an analysis about as follows: CaO, 3.40 per cent; SiO2, 51.9; Fe2O3, 1.25 ; FeO, 28.86; Al2o3, 1.82; MnO, 12.22. The high iron oxide content of the slag gives it a black appearance. The metal is high in carbon and some manganese and silicon will be present, depending on the amount in the original charge, the amount of

Jan 1, 1935

The Library belonging to the Institute is now administered as part of that of the United Engineering Society, the members of the Library Committee representing the Institute on the Library Board of the United Engineering Society. The main collection now consists of 115,900 books, 3680 pamphlets, 5811 maps, and 4402 searches, making a total of 129,793, a net gain of 7701 within the year. There is in addition a lending collection of 1004 volumes and one of duplicates amounting to 11,310. The library grows steadily both by gift and purchase. The cataloging is now substantially current covering 124,100 items represented by 362,145 cards. There are many rare and notable books, especially those relating to early engineering. It is truly a great treasure house of knowledge. While no severe effort is made to record all visitors the books showed 23,470 to have used the Library in 1928. In addition 5102 telephone requests for information were answered, 202 searches and 196 translations made and 34,964 photo prints furnished. The service department is maintained by small fees which cover the cost. The total amount appropriated for operating expense for the year was $46,300, of which $8,240.02 was furnished by the Institute, $5,399.45 being derived as income from the Douglas Library Fund and the remainder from current receipts. Within the year a slight change was made in the method of meeting the expenses of the Library, a flat charge of $5,000 per year being made against each of the four Founder Societies and this being supplemented by a surcharge based upon membership. The effect of this has been for the present to decrease slightly the amount that the Institute would otherwise need to pay. Placing in one collection all the books of the four societies greatly increases the number of books accessible to the members of each and opening the Library to the public is an important factor in keeping the tax exemption privilege enjoyed for the building. The Director and Staff of the Library make every effort not only to accommodate those who come in person to consult the collection but members resident elsewhere who communicate by letter or wire. The facilities of the Library are truly available to all.

Jan 1, 1929