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By E. J. Duggan

It is a coincidence that the two plants in this country for treating copper ores by ammonia leaching came into existence at almost the same time, that of the Kennecott Copper Corporation at Kennecott, Alaska, in March, 1916, and that of the Calumet & Hecla Mining Co. in July of the same year. The success of both from their very beginning attests the merits of the process under widely different sets of conditions. As would be expected, in the time they have been operating these two pioneers in this field have greatly perfected their methods and improved their technic. The early difficulties inevitably encountered in undertakings of this nature have been largely surmounted and the process may now be considered to be well seasoned and matured. There have been no other commercial plants built in this country and but one elsewhere, the Bwana M'Kubwa in Northern Rhodesia, for the reason that this method of treatment may be employed on comparatively few ores. However, it has certain advantages, some of which are inherent to sand leaching processes generally and some to ammonia leaching in particular. Among these may be enumerated: (1) the avoidance of fine grinding; (2) the small amount of water required; (4) a high-grade product; (5) little likelihood of deleterious gangue constituents and fouling of solutions. It is true that great progress has been made in recent years in the flotation of the ores that come within the province of ammonia leaching. Nevertheless ammonia leaching has its possibilities and these may be overlooked in the present tendency toward the use of flotation for all ores. Probably the chief requisite to its further extension to suitable ores will be a cheap source of steam. Ammonia, the only reagent required, is unlimited in supply, readily transported and the price that is likely to obtain in the future should not make its cost at all onerous. Choice of Method for Kennecott Ores The Kennecott ores are typical limestone replacement deposits. The milling ores have a copper content of approximately 8 per cent in a limestone dolomite gangue. About half the copper occurs as sulfide, mostly chalcocite with some covellite, and the remainder in the form of the two carbonates, malachite and azurite. A comparatively coarse grind followed

Jan 1, 1934

By S. Floreen, R. M. Pilliar, H. W. Hayden

The fracture behavior of a 50 pct Cu-50 pct Fe mi-croduplex alloy, laminated composites of copper and iron and an extruded 50-50 Cu-Fe elemental powder composite was studied. Very low ductile-brittle transition temperatures were achieved in all cases, but for different reasons. In the microduplex alloy both the initiation and also the propagation of cleavage fractures appeared retarded by the very small in-terphase distances. In the composites, crack propagation through the sumples was prevented in most cases by delamination fractures perpendicular to the advancing cracks. These delaminations occurred at different regions and by different mechanisms in the various composites. In the extruded powder composite, de-lamination appeared to take place along preexisting flaws. In the crack arrest geometry of the laminated plates, delamination took place by localized shear fractures within the copper near the Fe-Cu interfaces. In this case delamination was enhanced by thicker laminate layers, and by having the resistance to shear failure of the copper sufficiently low compared to the toughness of the iron. BRITTLE fracture in engineering materials has long been a problem, and many different ways of preventing it have been considered. One method that has been of growing interest lately is to prevent crack propagation by the introduction of mechanical discontinuities into the structure. These discontinuities may act in several ways. They may simply act as crack stoppers. They may introduce secondary fractures such as de-laminations that deflect the initial crack into new, less damaging directions. Alternatively, they may subdivide a fairly large bulk sample that would have been loaded in plane strain, for example, into a number of subunits that are individually loaded in plane stress and thus are more resistant to fracture. Other mechanisms, or combinations of mechanisms, are also feasible. A number of methods exist for introducing mechanical discontinuities into a structure. Composites by their nature have discontinuities in structure, and numerous studies have shown that fracture propagation in materials of this type can be radically changed by suitable control of the composite parameters. Of particular significance to the present work are recent investigations of layered composites made by joining high strength steel sheets by various means.'-4 These studies have shown that through proper control of the mechanical properties of the bonds joining the sheets it was possible to introduce delamination fractures that markedly improved the overall toughness of the composites and in some cases completely prevented through-the-thickness fractures. Another technique for introducing structural discontinuities is simply to use a two-phase alloy. It has been recognized for many years that a small amount of a second phase may improve toughness either by homogenizing plastic flow and thus preventing localized stress concentrations that nucleate fracture, or by interacting with an advancing crack. In most of these studies of two-phase materials, the decreases in ductile-brittle transition temperatures produced by the second phase were relatively small. More recently, work on two-phase stainless steels having a very fine grain microduplex structure has shown that the presence of on the order of 40 to 50 pct of a tougher second phase may lower the ductile-brittle transition temperature of the brittle phase by approximately 300°F. 5-7 In these alloys delaminations were seldom observed. The tougher second phase appeared to minimize the ease of both the initiation and the propagation of cleavage fractures. These results show that both the composite approach and the microduplex alloy approach are effective methods of preventing brittle fracture. Therefore, it was of interest to compare the fracture behavior of a microduplex alloy with composites made from the two-phases that were present in the alloy. To simplify this comparison the 50 pct Cu-50 pct Fe system was selected for study. At low temperatures the equilibrium tie line phases in this system are essentially pure ferrite and pure copper. A 50-50 alloy was cast and hot worked to produce a microduplex structure. Two types of composites were studied; laminated structures prepared by roll bonding iron and copper sheets of the tie line compositions, and an extruded powder composite made from high purity elemental powders. The fracture behavior of these materials was then compared. EXPERIMENTAL PROCEDURE Alloy Preparation. The 50-50 Fe-Cu alloy and the components for the roll bonded composites were prepared by vacuum induction melting 30-lb heats using electrolytic grades of iron and copper as charge materials. A carbon boil was used to deoxidize the melts. Small additions of copper and iron were made to the iron and copper heats, respectively, to approximate

Jan 1, 1970

By Thomas O. Ziebold, Robert E. Ogilvie

Experimental analysis of diffusion samples covering the entire Cu-Ag-Au system at 725°C has been carried out. Experimental coefficients are computed at twenty-eight points in the lermary system. It is found that the direct coefficienl for copper is nearly independent of the silver, content for 1ow-silver alloys and that the cross coefficient for silver correlates with the ther-nzodynatnic properlies. This lalter observalion leads to the conclusion that the mobililies of copper and gold are nearly equal. Thermodynarmic actiuilies for Cu-Ag-Au were computed from binary data and adjusted to be consistent with neasured tie lines across the two-phase region which extends into the ternary diagram at 725°C. Application of these therknodynarnic calculaliorls to the dijftcsion data terifies the Onsager reciprocal relations to the extent that experimental uncertainlies will allow. It is jound that diffusion neav the critical point of the 1200-phase field in the isothermal section at 725°C causes the composition gradients for copper and silver to approach infinity while the direct and cross coeficients become equal. From the standpoint of experimental Procedures, it has been shown that microanalysis of ternary samples may be carried out using a simple expression for the conversion of X-ray zntensily to composilion. The accuracy of' this method has been demonstrated by the analysis of standard alloys and by the reproducibility of composition determinations using differed X-ray lines. DIFFUSION in a ternary alloy system is basically and significantly different from diffusion in binary alloys. When only two elements are present there is just one independent composition variable, and the diffusion profile of composition vs distance across a sample must change monotonically through all solid solutions bracketed by the terminal alloys. If two-phase regions are stable for compositions between the terminal values, these must appear as planar interfaces in the diffused sample, with the composition profile exhibiting sharp discontinuities. Adding a third element may alter this picture completely. Because of the additional degree of freedom in the composition, we may see composition profiles which do not change monotonically through solid-solution ranges, and stable, nonplanar phase interfaces. Even though two-phase regions may lie between the terminal compositions of a diffusion sample on the constitution diagram, they will not necessarily appear in the diffusion profiles. In binary diffusion only one coefficient is needed to describe the interdiffusion process. From Fick's law this coefficient relates the diffusive flux of one component to its own composition gradient. In ternary diffusion we must allow for cross interaction between the two independent species. By a linear extension of Fick's law we introduce "cross" or "off-diagonal" diffusion coefficients which relate the flux of one component to the composition gradient of the other independent constituent. Thus, we require four interdiffusion coefficients to describe the transport process in a ternary system. In its most general form,1,2 the rate equation for mass transport by isothermal diffusion in a system of s components states that the diffusive flux of component i, Ji, is a linear summation of all driving forces, Xk, each force being multiplied by an appropriate compliance coefficient:

Jan 1, 1968

By T. H. Alden

T. H. Alden (General Electric Research Laboratory)—This paper as well as earlier ones of Dr. Wood represent an important contribution to the experimental description of fatigue fracture. The mechanism of fracture proposed by the authors, however, is not established by this data nor supported by other data existing in the literature. Although taper section metallography provides a rather detailed picture of fatigue crack geometry, photographs so obtained must be interpreted with care. The narrow bands revealed by etching, frequently associated with surface notches, are labeled by the authors "fissures". Measurement shows, taking into account the 20 to 1 taper magnification, that the depth of these structures is at most 2 to 3 times the width. This distinction is important in the conception of a mechanism of crack formation. It is difficult, for example, to imagine a deep, narrow fissure arising from a "ratchet slip" model. A surface notch, on the other hand, may form easily by this mechanism. The notches observed in the present work are the subsurface evidence of the surface slip bands or striations in which fatigue cracks are known to originate.4-6 It is clear that an understanding of the structure of these slip bands is of key importance in understanding the mechanism of fracture. The evidence presented shows that these regions etch preferentially, possibly because they contain a high density of lattice defects, or as the authors state equivalently, because they are "abnormally distorted." However, it is not possible to conclude that the distortion consists of a high density of vacant lattice sites. The fact of a high total shear strain in itself does not assure a predominance of point defects as opposed to other defects, for example, dislocations. Other evidence in the literature which suggests unusual densities of point defects formed by fatigue7-' refers not to the striations or fissures, but to the material between fissures (the "matrix"). If a choice must be made, the preferential etching would seem to be evidence for a high dislocation density, since dislocations are known to encourage chemical attack in copper;g no such effect is known for the case of point defects. A third alternative is that the slip bands are actually cracked, but that near its tip the crack is too narrow to be detected by the authors' metal-lographic technique. In this case the rapid etching can be readily understood in terms of the increased chemical activity of surface atoms. Unless a vacancy mechanism is operative, the motion of dislocations to-and-fro on single slip planes will not lead to crack growth. Point defect or dislocation loop generation are the principal non-reversible effects predicted by this model. In any case, the nonuniform roughening of the surface in a slip band6 requires a flexibility of dislocation motion which is not a part of the to-and-fro fine slip idea. The same is probably true of crack growth by a shear mechanism. Either some dislocations must change their slip planes near the end of the band and return on different planes,'0 or dislocations of opposite sign annihilate." The mechanism by which these processes occur in copper at room temperature or below is that of cross slip. Thus cross slip appears to be essential to fatigue crack growth.6'10"12 The fact that a tensile stress opens the slip bands into broad cracks does not indicate the structure of the bands or the mechanism by which cracks form. The charactersitic concentration of slip into bands during fatigue shows a low resistance to shear strain in these regions. (This fact in itself may be inconsistent with a high concentration of vacancies.) The authors contend also that continuing shear produces an additional mechanical weakening so that the bands fracture easily (are pulled apart) under the influence of the superimposed tensile stress. It is equally possible that the only weakness is a weakness in shear, that the crack propagates by a shear mechanism, and that subsequently the tensile stress pulls the crack apart. Even the direct observation of bands opened by a tensile stress would not be conclusive since, as argued above, they may be fine cracks. The same argument applies to internal cracks, their existence in the presence of a tensile stress not indicating the mechanism of formation. Internal cracks originating in regions of heavy shear have also been seen following tensile deformation of OFHC copper,13 so that this mode of fracture is not unique to combined tensile and fatigue straining. The authors point out in their companion report14 that 90 pct of the cracks formed during pure tor-sional strain were within 8 deg of the normal to the specimen axis. If the tensile stress were an important factor in crack propagation, it is surprising that the cracks cluster about the plane in which the normal stress vanishes. Similarly, a study of zinc single crystals showed that for various orientations the life correlated well with the resolved shear stress on the basal plane,'= and was not dependent on the normal stress across this plane. W. A. Wood and H. M. Bendler (Authors' reply) -Dr. Alden's discussion emphasizes the essential point in the relation of slip band structure to

Jan 1, 1963

By R. Maddin, A. Lawley

Single crystal Mo-Re alloys (99.99+ purity), grown by electron bombardment floating zone heating, were deformed in tension at temperatures from -196° to +200°C. At -196oC, Mo-6 pet Re and Mo-20 pct Re alloys deform by slip on systems of the type (101) [1ll]. Above-78oC, the operative slip system is of the type (112) [111], (101) [1ll], or (211) [1ll], depending upon orientation. Mo-39 pct Re alloys deform by twinning and slip at all test temperatures with a (112) [111] type twinning system. Critical resolved shear stress for slip and twinning is calculated as a function of composition and temperature, and the mechanical properties compared with those of less Pure polycrystalline alloys. HEXAGONAL close-packed rhenium, c/a = 1.615, is highly soluble in molybdenum. The bee molybdenum-rich solid solution extends to approximately 42 at. pet Re* at 2500°C,' Fig. 1. Recent work on polycrystalline alloys has shown conclusively that the addition of rhenium to molybdenum improves both the fabricability and the low-temperature ductility.2"5 Similar behavior is observed for W-Re and Cr-Re alloys.5 Initially, Geach and Hughes2 found that the Mo-30 pct Re alloy could be cold rolled to approximately 90 pct reduction before the onset of cracking. The remarkable effect of the rhenium was later confirmed by Jaffee et al. 3-5 with an optimum condition of maximum strength combined with maximum ductility at the Mo-35 pet composition. At higher rhenium contents, the ductility was severely impaired due apparently to the presence of brittle tetragonal s phase, Fig. 1. In the Mo-35 pet Re alloy, at least 110 ppm (parts per million) oxygen could be tolerated before cold workability was reduced. By comparison, the corresponding tolerance figure in unalloyed molybdenum is ~ 10 ppm. The effect of rhenium was considered in terms of: 1) a reduction in oxygen solubility in the lattice; 2) a redistribution of intergranular oxide from grain boundary films to isolated spheres; and 3) the promotion of twinning as a further mode of plastic deformation. Paradoxically, twinning is often associated with brittle fracture in iron and the silicon irons.6'7 Work to date has been restricted to are-melted and powder metallurgy polycrystalline material of ~ 99.9 pet purity. The present investigation was initiated for the purpose of determining the mode and crystallography of plastic deformation of a series of bee Mo-Re alloy single crystals over a wide temperature range from -196o to +200°C. Using high-purity zone-melted material (~ 99.99 + pet purity), the specific role of rhenium in the molybdenum lattice may be understood more fully since effects due to grain boundaries and oxide redistribution will be absent. At the same time, the study provides a comparison of single and polycrystalline deformation behavior. EXPERIMENTAL TECHNIQUES A) Preparation and Purity of Single Crystals. Alloys in the form of either are-cast and swaged or sintered and ground bar, 0.120 in. diam, were obtained from the Chase Brass and Copper Co. Alloy single crystals ~ 8-in. long were grown from the

Jan 1, 1962

By J. McLaren Forbes

Geologists and engineers in charge of diamond drilling often have no practical experience in the work, yet they must direct the drillers. In discussing some of the problems that arise, the author of this paper has tried to remember the things he did not know about diamond drilling when he first came in contact with that work. The basic reason for most diamond-drill holes is to obtain information. The more thorough the understanding of the geological and engineering problems involved, the greater will be the benefit derived from a drilling program. One of the best methods to ensure some thinking before drilling is to record on the permanent drill log, before the hole is collared, the reasons for the work and the information desired from that particular hole. When the hole is finished, the information obtained should be recorded. Driller The choice of a diamond driller is very important. If no experienced driller is available, a competent miner who has a sense of responsibility and better than average mechanical ingenuity can do the work. The best answer to most practical drilling problems, from the standpoint of the person in charge of the drilling program, is the service of experienced diamond drillers or drilling firms. Equipment Drilling equipment should be adequate to put down the longest hole desired and handle the toughest ground encountered. The type of bit used depends upon the ground drilled. Experimenting with various bits and careful study of footage records are the best means of determining which to use. Under ordinary circumstances it is best to drill using an EX barrel when possible. The length of rod and core barrels that can be used depends on the size of the drill station. Also, the length of core barrel depends on the way the ground cores. In good ground as much core will be recovered with a 10-ft. barrel as with a shorter one, and with considerable saving of drilling time. A water pump is needed if the hole is so deep that the water pressure is not strong enough to wash out the cuttings, or if it is drilled at an angle that prevents full force of the water pressure. Instructions For an Inexperienced Driller 1. Never run a bit too long a time. When a bit seems to be "good for one more run," discard it. 2. Always let the rods down on bottom easily. Protect the bit from sudden shock. 3. Start the drilling slowly and easily. Do not put pressure on the bit too fast. Diamonds can break. 4. Be sure the water pressure is strong enough to clear the bit, but do not use more water than is needed, as it may wash away the core. Usually, if no core is recovered the hole is a total loss. 5. When dry-blocking, do not run without water longer than necessary as the bit may burn. 6. Be sure the rods are well caulked and tightly screwed together. If not well caulked they will lose water, and if not

Jan 1, 1946

By V. J. Decarlo, J. J. Gilman

POLISHING pure zinc differs somewhat from polishing less reactive metals. The problem is not that of finding a suitable reagent, but rather of producing the polish in such a way that the surface remains polished after it is removed from the polishing bath. In other words., the anodic film that is vital to the polishing mechanism' must be tightly adherent and nonporous. It is usually desirable that it be thin. Polishing solutions consist of proper proportions of an acid and a strong oxidizing agent. In electro-polishing, the external circuit acts as the oxidizing agent. The proportions are critical because the essential surface film must be maintained at approximately constant thickness during the polishing process. In the case of zinc, chiefly two oxidizing agents, chromic and nitric acids, have been used. The simplest polishing reagent is concentrated nitric acid. However, it has certain disadvantages. It tends to pit: an excessive amount of heat is evolved during polishing; and the oxide film that it produces is not very stable, so that the polished sur-

Jan 1, 1957

By W. W. Anderson, D. G. Girton

The photoluminescence of Pr, Nd, Ho, Er, Tm, and Yb in CdS, and Ho, Er, Tm, and Yb in ZnSe has been observed from crystals Prepared by diffusion using rare earth metals and an excess chalcogen pressure. For a given temperature, time, and chalcogen pressure the spectral characteristics were very reproducible from run to run, and the emission intensity for Nd, Er, and Yb in CdS was as high or higher than the best vapor phase doped crystals we have grown. For a few rare earths it was found that certain conditions of diffusion tend to yield optimum rare earth emission intensity with respect to the background lattice emission. Photoluminescence measwements of Yb in CdS as a function of depth gave a profile which was neither a Gaussian nor complementary error function. Part of the profile appears to arise from a fast component of the diffusion and the other part from a slow diffusing component. At 960°C and 33 atm S pressure, a com -plimentary error function approximation of the slow diffusing component gave a diffusion coefficient of D = 1.3 x 10-9 sq cm per sec. MOST of the studies of emission from rare earth ions in II-VI compounds have been reported on crystals doped during growth,1,2 although Kingsley and Aven prepared ZnSe:Er by diffusion for paramagnetic resonance and fluorescence studies. Pappalardo and Dietz prepared CdS:Yb by diffusion, but they made optical absorption measurements., We know of no study on the properties of rare earth diffusion in the II-VI compounds. To date we have diffused Pr, Nd, Ho, Er, Tm, and Yb into CdS, and Ho, Er, Tm, and Yb into ZnSe and observed the rare earth emission spectra. For a given temperature and chalcogen pressure, the emission characteristics are very reproducible from run to run and for Yb, Nd, and Er in CdS, as good as the best crystals we had prepared by doping during vapor phase growth.2 The emission of Pr, Ho, and Tm has been observed in CdS prepared by diffusion for the first time. Previous attempts2 to prepare these later three materials by vapor phase growth were unsuccessful. The problem of obtaining reproducible characteristics in II-VI semiconductor compound work is well known.5 Not only is it difficult to reproduce results from one laboratory to another but it is sometimes difficult to reproduce results from one growth run to another under ostensibly identical conditions within one laboratory. This situation has been particularly bothersome in research on the luminescence of rare earth activated ZnS1 and Cds2. Crystals from one vapor phase growth run would show very strong rare earth line emission while crystals from a nearly identical run would show no rare earth emission. It was also observed on occasion that the intensity of the rare earth emission was not constant over the entire volume of a single crystal. MATERIAL PREPARATION AND INSTRUMENTATION Vapor phase grown boules of CdS were supplied by Dow Corning. This material was characterized by a free electron concentration of n - 3.5 x 1015 cm-3 and Hall mobility of 350 sq cm per v sec at room temperature. There were microscopic voids and decorated precipitates in some samples. The precipitates annealed out at diffusion temperatures but the voids remained. Single crystal rectangular samples of mm dimensions were sawed from the boules. The ZnSe was polycrystalline, UHP grade from Eagle-Picher. Poly-crystalline samples were sawed from the ingots. The samples were lapped, polished on one side, etched in a solution of 0.5 M K2Cr2O7 in 16 N H2SO4, and thoroughly washed in distilled water. A sample, excess sulfur (or selenium), and 5 mg of rare earth metal (turnings) were sealed in a 3.6 cm3 quartz ampoule at about 2 X 10-5 torr. The high chalcogen pressure used (1 to 30 atm) prevented thermal etching of the crystals and affected the diffusivity and solubility of the rare earth ions in the crystal lattice. For meaningful or reproducible results, it is thus necessary to specify the vapor pressure at which the diffusion was carried out. It is assumed that a negligible amount of the chalcogen was used in the formation of rare earth sulfides or selenides Our sulfur vapor pressure calculations are based on data assuming S2, S6, and S, molecules only in which case the equilibrium constants are given by6 where the pressures are expressed in torr. Selenium vapor consists of a mixture of Se2, Se4, Se6, and Se6 molecules. The selenium vapor pressure was calculated using equilibrium constants given by The status of the rare earth source during diffusion is unknown, i.e., the partial pressures of the rare earth metal and of the rare earth chalcogenides has not been determined. All emission spectra were recorded at 77°K on a Perkin-Elmer model 98-G spectrometer using a 640 line per mm grating. No correction was made for the spectrometer and detector spectral sensitivity. Excitation was by means of an XBO 1600 w xenon arc

Jan 1, 1970

By G. E. Burpee

A COMPREHENSIVE study of insoluble residues in the productive Permian limestone in the Hobbs and Eunice fields, Lea County, N. M., has been conducted by Shell Petroleum Corp. engineers {luring the past two years. This study was prompted by the belief that the stratigraphy of the producing formation might be worked out in detail and that some relationship might be established between the permeable oil, gas, and water zones and correlatable lithologic horizons within the productive formation. As a result of the study, correlations have been established which have proved of great value to both an orderly development and corrective program.

Jan 1, 1935

By Odmund Ljone

FAR north of the Arctic Circle is a totally industrial community which until 1945 could not boast a single specimen of the rat family, and where today you will be awarded a bottle of fine cognac for every rat-dead or alive. Amazing but true, the spot is Longyear City, the Norwegian mining town on the arctic island of Spitzbergen. Perhaps you have also heard of the town built on soil that never thaws, where huge blocks of ice must be melted to fill the city's fresh water reservoirs, and where the Far North dictates a way of life all its own. Here, coal is king and men must work hard for their "black gold." Spitzbergen is a rough, tough piece of Norway, made up of a half dozen isolated islands between 74 and 81 degrees north latitude. Covering twice the area of Belgium, they are home to

Jan 1, 1948

By J. E. Gould, H. J. Hand

Many independent studies are being made on slag-metal relationships in the open-hearth furnace, and these studies cannot help but result in an ultimate improvement in the quality of open-hearth steel of both the open and killed types. In maintaining quality control at the National Tube Company's plant, emphasis has been placed on an evaluation of the iron oxide content of the steel in as quantitative a manner as possible, in order that the most desirable level of oxidation might be obtained for a given type of steel, and to secure a more precise basis for final de-oxidation. In the past, various methods were used for estimating FeO content of the metal at tap to ensure uniform and thorough deoxidation of killed steel, avoiding overdeoxidation to minimize the amount of inclusions present and to make as sound a steel as possible. For the open-type steels, such control involves obtaining the necessary level of oxidation for the most suitable action of the steel in the molds to provide good surface quality and cross section for the specific grade involved. While rapid analytical methods are available for determination of FeO in the liquid metal, such methods are still not sufficiently rapid for routine control on the open-hearth floor, nor do such analyses provide information as to what causes high or low FeO values. The method of sampling can still be considered a problem in view of the variability encountered in taking simultaneous duplicate tests. With the accurate rapid methods now available for determining carbon in the metal, estimating slag basicity and obtaining temperatures of liquid metal, it was believed possible to determine the influence of the various furnace reactions in establishiug the state of oxidation at a given time. Simultaneous slag and metal tests were used in this analysis, aided by statistical methods, to determine the factors that affect the metal FeO, and also to make a quantitative evaluation of these factors. Data obtained are from actual iurnace operations, the metal test being of the I spoon, Herty type, and taken in duplicate. Metal temperatures were taken with the open-tube bath pyrometer developed by the Research Laboratory of the United States I Steel Corporation. This method of taking open-hearth metal temperature was invented by Collins and Oseland,l and was developed into its present form by L. 0. Sordahl,2 of the Research Laboratory. The instrument and its mode of operation have been fully described by Sordahl and Sosman in three publications.3,4,5 lag components were obtained by chemical analysis. Data were taken from four 165-net-ton furnaces during the working period of the heat. Recognizing that additions of ore affect the metal FeO. no tests were included within 30 min. after ore additions. In all, 65 tests (48 heats) were used in this study.

Jan 1, 1942

By J. E. Gould, H. J. Hand

Many independent studies are being made on slag-metal relationships in the open-hearth furnace, and these studies cannot help but result in an ultimate improvement in the quality of open-hearth steel of both the open and killed types. In maintaining quality control at the National Tube Company's plant, emphasis has been placed on an evaluation of the iron oxide content of the steel in as quantitative a manner as possible, in order that the most desirable level of oxidation might be obtained for a given type of steel, and to secure a more precise basis for final de-oxidation. In the past, various methods were used for estimating FeO content of the metal at tap to ensure uniform and thorough deoxidation of killed steel, avoiding overdeoxidation to minimize the amount of inclusions present and to make as sound a steel as possible. For the open-type steels, such control involves obtaining the necessary level of oxidation for the most suitable action of the steel in the molds to provide good surface quality and cross section for the specific grade involved. While rapid analytical methods are available for determination of FeO in the liquid metal, such methods are still not sufficiently rapid for routine control on the open-hearth floor, nor do such analyses provide information as to what causes high or low FeO values. The method of sampling can still be considered a problem in view of the variability encountered in taking simultaneous duplicate tests. With the accurate rapid methods now available for determining carbon in the metal, estimating slag basicity and obtaining temperatures of liquid metal, it was believed possible to determine the influence of the various furnace reactions in establishiug the state of oxidation at a given time. Simultaneous slag and metal tests were used in this analysis, aided by statistical methods, to determine the factors that affect the metal FeO, and also to make a quantitative evaluation of these factors. Data obtained are from actual iurnace operations, the metal test being of the I spoon, Herty type, and taken in duplicate. Metal temperatures were taken with the open-tube bath pyrometer developed by the Research Laboratory of the United States I Steel Corporation. This method of taking open-hearth metal temperature was invented by Collins and Oseland,l and was developed into its present form by L. 0. Sordahl,2 of the Research Laboratory. The instrument and its mode of operation have been fully described by Sordahl and Sosman in three publications.3,4,5 lag components were obtained by chemical analysis. Data were taken from four 165-net-ton furnaces during the working period of the heat. Recognizing that additions of ore affect the metal FeO. no tests were included within 30 min. after ore additions. In all, 65 tests (48 heats) were used in this study.

Jan 1, 1942

By W. F. Holbrook, C. E. Wood, E. P. Barrett

The Blast Furnace Studies Section, Metallurgieal Division, Bureau of Mines, has been working for several years on the mechanism of desulphurization of iron and steel by slags. The usual assumption that desulphurization takes place by diffusion of FeS from metal into slag and subsequent reaction of this FeS with CaO to produce CaS has seemed to us inconsistent with a number of experimental results we have obtained. We undertook, for example, to determine the proportion of sulphur in a slag present as FeS. An entirely satisfactory method of doing this has not yet been evolved. The results of extraction with metallic antimony led to an interesting conclusion, however. FeS is readily soluble in metallic antimony, either physically or by chemical reaction. On the other hand, CaS was found to be insoluble. Hence it would appear that by rapid extraction of the slag with antimony we might expect to determine the distribution of sulphur between iron and calcium. The results showed that much of the sulphur was present as FeS. In some instances the extraction of sulphur as FeS was almost quantitative. For example, in a slag containing 3.8 grams Fe and 3.7 grams S, extraction removed 1.18 grams S and 2.12 grams Fe. If all the iron present in the antimony had been FeS, 1.21 grams S would have been extracted. In another slag with 8.6 grams Fe and 0.06 gram S present, 0.14 gram Fe and 0.08 gram S were extracted. This was obviously extraction of sulphur as FeS within the analytical error and showed that FeS was present either in solution or as a dispersion. Attempts to determine the solubility of FeS and CaS in slag by quenching and ultramicroscopic investigation have indicated that the solubility of FeS is very low, and that reactions in the slag are probably not to be considered as homogeneous. A more detailed report on these theoretical considerations will be made at a later date.

Jan 1, 1940

By W. F. Holbrook, C. E. Wood, E. P. Barrett

The Blast Furnace Studies Section, Metallurgieal Division, Bureau of Mines, has been working for several years on the mechanism of desulphurization of iron and steel by slags. The usual assumption that desulphurization takes place by diffusion of FeS from metal into slag and subsequent reaction of this FeS with CaO to produce CaS has seemed to us inconsistent with a number of experimental results we have obtained. We undertook, for example, to determine the proportion of sulphur in a slag present as FeS. An entirely satisfactory method of doing this has not yet been evolved. The results of extraction with metallic antimony led to an interesting conclusion, however. FeS is readily soluble in metallic antimony, either physically or by chemical reaction. On the other hand, CaS was found to be insoluble. Hence it would appear that by rapid extraction of the slag with antimony we might expect to determine the distribution of sulphur between iron and calcium. The results showed that much of the sulphur was present as FeS. In some instances the extraction of sulphur as FeS was almost quantitative. For example, in a slag containing 3.8 grams Fe and 3.7 grams S, extraction removed 1.18 grams S and 2.12 grams Fe. If all the iron present in the antimony had been FeS, 1.21 grams S would have been extracted. In another slag with 8.6 grams Fe and 0.06 gram S present, 0.14 gram Fe and 0.08 gram S were extracted. This was obviously extraction of sulphur as FeS within the analytical error and showed that FeS was present either in solution or as a dispersion. Attempts to determine the solubility of FeS and CaS in slag by quenching and ultramicroscopic investigation have indicated that the solubility of FeS is very low, and that reactions in the slag are probably not to be considered as homogeneous. A more detailed report on these theoretical considerations will be made at a later date.

Jan 1, 1940

By C. E. Wood

THE Blast Furnace Studies Section, Metallurgical Division, Bureau of Mines, has been working for several years on the mechanism of desulphurization of iron and steel by slags. The usual assumption that desulphurization takes place by diffusion of FeS from metal into slag and subsequent reaction of this FeS with CaO to produce CaS has seemed to us inconsistent with a number of experimental results we have obtained. We undertook, for example, to determine the proportion of sulphur in a slag present as FeS. An entirely satisfactory method of doing this has not yet been evolved. The results of extraction with metallic antimony led to an interesting conclusion, however. FeS is readily soluble in metallic antimony, either physically or by chemical reaction. On the other hand, CaS was found to be insoluble. Hence it would appear that by rapid extraction of the slag with antimony we might expect to determine the distribution of sulphur between iron and calcium. The results showed that much of the sulphur was present as FeS. In some instances the extraction of sulphur as FeS was almost quantitative. For example, in a slag containing 3.8 grams Fe and 3.7 grams S, extraction removed 1.18 grams S and 2.12 grams Fe. If all the iron present in the antimony had been FeS, 1.21 grams S would have been extracted. In another slag with 8.6 grams Fe and 0.06 gram S present, 0.14 gram Fe and 0.08 gram S were extracted. This was obviously extraction of sulphur as FeS within the analytical error and showed that FeS was present either in solution or as a dispersion. Attempts to determine the solubility of FeS and CaS in slag by quenching and ultramicroscopic investigation have indicated that the solubility of FeS is very low, and that reactions in the slag are probably not to be considered as homogeneous. A more detailed report on these theoretical considerations will be made at a later date.

Jan 1, 1939

By O. W. Ellis

CERTAIN alloys1 that, as a result of quenching, are retained in the form of homogeneous solid solution are known to increase in hardness and strength on standing at room temperature or on heating at slightly elevated temperatures. Other alloys" that, on rapid cooling, are held in the form of homogeneous solid solution (as, for example, certain steels) behave in like manner on heating to somewhat higher temperatures. The observed increase in the hardness and strength of these alloys, referred to as "aging" or as "secondary hardness," is widely accepted as being occasioned, either in whole or in part, by the precipitation in submicroscopic form of such constituents as were held in supersaturated solid solution as a result of cooling in excess of a certain critical rate. In earlier discussions of the cause of age hardening or secondary hardness, the question of the hardness of the precipitated particles does not appear to have been raised. At present, however, the general opinion appears to be that age hardening and secondary hardness are occasioned by the precipitation of hard particles within the supersaturated solid substance.3 The authors may be wrong in their belief that the last is a prevailing opinion. Nevertheless, it is thought that the following experiments,

Jan 7, 1924

By D. A. Schemnitz, O. W. Ellis

Certain alloys1 that, as a result of quenching, are retained in the form of homoaeneous solid solution are known to increase in hardness and strength on standing at room temperature or on heating at slightly elevated temperatures. Other alloys2 that, on rapid cooling, are held in the form of homogeneous solid solution, as, for example, certain steels, behave in like manner on heating to somewhat higher temperatures. The observed increase in the hardness and strength of these alloys, referred to as " aging"' or as "secondary hardness," is widely accepted as being occasioned, either in whole or in part, by the precipitation in submicroscopic form of such constituents as were held in supersaturated solid solution as a result of cooling in excess of a certain critical rate. In earlier discussions of the cause of age hardening or secondary hardness, the question of the hardness of the precipitated particles does not appear to have been raised. At present, however, the general opinion appears to be that age hardening and secondary hardness are occasioned by the precipitation of hard particles within the supersaturated solid substance.3 The authors may be wrong in their belief that the last is a prevailing opinion. Nevertheless, it is thought that the following experiments,

Jan 1, 1925

By W. R. Seyfried

THE -problem of extracting alumina from clay and low-grade bauxites has been the subject of considerable interest for some time. The basic reason, of course, lies in the fact that known reserves of high-grade bauxite are not inexhaustible and that the present commercial process cannot successfully cope with low-grade bauxites or clay. Ultimately it may be necessary to use these poorer raw materials for all commercial operations, An unprecedented demand for aluminum during the war emergency and the constantly threatened shortage of imported bauxite caused the United States Government to take an active role in this problem. Through the National Academy of Sciences, the War Production Board and the Defense Plant Corporation, it investigated processes and finally selected four to be used in the construction and operation of four experimental plants. Each plant was to be designed in such a way as to facilitate its incorporation into a larger commercial plant should the need arise. The Chemical Construction Corporation process, or "Chemico" ammonium sulphate process as it is better known, was one of the four selected. The extensive literature and patents on record before the war generally follow one of two process-types depending upon the extracting reagent used. One group uses an acid reagent, the other an alkali. The Chemico process uses an acid reagent. For those interested in other processes described in literature, there is a short bibliography at the end of this paper, The basic steps of all acid extraction processes are: (I) to make the aluminum silicates acid soluble, (2) to separate the released alumina from impurities and insoluble gangue, and (3) to recover the reaent for re-use. THE PROCESS AS PLANNED In April 1941, a group of chemists and engineers of the Chemical Construction Corp, became interested in the problem of extracting alumina from clays and low-grade bauxites and, under the leadership of Mr. Blakeslee Barnes, Vice President and General Manager of the Company, first drafted a process in July of that year-five months prior to Pearl Harbor. The work continued in our research laboratories and with a small pilot plant, By June 1943, the work had progressed to a point where it was possible to apply for a patent on the process which was U.S. patent 2,405,426, granted August 6, 1946. Immediately prior to the development of the Salem plant, the process was envisaged to be as follows: I. The first step was to make the aluminum silicates acid soluble. It was planned: (a) Clay or low-grade bauxite would be roasted at 700 to 800°C (1292° to 1492°F). (b) The roasted ore would then be leached .with hot aqueous ammonium bisulphate to form a slurry. In this way the

Jan 1, 1948

By Benjamin L. Miller

The essential differences expressed by the different speakers participating in this symposium concern merely the relative emphasis placed on the subjects that are commonly included under the term "geophysics" and the branches of science that form the basis for investigations in this field. In order to appreciate the present situation it may be profitable to briefly refer to a few historical matters. One can find almost countless descriptions of geological phenomena long antedating the introduction of the title of "geology," which has been credited to Richard de Bury in the fourteenth century. Interpretations, when they were offered, were generally pure speculation. Only toward the close of the eighteenth century do we find theories developed as the result of observations and tested by additional observations. It is difficult to select and give proper credit to the individual who was particularly responsible for turning geology into a distinctly observational science. william Smith, who has been called the "Father of English Geology," certainly represents the period when observation was the only method used. As he traveled through the British Isles, "sometimes 10,000 miles in a year," he was continually making notes of his observations. Geikie says: "His plain, solid, matter of fact intellect never branched into theory or speculation, but occupied itself wholly in the observation of facts." William Smith, with others of his time, definitely laid firmly the foundations on which modern geology has been built. Field and laboratory observations can no longer be said to constitute the sole basis for geologic contributions but we have not laid aside the methods of Smith and his followers. It is folly to underestimate the fundamental value of the observational part of geology in the present. The objection to purely observational geology is that it is mainly qualitative and not quantitative, general and not specific. No one can deny this charge and probably there are few who do not welcome every method or process whereby we can put aside generalities for definite established values. Physics is the science that has particularly come to the aid of the geologist in this respect. Contributions of PhYsics It is not the intent of the writer to enumerate or to evaluate all of the contributions to geologic advance in the field of. physics. A few only are used for the purpose of illustration, When Clarence King, Director of the United States Geological Exploration of the Fortieth Parallel, invited Ferdinand Zirkel to study 2500 thin sections of rocks collected from the western United States, the use of the microscope came into general use. Zirkel's report was published in 1876. He was not the first to use transmitted light for microscopic rock determination, some work having been done by Henry Clifton Sorby and others some years earlier, but he was the first to put into general use this method. We may well daim that this

Jan 1, 1946

By Benjamin L. Miller

The essential differences expressed by the different speakers participating in this symposium concern merely the relative emphasis placed on the subjects that are commonly included under the term "geophysics" and the branches of science that form the basis for investigations in this field. In order to appreciate the present situation it may be profitable to briefly refer to a few historical matters. One can find almost countless descriptions of geological phenomena long antedating the introduction of the title of "geology," which has been credited to Richard de Bury in the fourteenth century. Interpretations, when they were offered, were generally pure speculation. Only toward the close of the eighteenth century do we find theories developed as the result of observations and tested by additional observations. It is difficult to select and give proper credit to the individual who was particularly responsible for turning geology into a distinctly observational science. william Smith, who has been called the "Father of English Geology," certainly represents the period when observation was the only method used. As he traveled through the British Isles, "sometimes 10,000 miles in a year," he was continually making notes of his observations. Geikie says: "His plain, solid, matter of fact intellect never branched into theory or speculation, but occupied itself wholly in the observation of facts." William Smith, with others of his time, definitely laid firmly the foundations on which modern geology has been built. Field and laboratory observations can no longer be said to constitute the sole basis for geologic contributions but we have not laid aside the methods of Smith and his followers. It is folly to underestimate the fundamental value of the observational part of geology in the present. The objection to purely observational geology is that it is mainly qualitative and not quantitative, general and not specific. No one can deny this charge and probably there are few who do not welcome every method or process whereby we can put aside generalities for definite established values. Physics is the science that has particularly come to the aid of the geologist in this respect. Contributions of PhYsics It is not the intent of the writer to enumerate or to evaluate all of the contributions to geologic advance in the field of. physics. A few only are used for the purpose of illustration, When Clarence King, Director of the United States Geological Exploration of the Fortieth Parallel, invited Ferdinand Zirkel to study 2500 thin sections of rocks collected from the western United States, the use of the microscope came into general use. Zirkel's report was published in 1876. He was not the first to use transmitted light for microscopic rock determination, some work having been done by Henry Clifton Sorby and others some years earlier, but he was the first to put into general use this method. We may well daim that this

Jan 1, 1946