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By R. H. B. Jones

This paper reviews pertinent geology of the Biwabik iron formation, Mesabi Range, Minnesota. This iron formation is divisible into four members. Each member is distinctive and contains marker horizons, which are recog nizable throughout all phases of alteration from lean, fresh rock to high-grade iron ore. Some beds have a larger magnetite content than others. During the process of ore genesis, which is essentially an oxidation process, the magnetite content is lowered. Alteration from iron formation to ore includes both oxidation of iron minerals and silica removal by leaching and these distinct processes progress at variable rates for different locations and structures. Magnetic intensities, of each horizon of the iron formation are dependent chiefly upon its preoxidation magnetite content, upon the subsequent degree of oxidation, upon the character of the enclosing rocks, and on the extent of fracturing, folding, or faulting. The results of a number of magnetic surveys are described and are correlated with results of drill-hole and mine exploration and developmerit. The magnetic anomalies obtained are discussed in relation to phases of formation of ore within the iron formation. General Information One hundred years ago a party of surveyors, applying the principles of geophysical prospecting, discovered iron ore in the state of Michigan in the Lake Superior district. This event was officially reported as follows:' On Sept. 19 (1844) while running the east line of Town 47 North, Range 27 West, they observed by means of the solar compass remarkable variations in the direction of the needle, amounting to 87" from the normal. Ascribing this phenomenon to iron ore, they sought and found it in ledges or outcrops at several points. The solar compass referred to was invented by William A. Burt, deputy surveyor in charge of this party.2 It is used for determining the true meridian by an observation on the sun. Eight years later, on July 7, 1852, the first iron 're, consisting of 6 bbl. of Ore, was shipped from Marquette, Michigan. It was another 40 years before the first or> shipment left the Mesabi Range in Minnesota, in October 1892. It totaled 4245 tons. Fifty years later, 90 years after the original shipment, during 1942 the Lake Superior district shipped 93,495,392 gross tons of iron ore. Production came from Minnesota, Michigan, Wisconsin, and Ontario, Canada. Throughout the 90-Year period it was known that magnetic properties of most of the ore bodies, and of the iron formations in which they occur, affected the compass. This phenomenon, later to be made use of to outline areas of ground favorable for exploration, was at first a

Jan 1, 1949

By R. H. B. Jones

This paper reviews pertinent geology of the Biwabik iron formation, Mesabi Range, Minnesota. This iron formation is divisible into four members. Each member is distinctive and contains marker horizons, which are recog nizable throughout all phases of alteration from lean, fresh rock to high-grade iron ore. Some beds have a larger magnetite content than others. During the process of ore genesis, which is essentially an oxidation process, the magnetite content is lowered. Alteration from iron formation to ore includes both oxidation of iron minerals and silica removal by leaching and these distinct processes progress at variable rates for different locations and structures. Magnetic intensities, of each horizon of the iron formation are dependent chiefly upon its preoxidation magnetite content, upon the subsequent degree of oxidation, upon the character of the enclosing rocks, and on the extent of fracturing, folding, or faulting. The results of a number of magnetic surveys are described and are correlated with results of drill-hole and mine exploration and developmerit. The magnetic anomalies obtained are discussed in relation to phases of formation of ore within the iron formation. General Information One hundred years ago a party of surveyors, applying the principles of geophysical prospecting, discovered iron ore in the state of Michigan in the Lake Superior district. This event was officially reported as follows:' On Sept. 19 (1844) while running the east line of Town 47 North, Range 27 West, they observed by means of the solar compass remarkable variations in the direction of the needle, amounting to 87" from the normal. Ascribing this phenomenon to iron ore, they sought and found it in ledges or outcrops at several points. The solar compass referred to was invented by William A. Burt, deputy surveyor in charge of this party.2 It is used for determining the true meridian by an observation on the sun. Eight years later, on July 7, 1852, the first iron 're, consisting of 6 bbl. of Ore, was shipped from Marquette, Michigan. It was another 40 years before the first or> shipment left the Mesabi Range in Minnesota, in October 1892. It totaled 4245 tons. Fifty years later, 90 years after the original shipment, during 1942 the Lake Superior district shipped 93,495,392 gross tons of iron ore. Production came from Minnesota, Michigan, Wisconsin, and Ontario, Canada. Throughout the 90-Year period it was known that magnetic properties of most of the ore bodies, and of the iron formations in which they occur, affected the compass. This phenomenon, later to be made use of to outline areas of ground favorable for exploration, was at first a

Jan 1, 1949

By W. J. Garmoe

Distinct areas of mineralized and non-mineralized brecciated rock are found in the Ontario Unit of the United Park City Mines. These breccias contain an appreciable fraction of the present ore reserves and probably will become even more important as deeper levels are developed. Three ages of breccia have been recognized in the Ontario Mine to date: ( 1) Pre-mineral breccia that may or may not be mineralized, (2) early post-mineral breccia with mineralized fragments, and ( 3) late post-mineral breccia that is younger than and cuts through ( 1) and (2) above. These age ,relations are known from detailed underground mapping. Locally, both pre-mineral and post-mineral breccias have sufficient lead-zinc-silver content, either as matrix or fragmental material, to constitute ore. Ore-grade breccias occur throughout a vertical range of over 1000 feet and are found in both the Humbug and Deseret formations from above the Ontario 1300 level to below the Ontario 2200 level. The mineralized breccias, which are difficult to distinguish on mine maps, are not well delineated by underground workings, and their horizontal outline and vertical extent are not known beyond the immediate mining areas. The greatest amount of truly mineralized breccia is exposed on the 2200 level.

Jan 1, 1968

By W. F. Chiao

With the application of dislocation damping theory an attempt was made to determine whether the generation and extension of dislocations is inherently more difficult in a brittle steel than in a ductile steel. A ductile steel was compared with a brittle stee1 by simultaneously measuring the ultrasonic attenuation and velocity during tensile test, and the density of free dislocations and their mean loop length were then calculated as a function of strain. The results showed that in the ductile steel there was always a large generation of dislocations and great extension of loop length occurring at some stage within the early plastic region. In contrast, the brittle steel showed very little or no such sudden changes in dislocation dynamic states after the onset of plastic deformation. Furthermore, a strong temperature dependence of dislocation dynamic states was also observed in the ductile steel and a hypothesis was suggested that a thermally activated process of dislocation rearrangement could occur at higher deformation temperatures. The activation energy of dislocation rearrangement at room temperature was estimated as about 2030 cal per mole.C. DUCTILITY is an indispensible property in the application of engineering materials, especially steel. During the past two decades the theoretical and experimental approach to the understanding of flow and fracture of metals has been constantly undergoing changes and progress." while the fracture behavior of metals can be influenced by many factors such as chemical Composition,3 second-phase particle mor-phology,4 and dislocation arrangement,5 it is now a general belief that the fundamental understanding of the ductile-brittle fracture phenomena of solid materials must stem from the study of dislocation dv-namics developed under stress conditions.6,7 Most of the traditional ductility tests, such as Charpy impact test, slow bend test, and tensile fracture test, cannot by themselves reveal directly the mechanisms of ductile to brittle transition of materials. In the experimental investigation of tensile ductility it would be ideal to be able to study directly the dynamics of dis-locations in a bulk specimen during the process of deformation. Since the ultrasonic pulse technique is the only satisfactory method for studying dislocations and the fine details of deformation characteristics in metals in the course of a tensile test, it would appear that a comparative study of ultrasonic attenuation changes during tensile tests of metallic materials exhibiting different ductility might be very informative. So far no work comparable to this study has appeared in the literature. Recent progress in both theory and experiment has indicated the feasibility of studying the dislocation mechanisms of ductility behaviors by ultrasonic measurements during tensile test. Granato and Lucke8 have developed a quantitative theory that enables the calculation of dislocation density and their average loop length from the measurements of ultrasonic attenuation and velocity, and several investigators, including Chiao and Gordon,9'10 have shown that simultaneous ultrasonic measurements can be successfully made during a tensile test. Furthermore, many investigators11-13 have repeatedly proposed in the past several decades that deformation and fracture are mutually self-exclusive, and that the ability or inability of a material to deform plastically, i.e., to generate dislocations, is a major factor in determining whether the material will be ductile or brittle. Thus, in the present work an attempt was made to determine whether the generation and extension of dislocations is inherently more difficult in a brittle steel than in a ductile steel. This article is principally concerned with the study of the relation between the propagation of ultrasonic waves and tensile deformation in a steel series which displays quite different toughness at room tempera-turk. changes in attenuation and velocity of ultrasonic waves have been measured as a function of strain during the deformation process. The results have been interpreted in terms of the vibrating string model for dislocation damping as developed by Granato and Lucke, and it has been found that some of the more subtle predications of the model are in good agreement with the experiments. This would be especially meaningful because most of the previous experiments in testfying the model were carried out with single crystals of high-purity materials and little work has been done with polycrystalline steel alloys. EXPERIMENTAL PROCEDURES AND RESULTS Specimen Materials. The tensile specimens used throughout this experiment were of two compositions selected from a series of Fe-Mo-0.77 pct Mn-0.22 pct C steels prepared for a ductile-brittle fracture transition study. One steel contains 0.21 pct Mo and the other 1.03 pct Mo. These two compositions were chosen for the present study because they possess quite different toughness properties at room temperature. The 0.21 pct Mo steel is quite ductile while the 1.03 pct Mo steel is rather brittle, as measured by the standard Charpy impact test. The alloys had been prepared by vacuum induction melting and chill casting in steel molds. The ingots were hammer-forged into 1/2-in.-sq bars from which tensile specimen blanks were cut. These blanks were first normalized under argon atmosphere at 1700°F and then reaus-tenitized and isothermally transformed at 1050°F to a bainitic microstructure. The chemical compositions, heat treatments, hardness measurements, and Charpy transition temperatures of the two steels are listed in Table I.

Jan 1, 1970

By L. T. Larson, M. L. Picklesimer

The relationship between the apparent angle of rotation of monochromatic plane polarized light and the tilt of the basal pole from the surface normal has been experimentally determined for zirconium over the wavelength range of 500 to 655 mp. This relationship allows the determination of the spatial orientation of the basal pole of an individual grain in a polycvystal-ling zivrconium specimen to within ±3 deg by three simple tneasurements with a polarized-light metallurgical microscope. The method of measurement is discussed in detail. THE optical anisotropy of materials having noncubic crystal structures has long been used to reveal features by polarized-light microscopy. Petrographers have used measurements of certain optical properties to identify and classify transparent or translucent minerals. More recent work (i.e., Cameron1) has extended such measurements to opaque minerals in reflected light. Few attempts have been made to make similar measurements on noncubic metals. Couling and pearsall2 have reported that a sensitive tint plate can be used in a polarized-light metallurgical microscope to determine the position of the basal-plane trace in a grain of polycrystalline magnesium. Reed-Hill3 has reported that the same technique can be used for zirconium. We have found that the precision of measurement can be increased to about ±0.5 deg by using a Nakamura plate4,5 to determine the exact extinction position after the sensitive tint plate has been used to locate approximately the basal-plane trace. This report describes a method for measurement of another optical property, the apparent angle of rotation. This measurement permits determination of the angle between the basal pole of a grain of a hcp metal and the normal to the surface of the specimen. When the two measurements are combined, the orientation of the basal pole in space can be determined from three simple measurements on a single surface. One to two hundred such determinations will permit plotting of a basal-pole figure for the polycrystalline material with reasonable accuracy. When normally incident, monochromatic, plane-polarized light is reflected from the surface of an optically anisotropic material, the light may be converted to elliptically polarized light, the plane of vibration may be rotated, or both may occur. The el- lipticity, the angle of rotation, and the reflectivity can be related to the indices of refraction and the absorption coefficients of the material.6,7 Ellipticity values can be determined with an elliptical compensator, but not with the ease and precision desirable for the present purposes. Measurement of the angle of rotation requires only the determination of the angle from the crossed position (90 deg to the polarizer) that the analyzer must be rotated to obtain extinction when the trace of the optical axis in the surface is at 45 deg to the vibration direction of the polarizer. The angle of rotation of the analyzer is approximately 6/5 that of the true angle of rotation of the light as reflected from the specimen because there is a small amount of additional rotation produced during the passage of the reflected light through the mirror of the microscope. Since we are presently interested only in determining the tilt of the basal pole, the angle of rotation of the analyzer (the apparent angle of rotation of the light, i.e., uncorrected) can be used. Precision of the measurement can be increased substantially by the use of a Nakamura plate4,5 in determining the extinction position. In an optically uniaxial material (hcp or tetragonal crystal structure) the angle of rotation depends only on the optical properties of the material and the orientation of the optical axis of the grain relative to the plane of incidence of the plane-polarized light.7,8 Thus, in a metal such as zirconium, the apparent angle of rotation at the 45-deg position in any given wavelength of light is a direct measure of the tilt of the basal pole from the normal to the surface. If the optical properties vary with wavelength, the apparent angle of rotation for any given tilt of the basal pole will vary. None of the required information exists in the literature for zirconium nor for any other non-cubic metal. MEASUREMENTS ON SINGLE-CRYSTAL ZIRCONIUM A single-crystal sphere of zirconium 9/16 in. in diam was spark-cut from a single-crystal rod grown from iodide bar by an electron-beam zone-melting process.9 The damaged surface was removed by chemical polishing in a 45/45/10 mixture (by vol) of water, concentrated HNO3, and HF (48 pct) and then electropolishing at 50 v in a bath1' of methyl alcohol and perchloric acid (95/5 by vol) at -70-C. The single-crystal sphere was mounted in a five-axis goniometer stage having a removable eucentric X-ray diffraction goniometer head for the two inner orientation axes. The basal pole of the single-crysta sphere was aligned parallel to a third axis of the goniometer stage by using the sensitive tint method to determine the basal-plane trace at several rotational positions of the sphere. The alignment was then checked by removing the sphere and eucentric gonio-

Jan 1, 1967

By E. S. Fisher, L. C. R. Alfred

The elastic anisotropy factors, c4,/c6,, c3,/cll, and c12/cl,, for hcp metal crystals vary significantly among the dgferent unalloyed metals. Significant variations with temperature are also found. The effects of elastic anisotropy on the dislocation in an elastic continuum with hexagonal symmetry have been investigated by computing the elasticity factors for the self-energies of dislocations in fourteen different metals at various temperatures where the elastic moduli have been reported. For most of the metals the effects of the orientation of the Burgers vector, dislocation line, and glide plane are small and isotropic conditions can be assumed without significant error. Significant effects of anisotropy are, however, found in Cd, Zn, Co, Tl, Ti, and Zr. The elasticity factors have been applied in the calculations of dislocation line tensions, the repulsive forces between partial dislocations, and the Peierls-Nabarro dislocation widths. It is predicted that the increase in elastic anisotropy with temperature in titanium and zirconium makes edge dislocations with (a), (a + c), and (c) Burgers vectors unstable in basal, pyramidal, and prism planes, respectively. The probability of stacking faults forming by dissociation of Shockley partials in basal planes also decreases with increasing c4,/c6, ratio, when the stacking fault energy is greater than 50 ergs per sq cm. The widths of screw dislocations with b = (a) in titanium and zirconium increase very significantly in prism planes and decrease in basal planes as c4,/c6, increases. The effects of elastic anisotropy on various dislocation properties in cubic crystals have received considerable attention during the past few years. In the case of cubic symmetry the departure from isotropic elasticity depends entirely on the shear modulus ratio, A = 2c4,/(cl, —c12); i.e., the medium is elastically isotropic when A = 1. Foreman1 showed that an increase in the ratio A produces a systematic lowering of the dislocation self-energy for a given orientation and Poisson's ratio. ~eutonico~, has shown that large anisotropy can have a marked effect on the formation of stacking faults by the splitting of glissile dislocations in (111) planes of fcc and (112) planes of bcc crystals. ~iteK' made similar calculations for (110) planes of bcc metals. Both studies of bcc metals showed that the large A values encountered in the alkali metals tend to reduce the repulsive forces between Shockley partial dislocations. In fcc metals, however, A does not vary over the large range encountered in bcc metals; consequently, the effect of A on the forces between Shockley partials is masked somewhat by the differences in Poisson's ratio between metals. The effect of A on the line tension of a bowed out pinned dislocation has also been investigated for cubic crystals, first by dewit and Koehler5 and more recent- ly by Head.6 In both cases the line energy model is applied and the core energy is not taken into account, thus making the conclusions somewhat tenuous with regard to the physical interpretation. Nevertheless, the fact that a large A decreases the effective line tension is clearly evident and the tendency for large A to produce conditions that make a straight dislocation unstable (negative line tensions) also seem evident. Head, in fact, shows visual microscopic evidence that stable V-shaped dislocations occur in 0 brasse6 For hcp metals the definition of elastic anisotropy is more complex and, furthermore, significant deviations from an isotropic continuum are found among a number of real hcp metals, especially at higher temperatures. The present work was carried out to survey the effects of elastic anisotropy on the elasticity factors, K, that enter into the calculations of the stress fields around a dislocation core. Some isolated analytical calculations have previously been carried out for several hcp metals but they are restricted in the dislocation orientations and temperature.8'9 The present computations are based on single-crystal elastic moduli that have appeared in the literature and consider various orientations requiring numerical computations. The results are then applied to survey the effects of temperature on the dislocation line tension and dislocation splitting in hcp metals. PROCEDURE Anisotropy Factors. The degree of elastic anisotropy in hcp crystals cannot be described by a single parameter, such as the A ratio in cubic crystals. The following three ratios must be simultaneously equal to unity in order to have an elastically isotropic hexagonal crystal: The magnitudes of these ratios at several temperatures, as computed from the existing data for the elastic moduli of unalloyed hcp metals, are given in Table I. There are no cases of complete elastic isotropy, but the large anisotropy ratios encountered in the cubic alkali metals are also missing. There are, however, several significant differences among the hcp metals, the most notable being the relatively small A and B ratios in zinc and cadmium and the differences in the magnitudes and temperature dependences of A. It has been noted that the temperature dependence of A has a consistent relationship to the occurrence of the hcp — bcc tran~formation. For cadmium, zinc, magnesium, rhenium, and ruthenium, A is less than unity at 4'~ and, with exception for rhenium, decreases with increasing temperature. In the case of rhenium, A has essentially no temperature dependence between 923' and 1123"~, so that it is clear that A does not approach unity at higher temperatures. Cobalt is similar to the above-mentioned group of metals in that it also does

Jan 1, 1969

By S. Sumski, M. B. Panish, R. T. Lynch

The liquidus isotherms in the gallium-rich corner of the Ga-Al-P phase diagram have been determined from 1000" to 1200°C and at I100°C the corresponding solidus isotherm was obtained. A simple thermody-namic treatment which permits calculation of the solidus and liquidus isotherms is discussed. A technique which was previously used for the growth of GaxAl1-xAs was used for the preparation of solution epitaxial layers of GaxAl1-xP and ALP. An approximate value of 2.49 i 0.05 ev for the band gap of Alp at 300°K was obtained and the ternary phase data were used to estimate a value of 36 kcal per mole for the heat of formation 0f Alp at that temperature. The Gap-A1P crystalline solid solution is one in which there exists the possibility of obtaining crystals with selected energy gaps, within the limits imposed by the energy gaps of Gap and Alp. Such crystals are of considerable interest because of their potential value for optoelectronic and other solid-state devices. Furthermore, it has been amply demonstrated for GaAs and GaP,'-7 that device, or bulk materials grown from gallium solution generally have more efficient radiative recombination than materials prepared in other ways. This presumably due to the lower gallium vacancy concentration in such material.= Small crystals of GaXAl1-xP and A1P have been grown from solution,8-10 and A1P has been grown from the vapor," but neither have previously been grown by liquid epitaxy. In this paper we present the ternary liquidus-solidus phase diagram of the Ga-A1-P system in the region of primary interest for solution epitaxy, and discuss the thermodynamic implications of that phase diagram with particular reference to the liquidus and solidus isotherms in the gallium-rich corner of the GaxAl1-xP primary phase field and to the A1-P system. Several measurements of the absorption edge of GaxAl1-xP crystals have been made and the width of the forbidden gap of A1P has been estimated from these measurements. EXPERIMENTAL The differential thermal analysis technique used to determine the liquidus isotherms and the optical measurements used in this work are similar to those described previously12 for the Ga-Al-As system, ex- thermocouples in the thermopile for added sensitivity. The materials used were semiconductor grade Ga, Gap, and Al+ The composition and temperature range at which DTA studies could be done was quite restricted. The upper temperature was limited by the chrome l-alumel thermopile to about 1200°C, and the highest aluminum concentration to about 5 at. pct by low sensitivity caused by the reduced solubility of Gap with increasing aluminum concentration in the liquid. DTA studies were not possible at 1000°C and below because of the low sensitivity caused by low solubility of Gap in the Ga-A1-P system. The cooling rate for these studies was about 1°C per min. No heating studies were done because of limited sensitivity. Supercooling probably does occur, but our experience with other 111-V systems indicates that it is no greater than about 10 to 15.c. Solid solubilities were determined by analyzing epitaxial layers of GaxAl1-xP grown from the liquid, with an electron beam microprobe. The layers were grown on Gap seeds by a tipping technique in which the layer is grown over a short-temperature range (20" to 50°C) on the seed from a solution of known composition. The tipping technique reported by Nelsson1 for GaAs could not be used, particularly for solutions containing appreciable amounts of aluminum, because of the formation of an A1203 scum on the liquid surface. A system was therefore designed, which would effectively remove the oxides mechanically, so that uniform wetting and crystal growth could occur. This tipping technique has already been described in detail." The best control over the composition of the re-grown layer was obtained when the tipping was done at a temperature which corresponded to the temperature of first formation of solid for the solution being used. Generally, therefore, a solution was prepared by adding the amounts of Ga, Gap, and A1 required to yield a solution which would be completely liquid above the tipping temperature with solid precipitating below that temperature. For most of the work reported here, the 1100°C isotherm of the ternary was used. It was generally necessary to heat the solution to 50" to l00. C above the tipping temperature to dissolve all of the Gap in a reasonable length of time. The epitaxially grown layers were used both for optical transmission measurements to aid in the estimation of the way in which the absorption edge changed with aluminum concentration, and for the electron beam microprobe analyses to provide data for the determination of the solid solubility isotherm. RESULTS AND DISCUSSION Liquidus Isotherms in the Ga-A1-P Ternary Phase Diagram: Thermodynamic properties of the system. The only thermal effect studied in this work was that

Jan 1, 1970

By R. A. Vandermeer, J. C. Ogle

Two distinct types of depth-dependent variations in texture have been observed in niobium cold-rolled various amounts up to 99.5 pct reduction in thickness. These nonuniformities are thought to be the results of nonhomogeneous plastic dewmation during rolling. The first type is characterized by a zone at intermediate depths that tends to lack certain strong orientations which are present in the surface and center layers of the rolled stock. This type of texture modification seemed to be associuted with "high" body rolling and may be related to the shape of the zone of deformation in rolling. The second type of texture inhomogeneity found involved the formation of a unique texture in the surface layers of heavily rolled strip. High fiiction forces between work piece and rolls appear to be needed to generate and maintain this texture. We believe that this unique surface texture results from a shear mode of deformation in the surface layers. THE evolution of texture in both the surface and center regions of cold-rolled niobium as a function of increasing deformation from 43 to 99.5 pct reduction in thickness was reported in a previous paper.' It was noted that for strips rolled between 95 and 98 pct reduction a distinctly different texture appeared in the surface layers which was unlike the center texture. Certain other layer to layer textural variations were also detected during the experimental phase of that work but were not described in the paper. Surface textures have been reported previously for the bcc materials iron and Steel2-4 and are well known in the fcc metals.5 It is usually stated that these are shear textures which arise under conditions of high friction between specimen and rolls. Work by Mayer-Rosa and Haessner5 n niobium rolled under conditions presumed to be high roll friction gave no indication, however, of a surface texture in that material. This is indeed puzzling in view of our results.' Thus we undertook additional experiments designed to study the stability of the surface texture for certain rolling variables. The variables investigated were the presence or absence of lubrication, amount of reduction per pass, and reverse vs unidirectional rolling. It is the purpose of the present paper to describe the kinds of depth-dependent textural inhomogeneities that we have observed in rolled niobium as well as to present the results of our recent experiments on the stability of the surface texture. Possible explanations for the depth-dependent texture variations will be discussed in terms of nonhomogeneous plastic deformation during rolling. EXPERIMENTAL Specimens cut from the niobium rolled to different reductions in the previous study1 were examined at various layer levels throughout the strip thickness for textural inhomogeneity. The specimen surfaces were either etched or machine ground and etched to remove material to a specific depth. Textures were determined by means of the Schulz X-ray reflection pole figure method with a Siemens texture goniometer and Cum X radiation. Since the important intensity peaks of the textures in niobium are usually located on the normal direction (N.D.) to rolling direction (R.D.) radius of the (110) pole figures, it was sufficient in many cases to scan only along this radius. At selected depths or where additional information was required the entire (110) pole figure was also obtained. In studying the stability and formation of the surface texture, experiments were conducted on 0.400-in.-thick, fine-grained, randomly oriented niobium specimens extracted from the same starting stock as that used in the earlier study.' Two of these specimens were rolled at room temperature to a total reduction of 96.4 pct. One was rolled between cleaned and degreased rolls with no lubrication. The other was lubricated between passes with Welch Duo Seal vacuum pump oil. The rolling schedules of each were kept as nearly identical as possible. Drafts were of the order of 0.006 to 0.012 in. per pass. Other experiments consisted of rolling specimens at constant fractional reduction per pass, i.e., (ta- tb)/ta equals a constant where ta and tb are the entrance and exit thickness of the rolled stock, rather than at a constant draft, i.e., ta- tb equals a constant. Ten specimens were rolled at room temperature on a two-high, motor-driven rolling mill with 8-in.-diam rolls. These specimens were rolled to thicknesses of between 0.041 and 0.073 in. (82 to 90 pct total reduction) at approximately constant reductions per pass ranging from 9 to 45 pct. Kerosene was used as a lubricant. Half of the specimens were always rolled in the same direction while the other half were reversed end to end at each pass. The texture in the surface regions was determined with the X-ray technique described above. RESULTS The textural inhomogeneities noted in niobium rolled from fine-grained, randomly oriented stock 1.5 in. long by 0.75 in. wide by 0.40 in. thick can be classified into two types. The first may be discussed with the aid of Figs. 1 to 3. Fig. 1 is a three-dimensional plot of the X-ray intensity in units of times random vs f , the angle from the N.D. to any point along the N.D. to R.D. radius of the (110) pole figure, and depth, given as percent of the thickness (?t/to X 100, where at is the thickness of material removed and to is the as-rolled

Jan 1, 1970

By S. R. Goodman, Hsun Hu

A detailed study of texture developmenf in poly crystalline copper atzd 70-30 brass has been completed. Textural changes as a function of deformation are shoum by pole jigmres and by intensity measurements oF- various rejlectiotzs from the rolling plane and the rolling direction. These examinations were accompanied by measurements of stacking fault frequency, hardness changes, and microstructure. Some of the results were briefly presented earlier. Additional results reported here are consistent with the idea that deformation faulting or slip by partial dislocations is of primary importance in the formation of deformation textures in fcc metals. lo examine the idea that deformation faulting is of primary importance in determining whether the texture is the copper type or the brass type an extensive study of the development of polycrystalline textures in copper and 70-30 brass was initiated. Besides the determination of complete pole figures, the intensities of the various reflections from both the rolling plane and the plane perpendicular to the rolling direction, the peak shifts due to deformation stacking faults, and the hardness of the rolled specimens were examined at various reductions from 10 to 99 or 99.5 pct. Mi-crostructures were examined by transmission electron microscopy. Some of the results were briefly presented in an earlier publication.' Since then, additional information has been obtained. This is given in the present paper. EXPERIMENTAL PROCEDURE Material and Specimen Preparation. The material used was a commercial electrolytic copper bar 1i in. wide and 2 in. thick and a 70-30 brass bar la in. wide and 1i in. thick. Chemical analysis indicated a purity of 99.97 pct for the copper, with 0.025 pct 0 as the major impurity. The 70-30 brass was of higher purity with 0.0016 pct 0 as the major impurity. Extreme care was taken in the preparation of the starting material to insure uniformly fine grains with a nearly random initial texture. The two bars were first cold-forged and then annealed to eliminate any original texture. The grains were then refined by several cold rolling (approx 30 pct reduction) and annealing treatments. The + -hr anneals were carried out in a salt bath at 390" to 440°C for copper and at 490°C for brass. The resulting penultimate grain size was 0.06 mm for copper and 0.03 mm for brass, and both showed very little preferred orientation. The number of prior cold rolling and annealing cycles was such that the final thickness after various final reductions of 10 to 95 (for brass) or 99 (for copper) pct was the same (0.020 in.). These annealed strips were rolled in two directions by reversing end for end between passes according to the following schedule: 0.006 in. per pass to 0.100 in., 0.003 in. per pass to 0.050 in., 0.002 in. per pass to 0.025 in., 0.001 in. per pass to 0.020 in. Texture Determination. The development of rolling textures was studied by examining complete pole figures determined from the (111) reflection. Specimens thinned from one face of the strip to half thickness (0.010 in.) were used to obtain the central portion of the pole figures, while specimens thinned from both faces to 0.003 in. were used to obtain the peripheral portion. The reflection and transmission techniques have been described previously. In addition to X-rav pole figures, texture development was also studied b; examining the intensity variation of the (Ill), (200), (2201, (311), (331), (420), and (442) reflections from the rolling plane and from the plane normal to the rolling direction, as a function of deformation. The same specimens used for the central portion of the pole figures were used for the intensity measurements of the various reflections from the rolling plane. For intensity measurements from the plane normal to the rolling direction, composite specimens were prepared by mounting sections cut parallel to the transverse direction of the strip. An epoxy resin was used to bond these sections together, and the entire composite was then mounted in a cold-setting resin to facilitate subsequent polishing and etching to remove distorted metal at the cut. The intensities were expressed in units of the integrated intensities measured from an annealed copper specimen having almost no preferred orientation. Stacking Fault Frequency Determination. Following the analysis of Warren: the stacking fault frequency, a, was determined from the change in the peak separation (A%) of two neighboring reflections of a deformed specimen, as compared with the normal peak separations of a fully annealed specimen. To obtain sufficient intensities for the second-order reflections, (222) and (400), composite specimens were prepared from parallel sections cut from the strip at 30 deg to the rolling direction for copper and 25 deg for the brass.* From texture data, these sections are known to contain a large population of both (111) and (200) planes. Since residual stresses can also cause X-ray line shifts (the direction of line shifts depends upon the sign of the stress), the use of composite specimens consisting of sectioned planes should help compensate for these effects as the residual stresses change sign from the surface to the central section of a rolled strip. Since the amount of peak shift is almost un-measurable in brass rolled 15 pct and in copper rolled

Jan 1, 1969

By A. G. McGregor

IN THE Southwest a number of large steel chimneys discharge the gases from the copper smelting furnaces. Some of these chimneys show no deterioration after twenty years, others show serious deterioration after tour years service. A steel stack 20 ft. 7 ½ in. (6.3 m.) in diameter by 279 ft. (85 m.) high, Fig. 1, used for roaster gases only at the Calumet & Arizona Mining Co.'s plant at Douglas, Ariz., was lined to the top of the bell, 40 ft. (12 m.) from the base, with common brick placed on end, lime and cement mortar being used. Above the bell, the stack was lined with 4 by 4 by 8 in. (10 by 10 by 20 cm.) building tile, placed on end, making a lining 4 in. thick. The tiles were supported on angle-iron rings, riveted to the inside of the chimney shell about 15 ft. apart. The chimney was put into use in the latter part of 1913. Four years later, considerable of the tile lining had fallen out of place and mixed with the flue dust at the bottom of the chimney. About a year later, several . flattened and distorted sheets were noticed about 70 ft. below the top. An investigation showed that the thickness of these distorted sheets, which was originally ¼ in., had been reduced one half. One year later, or six years after the chimney went into use, several holes, a square foot and smaller in area, appeared near the flat spots mentioned. Soon afterwards, when the chimney was shut down for repairs, it was found that most of the tile lining for 125 ft. from the top had fallen out and that the steel shell was badly corroded; but where the lining remained in place the shell was undamaged. Many of the tile which had fallen out of place had become soft or flaky and crumbling, others were as hard as when placed. An analysis of the hard and soft tile is shown on p. 2. These tile were of a fireclay mixture, and were used instead of common brick on account of lower cost. The steel forming the upper 125 ft. (38 m.) was replaced, and a 4 ¼ -in. (11-cm.) lining of firebrick was laid from the bell to the top of the chimney. The brick were placed on end, wedges and keys being used. After each 8-in. course was set, keyed, and wedged tight, thin mortar -water, sodium silicate, and finely ground silica-was worked into the joints. The brick are supported on angle-iron rings, every 15 ft., in the same way as the tile.

Jan 1, 1921

By R. P. Smith

THE carbon content of iron-silicon and of iron-manganese alloys at fixed activities of carbon has been reported previously.' It seemed desirable to investigate a system which allows a more extended range of alloy composition within a single phase region. The iron-nickel system is ideal in this respect, in that all alloys from 100 pct Fe to 100 pct Ni are face centered cubic ("austenitic") at 1000 °C. The experimental procedure was similar to that previously described.1,2 The alloys, in the form of pieces about 2 by 2 by 0.2 cm thick, together with a similar specimen of pure iron, were equilibrated with each of a series carbon monoxide-carbon dioxide tnixtures of fixed composition, quenched in the carburizing gas in the top of the furnace and then analyzed for carbon. The carbon content of samples containing more than 0.3 wt pct C was determined by the usual combustion method; those with less carbon

Jan 1, 1961

The Library of the above-named Societies is open from 9 A.M. to 10 P.M., except on holidays. It contains about 70,000 volumes and 90,000 pamphlets, including sets of technical periodicals and the publications of scientific and technical societies. Members of the Institute, with few exceptions, are forced to spend a portion of their time in localities isolated from sources of information. To these the Library, through its Library Service Bureau, can render valuable service through correspondence; letters requesting information will receive especial attention. The Library is prepared to furnish references and photographic copies of articles on mining and metallurgical subjects; to determine the existence of mining maps, and to furnish general information on the geology and mineral resources of all countries. All communications should be made as definite as possible so that the information received may be what is desired and not include collateral matter which may not be of interest. The time spent in searching for such collateral matter will be saved, and the information will be sent more promptly and in more usable shape.

Jan 7, 1917

By A. D. Zunkel, A. H. Larson

Equilibrium antimony contents of pb-sb alloys in contact with PbO-Sb2O3 slags containing less than 45 mole pct Sb203 uleve determined at 650', 700°, and 750°C in an inert atmosphere. In this ten~pevature range, the antimony contmzt of the alloy increased with increasing temperature at all slag compositions. The PbO-Sb203 phase diagram below 28 mole pct Sb2O3 was determined by thermal analysis and by application of a log sbZ4/y$b0 us plot determined from the equilibrium-activity data. The resulting phase diagram showed a eutectic at a temperature of 604°C and a comfiosition of 21.6 mole pct Sb2O, with a maximum terminal solid solubility of Sb203 in PbO of 5.6 mole pct. These results are compared with existing data in the literature. In the past three decades, only a small amount of experimental work has been done on the slag-metal equilibria in the Pb-PbO-SbaO3 or the analogous arsenic and tin systems. These systems are important in commercial lead-refining processes such as softening and dross fuming since it is impurities such as antimony, arsenic, and tin in lead bullion and Sb2O3, As2O3, and SnOz in lead drosses which must be re-

Jan 1, 1968

By D. A. Crerar, R. L. P. Kleinmann, R. R. Pacelli

A bacterium, Thiobacillus ferrooxidans, is of prime importance in the formation of acid drainage from pyritic material. Above pH 4.5, T. ferrooxidans increases initial acidification; below pH 4.5, it allows acidification to continue by oxidizing Fe2 +. Below a pH of approximately 2.5, the activity of F3+ is significant and results in steady-state cycling between oxidation of pyrite by Fe3 + and bacterial oxidation of Fe2 +. Laboratory and field tests demonstrate that inhibition of T. ferrooxidans by controlled release of anionic detergents can inexpensively reduce pyrite oxidation and acid formation.

Jan 1, 1982

By David R. Poirier

Activity data of carbon as a function of both temperature and composition throughout the stable austenite range is correlated by mearts of an equation derived from a quasi-chemical model. The carbon activity data of austmite for temperatures between 800° and 1200°C are utilized in conjunction with the activity of carbon calculated for the y solidus using the activity of carbon in liquid iron and published austenite-liquid equilibria. The results agree very well with Chip-man's correlation; however, a small difference in the activity of carbon in the high-temperature range of the austenite field is evident. Excellent agreement is found for the heat of solution of graphite in infinitely dilute austenite; from this study the value is 10,550 cal as compared with Chipman's value of 10,680 cal. AS part of a program to study microsegregation in dendritic solidification of ternary Fe-C-Cr alloys, it was desirable to be able to describe the equilibria between austenite and liquid iron in Fe-C-Cr alloys. In this regard, it was necessary to correlate existing data on the activity of carbon in Fe-C austenite as a function of both temperature and composition. At that time, Chipman's analysis1 of the thermodynamics of binary Fe-C austenite was not available. It will be shown that this study and Chipman's study agree rather well throughout the stable austenite range of temperature and composition; however, some small differences appear at temperatures greater than the eutectic temperature. Benz and Elliott 2 presented isoactivity lines for austenite superimposed on their revised Fe-C phase diagram. Using an expression from Darken and Gury 3 representing Smith's4 activity data between 800" and 1000°C, they found that the activities extrapolated above 1000°C to the solidus did not agree with the activities determined from the corresponding liquidus compositions. It is the purpose of the following argument to reconcile carbon activity data of austenite with the activity in liquid Fe-C alloys as determined by Rist and Chipman. 5 In addition, a simple analytical expression is sought for computational convenience. ACTIVITY DATA OF CARBON IN ZRON Fig. 1 shows the activity of carbon in Fe-C austenite as determined by Smith, 4 Schenck and Kaiser, 6 Scheil et a1.,7 and Bungardt et al.' The lines are merely drawn to separate the data into the respective isotherms. These data are inadequate to determine the activity of carbon at temperatures greater than 1200°C. The activity coefficient in Fe-C liquid alloys was assumed by Rist and chipmans to obey the following

Jan 1, 1969

By George Hulst

PRIOR to 1914, there was little demand for antimony in this country; its use was limited almost entirely to the manufacture of type and bearing metals. Practically no antimony ore was mined here, the market being supplied principally from China, and the alloy was produced by a direct mixing of lead and antimony. The great world war, with its demand for shrapnel in hitherto undreamed of quantities, precipitated a great boom in the price of antimony. Nominally quoted at 6 c. to 7 c. in 1914, the price increased by leaps and bounds to 45 c. in March, 1916. Under the stimulus of high prices many shall mines were opened, for it became profitable to work ores containing as low as 20 percent. antimony. High-grade sulfide ores (stibnite), containing 55 per cent. to 60 per cent. antimony, were received from Bolivia, China, and Alaska. Low-grade sulfide ores, running from 20 per cent. to 45 per cent., were produced in Nevada, California, Idaho, Utah, and Mexico; much of this ore was fairly rich in silver. The principal oxide ores came from Mexico and Oregon. The following analyses are representative of various types of antimony ore: Se Pn Cu Ao Au SIC), Fe S CAO ZN As Oxide Ore 25.09 46.02 0.95 0.40 10.98 0.30 0.22 Sulfide ore 5.5.20. 15.12 1.05 19.87 ? 0.40 0.25 Sulfide Ore 37.16 11.30 0.10 34.0 7.60 0.50 17.05 7.40 0.36 0.10 Sulfide Ore 41.55 15.00 0.20 76.0 0.04 5.60 0.25 18.17 0.85 0.25 0.10 The International Lead Refining Co. fortunately was equipped to handle these ores through residue and blast furnaces. The charge consisted of a variety of sulfide ores containing Sb 20 to 60 per cent. and Si02 6 to 45 per cent., oxide ores containing Sb 20 to 40 per cent. and SiO2 10 to 45 per cent. Secondary materials, such as battery plates, battery mud, lead oxide, paint, etc., together with refinery skims, softener skims, and other refinery byproducts, were treated along with the antimony ore to furnish the lead required. All silver-bearing antimony ores were treated in the residue furnace, the sulfur, iron, and copper forming matte that carried part of the silver, the balance going into lead bullion. The

Jan 9, 1919

By A. B. Tanner

The effects of radon in drillholes on gamma-ray logs have been described by L. S. Hilpert and C. M. Bunker1 Since these effects may cause drastic error in the evaluation of uranium deposits, it is useful to know the conditions under which significant amounts of radon tend to accumulate in drillholes. In the studies described here, atmospheric conditions were found to dominate in the control of the behavior of radon in drillholes in the vicinity of a uranium orebody. The site of the investigation was in McKinley County, New Mexico, about 12 miles north of Grants. Drillholes of 4 1/4-in. diam, on 25-ft and 100-ft centers, penetrate ore in dry rock at a depth of about 100 ft. A geologic log of the drillhole of primary interest is shown in Fig. 1. Gamma-ray logs revealed three zones of ore-grade mineralization in the Todilto limestone. A 6-ft zone, the lowest of the three, assayed 0.20 pct U3O8 by chemical analysis. The limestone ores in this area contain disseminated uraninite and some yellow and orange secondary minerals. Only radon"", a member of the uranium'" series, was measured in this investigation. Radon is one of the chemically inert noble gases and is radioactive by alpha particle emission with a half life of about four days. In this discussion, amounts of radon are expressed in microcuries (1 microcurie equals 37,-000 disintegrations per sec) and concentrations of radon are expressed in microcuries per liter of drillhole air. Samples of air were obtained by lowering a sampling device (Fig. 2) into a drillhole and actuating the device at the desired depth. It was then raised to the surface and the sample was transferred to a storage tube. Within two days the sample was transferred to an ionization chamber, and the activ- ity of radon and its short-lived daughter products was measured at radioactive equilibrium with a vibrating-reed electrometer. The measurements were corrected back to the time of collection and involve errors estimated generally not to exceed + 5 pct to —15 pct. Radon Behavior in a Covered Hole: Fig. 3, a typical log of radon concentration vs depth in the covered drillhole, was made by using values of radon concentration at discrete depths. Continuous logs of alpha-particle radiation in the drillholes showed that such radon logs depict the continuous variation of radon concentration with depth quite accurately. Three features of radon logs were noted: 1) maximum

Jan 1, 1960

By J. K. Buehler

With the rapid acceleration of the cost of shovel dippers and major standard shovel clipper rebuild components, maintenance management at Kennecott Copper Corp.'s Bingham Canyon mine initiated a dipper maintenance and rebuild program. The program focused on extending the service life of the shovel dipper, reducing field labor in maintaining dippers, and lowering shovel dipper rebuild costs. While comprehensive evaluation of the program is still underway, preliminary benefits of the program indicate: •Reduced field ,gelding for shovel dipper field maintenance, •Fewer dipper rebuild units entering the shop, and •Reduced dipper rebuild costs per unit.

Jan 1, 1979

By J. Halpern, D. R. McKay

SOME of the most important hydrometallurgical developments in recent years relate to processes involving the oxidation of sulfide minerals in aque- ous suspension at elevated temperatures by air or oxygen under pressure. Among these is the acid pressure-leach process which has been developed, particularly for the treatment of pyritic uranium ores.1-5 In this process, an aqueous suspension of the ore is digested in an autoclave, in which an overpressure of air or oxygen is maintained, at temperatures above 100°C. Oxidation of the pyrite (FeS,)

Jan 1, 1959

By George H. K. Schenck

The investment analysis methods that are most generally accepted in the mineral industries in the mid-80's are presented along with their advantages and disadvantages. Also covered are current widely-used practices for introducing the uncertain nature of most of the important variables in an investment analysis, which is contrasted to the former dominance of deterministic analysis. Finally, the discussion turns to current practice for handling the two critical areas: cost of capital and inflation. The advice contained is reinforced with data from a survey of current practices in the petroleum industry.

Jan 1, 1985