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By Wallace W. Key

Problems of marketing industrial minerals to chemical manufacturers are manifold. In addition to the difficulty of establishing demarcation lines between "crude" and "processed" industrial (nonmetallic) minerals, and "industrial mineral compounds" further uncertainty exists because some chemical manufacturers do not talk the same language as the industrial mineral producer. For example, paint technologists use "rutile" and "anatase" to describe highly refined chemical compounds. The earth scientists use these terms to describe naturally occurring minerals. Further, marketing research problems are intensified because of the overlapping data of the Standard Industrial Classifications (SIC) groups, and the inexactness of "Chemical Industry," "Chemical and Allied Products Industries," and "Chemical Process Industries," which are widely variable in meaning but are often used interchangeably. Bureau of Mines information Circular 8244, "Minerals for Chemical Manufacturing," was the out¬growth of an attempt to unravel some of the problems caused by overlap of statistical data compared with actual industry practices. Using this study as a base, specific industrial mineral applications of some important sub-industry groups were analyzed for the; California chemical industry. Differences between local and national practices were compared. Practices usually differed, depending on cost and availability of alternate minerals, climate, idiosyncrasies, local regulations, and other conditions. Bureau of Mines Information Circular 8260, "Mineral Fillers for the California Pesticides Industry," is the first such analysis of, a sub-industry group. Other such studies are underway. Obtaining national data is easy, but to be able to compile meaningful information which can be revealed on a regional and State basis generally is difficult and often impossible. This paper will briefly emphasize some of the industrial mineral problems encountered, and bring out the needs and benefits being derived through the continued cooperation of authoritative officials concerned with supply and consumption of industrial minerals in government and industry.

Jan 1, 1965

By George R. Schottler

The objective of this research is to find the extent of the range of applicability of previously developed statistical methods for determining grade and tonnage of ore to bedded uranium deposits. Uranium assays obtained from gamma-ray logs of exploratory drill holes are used to compute grade and tonnage of ore in the deposit by a standard polygonal method and by statistical analysis. The results obtained by the two methods are compared. The uranium-assay frequency distributions are shown to be lognormal and a simple transformation permits the use of standard normal curve statistics. The effects on the assay frequency distributions of stratified sampling, a required minimum mining thickness, and increased assay-interval length are investigated. The addition of low-grade mineralization to make up the required minimum mining thickness results in a distinct change in the skewness of the assay frequency distribution. Any statistical inference regarding grade-tonnage relationships that will be produced, using the minimum mining thickness, should be made on the basis of this "revised" assay frequency distribution.

Jan 1, 1965

By Malcolm T. Hepworth

RECENT interest in thermoelectric devices has been directed toward studies of the properties of thermoelectric materials of semiconducting solid compounds with little attention given to ionic and semiconducting liquids such as aqueous solutions, fused salts, and mattes. One type of thermoelectric system is the thermocell: a nonisothermal galvanic cell with two identical electrodes at different temperatures connected by an electrolyte bridge. An electromotive force, v, is generated which is a function of the electrode reactions and the properties of the electrolyte according to the Eastman' equation: where S* is the entropy change of the system arising from the electrode reactions and by heat transferred by ion migration and by thermal conduction. The quantity nF is the product of equivalents passed and Faraday's constant. A value of S* of 23.06 cal per "C is equivalent to 1 mv-Faraday per "C. The symbol, a, is used for dV/dT in analog to the See-beck coefficient of solid-state thermoelements. de Bethune2 has calculated the temperature coefficients of the electromotive force of a large number of nonisothermal aqueous cells from measurements on the nonisothermal temperature coefficients of the standard hydrogen electrode, combined with data on the isothermal temperature coefficients of half-cells tabulated in the literature. Values of these coefficients (a) in de Bethune's compilation ranged up to 3 mv per C. In particular he reported a value of +2.059 mv per "C at 25'C for the cell: Fe (aqueous, unit activity) (aqueous, unit activity) written for the hot-electrode reaction. The positive sign indicates that the hot electrode is positive (an "n-type thermocell"). In analog to a solid-state p-n system, it would be possible to couple two thermocells together to form a system in which the figure of merit could be calculated by adding the temperature coefficients according to the relationship described by offee:' where a is the Seebeck coefficient in volts per "C, p is the specific resistivity in ohm-cm, and K is the thermal conductivity in watts per cm "C. Even though ionic systems have rather high electrical resistivities compared with semiconducting and metallic systems, it was felt that a preliminary study of one ionic system should be made to establish some basis for evaluating the possibility of a p-n thermocell for energy conversion. Accordingly the Fe", Fe"' system was studied as a possible component for a p-n system. A glass system was constructed consisting of two vertical water-jacketed tubes connected by a horizontal tube, Fig. 1. Platinum-black electrodes 1 cm by 1 cm in dimension were inserted in each vertical tube with thermometers to register the electrode-compartment temperatures. The temperature of the electrode compartments was controlled by circulating water from thermostatted baths around the electrode compartments. The electromotive force of the cell was then read by a potentiometer for zero current as a function of the temperature of the hotter electrode. Current output of the cell for varying external loads was also measured. The cell resistance was measured by means of a bridge circuit with 10,000 cps signal and oscilloscope. Resistance measurements were converted to specific resistivity by calibrating the cell with a solution of known conductivity.

Jan 1, 1965

By Claude H. P. Lupis, John F. Elliott

WAGNERL described the thermodynamic behavior of a metallic solution consisting of the solute components 2, 3,... at very dilute concentrations in the solvent, 1, in terms of the excess partial molar free energy, or alternatively the logarithm of the activity coefficient. In the Taylor expansion of FiE, by neglecting the second- and higher-order differential terms, he obtained the excess partial molar free energy as a linear function of the composition:

Jan 1, 1965

By W. A. Wood, W. H. Reimann, Maria Ronay

The basic mechanism of fatigue is studied in annealed a brass subjectecl to alternating torsion at room temperature, 100°, 200°, 300°, and 400°C, and in air. It is shown that the slip-zone micro-cracking which characterizes fatigue damage produced by small amplitudes at room temperature is progressively replaced by grain boundary cracking at elevated temperatures, replacement being complete at 400°C. Replacement occurs not because slip activity decreases hut because slip movements at elevated temperatures cease to concentrate in narrow zones and instead disperse. Decrease of amplitude at 400°C through permitting longer lives of specimens before fracture actually causes in- MOST studies of fatigue at elevated temperature have been concerned with data for design. Observations on the basic mechanism of fatigue have been largely incidental, though they have led to the interesting inference that this mechanism has features in common with that of creep.' This paper is concerned primarily with the mechanism itself. Advantage has been taken of mater- crease in pain boundary damage, an anomaly attributed to the greater difficulty at elevated tempwature of starting and propagating a crack. Surface corrosion was most pronounced along slip bands but since at elevated temperatures the slip hands showed no cracking the surface corrosion did not appear to influence onset and early spread of fatigue damage. Similarly the type of fatigue damage produced at room temperature by cyclic strain at large amplitudes, characterized by irregular mi-crocracks at zones between disoriented regions in a grain, was also replaced by mainly grain boundary cracking at elevated temperature, though not so completely. ials and procedures known to show readily how fatigue affects the microstructure of a metal at room temperature, so that direct comparison might be made with what the same procedures show when the material is subjected to fatigue deformation at higher temperatures. 1) MATERIAL This was 70/30 a brass, used extensively in previous studies at room temperature.' Specimens were turned from extruded rod to have parallel test portions 1-1/4 in. long and 7/32 in. diameter, annealed to a grain size -1/10 mm, and electro-

Jan 1, 1965

By J M. Gibbs

Craigmont Mines Limited mine 50,000 tons of ore and waste per day from the open pit at Merritt, British Columbia. An electric-powered "down-the-hole" drill, a diesel-powered rotary drill and two electric-powered rotary drills have been used. All primary drilling, as a result of cost and operating experience, is now performed with two electric-powered rotary drills. Trials with various loading techniques have increased the amount of AN-FO and decreased the amount of commercially prepared slurries used for primary blasting. Approximately 95 per cent of the primary blasting is accomplished with AN -FO, mixed at the hole. Introduction THE Craigmont mine is located near the village of Merritt, B.C., 240 miles northeast of Vancouver. The concentrator has been in production since September of 1961. Craigmont is a combined open-pit and underground operation. To date, slightly more than 95 per cent of the mill feed has been mined from the open pit. As underground development proceeds, the ore requirements from the open pit will decrease. The average milling rate from September, 1961, to April, 1964, was approximately 4,900 tons per day.

Jan 1, 1965

By C. A. Stickels

The preferred crystallographic orientations developed during recrystallization of polycrystalline electrolytic iron sheet, cold-rolled 90 pct, were ivestigated. Recrystallization at 500° or 565° C for relatively short limes produces a texture which is similar to the rolling texture. A duplex partial fiber texture, significantly different from the rolling texture, is found when the annealing time is increased. Recrystallization at 700°C also produces a sequence of textures with increasing annealing time. In order of their appearance, these textures are: 1) the duplex partial fiber texture found at lower temperatures, 2) a four-component texture "near {322}(296)", 3) a {112)(110) +(111)(110) texture, and 4) a two-component "near {554)(225)" texture. Secondary recrystallization, or discontinuous grain growth, accompanies the development of the latter texture. However, the "near {554} (225)" texture was nol observed when secondary recrystallization occurred under other conditions. All of the ideal orientations found in recrystallization textures can be accounted for by the growth of minor components of the deformation texture. IN recent years there has been increased interest in improving the drawability of metals by controlling the preferred crystallographic orientation of the sheet.1-l3 Since more low-carbon steel is drawn than any other material, considerable attention has been focused on the properties of sheet steel. Efforts to improve drawability through texture control have been hampered by the lack of any published systematic study of the recrystallization textures developed in iron annealed below Acl. The purpose of the present work was to supply some of this missing information, specifically, the recrystallization textures obtained by isothermal anneals of polycrystalline iron, cold-rolled 90 pct. LITERATURE REVIEW—DEFORMATION TEXTURES Barrett14 reviewed and summarized the investigations of rolling textures in iron and low-carbon steel prior to 1952. The texture of heavily deformed iron (rolled 90 pct or more) is described as consisting of two partial fiber textures. The dominant fiber texture (designated here as fiber texture A) has a (110) fiber axis in the rolling direction and includes the orientations (001)[110], {112}( 110), and {111}(110). The secondary texture (designated here as fiber texture B) is described as having a (111) fiber axis in the sheet normal direction, and includes the orientations {111)( 110) and (111)(112). Since the publication of Barrett's book, there have been two detailed studies of the deformation texture in polycrystalline iron. In both instances, the more sensitive diffractometer methods of pole-figure determination were used. Bennewitz15 studied the cold-rolling textures developed in polycrystalline low-carbon steel and a 3 pct Si steel. He determined (110), (2OO), and (222) pole figures for specimens reduced 30, 50, 60, and 90 pct and analyzed his results in terms of partial fiber textures. He distinguished three stages in the development of the final deformation texture. 1) Grains rotate to form two incomplete fiber textures, with (110) fiber axes inclined 30 deg to the sheet normal toward the rolling direction (fiber texture B). After 50 pct reduction, the highest density of poles is near an ideal orientation {554}(225), the two components of which are members of this duplex fiber texture. 2) With increasing amounts of reduction, grains rotate about the former fiber axes toward ideal orientations of the type {112)( 110) (common to fiber textures A and B). 3) Finally, grains rotate about their ( 110) axis in the rolling direction, clockwise and counterclockwise from the orientations {112}(110). This produces the range of orientations from (111)(110) to (001)(110) commonly found in the rolling texture of heavily deformed iron (fiber texture A). No significant difference was found between the deformation textures of low-carbon and silicon steels. A few years earlier, Haessner and weik16 had determined (110) pole figures for carbonyl iron rolled to 30, 60, 80, and 90 pct reduction in thickness. heir data agree quite well with the more complete data of Bennewitz, but a somewhat different description of the evolution of the deformation texture was given. The appearance of (110) poles in the transverse direction is ascribed to a (100)[011] component rather than "near {554}( 225) " components, and the (110) fiber axes of fiber texture B are described as located 35 deg rather than 30 deg from the sheet normal. Both of these studies agree that the secondary texture present in heavily rolled iron, the duplex fiber texture B, has (110) fiber axes and not a single ( 111) fiber axis normal to the sheet, as

Jan 1, 1965

By W. Bonfield

A study has been made of the dislocation substructures produced in hot-pressed beryllium specimens strained to various levels in the range from 800 x 10-6 In. pev in. to fracture. A number of distinctive dislocation configurations were observed in this region which had not been noted at lower levels of strain. These included dislocation-dislocation interactions to form networks, dislocation "walls", subgrain boundaries and complex arrays, interactions between dislocations and large beryllium oxide particles, and the generation of dislocations from certain particles. The nature of these differences in substructure and their relation to the stress-strain characteristics of polycrystalline beryllium are discussed. In a previous study1 of the plasticity of commercial-purity, hot-pressed beryllium a transition was found in the deformation characteristics in the mi-crostrain region. The initial plastic deformation could be represented by a parabolic stress-strain equation, but above a critical stress there was a complete departure from this relation and a reduction in the strain-hardening rate. The dislocation configurations produced by various levels of micro-strain in this region were examined by transmission electron microscopy and a general correlation was established between the observed transition in deformation characteristics and the dislocation structure of the material. The two stages in the micro-strain region distinguished in these experiments were designated as Stage A' and Stage B'. Stage A' type deformation generally was noted up to a plastic strain of -80 x 10"6 in. per in. and Stage B' type from -80 x 10-6 to -800 x 10'6 in. per in. The discovery of two stages in the microstrain region naturally posed pertinent questions as to the existence of any further distinct stages in the subsequent plastic deformation. The purpose of this paper is to present a study of the dislocation configurations produced in similar beryllium specimens strained to various levels in the range from -800 x 10 in. per in. to fracture and to discuss the relation between substructure and the stress-strain characteristics. It is concluded that this region of strain can be considered as a distinct stage in the plastic deformation of polycrystalline beryllium. Tensile specimens of gage length 1 in. and cross section 0.18 by 0.06 in. were prepared from commercial-purity, hot-pressed QMV beryllium and then annealed at 1100°C for 2 hr. 2 followed by a careful chemical polishing procedure.3 The specimens were strained at a constant rate to various levels of strain in the range from -800 x 10-6 in. per in. to fracture (at 0.5 to 2 pct elongation), using the Tuckerman strain-gage technique1 to measure plastic and total strain. Thin foils were obtained from the strained and fractured specimens by chemical polishing3 and were examined using an RCA-EMU 3 electron microscope. Considerable care waS taken to avoid both accidental deformation during the preparation of the thin foils and excessive heating during their examination. Selected-area diffraction patterns were determined for each micrograph. Tilting experiments were also performed whenever appropriate to establish the dislocation zero-contrast position and hence determine the Burgers vector. This operation was sometimes not possible due to the rapid contamination of the foils which occurred in the electron microscope. RESULTS AND DISCUSSION To enable the distinctions between the dislocation arrays at high and low strain levels to be adequately made, the main characteristics of Stage A' and Stage B' deformation are briefly reviewed. 1) Stage A'. In the annealed starting condition there was a variable density (5 x 107 to 3 x 10' cm per cu cm) of isolated dislocations within a grain. The initial deformation in a tensile specimen was heterogeneous, with the dislocation density increasing in a few grains to 5 x 10g to 1.5 x 101° cm per cu cm. The deformation occurred exclusively on the basal plane by the movement of one or more 1/3 (1130) type dislocation systems. The dislocations were long and regular in form and nearly all the intersections exhibited a simple four-point node configuration. No interactions between glide dislocations and beryllium oxide particles were observed. 2) Stage B. In Stage B' there was a large increase in the number of grains exhibiting dislocation movement and also a change in the nature of the deformation, in which jogged dislocations and elongated loops became the characteristic feature. The splitting up of the elongated loops into smaller loops and the possibility of source action from the re-

Jan 1, 1965

By L. H. Wolfe, J. O. Thieme

The tensile and shear strengths of frozen soil and the compressive strengths of ice and frozen soil were measured These tests showed that the strength of ice and of frozen soil increased as the temperature was decreased. A method is presented for the measurement of thermal conductivity and specific heat of earth and ice. Using the parameters thermal conductivity, specific heat and density, the thermal diffusivity was calculated. Results of thermal property tests establish water as the major variable contributing to thermal property values. INTRODUCTION During the last few years, a considerable interest has developed in underground storage of cryogenic liquids such as liquid natural gas. Because of its economy and safety, underground storage is being used. Before underground caverns could be seriously considered, however, the strength and thermal characteristics of the soil had to be obtained. Methods are presented herein for measuring tensile, compressive and shear strengths, specific heats and thermal conductivities. The tests were performed on two soils at temperatures from ambient to -195C. Because it is difficult to find data in the literature that pertain to a particular soil, ice was used to evaluate some of the experimental procedures. Some of our ice data are compared to the published values. PHYSICAI, PROPERTIES SOIL SELECTION AND SAMPLE PREPARATIONS The physical and thermal tests were performed on recompacted samples of two typical soils that might be encountered in underground caverns: a gray, fire clay that had been pulverized and mixed with water into a pliable mud; and a brown, sandy silt that was dug from a dry river bank and subsequent1y mixed with tap water. The moisture content of the test specimens was 17 to 22 per cent (based on the wet weight of the soil). This amount of water nearly saturated the silt, but the clay was well below the saturation point. The soils are partially described by the sieve analyses (Fig. 1) which show the particle size distribution of the coarser than 44 micron portion of the soils. The curves also show that approximately 75 per cent of the clay and 20 per cent of the silt are finer than 44 microns. The particle size seems to affect some of the physical properties, and the finer than 44 micron portion is important in the thermal conductivity test. Physical specimens were cut with a bandsaw from frozen blocks of the soil. The specimens were then sanded and kept frozen until after they were tested. They were stored at the approximate test temperature for several hours. Then, to equilibrate the samples to the test temperature, they were stored at the temperature at least an hour before they were tested. TEST EQUIPMENT An Instron, which is a constant speed gear-driven instrument, applied force to the samples and drew stress-strain plots of the test. All of the samples were strained at 0.02 in./min. All of the physical tests were conducted in a temperature cabinet that controlled the temperature to 1C. TENSILE STRENGTH Briquette or "dog-bone" shaped tensile specimens were pulled with suitably shaped jaws. This shape of specimen, which is usually used for tensile tests of concrete, is satisfactory for testing frozen soils except that the samples tend to

Jan 1, 1965

A drive, 3,500 ft long, was planned to explore mineralization exposed by diamond drilling. A rate of advance of 150 ft per fortnight, approximately double previous Broken Hill rates, was required. Subsequent to the completion of this drive its extension for a further 6,200 ft was planned to provide a main haulage way along which ore could be transported from a newly acquired lease back to the main hoisting shaft, a total distance of 13,500 ft.This paper describes the working conditions, relationships, manning and costs, and gives details of the cycle and equipment used to achieve rates up to 170 ft per fortnight.OBJECTIVEDiamond drilling from the 1,000 ft level at the Delprat Shaft section had indicated that the zone of mineralization, about 150 ft wide, which had been explored on the 1,000 ft level for a length of 2,600 ft, continued downwards with a westerly dip. The drilling results showed that within this wide zone there were arrower lenses of mineralization of possibly payable grade (see composite plan, Fig. 1).Diamond drill holes of 2,000 ft and over, particularly through heavily sheared areas of sericite schist, had been found to be costly, slow, and inadequate in testing the potential and trends of these smaller concentrations of mineralization.It was therefore decided that an exploratory drive should be advanced from the northern limit of the 1,480 ft level into the western mineralization, and that from this drive diamond drill holes should be drilled at dose intervals to outline the ore.The 1,480 ft level was chosen for the following reasons.1. It had the greatest northerly reach of the accessible levels at No. 7 Shaft section below the 1,000 ft horizon and therefore would enable the test to be made most quickly.

Jan 1, 1965

By R. C. Hepworth

Heaving in roads built on the Mancos Shale is a serious problem in east-central Utah. Heaves are expressed as local bumps, general rises and severe cracking of the pavement. The heaves usually occur in shale road cuts and generally show a seasonal cycle, which reaches a maximum development in the winter. The presence of certain salts, absorption of moisture and physical properties of the subgrade materials were considered, in Utah, to be the main factors in the heaving mechanism. Work done on similar problems elsewhere and studies conducted by the author indicate that the latter two factors are the most important. Results of this investigation indicate that heaving areas are associated with slaking shale or expansive clays, with and without salts present. Laboratory studies show that the initial moisture content of remolded samples and the desiccation history of un- disturbed samples have a major effect on swelling. Swell tests on compacted samples at various temperatures indicate that water has more influence on swell than temperature, except for samples containing sodium sulphate, which swelled with decreasing temperature. Chloride salts inhibited swelling. Tests on shale cores indicate that the stability of slaking shale can be preserved by maintaining its original moisture content. It is concluded that shales and expansive clays, when exposed in road cuts, become desiccated and are subject to expansion when moisture is subsequently available. The seasonal cycle of heaving may possibly be explained by the annual moisture excess and deficiency. To minimize the problem, freshly exposed shale should be kept wet, and the thickness of the subbase and base courses should be increased. The Utah State Department of Highways has been plagued for many years with a distressed condition that develops in roads constructed on the Mancos Shale. Locally these distressed areas are known as heaves, frost boils and alkali boils. These names refer to the surface expression, time of year

Jan 1, 1965

By Sofoulis J

In the Archaean of the Kalgoorlie-Norseman area, the layered rocks have been subdivided into two sequences, both containing basic igneous rocks and sediments. The lower sequence is distinguished by the presence of acid volcanic flows and large acid sills. The upper sequence is unconformable on the lower one.In some areas, clastic sediments become coarser and pass into conglomerates. Th:s passage is accompanied by thinning of the beds.These features and their distribution suggest a basin of subsidence flanked by areas of shore-line conditions.Repeated igneous activity, including vulcanism, has occurred along the flanks of this basin. These different igneous and sedimentary environments have played an important part in the primary distribution of metals.A chronology of all basic and acid igneous activity, as well as sedimentat:on, has been established for the Precambrian of this area.INTRODUCTIONThe subdivision of Archaean rocks into those of basic igneous or of sedimentary origin has formed the basis for the nomenclature appearing in past literature. These subdivisions were distinguished as greenstones (predominantly basic igneous rocks) and whitestones (predominantly sediments), and it was generally accepted that the greenstones were stratigraphically lower in the sequence than the whitestones.Recent studies show that, between Kalgoorlie and Norseman, basic igneous rocks interfinger with and pass laterally to sediments, and that basic volcanic rocks occur at different stratigraphic levels. Younger Precambrian. units are also...

Jan 1, 1965

Jan 1, 1965

By R. J. Wasilewski

The variation of elastic modulus with terrzperature between -150° and 600°C has been investigated. Compounds close to equiatomic cornposition exhibit very low modulus values and very high damping near room temperature. The modulus rises steeply with both decreasing and increasing temperature. The modulus minimum and the high damping are believed to be connected with a martensitic transformation of TiNi. In bulk material this transition takes place slightly above room temperature quite rapidly and reversibly, with a hysteresis of some 30°C, depending on the Ti:Ni ratio. Oxygen impurity affects the reaction time. THE inter metallic compound TiNi has been reported to exist in an ordered CsCl (B2) structure,l-6 the homogeneity range varying rather markedly with temperature.7 Some investigators reported this compound to decompose peritectoidally to Ti2Ni and TiNi, between 650° and 800°C,3 or below,',g the latter workers also suggesting the decomposition to be strain-sensitive. Purdy and Parr were the first to report a structural transformation to a new, possibly hexagonal, structure at 36°C,7 a temperature indubitably too low to allow the significant amount of diffusion necessary for a peritectoid reaction. Mechanical-property investigations of compositions close to TiNi just above room temperature have qualitatively shown remarkable anomalies, particularly with respect to clamping,' and to a "memory" effect, that is, plastically deformed material returning to its original shape on being heated through the "decomposition" temperature.9 The original explanation of this effect—based on the apparent experimental observation of Ti2Ni or TiNi, formation in the material subjected to tensile or compressive stresses, respectivelp—does not appear plausible. It appeared more probable that the change involved may be a martensitic, diffusionless structural transformation, similar to those observed in other B2 structures such as 0 brass,'' AuCd,ll and AuZn.12 The existence of such transformation has been established recently,', although the symmetry of the low-temperature structure is not yet known. The present paper describes the elastic modulus and damping behavior of polycrystalline TiNi in both structures. EXPERIMENTAL METHOD 1) Specimens. All the specimens to be investigated were prepared from premelted electrolytic nickel and iodide titanium by nonconsumable arc melting and casting in a water-cooled copper mold. The cast billets were canned in mild steel, extruded, and swaged to approximately 0.375 in. diam. The cans were then removed by pickling or machining. Preliminary material balance checks indicated no significant weight losses on melting (less than 5 mg on a 50-g button); hence nominal compositions have been used throughout. In agreement with previously reported observations7 no single-phase material was obtained at—or close to—Ti 1.00 Ni1.00 a small amount of finely divided second phase always being present. It was found that most of the oxygen impurity was associated with this minor phase, which was identified as oxygen-bearing Ti2Ni—possibly Ti,Ni,O. The amount of this phase—at any given Ti:Ni composi-

Jan 1, 1965

By D. L. Creighton, S. A. Hoenig

The field-emission microscope has been adapted for the study of microcrack growth during the early stages of fracture in metal wires. Cracks as small as 6 1 in length can be detected and their growth can be followed to specimen failure. The system is quite useful in searching for microcracks since only sharp-edged surface defects will emit electrons under the experimental conditions. THE conditions leading to brittle fracture were discussed a number of years ago by Griffith1 and the term Griffith Cracks is often used for the small surface cracks which are responsible for brittle fracture. Griffith's theory has been modified by stroh2 and more recent results on metals are discussed by Allen,3 pp. 123-40. At present the phenomenon is not completely understood but there is general agreement that at least in certain materials the sequence leading to brittle fracture involves several stages. The initial microcracks are present because of cooling or working stresses, Hahn et al.,3 p. 95. When a stress is applied to the specimen the cracks grow slowly until the release of stored elastic energy is large enough to accelerate the crack and provide the necessary surface energy for crack growth. At this point the growth rate appears to increase rapidly to some new equilibrium velocity, and failure occurs. Since the microcracks are usually about the size of a single metallic grain (Ref. 3, p. 99) it is not easy to find them and it is very difficult to follow their growth under stress. This paper will report on the use of a cylindrical field-emission microscope for observation of the formation and growth of microcracks. I) THE FIELD-EMISSION MICROSCOPE The field-emission microscope (FEM) has a high magnification and resolution and is almost uniquely suited for observations of microcracks. Since the FEM is relatively new as a metallurgical instrument, a short description will be given here. Normally metals at room temperature do not emit electrons; however in the presence of a strong electric-field gradient, electrons can tunnel out through the reduced potential barrier. Since this tunneling is a function of the local field gradient and the local work function, the emitted electrons can be used to produce a highly magnified image of the surface by allowing them to strike a phosphor screen. Because the electron emission is dependent upon the local field gradient, smooth surfaces emit few electrons except at very high fields. On the other hand cracks, extrusions, or other surface defects, having sharp edges, emit strongly since the field gradient is very high in the vicinity of these defects. This indicates that the FEM should be most useful for detection of microcracks on otherwise smooth surfaces. A field-emission microscope was first used by Muller4 in 1936 for observation of metal surfaces, and recent reviews have been given by Muller5 and Gomer.6 The instrument has been used for metallurgical studies in the area of surface diffusion,= recrystallization,7 and grain growth 8 (Ref. 8 is directed specifically at metallurgists). In the work of Muller4,5 and Gomer 6 the specimen was in the form of a sharp metal point at the center of a phosphor-coated glais sphere. The impact of the emitted electrons on the phosphor produced a highly magnified image of the specimens. Such a system is not practical for applying a controlled stress to the specimen and a cylindrical geometry has been used in this investigation. This allowed the application of a controlled tensile stress to the wire specimen. Normally a cylindrical FEM geometry produces magnification only in the radial direction. This is the case because a smooth wire at the center of a cylinder produces a purely radial electrical field. However, if there is a break in the smooth surface of the inner cylinder, the field near the break becomes three-dimensional and the area of the break is highly magnified. The reason for this is clear if it is recalled that the field gradient depends on the relative radii of the inner and outer cylinders; if a crack forms, its edge radii are of atomic dimensions and a very high field gradient is formed near these crack edges. Since the electrons receive most of their acceleration near the crack edge and are always traveling perpendicular to the field lines, they tend to spread out and produce the magnified image observed in the cylindrical field-emission microscope. 11) BRITTLE-FRACTURE STUDIES A) Experimental Apparatus. The geometrical arrangement chosen was that used earlier by Gifford

Jan 1, 1965

By E. T. Turkdogan

This paper deals with an analysis of the conditions leading to the formation of blowholes and surface and subsurface defects in cast low-carbon steels. The theoretical analysis of the problem is based on the concept of the occurrence of deoxidation reactions during cooling of liquid steel and during its solidification. The reaction equilibrium data are given on deoxidation of steel by carbon, silicon, and manganese. The details of the calculations are given on the simultaneous deoxidation of steel by silico-manganese additions to produce a desired level of deoxidation at certain residual concentrations. Based on an idealized model, an attempt is made to calculate the enrichment of solutes in the solidifying liquid entrapped within the interdendritic cells which are known to be less than 200 µ thick. Formulae are derived for the calculation of the change in the residual oxygen content of the enriched liquid steel, controlled by Si/Mn deoxidation. It is shown that for every particular initial silicon, manganese, and oxygen concentration in steel (as residuals in liquid solution at the beginning of solidification) there is a particular carbon concentration below which carbon monoxide, leading to blowholes or pinholes, is not expected to form. There are a number of independent variables which have a decisive influence on the formation of blowholes. For example, it is shown that the position of the curve depicting the critical relation between initial silicon and carbon content for suppression of the evolution of carbon monoxide) can be shifted to lower silicon or higher carbon levels by: increasing manganese content; decreasing oxygen, hydrogen, or nitrogen content; or increasing external pressure on the solidifying mass. FOR the production of sound castings it is essential to prevent the formation of interdendritic worm-holes or pinholes brought about by gas evolution during solidification. Another major problem encountered in solidification of ingots is the formation of surface defects. These problems are thought to be closely associated with the deoxidation reaction occurring in liquid steel during cooling and subsequent solidification. As the liquid becomes richer in impurities during dendritic solidification of steel, a series of reactions may occur in the liquid phase trapped within the branches of growing dendrite platelets. Because of the strong interaction between dissolved oxygen and impurities in liquid steel, the reactions most likely to occur are of the deoxidation type. However, inherent to the extreme complexity of the problem in question, numerous simplifying assump-

Jan 1, 1965

J. H. Lord (Geological Survey of Western Australia): During the last few days in Kalgoorlie here we have heard on various occasions of the great job the mining engineers have done persisting against rising costs and increasing salaries without a rise in the price of gold. I think it has been somewhat overlooked that it has been difficult to find additional ore as well. I consider that geologists also should be commended on their action in persisting to search for more orebodies. This goes on in any mining community, but in Kalgoorlie in particular, I believe, over the last few years that it has been more difficult all the time to find additional orebodies and the Companies are calling for higher grades to offset the economic condition. I feel that this paper by Mr. Finucane shows that the geologists have persevered on an idea and discovered that they can find additional orebodies in the calc schist where previously it was thought that these did not occur. This has added many tons to the ore reserves, and although it is not very significant at the moment, the significance will probably improve as more work is done.The whole thing has shown us the importance of economic geology. Mr Finucane has had many years of experience here and he has given us a very able exposition of the economics of ore finding, and there are not many questions that one could pose to him, because most of the information he presented is obviously fact borne out by drilling, underground development and lining up the ore channels. He did briefly touch on ore shoots-the Oroya shoot and several others. It would be very good if we could, and I feel sure...

Jan 1, 1965

By T. S. Lundy, J. Askill

J. Askill and T. S. Lundy (Oak Ridge National Laboratory)—Moore has proposed a simple correlation between the activation energy for solute diffusion in fee metals and the atomic volume of the diffusing species using both tracer and chemical-diffusion data. The first point we wish to make is that it is wrong to attempt such correlations without separating the two types of data. Activation energies obtained using tracer techniques cannot, in general, be directly compared with those obtained from chemical-diffusion experiments. A knowledge of the variations of chemical potentials with composition is necessary and chemical-diffusion data must be corrected for such variations, even for dilute alloys, before a comparison is possible. Secondly, for nickel, iron, aluminum, and lead, Moore neglected a number of recently published works, e.g., Al26 and Mn54 in aluminum,46 cr51 in nickel,47 and Fe55 in iron.48 These and others should have been used. If one considers only the tracer diffusion data, there is left no simple correlation of the type proposed by Moore. For example, in the case of solute diffusion in aluminum the only reliable tracer data listed by Moore are for zinc and aluminum. The nickel, cobalt, and iron data of Agarwala49 are representative of near-surface diffusion-not bulk diffusion. In conclusion we suggest that for tracer diffusion data in these fee metals there is no justification for proposing any simple correlation of activation energy with atomic volume using the limited data that are presently available. R. H. Moore (author's reply)—The writer has proposed a simple correlation which is useful in estimating the internal consistency of diffusion data. The accuracy of the correlation is, of course, a function of the number of data available. Lundy and Askill take issue with the writer's decision to include data for the systems: nickel, iron, aluminum, and lead, taking the view that the data are insufficient to establish the correlation. The writer agrees that the data are insufficient and has cau- tioned the reader that the correlation is tentative in these instances. Inclusion of these systems is justified by the interesting trends the correlation reveals. For example, the distinction between interstitial and substitutional diffusion may be clearly established, Figs. 4 and 6, and the behavior of transition elements and nontransition elements is indicated to parallel the behavior illustrated by the silver and copper systems. Lundy and Askill have singled out the aluminum system for special criticism. The writer chose to discuss the data for diffusion of iron, nickel, and cobalt in aluminum in the terms used by the original authors9 and has included the comments of Balluffi.l0 The writer did not intend the reader to conclude that data for these elements should correlate with data for the nontransition elements as Lundy and Askill have evidently assumed. Iron, nickel, and cobalt form intermetallic compounds with aluminum, so the activity coefficients of these elements may be expected to deviate markedly from unity. This may account for the low frequency factors observed by Hirano.9 The nontransition elements, on the other hand, yield relatively simple phase diagrams with no evidence for intermetallic compound formation as in the case of iron, nickel, and cobalt. In dilute solution, Henry's law should be closely obeyed, the activity coefficients should not deviate markedly from unity, and the effect on the activation energy should not be large. The accuracy of the correlation applied to these systems will improve as the data is extended. It does not seem unreasonable to conclude that its extension should be encouraged.

Jan 1, 1965

By Desmond De Villiers Oxford, Peter H. Williams

Nchanga Consolidated Copper Mines, Ltd., is one of the four mines operated by the Anglo American Corp. in Northern Rhodesia, now the independent nation of Zambia. Today Nchanga is the second largest single producer of copper in the world, accounting for more than 200,000 long tons of copper annually at a monthly milling rate of 430,000 tons of ore. The average mill-head grade is about 5.20% total copper, of which approximately 60% is copper sulfide. The remainder, referred to as "acid soluble," is copper oxide. Nchanga mines three separate orebodies varying in grade and sulfide-to-oxide ratio. Ore is processed in two separate grinding circuits feeding into three separate flotation circuits. A fourth flotation circuit treats leach plant residue for additional recovery of sulfides.

Jan 1, 1965

By Richard H. Hopkins, R. W. Kraft

A new technique facilitating the rapid determination of the three-dimensional morphology of phases suspended in an opaque matrix is described. The vapidity of the technique is based upon continuous cinephotomicrographic recording of specimen microstructure as the specimen surface is removed under controlled conditions in an electrolytic cell. The advantages of the technique for determining spatial morphologies in opaque materials are illustrated by application of this method to the study of the configuration of faults in a specimen of directionally solidified CuAl2-Al eutectic alloy. A spatial model of the eutectic fault network deduced in this manner has substantiated the facts that faults in this alloy tend to lie parallel to one another in a direction close to that of the specimen growth axis and that the majority of faults tend to bridge lamellae rather than run parallel to them as growth proceeds. For the specimen studied fault density decreased as growth proceeded. ALTHOUGH metallographic observation is a powerful tool for investigating the correlation between structure and properties in metallic alloys, ordinary metallographic methods suffer the fundamental limitation that any conclusions concerning the three-dimensional structure of these opaque materials must rely upon inference from two-dimensional microsections. For this reason it is frequently impossible to make valid judgments regarding the true spatial distribution of the micro-constituents in specimens under investigation. Several techniques have been devised to circumvent the basic limitation of planar microsec-tioning and employed with varying success. These include construction of three-dimensional models of alloy microstructure from sequences of photomicrographs,1-3 quantitative deduction of spatial features based upon statistical studies of data from random and/or selected plane microsections,4-6 and selective dissolution of one phase in a two-phase alloy to reveal the topography of the phase remaining.' However these techniques also have certain obvious disadvantages. Construction of three-dimensional models is a very time-con- suming procedure due to the tedious polish-etch-photograph cycle needed to obtain the necessary photomicrographs to portray the spatial microstructure. Statistical methods by their very nature give only average values of the quantities being studied and cannot therefore give a detailed physical picture of the microstructure to be observed. Finally, the technique of selective dissolution is only applicable in systems where the phases are of vastly different chemical reactivity; it is of little use in the study of single-phase alloys. Since the determination of the three-dimensional structure of opaque materials is hindered by two facts—the materials are opaque to radiation in the visible spectrum and construction of spatial models of microstructure is quite laborious—two solutions to the problem suggest themselves: 1) use radiation of energy great enough to render the alloy transparent, i.e., some microradio-graphic method, or, 2) devise a rapid means to section and record alloy microstructure. Stereomicroradiography has indeed been used to study internal arrangements of phases in several materials8,9 but the method, in general, is limited to very thin specimens (due to X-ray absorption) and simple microstructures. It would seem then that development of a rapid, simple, and generally applicable technique for studying the details of alloy microstructures in three dimensions can best be undertaken by following the second approach above. Using this idea a new technique for rapid evaluation of spatial microstructures was developed based upon cinephotomicrographic recording of the micro-structure of a specimen undergoing controlled electrolytic dissolution. It was further felt that application of this technique to the careful study of the spatial configuration of faults in a CuAl2-Al eutectic alloy would yield information that could be correlated with the extensive data3,6,10-12 already compiled concerning the solidification and crystallography of this eutectic. The practicality and usefulness of similar methods for studying three-dimensional features in alloys has recently been illustrated by the study of dislocation loops in zinc13 and spheroidized structure in steel.14

Jan 1, 1965