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By J. B. Gayle

The Bureau of Mines studied the effects of air oxidation on the recovery of float coal. Both batch-and continuous-type tests were made on six bituminous coals, representing the range in rank of coals now commercially used for carbonization, and on one anthracite coal. The effects on flotation recovery of oxidation at 1000 C for periods up to 50 days were investigated using an alcohol-type frother and a kerosine-pine oil reagent. Two series of release analysis tests were made, using one medium-volatile bituminous coal. Float coal recovery was adversely affected by oxidation in all tests where the alcohol-type frother was used. Conversely, a small degree of oxidation improved recovery with kerosine-pine oil frother for some of the coals in continuous tests. Prolonged oxidation (beyond about 14 days) adversely affected float coal recovery for all coals, the effect being more pronounced for batch-type tests and for tests using alcohol-type frother. Reagent selectivity for the rejection of both ash forming and sulfur bearing minerals was reduced by oxidation. Severe reduction of reagent selectivity required only about 3 days' oxidation for alcohol-type frother but more than 10 days' oxidation when the kerosene-pine oil reagent was used.

Jan 1, 1965

By John F. Elliott, John R. Rawling

The rate of reduction of silica to silicon by carbon at 1550° to 1700°C in iron blast-furnace type slag-metal systems has been investigated. In the tower portion of the temperature range oxygen transport in the metal boundary layer at the slag-tal interface is probably rate limiting. A second step, which apparently involves a chemical process in the slag at the slag-metal interface, appears to be rate limiting when the oxygen-transport limitation is avoided. Above 1650°C rate control of the reduction by carbon probably is mixed between the two steps. INVESTIGATIONS1.2 into the equilibrium distribution of silicon between graphite-saturated slags and metals typical of iron blast-furnace practice show that, under the experimental conditions specified, the reduction of silica to silicon is relatively slow compared with the rates of other slag-metal reactions under similar conditions. For this reason, the reduction of silica in blast-furnace slag-metal systems was considered to be an interesting subject for further study. Investigations of the kinetics of the reaction3-5 suggest that several possible steps may be rate controlling, and that the rate-controlling step depends not only on the physical state of the systems but also on the configuration of the apparatus. The main objects of the investigation reported here were to sug- gest plausible reaction paths for the reduction of silica under the experimental conditions chosen and to determine the step or steps which control the rate of reduction of silica. EXPERIMENTAL Two types of experiments involving the reduction of silica from the slag were carried out. In the first, the only reducing agent present was carbon (graphite), for which the over-all reaction is (SiO2) +2C(gr) —Si + 2Co(g) [l] The second type was a graphite-saturated ferro-silicon-iron concentration cell. In it silica in the slag could be reduced either by carbon according to Eq. [I], or by a reaction of electrochemical nature in which silicon was oxidized at the ferrosilicon-slag interface and silica was reduced at the slag-iron interface without the formation of CO. The two types of experiment are described below. Reduction of Silica with Carbon as the Only Available Reducing Agent. The reduction of silica was accomplished by allowing a liquid lime-alumina-silica slag and graphite-saturated iron to react in an induction-heated graphite crucible. The crucible was 2.25 in. diameter and 5 in. deep; it was fitted with a graphite stirrer which penetrated through the slag and into the metal, Fig. 1. The slag and metal charges weighed 350 g each. Pure carbon monoxide at a pressure of 1 atm was maintained above the melt by passing the purified gas through the crucible at a rate of 0.5 liter per min. The gas did not stir either the slag or metal. Temperature measurements were made by sighting an optical pyrometer down the hollow stirrer rod into a 1/4-in. hole drilled in the stirrer blade. The crucible temperature was maintained within *15"C of the required value by manual control of the power supply to the

Jan 1, 1965

By B. W. Howlett, M. B. Bever, Somnath Misra

The heats oj- formation at 0°C of the compounds AuSn,, AuSn2, AuSn, and the £ phase were measured in a metal -solution calorimeter with liquid tin or a liquid Sn-Bi alloy as solvent. The melting point, heat of fusion, and heat capacities near the melting point of- the compound AuSn in the solid and liquid state were measured in a constant temperature gradient calorimeter. The free energy and entropy of formation of the compound AuSn at its melting point and at 298 °K were calculated from the experimental results and published data. The heats of formation are discussed in relation to the nature of the compounds. The heat capacity below the melting point, heat of fusion, and entropy of fusion of AuSn are interpreted in terms of processes oc-curring before melting. The atomic arrangement in liquid Au-Sn alloys and the bonding in the intermediate phases of. the Au-Sn system are discussed in the light of the measured thermodynamic properties. THE available thermodynamic information on the intermediate phases in the Au-Sn system consists of the heats of formation of the compounds AuSn4, AuSn2, and AuSnly2 and of one composition of the < phase2 besides values of the heat content of the compound AuSn from 0" to 635".&apos; However, the heats of formation refer to different temperatures ringing from 90" to 450°C. Also, the reported error limits of some of the values are large and several inconsistencies are apparent. In the investigation reported here the heats of formation of the compounds AuS-, AuSnz, and AuSn and of three compositions of the < phase were determined for a single reference temperature of 0°C by liquid metal-solution calorimetry. The compound AuSn, which is the only congruently melting intermediate phase in this system, was further investigated in a constant temperature gradient calorimeter by measuring its heat of fusion, melting point, and heat capacity in the solid and liquid states near the melting point. From these data and published free energies of the liquid of composition Au~n,&apos; the free energies of formation of the compound AuSn at the melting point and at 298°K were calculated. The results shed light on the solid-liquid transition of AuSn and on the atomic bonding and state of association of gold and tin in the solid and liquid phases. 1) EXPERIMENTAL PROCEDURES 1.1) Preparation of Samples. Stoichiometric amounts of gold and tin, each 99.99+ pct pure, were melted in evacuated Vycor capsules (12 mm ID). The melts were maintained approximately 150°C above the liquidus for about 12 hr and shaken repeatedly. Samples of the compound AuSn were cooled slowly to room temperature. Melts of the other phases, all of which solidify by peritectic reactions, were transferred to the narrow end (5 mm ID) of the capsule, which was then quenched into iced brine. The solidified samples were annealed in the unopened capsules for 10 days at 30" to 50° C below the respective solidus temperatures. The absence of microsegregation and second phases was confirmed by metallographic examination. At least two batches of each composition were prepared. 1.2) Solution Calorimetry. The heats of formation were determined by liquid metal-solution calorimetry. In this technique, the difference between the heat effects on dissolution in a liquid metal, or alloy bath, of the compound and a mechanical mixture of its annealed components, adjusted for changes in composition of the bath, is the heat of formation of the compound at the temperature from which the samples are added. Details of the equipment and technique have been described."&apos; A tin bath at 300" or 350°C was used with the compounds AuSn,, AuSnz, and AuSn. The high gold content of the £ phase would have caused it to dissolve with an appreciable exothermic heat effect. In order to achieve thermal compensation, the samples were added from 0°C to a bath at 350°C consisting of 66.2 wt pct Bi (99.999+ pct pure), balance Sn (99.99+ pct pure). This solvent gives thermal compensation because gold dissolves exothermically in tin and endothermically in bismuth. The calorimeter was calibrated by adding from 0°C approximately 0.015 g-atom of the solvent.

Jan 1, 1965

By D. L. Feucht, R. L. Longini

The semiconductor heterojunction is considered in terms of simple models which may lead to an understanding of move complex heterojunctions. Metallurgical and electrical properties of hetero-junctions aye discussed including the interface structure, energy -band diagram, and carrier transbovt across the interface. It is found that in a heterojunction all mechanisms such as injection, tunneling, and junction recombination found in simple junctions play modified voles. INTERFACES between materials (grain boundaries, the electrical junction between two differently doped materials in a single crystal, the oxide-metal interface, or metal-metal junctions) are of considerable importance in many situations. These various interfaces all have one very fundamental thing in common. Quantum mechanically speaking, the wave functions of the electrons in one material may penetrate the other material but, in general, only to the extent of angstroms. From an electrical point of view the conduction mechanism changes as a current passes through such junctions. In some cases the change is tremendous, in others almost negligible. The interface, then, is the locus of a change of conduction mechanisms. Some of these, particularly in semiconductors, are well-understood. The ordinary p-n junction in a single crystal can be the locus of an injection mechanism or a tunneling process, depending on conditions. The mechanisms are probably best understood in semiconductors because of the possible simplified view of particlelike conduction. The bands are either nearly filled or nearly empty and band overlap is seldom involved. The same fundamentals are probably important in other situations too but they are very difficult to look at naively. Although the simple look at the semiconductor case only gives us a relatively rough picture which must then be refined, the other systems, which involve a more complex situation, immediately are in many ways too difficult. There are too many initial choices of complex systems and therefore it is not possible to be even reasonably certain of any one model. Because of the relative simplicity of semiconductors, their good and controllable structure, and because of the ability to make many measurements on them not normally available to either metals or insulators! they are probably the best understood materials. It is therefore desirable to use them as a tool to further the understanding of interfaces in general. Semiconductor-heterojunction concepts were first proposed by kroemer1 in 1957. This was followed several years later by reports on the fabrication and experimental characteristics of heterojunction structures by Anderson2 and Diedrich and jotten.3 I) THE HETEROJUNCTION STRUCTURE To get down to hardware, when we refer to a semiconductor heterojunction we imply that there exists an intimate contact between different semiconductor materials. We could put two pieces of material together, complete with oxide layers, we could remove the oxides, or we could even melt the interface and hopefully get wetting and a good "bond" on solidifying. In fact we could by some means grow a crystal of one material using the other as a seed. Essentially we are interested only in the last two because they are the simplest to look at analytically. The degree of perfection of fit varies greatly and is reflected somewhat in the arc welder&apos;s joint strength. The lattice match of the two materials, their orientation, and so forth. is obviously necessary for a good bond but so is the continuity of any polar bonds which are involved such as in the III-V semiconductors. The mechanical misfit between two similar lattices can be described in terms of edge dislocations. The edge-type dislocations must be very close together for the usual misfit and there must be dislocations for each of several different Burger&apos;s vectors in order to produce a lattice match. The .&apos;dangling bonds&apos;&apos; resulting will be involved in producing interface charge. Order of magnitude estimates of the charge density extrapolated from low densities of dislocations in homogeneous materials give 5 x 1013 cm-2 Ge-Si and 1 X 1012 cm-2 Ge-GaAs electronic charges. Edge dislocations also act as very active recombination centers between holes and electrons. One lattice "matching" difficulty usually exists even if two structures have essentially the same lattice constants as they will have different coefficients of therma1 expansion. Thus, on cooling from the usually high temperature of fabrication to room temperature, dislocations are produced, a good fit not existing at both temperatures. In brittle materials this shrinkage may even result in cracking. For the Ge-Si interface the mismatch is about 2 x 10 -6 per degree whereas it is less than 10"7 per degree between germanium and GaAs. The exact effect of the misfit is dependent on the thickness of the materials involved. For a very

Jan 1, 1965

By S. J. Gasior

A method for destroying the caking properties of bituminous coal was developed by the Bureau of Mines. Coal is treated in a fixed bed by heating through its plastic range under controlled temperatures in mildly oxidative atmospheres composed of inert gas and/or steam containing about 1 volume-percent oxygen. High-volatile A (hvab) and high-volatile B (hvbb) and low-volatile bituminous (lvb) coals in the size range 1/8 to 1-1/2 inches were successfully treated at 0 (atmospheric pressure) to 300 psig in static beds 6 to 18 inches deep. Conditions of treatment depended on the coal and ranged from 80 to 200 minutes at 350° to 510° C. Char produced in this manner from hvab coal was gasified with steam at 800° C and 100 psig in a fixed bed in one series of tests and in other tests was exposed to hydrogen in a dilute co current free-falling-bed system at 750° C and 3,000 psig without agglomerating.

Jan 1, 1965

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&apos; 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&apos;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&apos;s compilation ranged up to 3 mv per C. In particular he reported a value of +2.059 mv per "C at 25&apos;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:&apos; 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"&apos; 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.&apos; 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.&apos; 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&apos;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&apos; and Stage B&apos;. Stage A&apos; type deformation generally was noted up to a plastic strain of -80 x 10"6 in. per in. and Stage B&apos; type from -80 x 10-6 to -800 x 10&apos;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&apos; and Stage B&apos; deformation are briefly reviewed. 1) Stage A&apos;. In the annealed starting condition there was a variable density (5 x 107 to 3 x 10&apos; 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&apos; 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,&apos;,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,&apos; 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,&apos;&apos; AuCd,ll and AuZn.12 The existence of such transformation has been established recently,&apos;, 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&apos;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