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A method for determining the relative degree of oxidation of concentrate samples was established, and various surface-active materials and protective systems were examined as oxidation inhibitors. Sodium oleate was-the most effective of the materials tested, and a plant trial

Jan 1, 1963

By L. D. Keller

The application of hydraulic concentration to large scale operations has been effectively accomplished by the use of the SiphonSizer. Operation has been simple, automatic and essentially trouble free. The use of the primary desliming SiphonSizer on magnetic taconites has shown an improvement in grade of concentrate and an increase in recovery over conventional hydroseparators. Magnetic concentrates have been further deslimed and upgraded in SiphonSizers by floating a coarse middling product away from the heavier concentrate. The application of the Siphon-sizer to closed circuit grinding has met with only partial success to date. Hydraulic concentration of minerals has been practiced for a good many years. Until recently, however, the practice has been limited to equipment using a multiplicity of small pockets and relatively low tonnages and flows. The adaptation of the SiphonSizer to the concentration and classification of magnetite has changed this concept. Some fifty commercial units varying in size from a 16-ft diam circular unit to a 25x100-ft rectangular unit are currently in operation on magnetic taconites. Additional units up to 38 ft diam are under construction. Depending upon the application in the flowsheet, upgrading varies from 0.75% to 14% Fe in a single stage. To those not familiar with taconite processing, the importance of the struggle to remove economically as much silica as possible may not be fully appreciated. Perhaps some figures pertaining to transportation costs will underscore this important process. If the silica content of the concentrate from a 10,000,000 ton per year plant could be reduced by I%, a savings in boat freight, at $2.00 per ton, would amount to $200,000 annually! THE SlPHONSlZER The SiphonSizer, as illustrated in Figs. lA, 1B and 2, is a hydraulic classifier in which the hydraulic water is distributed uniformly across the bottom of the vessel by means of a system of headers (1 and 2), jet pipes (3), and nozzles (4). The depth of the teeter bed is automatically maintained by the siphon-float assembly. The feed is introduced through a feed well (5) and separated into two fractions by the effects of rising water and the density of the teetered bed. The magnetite fraction is discharged by the siphon (12) while the fine slime and light middling overflow a peripheral weir (9) to the overflow launder (6). The bed depth is controlled automatically by float valves (7), which are responsive to changes in the height of clear water supported in the superelevation tubes (8) by the density of the teetered bed. On top of the float (7) is a needle valve (10) which permits

Jan 1, 1963

In April, 1961, a large pillar was removed by blasthole mining methods at Inco's Murray mine. More than half a million pounds of explosives were used to break 2,120,000 tons of ore in a single underground blast. The 5, 10 2-inch boreholes, involving 435,815 feet of drilling, were loaded over a three-week period, using conventional explosives and short-period electric caps. From this blast, more than half a million tons of ore have been removed to date (April, 1962) through slusher trenches situated in the footwall of the ore body. T HE Ontario Division of The International Nickel Company of Canada, Limited, operates six underground mines and two open pits in the Sudbury district in the north-central part of the Province. This paper describes the removal of a large pillar at the Murray mine (Figure 1), where 2,120,000 tons of ore were broken in a single underground blast by the blasthole mining method. This is the largest underground blast achieved to date (April, 1962) at Inco mines.

Jan 1, 1963

By J. J. Kramer, W. A. Tiller, G. F. Bolling

THE axial orientations of columnar crystals in unidirectionally solidified ingots of zone-refined zinc and tin have been examined using the techniques recently described by us.' Both metals had an initial purity of 99.999+ pct before zone refining and satisfied all qualitative guides for very high purity after zone refining. Fig. 1 presents the orientations of the columnar crystals for tin and zinc, respectively. For tin, there is a preference for grains growing in the [I101 direction, i.e., the dendrite direction.' For zinc, a weak preference for the [0001] direction is seen (a random population in the unit triangle would give equal density on either side of the 60-deg circle centered on [0001]).' There was no apparent evidence for dendritic growth in either metal. These results, and those previously reported,' confirm the recent investigation by Hellawell and Herbert of casting textures observed for zone-refined lead, zinc, and tin.4 The preferred casting orientations for these metals in both the impure and zone-refined states are given in Table I. In the experiments on zone-refined lead,' it was shown that two separate textures existed: a preferred (111) nucleation texture existed at the chill surface and a preferred (111) texture developed during solidification. Either effect is sufficient to produce the result recorded in Table I. Similarly the results recorded for tin and zinc may be attributable to either a preferred nucleation or a preferred growth phenomenon and additional experiments are required to separate these two possible explanations. Hellawell and Herbert' attribute their results to a preferred growth process and account for it on the basis of a "layer-growth" model proposed much earlier by one of the present authors.5 An equally satisfactory growth model would be that based upon anisotropic surface energies. However, both of these growth models would indicate that the preferred growth direction for very pure metals should be normal to the plane of closest packing in the metal. This is consistent for zinc but, contrary to the conclusion of Hellawell and Herbert, it is not consistent for tin since here the (100) is expected to exhibit a greater density of packing than the (110). Although tin is expected to exhibit an anisotropy of thermal conductivity, we would expect the thermal conductivity to be the same in the [1101 as the [l00]

Jan 1, 1963

By B. D. Cullity

A distribution of residual stress after plastic elongation is proposed, in which the bulk of the material is strained in compression and a very small portion in tension, This distribution is shown to account both for the X-ray observations and for the effect of plastic straining on magnetic losses in silicon steel. The regions left in compression are tentatively identified with the interiors of the sub-grains revealed by the electron microscope. THIS paper is concerned with the general problem of the nature of the residual stress which is produced in metals by plastic elongation. A particular stress distribution will be suggested which accounts for the main X-ray diffraction observations which have been made. It will also be shown that certain magnetic measurements made on silicon steel can be understood in terms of this stress distribution. X-RAY OBSERVATIONS Uniform straining of a crystal lattice (macro-strain) causes a diffracted X-ray beam to shift its position, and nonuniform straining (microstrain) causes line broadening. If a bar of metal is plastically elongated in the longitudinal x direction and then unloaded, diffracted X-ray lines are observed to be both shifted and broadened.'-= Although the observed line shift indicates the presence of macro-strain, experiments have shown that no macrostrain, in the usual engineering sense of the term, exists.5"7 For example, removal of a layer from one surface of a stretched and unloaded bar does not produce curvature in the remainder of the bar 5'7 Fig. 1 shows the variation of lattice strain in the x direction, as determined from X-ray line shifts, with the applied stress in the same direction. The curve ABC is the normal stress-strain curve of the material, AB being the elastic portion and BC the plastic. In the elastic region AB, the strain measured by X-rays, called the lattice strain, and the strain measured mechanically are both proportional to the applied stress, and both return to zero when the applied stress is removed. Above the elastic limit the lattice strain would be expected to continue to increase along the line BD. Actually, it increases less rapidly with respect to stress, or even decreases, as shown by BE. If the applied stress is then decreased, the lattice strain decreases along EF, which is parallel to AB. As a result, there is a compressive residual lattice strain FA after unloading. STRESS DISTRIBUTION. Since a stretched and unloaded bar does not contain macrostress, it follows that the observed line shift must be due to a special distribution of mi-crostress. Such a distribution is shown in Fig. 2, which shows the variation of the stress u, across a stretched and unloaded bar. The material is assumed to consist of two kinds of regions: regions C, stressed more or less uniformly in compression, comprising the bulk of the volume of the material and responsible for the observed diffrac-

Jan 1, 1963

By Douglas N. Kendall

There are three definite steps in the making of a mining industry in any country. These are as follows: Step A - Geological Mapping This step covers the basic geological mapping of the country at scales of 1/250, 000 up to l/50, 000. This step eliminates territory and directs the exploration teams to the areas of potential interest. Step B Prospecting This step includes all phases from detailed geology through geophysics and drilling up to the point of proving that an economic ore body exists. Step C - Mine Development This is the expensive step, involving the creation of the mine, including shaft-sinking, ore treatment plant, etc.

Jan 1, 1963

By D Marshall

The sub-level blasthole benching method of mining has been proved to be economical at Willroy Mines. How-ever due to the nature and attitude of the wall rock, this method is susceptible to serious hanging-wall dilution of the ore. Attempts to solve the dilution problem by various means were not satisfactory until long Stressteel bars were employed as rock bolts. The adoption of this de-vice does not require any special skill, and has become routine in the under-ground operation. Since the inception of this method, the dilution of the ore has been greatly reduced and the ov1!r-all costs of controlling this dilution are much lower. INTRODUCTION T HIS is a report describing the successful use of long Stressteel bars as rock bolts in preventing l1anging-wall failure and consequent dilution in open stopes. Willroy Mines Limited is located (Figure 1) near the town of Manitouwadge, Ontario, approximately l1alf-way between Sault Ste. Marie and Port Arthur.

Jan 1, 1963

By G. W. Birge

Twenty-eight samples, representing the Pittsburgh, Lower Kittanning, Stockton-Lewiston, Coalburg, Winifrede, Cedar Grove, Peerless, No. 2 Gas, Powellton, and Eagle beds, were carbonized by the Bureau of Mines--American Gas Association (BM-AGA) method, and yields of products and physical properties of cokes were determined. Expanding characteristics of 22 of the samples were determined in the Bureau of Mines sole-heated oven. The Kanawha County coals tested were high-volatile A bituminous in rank, with dry, mineral-matter- free fixed- carbon contents ranging from 53.9 to 66.3 percent. With few exceptions, they were chemically satisfactory for metallurgical use, and most of the coke-strength indexes were within the industrially accepted range for high-volatile blending coals.

Jan 1, 1963

By A D. Turnbull

In Canada, although some research on extraction metallurgy is carried out by the universities and by government, the primary responsibility for the research necessary to the mining industry rests on the industry it-self. Automation is coming more slowly to the mining industry than to others, partly because of the problems of instrumentation. Operations research methods are, however, coming into use. Some new developments in the extraction of aluminum, in iron and steel, in pyrometallurgy and in pressure leaching of nickel, copper, zinc and lead are briefly outlined. Mention is made of uranium and the reactive metals. The importance of the by-product metals, notably antimony, bismuth, gallium, germanium, indium and tellurium, in the development of the electronics industry is also mentioned. The trend toward co-operative research by groups of producers, to develop markets for their products, is noted. In conclusion, there are a greater number of trained scientists, as well as larger amounts of scientific knowledge, available to the mineral industry than ever before, and, if properly used, this will result in great benefits to the industry and to Canada.

Jan 1, 1963

By L. G. Marshall

The geology, mining, beneficiating, types of products, and costs in terms of percent of total costs and of labor, power, and supplies of two crushed-limestone operations in Madison County, Iowa, are described in this paper. The operations are basically similar, differing in refinements in mining, product types, and markets. The operations are comparable as to personnel and as to weighted costs in terms of percent of total costs and in terms of man-hours, power, and sup-plies. The waste-to-stone stripping ratio is 1 to 0.8 at both operations, the powder factor is 0.29 pound of explosives per ton of stone, and daily production is 95 tons per man-shift. Both companies use crawler-mounted diesel shovels for loading, truck transportation, wagon drills, and dry screening.

Jan 1, 1963

By Kenneth A. Moon

An exact statistical treatment of a one-dimensional model is used as a basis for evoluating the reliability of certain simplified expressions for the activity of the solute in interstitial solutions, including one obtained from the exact expression by setting the repulsive interaction equal to infinity. The latter approximation is found to be satisfactory at low and moderate concentration if the repulsive interaction is large, even though not infinite. A similar expression (identical if the co-odination number is two) is derived from the quasichemical expression of Lacher, and is recommended as the best available expression for the excess configurational entropy of interstitial solutions with excluded sites. Some reasonable models are discussed, and the nature of the saturated solutions is determined by inspection. Some of the models reduce to the one -dimensional case. An analysis is given of the excess partial entropy of hydrogen in V-H; Nb-H; and To-H solutions. MOST treatments of the statistical thermodynamics of interstitial solid solutions have followed the classic paper1 of Lacher in making the simplifying assumption that the configurational entropy of the solution is ideal. However, it is becoming increasingly apparent that there are many interstitial solutions with very large so lute-solute repulsions, and for these the assumption of ideal entropy is not valid or useful. It is important to realize that with substitutional solutions large repulsions between the component atoms must lead to phase separation, whereas in interstitial solutions the free energy of the solution is not drastically increased by large solute-solute repulsions until intrinsic saturation is reached at the concentration where further solute would be forced to enter a site in which it would experience the repulsive effect of one or more solute atoms already present. In the limiting case of an infinitely large repulsive interaction, the excess free energy would be attributable entirely to excess entropy, the enthalpy of mixing being zero. AS will be shown below, even if the repulsions are less than infinite, a treatment based on an assumption of infinite repulsions may be very satisfactory up to moderately high concentrations of the interstitial component. Often in solutions where large repulsive interactions exist, there are also small interactions — often attractive—between solute atoms in configurations other than that corresponding to the large repulsion. In such cases the excess free energy will consist of an excess entropy term attributable to the large repulsive interactions, and an enthalpy term corresponding to the other small interactions. Nomenclature to differentiate succinctly between important cases would be a convenience. In this paper the nomenclature shown in Table I will be used. In Table I, and in the preceeding discussion, excess quantities are defined in terms of standard states which are pure solid solvent and pure (possibly hypothetical) solid saturated phase of the structure in question. In practice, it is more convenient to choose the interstitial element as a component, and its conventional standard state. This will add a composition-independent term to the excess entropy and the enthalpy. The earliest paper known to the present author which treats the thermodynamics of athermal interstitial solutions was given by schei12 in 1951, but the statistical derivations in that paper are open to criticism. Speiser and Spretnak were the first to give a correct statistical treatment,3 limited, however, to concentrations sufficiently low that the number of empty sites excluded from occupancy by more than one filled site is negligible. The purpose of the present paper is to extend the statistical treatment to more concentrated solutions, and to examine the magnitude of the errors introduced by assuming that the repulsive interactions are infinite when in fact they must be finite. THE QUASICHEMICAL APPROXIMATION Fortunately, a standard method already exists for taking into account the effect of large interactions upon the entropy of mixing. This is the quasi-chemical method, in which the probability of existence of a given pair of solute atoms in a certain proximate configuration is assumed to be proportional to exp(-w/kT), where w is the energy increase of the solution when the two atoms are moved from isolated locations in the solution to the configuration in question. A quasichemical treatment of interstitial solutions was given in 1937 in a widely neglected paper by Lacher.4 The result comes out

Jan 1, 1963

By R A. Burwash

In the Yellowknife geologic province, 2,600-million-year-old granites are cut by three sets of diabase or gabbro dyke : (1) large dykes striking 70°E to E-W, (2) rare dykes striking N-S to 30°E and (3) an abundant swarm striking N 10°-300W. Preliminary potassium-argon dating has been carried out on whole-rock samples of the chilled margins and coarse centers of the dykes, and on mineral separates from the dykes and contact aureoles. Data from seventeen dated samples suggest that the dyke sets were intruded during three periods of basaltic magmatism -2,200, 1,500 and 1000 million years ago. The two earlier periods closely follow the time of emplacement of granites in the Yellowknife and Churchill geologic provinces. The latest diabase dykes occurring in the Yellowknife province are temporally related to a widespread basaltic magmatism, for which the term Keweenawan is not appropriate. D DRING the past ten years, methods of physical age determination have been widely applied to date the time of intrusion or metamorphism of Precambrian rock

Jan 1, 1963

M INE production requires the coordination of the talents of men and the use of equipment. Mine operators maintain a continual surveillance of equipment, looking for improvements and modifications that will benefit them. Few give similar attention to the advances made in the education of mining engineers since they themselves graduated. That is not surprising. Education lacks the advertising budget available to manufacturers. A modification to improve a mechanical contrivance is advertised, and an advertiser's press releases get attention by publishers. The whole program for mining engineering education could be revolutionized and no one, except a few professors, would know about it. The Canadian Institute of Mining and Metallurgy's newly established General Commit-tee on Education can improve that situation. Nine groups of engineers in Canadian universities are trying to give undergraduates an education that will make them useful to the mineral industry as mining engineers. The tabulation offered here (Table I) is an analysis of the distribution of the undergraduate-teacher contact time.

Jan 1, 1963

By James C. M. Li, J. Weertman

James C. M. Li (United States Steel Covp.)—The author has discovered a single analytical relation between the minimum, or the steady-state, creep rate and the applied stress confirming a statement made earlier by orn" that such relation should exist and should reduce to the power law at low-stress levels and to the exponential law at high-stress levels. However, as pointed out by the author, all the available theories of creep are not adequate to explain such a single relation. Inspired by such a statement, I have made a suggestion concerning a possible explanation13 of the new relation. This is based on the concept that the rate-controlling step is the cooperative motion of a short dislocation segment. The nature of and the reason for the cooperation have been discussed13 as well as the reason why the motion of the dislocation could be controlled by the mobility of the short segments. A natural short segment has been proposed13 to be the node formed at the intersection of two dislocations. The reason why the node may contain only a few atoms has not been discussed and the application of the proposed model to all the metals and alloys reported in this paper has not been attempted. It seems appropriate to include these in this discussion. The model was partly inspired by the substructure recently observed in the electron microscope on creep specimens. One such example is shown in Fig. 48 in Darken's Campbell Memorial Lecture. The substructure is a collection of dislocation intersections and irregular networks. No pileups have ever been observed in such specimens. A closer look at the network indicates that one set of dislocations is more straight than the other set sug- gesting that the other set may be mobile in the plane of the net. Since, for the network to survive the creep deformation, some dislocation reaction has to take place at the intersection of the two sets of dislocations, the mobile dislocation, even if it can slip in the plane of the net, will have difficulty in moving at these intersections. To illustrate, an idealized network is shown in Fig. 9. The thin lines represent the set of dislocations which are mobile and can slip in the plane of the net except at the nodes which are formed at the intersection of the two sets of dislocations. The other set of dislocations, represented by the thick lines, may have a Burgers vector which is not parallel to the plane of the net, and therefore may be immobile. Because of this nonparallel Burgers vector, the Burgers vector of the node, which is avectorial sum of the Burgers vectors of the two sets of dislocations, will also be nonparallel to the plane of the net. Therefore, the node cannot slip in the plane of the net and the set of mobile dislocations will have to drag the node along as indicated in Fig. 9. Now the problem is how many atoms could be involved in the nodes. Exact calculation of the length of the node is a difficult task especially since the length should be a steady-state length and not an equilibrium length. An estimate of the equilibrium length can be made by balancing the line tension of all the dislocations. The results would be a small fraction of the length 1 between nodes as shown in Fig. 10. In some instances such a calculation shows that the node will not be formed. But, since the calculation is only approximate, it does not rule out the possibility of the formation of a short node. In other instances the equilibrium length of the node is an appreciable fraction of I. Such a node would

Jan 1, 1963

By T. P. Meloy

In a recent paper, Gaudin and Meloy1 derived a size distribution function for single, impact fracture. Mular2 extended the use of this size distribution to describe the output of carefully controlled grinding experiments. As it stands, the function is difficult to compute. Consequently, a series of tables of the function are presented below: where M(x) is the cumulative fraction finer than size x when x is particle size. Weight percents are tabulated for the single parameter, r, in three different size ranges: from 0 to 1, from 1 to 10 and from 10 to 100. Tables I, II and III are cumulative percent finer and Tables IV, V and VI are for weight percent passing screen size x, retained on the screen below. A number of conditions from the table are plotted in Figs. 1 and 2. Fig. 1 is a plot of the cumulative percent finer vs. size, and Fig. 2 is the weight per-

Jan 1, 1963

By L. F. Willmott

The Bureau of Mines at Morgantown, W. Va., has been investigating, on a pilot plant scale, various methods of gasifying bituminous coal with oxygen and superheated steam to produce synthesis gas, as part of the broader program of finding new uses for coal. Differences in the pressure gasification methods used have depended on differences in the manner in which the pulverized coal is fed to the gasifier. One of the methods of feeding the coal that was investigated was the continuous, integrated coal-water slurry system. Goal and water were first mixed to produce a slurry; then the slurry was pumped through a heated coil. to evaporate the water fraction; the resulting steam was superheated, and some of it was separated so as to adjust the ratio of the residual steam to the coal fraction and make the resulting mixture suitable for partial combustion with oxygen in a pressure gasifier. Both before and during this reported3 developmental work it was necessary to make an extensive literature search into the technology of aqueous slurries in order to establish design criteria for the pilot plant and to correlate results of various phases of the work with that of other investigators, The pilot work coincided with the commercial development of a long-distance pipeline for the transportation of coal as a coal-water slurry, and this fact tended to broaden the scope of the pilot plant work and the extent of the literature search. This bibliography is the compilation of the material that was collected.

Jan 1, 1963

By M. J. Hordon

Measurements of the 103 yield stress of ordered and disordered poly crystalline Cu ,Au were related to the ordered antiphase domain size determined by resistivity measurements. For undeformed material, a yield stress maximum wa obtained at a critical domain diameter of about 40A. Plastic deformation resulted in a marked increase in the yield stress and electrical resistivity of the ordered alloy compared to the disordered, the strain hardening rate increasing regularly with initial antiphase domain size. Order hardening was accompanied by a sharp reduction in size of the initially large domains. It has been observed that the yield stress of ordered and partially ordered Cu3Au alloy varies sensitively with antiphase domain size aid degree of order.ly2 In addition, ordering of the lattice leads to a marked increase in the strain hardening rate (order hardening) as compared to the rate for the disordered alloy. In the present investigation, changes in the electrical resistivity and yield stress of ordered polycrystalline Cudu with varying initial domain diameters were measured after tensile plastic deformation in order to examine the effect of cold work on the antiphase domain size. EXPERIMENTAL PROCEDURE Au-Cu alloy of 99.99 pct purity analyzing 50.85 wt pct Au-balance copper was obtained from the Handy-Harmon Co., N. Y., in the form of 0.061 in. diam drawn wire. Wire specimens 3 in. in length were given the following annealing treatment in nitrogen: 500" for 72 hr, 820" for 15 hr, and 450" for 5 hr, followed by a water quench. The annealing sequence resulted in a completely disordered structure with a grain size of about 0.2 mm. The disordered specimens were then reannealed at 360' in nitrogen for periods varying from 10 min to 150 hr followed by quenching to produce ordered structures with varying domain sizes. The degree of ordering and variation of domain size was followed by electrical resistivity measurements made at room temperature using a low resistance precision Kelvin double bridge apparatus. The specimen resistance was determined over a length of 4.0 cm between two brass knife-edge contacts while the specimen was immersed in an oil bath to minimize temperature variations. In addition, the current flow in the circuit was minimized by a current pulse technique in balancing the bridge in order to avoid heating the specimen. Using a sensitive galvanometer to detect the bridge null, the accuracy of the resistance measurement Wire specimens were plastically strained in tension with an Instron tensile unit at strain rates in the range 5 x 10"5 sec-' to 2 x 10"4 sec-'. Stress and extension data were fed into the Instron chart drive amplifier to obtain the actual stress-elongation curve from which the yield stress at 10"3 strain was determined. The maximum resolution of the apparatus was approximately 50 psi stress and 3 x 104 strain. At various plastic strain levels, deformation was interrupted and the electrical resistivity determined after removing the stress. RESULTS AND DISCUSSION 1) Yield Strength of Ordered Cudu. In order to determine the effect of the ordered antiphase domains on the initial yield stress, specimens were prepared with varying domain sizes ranging from zero for 5 completely disordered structure to about lo5A for a completely ordered structure by suitable annealing treatment. Domain sizes were estimated by comparing room temperature electrical resistivity data with the original data of Jones and sykes3 as modified by rdle.' In agreement with previous work, the resistivity varied sensitively with domain diameter and degree of order, decreasing from approximately 11.6 x l0- ohm-cm for the disordered structure to about 5.9 x l0- ohm-cm for ordered domains above 10"3 cm in diameter. Fig. 1 shows the change of the 103 yield stress with ordered domain size. It is evident that the maximum

Jan 1, 1963

By J. Mizrahi, A. M. Baniel, A. Mitzmager, S. Star

This article gives an account of the latest developments in the use of TBE for sink-float separation of silicate minerals. A number of minerals for which the process has been tested and found suitable are reviewed. Specific examples are discussed in relation to the particular problems of sink-float separation and recovery of TBE as compared with non-silicate minerals. The economic aspects are outlined. Silica and silicates comprise the most common and abundant group of minerals, and since they are present in variable amounts in most ores, they constitute an appropriate subject for the review and discussion of the recent developments in the use of TBE for mineral concentration. The silicates considered as a group have an extremely wide range of chemical and physical properties. Some of these properties, which are common to all minerals, are of importance to concentration by TBE and are discussed in some detail in this paper, as well as the development of methods and apparatus for concentration and recovery of TBE and several examples of concentration of silicates. PROPERTIES OF MINERALS WITH RESPECT TO CONCENTRATION BY TBE The properties considered as most important to concentration by TBE are specific gravity, structure, surface and shape. The specific gravity of a mineral is a fundamental property and is constant between very close limits for the same species of different sources if particles are pure and free from cavities or cracks. In many species, however, solid inclusions and changes in chemical composition due to replacement of elements cause variations in the specific gravity. The plagio-clase series of feldspars between albite and anorthite illustrate this point (specific gravity from 2.60 to 2.77). Fig. 1 shows the specific gravity distribution of some of the common silicate minerals.' The highest specific gravity is about 4.7 (zircon) and the lowest is 2.0 (sepiolite), with most of them ranging between 2.6 and 3.5. Although most of the silicates given in Fig. 1 are found as constituents of rocks, those generally considered as rock making minerals are comparatively few. They include quartz, feldspars, nephelite, sodalite, leucite, mica, pyroxenes, amphiboles, chrysolite, kaolin, talc and serpentine. These minerals may appear in igneous rocks as coarse crystals in granites, syenites and diorites or as very fine grained dispersions in basalt and felsite. When the latter rocks occur in an ore, their specific gravities depend on the minerals present and structure. The same is true for the sedimentary and metamorphic rocks (sandstones, shales, gneiss, slate, schists). A comparison of specific gravities for the minerals listed in Fig. 1 with that of TBE (see Table I) shows that the important rock-forming minerals, with the exception of pyroxenes, amphiboles and chrysolite (olivine), lie in the specific gravity range of less than 2.96 and can therefore be separated by TBE. The ore structure is important both in determining the apparent specific gravity and the efficiency of TBE recovery. The structure can be compact (as in

Jan 1, 1963

By F. Weinberg

The relative concentration of 1" at grain boundaries in controlled orientation bicrystals has been examined by autoradiographic techniques, and by activity measurements of grain boundary surfaces exposed by preferential ,melting. The autoradio-graphs indicate that thallium is concentrated at grain boundaries in as-grown bicrystals, but not in zcell-annealed bicrystals. They also indicate that the solute concentration and the distribution on as-grown bicrystal surfaces are markedly different than that of the bulk material. The boundary surface measurements are in agreement with the autovadiographic evidence. On the basis of these measurements, as-grown bicrystals containing approximately 100 ppm of Tl, solidified at rates between 5 and 30 cm per hr and with tilt boundaries greater than 10 deg, exhibited grain boundary segregation equivalent to roughly 10 atomic planes of pure solute. Higher solute concentrations (equivalent to 140 atomic planes of pure solute) were obtained in bicrystals solidified slowly (0.6 cm per hr); slightly higher values were obtained in specimens containing a large angle nantilt boundary. Annealing for various times over a range of temperatures eliminated grain boundary segregation within the experimental uncertainty of the results (equivalent to 1 atomic Plane of pure thallium at the boundary). The results for the as-grown bicrystals can be qualitatively accounted for by assuming the presence of a groove on the solid-1iq;id interface, at the grain boundary. SOLUTE segregation at grain boundaries may be considered in two parts, namely, nonequilibrium segregation associated with the solidification process, and equilibrium segregation in fully annealed materials.' There is much indirect evidence for nonequilibrium segregation, based on preferential etching at grain boundaries and the mechanical properties of as-cast alloys. In addition, some direct observations have been reported in which radioactive tracers were used as solute additions and segregation detected at the grain boundaries by autoradiographic techniques. However, there is little detailed quantitative data on solute concentrations related to grain boundaries, particularly for different freezing conditions and grain boundary configurations. Equilibrium segregation at grain boundaries has been considered both theoretically and experimentally. cean' has made an estimate of the maximum equilibrium solute concentration that might be expected at a grain boundary, based on the lattice distortions in the boundary region. He arrived at a concentration which was equivalent t a monatomic layer of pure solute. A similar value, based on thermodynamic arguments, was calculated by Cahn and Hilliard for the segregation of phosphorus in iron. Experimentally, much higher values of solute concentration at grain boundaries have been reported recently by both Inman and iler' for phosphorus in iron, and Ainslie et 1.' for sulfur in iron. They observed concentrations equivalent to as much as 20 to 100 atomic layers of pure solute at the grain boundaries. However, in both cases it was shown that the observed segregation was not due solely to equilibrium segregation at the grain boundary. In the former case, precipitation effectss due to trace impurities in the material were believed to account for the large amount of solute present at the grain boundary. In the latter case it was shown that a high density of dislocations in the boundary region could provide a large number of additional sites for solute atoms, other than at the grain boundary. Thomas and chalmera have reported on the equilibrium segregation of po210 in grain boundaries of Pb-5 pct Bi alloys. Using autoradiographic techniques, they observed a concentration of polonium along the boundary trace on the surface of annealed bicrystal specimens grown from the melt. The concentration only appeared after annealing, and varied with boundary angle, increasing as the boundary angle increased. Their conclusions have been questioned by Ward," who pointed out that the segregation they observed along the boundary trace was much too wide to be compatible with the usual concepts of the thickness of a grain boundary of several lattice spacings. Also, Maroun et al.,l1 with specimens similar to those of Thomas and Chalmers, found that segregation could only be detected on the specimen surface, suggesting that Thomas and Chalmers' results were associated with an oxidation effect of polonium, and not equilibrium segregation. Thomas and Chalmers replied12 that they did observed segregation at the grain boundary in the bulk material and suggested further experiments were necessary to resolve the difference. The purpose of the present investigation was to examine both nonequilibrium and equilibrium grain boundary segregation in melt grown bicrystal specimens as a function of boundary angle, growth rate, and solute concentration, and to de-

Jan 1, 1963

By L. J. Buteau, R. E. Reed-Hill, W. A. Slippy

In a zirconium {1121} twins tend to have coherelzt boundaries and thus do not usually taper to a point when they intersect a grain boundary. Under the proper conditions, a (1121) twin may deform a boundary in such a manner as to clearly rcveal the twinning shear. Measurements of these grain-bounrlary rotatzons yield a value of 0.63 for the (1151) twinning shear. The magnitude of the observed shear and its shear sense are in excellent agreement with the assumption that the second undis-torted plme (K2) for this form of twinning is the basal plane (0002). The present value of the tzvinninz shear, which is approximately three limes larger than Rapperport&apos;s value? is in excellent agreement with reported results of Sokuskii and Prolsenko.5 RECENTLY westlake&apos; reported a study of the twinning modes of zirconium based on ~ap~er~ort&apos;s2 values for the twinning elements. He observed that two of the modes, (1012) and {1122), can be explained by relatively simple dislocation models. A workable model for (1121) twinning, however, proved to be very complex and questionable. Because Rapperport&apos;s second undistorted plane, (K2), for (1121) twinning has large indices, {ll2l6), it is possible that the difficulty in defining a model for (1121) twinning lies in an incorrect value for K2. A measurement of this twinning element has therefore been made, using a method based on observations of the shear displacement of grain boundaries at positions where they are intersected by (1121) twins. EXPERIMENTAL PROCEDURES The zirconium specimens were deformed in tension on an Instron machine either at the temperature of liquid nitrogen (77ºK), or prestrained at liquid nitrogen temperature and then further deformed at room temperature. Straining at 77°K was employed in order to nucleate (1 121) twins in large numbers, since simple ropm-temperature tensile deformation favors (1012) twinning. Specimens were machined from 1/2-in.-thick plate. The material was arc-melted sponge zirconium annealed to an ASTM grain size 4 and containing, in parts per million, 380 Fe, 880 0, <40 Hf, 32 N, and < 5 H. The specimen gage length and diameter were 1.25 and 0.130 in., respectively. To insure a gage section initially free of twins, the last 60 thousandths of the specimen diameter was removed by acid machining.

Jan 1, 1963