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By D. W. Fuerstenau, P. C. Kapur

The kinetics of green pelletization in a laboratory balling drum have been studied, using pulverized limestone as a model system. The growth characteristics of green pellets were found to be extremely sensitive to the moisture content of the material. Empirical kinetic equations, which incorporate a function of specific surface of the pellets as the criterion for growth potential, have been found to describe growth in a nucleation region and in a ball growth region. The rate constants in the kinetic equations are strongly dependent on the moisture content of the material being pelletized. Size distributions of the balls at different stages of pelletiz-ing are also discussed. In many industrial chemical processes, particulate matter can only be utilized if it is in an agglomerated form, such as pellets. Pelletizing is now widely used in iron ore technology1, and it has also been applied to a number of diverse fields such as the production of cement-kiln feed2, fertilizers3, and fluorspar4. Recently, it has been proposed to pelletize dispersion-type ceramic nuclear fuel elements5. In iron ore technology, for example, the production of agglomerates by pelletizing involves two major steps: 1) the preparation of green balls by rolling particles in a suitable balling device and 2) the firing of the green balls to form compact, strong bodies upon sintering. The critical step in a successful iron ore pelletizing operation is generally considered to be the balling operation1. In this paper, which is not concerned with the sintering of green pellets, the words green pelletizing and balling will be used interchangeably. Green pelletizing, or balling, will be defined as the process of forming larger bodies by rolling fine particles on a surface without the application of direct pressure. Two recent literature surveys6" indicate that in spite of the considerable amount of industrial pelletizing, very little is known about the fundamental principles of balling and its kinetics. The first reported research on the kinetics of pelletizing is the work of Newitt and Conway-Jones8. Using silica sands of different sizes in a batch laboratory balling drum, they found that the average green pellet diameter increased linearly with time at constant drum speed, and qualitatively the growth rate increased with moisture content. Generalized conclusions cannot be drawn from their research since the materials which they pelletized were sand and sand-silt mixtures rather than comminuted materials. Moreover, Newitt and Conway-Jones used testing sieves to estimate the size distribution of the green pellets, and this technique limited the range over which they could study the growth kinetics of the pellets. Bhrany and co-workers9 investigated the kinetics of balling iron ore fines on disk pelletizers ranging in diam from 1 to 18 ft. In their investigation, balling was carried out as a continuous operation, and growth kinetics were studied in terms of retention time of the material on the disk. Although the feed material in their study was quite coarse (the maximum size being about 1/2 in.), they also found qualitative relationships between pellet growth and water content, and feed size. In the present investigation, a number of innovations were introduced that refined the experimental measurements and established the reproducibility of balling experimentation. This enabled extension of the range of measurements to include study of agglomerate nucleation phenomena in the fractional mm size. This paper presents a detailed analysis of the nucleation and growth of green pellets in a laboratory balling drum. MATERIALS AND METHOD Pulverized limestone of specific gravity 2.72 was used as a model system in these studies. It has already been established that the balling characteristics of limestone and silica are similar to those of iron ore concentrates 2,8,10, depending on physical, rather than chemical, properties of the particles. The size distribution of the limestone was determined by a wet-dry sieving technique in the sieve range and by a sedimentation balance in the sub-sieve range. Fig. 1 presents the size distribution of the limestone used in this research. This figure shows that the material is finer than 200p (65 mesh) and that 25% of it is finer than 12. The specific surface area of this powder, as measured by BET gas adsorption methods,

Jan 1, 1964

By Leslie W. Austin

ROTARY kiln operators will agree that some of the most severe conditions a refractory must stand occur in the hot zone of a kiln burning Portland cement, dead burn dolomite, magnesite, periclase, and similar materials. Frequently the operator is faced with factors beyond his control which drastically shorten the life of refractories. Shutdown due to mechanical failure can be serious if the period is of sufficiently long duration to cause the dropping of coating or the loosening of the lining. A change in slurry can affect the coating and cause ring buildup. A change in type of fuel and its effect upon the flame can cause a shift in location of the hottest zone. Weekend shutdowns or any other interruption can cause the operator trouble and may damage the refractories, since stopping and starting a rotary kiln is certainly more difficult than stopping and starting a motor. Some operators have tried to set an estimate of damage for each shutdown in equivalent days of running time. Conditions affecting the refractory may be roughly grouped in four classes: chemical attack, mechanical stress, thermal shock, and abrasion. Chemical Attack: The drive to obtain maximum production through a kiln demands maximum operating temperatures, temperatures which are limited more by the ringing up or melting of the clinker. This can cause interface temperatures at the junction of coating and refractory which require the use of a basic kiln block to withstand the chemical attack. Chemical changes take place within the refractory itself, especially in chemically bonded or unburned kiln blocks: These changes cause the formation of the ceramic or burned bond. Migrating liquids or fluxes from the kiln charge have an effect within the refractory and lead to mineral or glass formation. The alkalies, sodium and potassium, migrate into the refractory as silicates, chlorides, sulphates or other salts. They may move under capillary action or may be caused to move by volatilization with condensation in the cooler portion. Mechanical Stress: Concentrated stress may be caused by several factors or combinations thereof. 1-The rings of refractories must be kept tight and rigid within the kiln, and this alone demands considerable force to hold the blocks in place. So that the force will not be concentrated, the blocks should fit the circle as perfectly as possible, with the faces in contact overall. 2-As the kiln is heated, thermal expansion takes place at the hot end of the kiln block. Since this disturbs the plane face it too can cause a concentrated stress at the two ends of the block, and shearing stress can be set up within the brick itself because of the difference in expansion between the two ends. 3-If a lining becomes loose and moves in the shell very severe stress can be set up, and as the kiln rotates this load changes and gives the effect of repeated loading. Permanent expansion of the refractory can also cause severe loading. 4-Not least important, flexing of the kiln is frequently the cause of concentrated stresses. Thermal Shock: Thermal shock, the result of heating and cooling too rapidly, occurs on starting and stopping or when a large patch of coating drops, exposing the bricks. Again, its destructive effect is often the result of phase change, liquid to solid or the reverse; dense refractories loaded with glass-forming impurities are particularly susceptible. Thermal shock is a problem with refractories set in the wall or roof of a stationary furnace, and becomes even more serious in a rotary kiln, the tendency to spall being magnified with movement and concentration of stress. Uniform rate of feed and loading insures both better coating and a more uniform stress. Abrasion: If the refractories do not take a coating, abrasion can become a most destructive factor. Movement of the lining in shell or movement of loose blocks causes abrasion, which is also most destructive if the refractories do not take a coating. An analysis of the problem of basic lining for the hot zone reveals, therefore, a number of desirable characteristics: high refractoriness, basic chemical reaction, resistance to spalling, good strength at all stages, ability to take coating, true sizing, volume stability, and abrasion resistance. Increased demand

Jan 1, 1952

By D. Kunstelj, M. Stubicar, A. Tonejc, A. Bonefacic

A. Bonefafcic, D. Kunsfeli, M. Stubicar, and A. Tonejc The present communication is concerned with the variation of the texture in aluminum wires with die angle and temperature, at constant speed of extrusion. Experiments were carried out concurrently on refined samples, with a stated purity of 99.997 pct pure A1 and commercial samples of 99.5 pct Al. Ingots of refined aluminum samples were machined to 30-mm-diam by 150-mm-long billets. These billets were transformed to 5-mm-diam wires by drawing. The final form, suitable for examination, was obtained by extrusion through conical-face dies with a 1-mm hole diam and extrusion ratio 5:l in diam. The initial form of the commercial aluminum samples was drawn wire 5 mm in diam. These samples showed a poorly defined texture with (111) as a major and (001) as a minor component. A similar defined texture appeared in the refined aluminum samples after drawing to 5 mm diam. Conical-face dies with different angles (defined by the axis and the generating line of the cone) were used in our experiments. The values of the angles were 27, 35, 45, 57, 63, and 90 deg. The extrusion container was fitted with a heating element and controller permitting temperatures up to 600°C to be maintained within i5"C. Extrusion was performed at 250°, 300°, 350°, 400°, and 500°C at constant speed (approximately 1 mm per sec) and constant die reduction. The extrusion product was a wire 1 mm in diam and approximately 20 cm long. In order to remove the surface layer with the "conical" texture and to reduce the absorption by the X-ray examination of the samples, the extruded wire was etched to 0.22 mm in diam. Experiments were performed in the middle sections of the 20-cm-long wires. In addition to the die of l-mm hole diam, dies with a 1.5-, 0.7-, 0.6-, 0.5-, and 0.4-mm hole diam and 63-deg die angle were constructed. In our experiments we did not find in these ranges any important difference concerning the texture of the extruded wires and we continued our work solely on the 1.0-mm die. The diffracted X-rays (Cu K radiation) were recorded photographically. Diffracted intensities were measured on the (111) reflection with a microphotometer. The relative amounts of texture components were determined from the areas under the diffracted maxima. We found the texture of extruded aluminum wires to be strongly influenced not only by the temperature of extrusion and the purity of the sample but also by the form of the die. It is generally admitted that cold-drawn aluminum wires have mainly a (111) texture with a small amount of (001) component, Table I of Ref. 1. In our experiments with wires extruded in conditions represented by Fig. 1, in some cases a single (001) texture was obtained. If these wires were drawn repeatedly at room temperature, X-ray measurements revealed a duplex (001)-(111) fiber texture. Further drawings increased the (111) and decreased the (001) texture component. In Fig. 1 the percentage of material oriented with (001) parallel to the extrusion direction is represented as a function of the temperature and the die angle (a), for commercial and refined aluminum samples, respectively. From these diagrams we may draw the following conclusions. The slope of the die (a) influenced more strongly the texture at the lower rather than the higher temperatures. Again, a stronger influence was found in the case of the commercial in comparison with refined aluminum samples. In the case of the commercial aluminum samples the amount of material with (001) texture increases with increasing wire temperature in an approximately linear manner. This effect is less pronounced in the pure aluminum samples, with the exception of the die with a = 45 deg. In this case the (001) texture decreases with increasing temperature, as shown in Fig. 1. Component (001) is more pronounced in higher-purity aluminum samples. Our experiments led to the conclusion that both (001) and (111) components are essentially stable in extruded aluminum wires. As we obtained a single (001) texture starting with a sample of drawn wire in which the (001) component was very weak, our experiments revealed that the (001) component is not a remnant of the initial texture; this is in disagreement with the findings of Vandermeer and McHargue.1 We gratefully acknowledge discussions with Professor M. Paic. 1 R. A. Vandermeer and C. J. McHargue: Trans. 7MS-AME, 1964, vol. 230, p. 667.

Jan 1, 1969

By C. S. Smith, L. Guttman

It is shown, from a study of geometric probabilities, that the average number of intercepts per unit length of a random line drawn through a three-dimensional structure is exactly half the true ratio of surface to volume. Since the surfaces can be internal or external, the area of grain boundary or of the interface between any two constituents in a micro-structure can be measured. Other metric relations are tabulated that may be of use in studies of the microstructure of polycrystalline, cellular, or particulate matter generally. IN many fields of scientific investigation the structure of cellular aggregates or random arrays of discrete particles imbedded in some matrix is observed on a two-dimensional section and inferences are drawn therefrom as to the real structure in three dimensions. The biologist's microtome slice, the petrologist's thin section, and the metallurgist's plane polished and etched sections are common examples, although the problem is a general one. Scientists have commonly limited their thinking to the same dimensionality as their structures, and the few attempts that have been strictly three-dimensional in character have been laborious and noteworthy. From a metallurgical standpoint it is often of considerable importance to know, in addition to the volume fraction of two or more components in an alloy, the amount of two-dimensional interface between crystals. Such grain boundaries (which may separate either two identical crystals differing only in orientation or two crystals differing in structure, and possibly also in orientation) have a determining factor upon the mechanical behavior. It is at these boundaries that melting commences, that stress-induced corrosion occurs, and that various precipitates (harmful or otherwise) first appear. The boundary is doubtless of equal importance in nonmetallic crystalline aggregates such as rocks, ceramics, and concrete, and the biologist is deeply concerned with the area of cellular membranes. Many synthetic cellular foams involve similar structural problems. The very term structure usually implies the presence of interfaces and a complete understanding of structure involves nothing but an analysis of the geometrical, metrical, and topological relations between the various interfaces (zero, one and two-dimensional) that exist in a three-dimensional structure. Even systems lacking sharp physical interfaces often have interrelated gradients of composition or velocity (as cored crystals or turbulence cells) in which a neutral surface can be treated as a two-dimensional interface. In an earlier paper by one of the authors' the question of cell shape was considered in terms of simple topological principles without regard to physical dimensions. The determination of the actual size of grains in two dimensions is carried out in a routine fashion in innumerable metallurgical laboratories (see, for example, the ASTM standard methods of grain size determination2), though this is done merely to check the uniformity of a product and has no relation to the actual three-dimensional shape or size of the grains. Some authors have discussed the three-dimensional problem but only on the basis of assumptions as to idealized grain shapes.:'-' Quantitative measurements of microstruc-tures to obtain the volumetric relations of various phases have been carried out by petrographers for many years and are of increasing popularity among metallurgists." The present paper will show how, on the basis of no assumptions other than randomness of sectioning (usually realizable in experiment), it is possible to learn a great deal about the three-dimensional structure. The relations to be derived will generally be used on random arrays of cells or other particles, although they are equally applicable to ordered arrays and even to isolated objects of complex shape provided that suitable random sections can be made. Total Area of Interfaces in a Sample Consider a typical microstructure of a single-phase polyerystalline metal, such as that shown pres- in Fig. 1. The plane cross section shown contains a network of lines which subdivides the area into two-dimensional cells. The lines, of course, represent merely the intersection of the two-dimensional plane of sectioning with the two-dimensional interfaces between adjacent three-dimensional cells. The structure also contains points at which two or more lines intersect: in three dimensions the points are, of course, lines. In the more general case there may be in three dimensions isolated particles surrounded by a single interface without contact with others, and both two and one-dimensional features which do not necessarily connect with others. On the two-dimensional section these will appear as areas delineated by a closed line (as at a and b, Fig. 2), as isolated lines

Jan 1, 1954

By WM. P. BLAKE

THE salt-beds at Salton, on the line of the Southern Pacific railway, in San Diego county, California, have been successfully worked for many years by the corporation known as the East Liverpool Salt Co., and the salt has been largely used upon the Pacific coast generally and in the interior. But the industry has lately been destroyed by the overflow from the Colorado river. The salt is dissolved, and the waves of the Salton sea now roll 50 ft. above the site of this once thriving and growing business. The salt-bed was evidently the residual accumulation from the waters of an ancient lake, which I have named Cahuilla, from the name by which a large part of the valley-the home of the Cahuilla tribe of Indians-is known. The deposit covered a comparatively small area in the lowest part of the valley, 280 ft. or more below the sea-level. This depressed area is now generally known as the Colorado desert, but has a soil of wonderful fertility wherever water can be had on its surface. The deserted beaches, and the water-lines, only a few feet above tide-level, upon the rocks of the bordering mountains, as well as a great abundance of shells in the soil, all bear decisive testimony to the former occupation of the valley by water. The depression is topographically the northern end of the Gulf of California, from which it is now separated by the delta of the Colorado river, extending practically from the mouth of the Gila river across the valley to the coast mountains on the west side. We may conclude that the imprisoned salt water was gradually displaced and freshened by the inflow and outflow of the river, so that the lake was changed to fresh or brackish water, with enough salt in it to give a bed at the bottom upon

Jan 1, 1908

By S. A. Lever, R. Hultgren

The solidus is usually the least satisfactorily determined portion of a phase diagram. Cooling curves, which succeed well with the liquidus, show the solidus inaccurately or not at all because of segregation which occurs during freezing. Heating curves of carefully homogenized alloys might be expected to indicate accurately the solidus, but they are seldom used. Dynamic methods involving heating or cooling are never completely satisfactory because of uncertainty as to whether equilibrium is attained. A static method in which the specimen may be allowed hours, days, or even weeks to attain equilibrium is to be preferred. In a static method a solid solution, for example, is first made thoroughly homogeneous, then heated to successively higher temperatures. After sufficient time at each temperature to assure equilibrium, some property is measured which should alter strikingly when melting begins. Microscopic examination can be used to detect the beginning of melting, but the method is tedious since the specimen must be quenched, sectioned, polished, and etched before each examination. Of all the physical properties which change on melting, electrical resistance is probably the most satisfactory to measure. The measurement may be made while the specimen is at temperature without damage to the specimen. It may be repeated indefinitely to ascertain when equilibrium has been achieved. Measurements may be made on a single specimen over the whole range of temperature. Most metals approximately double their resistance on melting. Since an accuracy of a few tenths of a percent is easy to achieve, the method is highly sensitive to the beginning of melting. In spite of these advantages, which have been perceived for a long time,l,2 a reasonable search of the literature has failed to reveal a single case in which the method has been satisfactorily applied in practice to the determination of solidus temperatures. The use of electrical resistance measurements appears to have been confined in practice to changes in the solid state. In the work described in the following pages we have applied the electrical resistance method to the solidus of the lead-tin system. We have found the method to be convenient, reproducible, and highly sensitive. We chose the lead-tin system because it leads to few technical difficulties. Furthermore, a number of determinations of solidus have been made in this system by various methods and results could be checked against them. However, all published results are not in good agreement with one another, so this work should help in determining the solidus more precisely. The Lead-tin Diagram Because of its commercial importance, there have been numerous investigations of the lead-tin diagram. The results of the most recent work on the solidus are indicated in Fig 7, as well as the results of the present work. The works of Honda and Abe3 and of Stockdale4 agree fairly well with each other and with the present work. Jeffery's5 data indicate the solidus to be about 50°C lower. Honda and Abe3 used differential thermal analysis on both heating and cooling cycles. Stockdale4 used the microscopic method and also differential heating curves. Stockdale's results were about 4" higher than those of Honda and Abe at low tin contents and lower at higher tin contents. These results also agree with those of Rosen-hain and Tucker.= Jeffery5 used electrical resistance measurements of the alloy as it was being heated or cooled. Apparently he did not attain equilibrium as his results are about 40°C lower than those of Stockdale4 or Honda and Abe.3 MATERIALS AND METHODS The lead and tin used were of high purity. They were supplied by the American Smelting and Refining Co., who gave the following analyses: Lead: silver, 0.0016 oz per ton; copper, 0.0008 pct; cadmium, 0.0007 pct; zinc, 0.0002 pct; arsenic, 0.0003 pct; antimony, 0.0002 pct; bismuth, 0.0005 pct; tin, 0.0001 pct; iron, 0.0020 pct; lead (by difference), 99.995 pct. Tin: antimony, 0.037 pct; arsenic, 0.020 pct; bismuth, 0.004 pct; cadmium, trace; copper, 0.025 pct; iron, 0.004 pct; lead, 0.020 pct; nickel and cobalt, 0.005 pct; silver, 0.0005 pct; sulphur, 0.005 pct; tin (by .-difference). 99.88 pct. One hundred grams of metal with the desired proportions of lead and tin was weighed out to the nearest one-tenth of a milligram. The mixture was placed in a silica crucible, covered with charcoal, and melted in a reducing atmosphere in a gas-fired furnace. The alloy was well stirred. Chemical analysis of two of the alloys checked closely with the weighed portions. The compositions of the remainder of the alloys were taken directly from the weighings, without chemical analysis.

Jan 1, 1950

By F. R. Jones

AT Tahawus, N. Y., National Lead Co. operates the MacIntyre development. Here the world's largest titanium mine produces 5200 long tons of ore per day and pours 8000 long tons of waste rock over its dumps. Concentrated ilmenite is sent by rail to National Lead Co. pigment plants, and a second product, magnetite, is sold to steel producers in raw form or is agglomerated and shipped as sinter. Several earlier attempts had been made to produce iron from the deposits, which have been known since 1826. These attempts failed, chiefly because of titanium impurity. In 1941 the present owners reestablished the operation for production of war-scarce ilmenite, and the impurity became the main product. The Ore: The MacIntyre ore zone is about 2400 ft long and 800 ft wide in horizontal measurements. Ore outcrops were found on the northwest side of Sanford Hill, 450 ft above Sanford Lake and 2500 ft southeast. The zone dips at about 45" toward the lake and plunges to the southwest. The ore minerals, ilmenite and magnetite, are unevenly distributed in bands roughly parallel to the long axis of the ore zone and are interspersed with bands and horses of waste. Hanging wall ores are fine grained and grade from rich ore to waste rock or gabbro. Footwall ores are coarse grained and are almost entirely ilmenite and magnetite. The foot-wall waste rock, anorthosite, is the common country rock. Several faults cut the ore zone. These faults have no great displacement but do contribute to the great physical variations in ore rock and surrounding waste. The Mine: The MacIntyre mine is an open pit operation, with benches at 35-ft intervals. The lowest bench is now 54 ft below lake level. Loading equipment consists of three electric-powered shovels (a P & H model 1400 with 4-yd dipper and two Bucyrus-Erie models 85-B with 2%-yd dippers) and one diesel-powered shovel (a Northwest model 80D with 2%-yd dipper). Ore and waste are transported to a 48x60-in. jaw crusher in ten 22-ton Euclid trucks with 300-hp diesel engines. Ordinarily the two Bucyrus-Erie 2 % -yd shovels load ore into a fleet of three or four trucks. This combination works two 8-hr shifts per day, moving 5200 long tons of ore to the crusher and removing a small portion of the waste rock. The P & H model 1400 shovel, with a fleet of four trucks, loads waste on three shifts per day. The mine operates on a 5-day week, with a small maintenance crew working Saturday. Oversize rock is broken by a dropball handled by an Osgood model 825 rubber-mounted crane.' Ore and waste are broken by drilling and blasting 9-in. diam vertical holes behind the benches. Bucyrus-Erie 42-T churn drills are used to drill the holes, which are extended 4 ft below the bench level on which the broken rock will fall. Drilling and Blasting History: In its early years the mine was equipped with Bucyrus-Erie 29-T churn drills, which drilled 6-in. holes. To keep up with production requirements the hole diameter was soon increased to 9 in., and by 1950 the three 42-T drills now in use had been acquired. Early blasting experiments with different kinds and grades of explosive led to adoption of 90 pct straight gelatin dynamite as standard. It was recognized that this explosive was expensive, and from the start of operations until 1950 extensive experiments were made using blasting agents of the ammonium nitrate family. Results were recorded as uniformly poor, with great build-up of oversize rock. The expense of these experiments, and the discouraging results, caused the abandonment of any expectation of breaking MacIntyre rock with anything but 90 pct straight gelatin dynamite. Further standardization led to 9-in. well drillhole spacings set at 16 ft in ore and 18 ft in waste, exceptions being permitted only for unusual conditions. The hole burdens were theoretically about 22 ft. Due to the extreme back-slope of bench faces, caused by blasting with heavy charges of dynamite, actual burdens were commonly well over 30 ft. Lack of precise control resulted in many holes having a burden as light as 15 ft. General practice was to stem 6 or 7 ft of hole with magnetite concentrate, the amount of stemming being left to the discretion of the pit foreman. Usually all holes in a row were fired instantaneously with Primacord detonating fuse. Millisecond delays were

Jan 1, 1957

By R. D. Daniels, T. W. Wood

The tensile properties of columbium and Cb-H alloys containing up to 455 ppm H were studied as a function of temperature and strain rate. Hydrogen, introduced into columbium at elevated temperatures, using a thermal -equilibrium technique, embrittled columbium most severely at about —77°C. This elnbrittle ment occurred even at hydrogen concentrations of an order of 20 ppm. At higher temperatures, the hydrogen tolerance of columbium increased in relation to the increased solubility of hydrogen in tile metal. Below this temperature hydrogen tolerance, as determined by ductility and fracture stress, increased slightly. Strain rate had little effect on the tensile results for cross-head speeds over the range 0.002 to 2.0 in. per min. Strain aging during the tensile test appears to explain the ductility mininmum at —77°C. The apparent increase in hydrogen tolerance at lower temperatures is attributed to the low mobility of hyhogen. Experiments were performed in which samples were prestrained in tension at room temperature and tested to failure at —196°C. Results suggest that hydrogetz segregation to preformed crack nuclei can cause subsequent embrittlement even at temperatures where hydrogen mobility is too low to cause embrittlement in a normal tensile test. COLUMBIUM is an example of the class of bcc metals with ductile-brittle transition temperatures sensitive to the presence of interstitial atom contaminants. Hydrogen is one of these embrittling contaminants. The embrittling effect of hydrogen is less potent, perhaps, in columbium than in some of the other bcc refractory metals, but it is still a problem of both theoretical and practical interest. Unlike hydrogen in iron and steels, hydrogen in columbium is exothermically rather than endo-thermically occluded. The embrittlement process in exothermic systems has not been studied as extensively as that in endothermic systems, especially at hydrogen concentrations below the limit of solubility. The purpose of this investigation was to evaluate the embrittlement process in initially pure columbium as a function of hydrogen content, temperature, and strain rate. The Cb-H phase diagram, according to Albrecht et al.,1 is shown in Fig. 1. Columbium reacts exothermically with hydrogen producing a solid solution at concentrations of less than about 250 ppm (parts per million by weight) H at room temperature. At concentrations above the highly temperature-dependent solvus a second phase is formed. Like many similar hydrogen-metal systems,2 his system exhibits a miscibility gap with respect to hydrogen solution. Albrecht found the critical temperature of the miscibility gap to be about 140°C, the critical concentration to be 0.23 atom fraction hydrogen, and the critical pressure to be 0.01 mm Hg. Above 140°C there is a solid solution of increasing lattice constant extending across the phase diagram. Hydrogen concentrations of particular interest in this investigation were those below the limit of solubility in columbium. At hydrogen concentrations above the limit of solubility, columbium will contain the hydrogen-rich second phase and will be brittle under most testing conditions because the hydride generally precipitates as platelets with coincident matrix lattice strains.1'3 At hydrogen concentrations below the limit of solubility, the tensile behavior of columbium is expected to be more sensitive to the interrelationships between hydrogen concentration and mobility and the testing variables such as temperature and strain rate. Literature references to the hydrogen embrittlement of metals, especially ferrous alloys and titanium alloys, are too voluminous to mention. It is only recently, however, that detailed studies of the hydrogen embrittlement of columbium have been undertaken. Wilcox et a1.4 studied the strain rate and temperature dependences of the low-temperature deformation behavior of fine-grained are-melted columbium (1 ppm H) and the effect of hydrogen content (1,9, and 30 ppm H) on the mechanical behavior of columbium at a series of temperatures for a single strain rate. A strain-aging peak was ob-served at about -50°C which was attributed to the presence of hydrogen in the metal. Eustice and carlson5 studied the effect of hydrogen on the ductility of V-Cb alloys at a series of temperatures over the range -196° to 25°C. Pure columbium was embrittled by 20 ppm H which produced a ductility transition at approximately -70°C. Ingram et al.6 studied the effect of oxygen and hydrogen on the tensile properties of columbium and tantalum. A minimum in the notched-to-unnotched tensile ratio of hydrogenated columbium was obtained at about -75°C, but because of the relatively large hydrogen content employed (200 and 390 ppm) the ductility

Jan 1, 1965

By J. M. Eldridge, P. Balk

Phosphosilicate glass films were formed, by reacting gaseous P2O5 with SiO2, over a large range of temperature (800° to 1200°C) and gas phase composition (nearly two orders of magnitude of effective P2Ospressure). The film compositions generally corresponded with the liquidus curve, delineating the maximum solubility of the tridymite Phase of SiO 2 in phosphosilicate liquid solution at the temperature of film formation. It is shown that the P2O5 concentration of the phosphosilicate liquid film tends to decrease by reaction with the underlying SiO 2 layer until the liquidus curve is reached. The validity of the thermodynamic argument used in this explanation is supported by the results of a determination of the composition of borosili-cute films, prepared by reacting gaseous B2O3 with SiO2 at different temperatures. The kinetics of phosphosilicate film formation were described by a model predicated on a steady-state diffusion of P2O5 through the film. UNDERSTANDING of the processes leading to formation of phosphosilicate and borosilicate glasses is of great importance for producing passivating layers on FET devices. Passivating films with optimum characteristics are preferably formed in a separate step, independent of the doping of the semiconductor.' The results of an investigation carried out to gain improved insight into the mechanism of glass formation are presented in this paper. It would be expected that application of the known Pz05-Si02 and B 2 O 3-SiO2 phase diagrams should be useful in extending understanding of the glass-forming processes. However, the question of the propriety of treating thermally grown SiO2 in these binary oxide systems by the methods of equilibrium thermodynamics must be considered when this application is attempted. Although Sah et a1.' and Allen et al. 3 investigated the kinetics of formation of phosphosilicate glass (PSG), they failed to adequately relate their diffusion models to the occurrence of experimentally observed phases in the PSG/SiO 2/Si system. Horuichi and yamaguchi4 investigated the diffusion of boron through an oxide layer and described their results in terms of a model similar to that of Sah and coworkers. More recently, Kooi 5 and Snow and Deal6 reported the compositions of PSG films formed by depositing P2 O 5 onto SiO2. These compositions apparently coincide with those at the liquidus curve delineating the maximum solubility of crystalline SiO2 in phosphosilicate liquid solutions. These authors did not discuss the thermodynamic implications of their results on the structure of thermally grown SiO2 films. The structure of thermally grown Sio2 films and that of vitreous silica are generally thought to be quite similar. Since the solubility of a substance depends on its structure, it is relevant that the solubility of vitreous silica in water7 is highly reproducible, like the solubility of thermally grown SiOz in phosphosilicate liquid. Furthermore, the vitreous silica-water system appears to be in true thermodynamic equilibrium (viz., the same solubility value can be approached from both supersaturated and under-saturated solutions). Sosman7 suggested that a type of two-dimensional lattice may form at the silica/solution interface, resulting in the observed solubility behavior that is characteristic of a crystalline solid. An alternative explanation may be that vitreous silica has a microcrystalline grain structure. Other investigators have suggested that vitreous silica has essentially the structure of B cristobalite,' or is composed of microcrystals of p tridymite or cristobalite, or a mixture of both. Presumably the grain size would be sufficiently large to minimize any appreciable contribution of the grain boundaries to the solubility of the crystalline matrix. The present investigation was carried out to clarify the significance of the boundaries in the Pa,-SiO, and B2O3-SiO2 Systems in determining PSG and BSG (borosilicate) film compositions. Furthermore, the kinetic data for PSG film formation were extended, using a wider range of formation parameters than were previously reported. One model describing the kinetics of film formation will be presented that is compatible with the thermodynamics of the Pa5-Si02 system. EXPERIMENTAL PROCEDURE Glass Film Preparation. SiO2 films (1000 to 8000A thick) were obtained by oxidation of silicon substrates in dry O2 at 1100°C. PSG and BSG films were prepared by exposing these layers to gaseous oxides obtained by reacting high-purity POC13 and BBr3, respectively, with O2. A double-columned saturator was used to ensure complete saturation of the N 2 carrier

Jan 1, 1969

By G. R. Leverant, C. P. Sullivan

Re crystallized TD-nickel mi-2Th0,) in both coated und uncoated conditions was fatigued at 1800°F at total strain ranges varying .from 0.2 to 0.75 pct. The fatigue life of uncoated inaferal, Nf, was related to the total strain range, ?eT, by (2Nf/021AeT = 0.014. A duplex Al-Cr pack coating increased the fatigue life by about a factor of two. The cracks that led to failure in both coated and uncoated material were initiated at the outer surface, indicating that the mechanical properties of the surface layers were important in determining fatigue life. Crack propagation and subsurface crack initiation in the TD-nickel occurred preferentially at grain boundaries with cavitation at thoria particle-matrix interfaces an integral part of the grain boundary fracture process. The importance of both the grain morphology developed during thermome chanical processing of TD-nickel and the distribution of thoria particle sizes to fatigue resistance are discussed. THE fatigue properties of only a few dispersion-strengthened metals have been studied at temperatures 0.5 Tm;1,2 among these have been lead and aluminum containing oxide dispersions. TD-nickel is a material of interest for application in aircraft gas turbine engines, but little fundamental information is available on its behavior under cyclic loading conditions. In this study, the low-cycle fatigue properties of TD-nickel were determined at 1800°F with emphasis on the 101-lowing; 1) the relation of the grain morphology produced during thermomechanical processing to crack initiation and propagation; 2) the role of thoria parti-cles in the fracture process; and 3) the effect of an oxidation resistant coating on fatigue life. I) MATERIAL AND EXPERIMENTAL PROCEDURE The TD-nickel was supplied by DuPont as a 5/8-in. thick plate which had been subjected to a proprietary series of thermomechanical treatments with a final anneal at 2000°F for 1 hr in hydrogen. The composition of the material is given in Table I. At the test temperature of 1800°F, the 0.2 pct offset yield stress was 15,000 psi, and the elongation and reduction in area were 4.6 and 3.0 pct, respectively. The microstructure of this material has been previously described.&apos; Briefly, it consists of an array of lath-shaped grains, about 0.15 mm in thickness, with the long dimension of each grain parallel to the primary working direction, Fig. 1(a). The presence of very small annealing twirls, Fig. l(b ), together with the absence of extensive dislocation networks, Fig. L/C), indicated that the material was in the recrystal- Table I. Composition of TD-Nickel ThO2 2.3 vol pct C 0.0073 wt pct lex 0.01 wt pct Cr 0.01 wt pct Cu 0.004 wt pct S 0.001 wt pct Ti <0.001 wt pct Co <0.01 wt pct Ni bal lized condition. Commercial TD-nickel sheet has a similar grain size and shape, but unlike the present material is not recrystallized as evidenced by the absence of annealing twins and the presence of a well-developed dislocation substructure.4 The plate material had Young&apos;s moduli in the rolling direction of 22 x 106 psi and 13 x 106 psi at room temperature and 1800°F, respectively, indicating a texture with a strong {100}<001> component in agreement with previous observations on recrystallized TD-nickel sheet.596 The 2.3 vol pct of thoria particles were uniformly distributed although some clustering and stringering of larger particles was occasionally seen. The average diameter of the particles was 450 and the calculated mean planar center-to-center spacing was 2100Å. Two specimens were coated with a duplex A1-Cr pack coating. The coating was somewhat nonuniform from one position to another along the gage length. An area of the coating after testing is shown in Fig. 2. Electron microprobe analysis revealed the following zones in the various lettered regions indicated in Fig. 2: A) a bcc matrix of B-NiA1 with some chromium in solid solution along with a fine dispersion of a chromium-rich second phase which was probably precipitated during cooling from the test temperature to room temperature; B) fcc y&apos;-Ni,Al with some chromium in solid solution; C) porosity; D) a two-phase mixture of a chromium-rich solid solution containing nickel and aluminum and a small volume fraction of a nickel-rich solid solution having approximately the same composition as the immediately adjacent portion of region E, E) the TD-nickel substrate containing chromium in solid solution to a depth of 5 to 10 mils. As expected from the nature of the diffusion processes involved,7 the thoria particles were present only up to the layer of porosity, region C, Fig. 2. The measured thickness of the coating proper, zones A to D, after testing was 1 to 2 mils. The specimen design and testing techniques have been previously discussed.&apos; Stressing was axial and parallel to the lath-shaped grains (i.e., parallel to the rolling direction). The total strain range was controlled between zero and a maximum tensile strain varying from 0.2 to 0.75 pct. (The test at 0.2 pct total strain range was switched to load control at 1030 cycles at which point the peak tensile and compres-

Jan 1, 1970

Jan 1, 1903

At Asarco&apos;s Mission mill. located near Sahuarita, Ariz., the 20 500-t/d (22,500-stpd) throughput of highly abrasive and corrosive copper ore can play havoc on equipment wear parts. To minimize frequent replacement work and extend life on key components, Asarco engineers have over the past five years utilized liners made of "Towniprene" in the secondary grinding and flotation area of the plant. Results to date have indicated that these liners last between three and five times longer than those made of metal or ordinary rubber.

Jan 8, 1978

"In 1899 the American Refining and Smelting Company obtained control of the East Helena Smelter, and have added improvements from time to time.The plant is four miles east of Helena, on the Northern Pacific and Great Northern railroads, with hourly street car service from Helena.Electric power is obtained from Canyon Ferry dam, twelve miles east on the Missouri river, and about 800 h-p. is used in the blowing engines, crushing machinery, cranes and locomotives.Besides the Montana ores convenient to the above railroads, a large part of the ore supply comes from the Coeur d'Alene district, Idaho, and is mainly lead ore and concentrates.A modern automatic sampling mill, with Vezin samplers and a capacity of 50 tons per hour, was completed in 1912.Three blast furnaces, each 48 inches by 136 inches, are now in continuous operation, and the monthly production of silver-lead bullion is six thousand tons.A part of the ore roasting is done in Godfrey furnaces, in connection with the Huntington-Heberlein process, 12 pots being in use, with a capacity of 300 tons per day.Four Dwight-Lloyd sintering furnaces, each 42 inches by 264 inches, and a smaller experimental machine, with a combined capacity of 440 tons per day, are in steady operation, and are successfully roasting ore as well as sintering flue dust. These machines are in great favor and results are being carefully watched.Three bag houses are used in connection with the 1,800 brick flue chamber, and each bag house contains 1,260 cotton bags, each 18 inches in diameter by 30 feet long, suspended on vertical roads. The product saved by the bags contains about 50 per cent lead and is retreated in the blast furnace after sintering.About 450 men are employed."

Jan 1, 1913

By J. A. Hren, C. M. Wayman

RECENT investigators have noted anomalous behavior in the electrical resistivity of vanadium below room temperature. Rostoker and Yamamoto1 in studying the vanadium-oxygen system hypothesized that the body-centered-tetragonal phase existing from 15 to 34 at. pet O at approximately 800°K was really a low-temperature allotrope of vanadium that was stabilized by oxygen. In measuring the electrical resistance of cold-swaged vanadium rod over a range of temperatures, a small discontinuity was observed at approximately 240°K, supporting their notion of allotropy. However, the magnitude of the observed discontinuity was extremely small. Loomis and Carlson2 in studying the ductile-brittle transition in vanadium also made resistance measurements and reported a discontinuity near 200°K. More recently, White and Woods3 showed that the electrical resistivity from room temperature to approximately 100 °K was not linear and at variance with the Bloch-Griineisen law. Instead of finding a discontinuity, they observed a deviation from linearity below 200°K. In discussing their results they pointed

Jan 1, 1961

By George Dyott

THERE are many who may consider a paper on aerial transport and its possibilities in connection with mining operations somewhat premature. Nevertheless, as there is considerable interest manifested in the subject at the present time and the amount of information available is both scanty and misleading, the result of investigations in some of the remote mining districts of Peru will not only be of interest, but will help crystallize, in the minds of many, a more correct conception of just what an airplane is capable of doing. By way of introduction, I will deal briefly with the types and varieties of airplanes now in use, and the developments of the past few years, pointing out -how the war has encouraged machines. of startling performance rather than those of commercial utility. I will then take up aerial transport in general, showing how airplanes may be employed to advantage and the particular kind of work for which they are best suited. This will cover a preliminary discussion on cost, which is one of the most important phases of the subject. In passing on from a general survey of the situation, I will deal with actual observations and investigations made in Peru. This part of the paper will be divided into two sections: the first, covering the mountainous districts of the Andes (Tamboras, Pataz, Soledad, etc.); the second, the alluvial deposits in the rivers, Chinchipe, Santiago, and Napo. In each case the question of atmospheric conditions, altitude, landing grounds, motors, cost, etc. will be discussed. While it is my intention to deal chiefly with mining in the sections mentioned, the same line of argument will be applicable to any other districts in the world. In conclusion, I will touch on the possibilities of using lighter-than-air craft of the Zeppelin type, followed by a summary of the most salient points brought out in the paper.

Jan 2, 1919

By A. K. Sinha

The annual production and productivity of underground coal mines in recent years declined from 334 Mt (368 million st) and 14.5 t (16 st) per man per shift in 1969 to approximately 254 Mt (280 million st) and less than 8 t (9 st) per man per shift in 1977. Productivity is still hovering at about 7.25 t (8 st) per man per shift. According to US Bureau of Mines, the estimated US coal reserve is about 396 Gt (437 billion st), 68.65% of which is obtainable by underground mining methods. Approximately 153 Gt (169 billion st), or about 85.2% of the high Btu premium coking coal of the eastern US, would need to be extracted by underground mining methods. It is thus apparent that under- ground mining will continue to play a major role in total US coal production, which is expected to rapidly increase to about 1.1 Gt (1.2 billion st) by 1985, with about 606 Mt (668 million st) being contributed by underground mines. Production Potential of Continuous Mining The production potential of a continuous mining section depends primarily on the producing ability of the miner, transporting ability of the face haulage, and the matching of the two systems. The producing ability of the continuous miner depends on its actual cutting ability and the time available for cutting coal. The performance of 10 continuous miners operating in coal seams of various thicknesses were monitored in Pennsylvania and West Virginia, using continuous electrical power analyzers and time studies. The recordings on current and power strip charts yielded an accurate analysis of the cutting, trimming, and idle times of the machines on a full shift basis. Continuous miners of various models and sizes from 112-298 kW (150-400 hp) were monitored. Based on actual cutting time, the average cutting ability of the machines, as shown in [Fig. 1], ranged from

Jan 1, 1983

By T. L. McCall

This is a continuation of the paper on bumps presented by the late Mr. Herd in February, 1929. The seam worked consists of bituminous coal, 9 ft. thick, pitching 20°, and now under a depth of cover of 2800 to 3200 ft. Full particulars are given of two bumps that happened in November, 1931, with an interval of only 9 hr. between them. The first was a "district" bump affecting an area of 1000 ft. on the strike by 700 ft. on the dip and rise, beginning at a distance of 1000 ft. from the long-wall faces. The second, which caused much greater damage, was localized to two levels 200 ft. apart, in the area left undisturbed by the first bump next to the longwall faces. Observation stations had been established in the workings in 1931 and definite records were obtained on the flow of coal taking place from the edge of large pillars developed for retreating work, into the open roadways. The records also gave evidence that "advance weighting" or "underdraw " was affecting the coal at an average distance of 260 ft. in advance of the longwall faces. The author propounds the theory that the sandstone bed varying from 0 to 75 ft. in thickness and lying 14 ft. above the coal acts as a slab in distributing the superincumbent weight. The weight is thereby concentrated on the pillars in advance of the longwall faces and this load, in conjunction with a pavement strong enough to resist the reaction, leads to overstressing the pillars, which finally collapse suddenly, thus giving rise to this particular type of low side bump. The overlying sandstone bed, which is apparently a condition common to all coal mines in which bumps occur, is not necessarily a massive bed, as the thickness of this bed at Springhill in the area that has experienced these severe low side bumps is only 25 to 31 feet. A list of 43 minor bumps occurring in the past 2½ years is appended

Jan 1, 1934

By Martin Coryell

EHRENBERG was the first to publish and direct attention to the peculiarities of the diatomaceous deposit of Richmond; but how and by whom he was supplied with the material for his microscopical investigations, is not generally known; but we may presume W. B. Rogers, formerly State Geologist of Virginia, furnished the material, and may have given the geological position or horizon. O£ these facts we have no available evidence, nor have we any estimate of the thickness of this stratum of diatomaceous or infusorial earth. At the request of a member of this Institute, I have investigated the subject, and offer the following facts as the result, derived principally from information supplied by Mr. John Ott, of the Southern Fertilizing Company, Dr. William Taylor, State Chemist, C. Peticolas, microscopist, Captain Robert H. Temple, civil engineer, Major C. M. Bolton and Mr. C. M. Smith, civil engineers, and formerly engaged in constructing the tunnel under Church Hill, in Richmond. The city of Richmond is generally described as being built on seven hills. This is not the fact, geologically speaking. Originally, there was an immense plateau of land, about two hundred feet above tide, in which a deep excavation was made from the west to east by the James River cutting down to the granite. Opening southward and meeting the valley of the James are various ravines and gullies, in the principal of which are Shockoe and Gillies Creeks. The formation is tertiary, subdivided into all the classified divisions, but at the present moment no one has been found to make this section a special study. Rogers&apos;s early classifications and diagrams, with all their imperfections, are the only published records, and the printed editions are long since exhausted. The city of Richmond is really situated in these ravines of the James, Shockoe, Gillies, and their connections. The profile marked A, Plate V, represents the section of the plateau

Jan 1, 1876

By F. J. Tuck

THE Hayden mill of the Ray Mines Division, Kennecott Copper Corporation, is now equipped with two 9 by 12-ft. rod mills having a daily capacity of 6000 tons of coarse-crushing plant product from the mine. These two mills crush a 3/4-in. product to approximately 19 per cent on 14 mesh, with only one pass through the mills. Each rod mill has taken the place of four sets of 42-in. Garfield rolls with their attendant screens, and is making a product for the fine-grinding department comparable to that formerly made by rolls in closed circuit with screens. The rod mills are lined with wave-type liners of white iron, varying in thickness from 2 to 3 in. The shell and end liners last approximately 600 to 700 clays. Manganese-steel lifter bars, 3 5/8 in. thick, are used, spaced about 11 in. apart, and they give a life of 350 to 450 clays. Fig. 1 shows the general design and thickness of the wave-type liners and lifter bars; 1 1/2 -in. liner bolts are used to fasten the lifter bars to the shell. The shell liners are held in place by the tapered lifter bars. A ¾-in. wood hacking is used between the shell and the liners. The rod-mill scoop has removable manganese-steel lips, which last 250 to 300 days. The scoop proper has shown some wear in spots; and these spots have been protected by rubber bolted over them. Water and milk of lime are added to the elevator feeding the mill, but not enough water to cause a pounding of the rods against the shell. Roughly, the water added amounts to 2.5 to 33 per cent of the ore. Addi-tional water is added to the mill discharge to facilitate distribution to the classifier bowls in the fine-grinding department.

Jan 1, 1938

By Martin Coryell

Ehrenberg was the first to publish and direct attention to the peculiarities of the diatomaceous deposit of Richmond; but how and by whom he was supplied with the material for his microscopical investigations, is not generally known; but we may presume W. B. Rogers, formerly State Geologist of Virginia, furnished the material, and may have given the geological position or horizon. OF these facts we have no available evidence, nor have we any estimate of the thickness of this stratum of diatomaceous or infusorial earth. At the request of a member of this Institute, I have investigated the subject, and offer the following facts as the result, derived principally from information supplied by Mr. John Ott, of the Southern Fertilizing Company, Dr. William Taylor, State Chemist, C. Peticolas, microscopist, Captain Robert H. Temple, civil engineer, Major C. M. Bolton and Mr. C. M. Smith, civil engineers, and formerly engaged in constructing the tunnel under Church Hill, in Richmond. The city of Richmond is generally described as being built on seven hills. This is not the fact, geologically speaking. Originally, there was an immense plateau of land, about two hundred feet above tide, in which a deep excavation was made from the west to east by the James River cutting down to the granite. Opening southward and meeting the valley of the James are various ravines and gullies, in the principal of which are Shockoe and Gillies Creeks. The formation is tertiary, subdivided into all the classified divisions, but at the present moment no one has been found to make this section a special study. Rogers&apos;s early classifications and diagrams, with all their imperfections, are the only published records, and the printed editions are long since exhausted. The city of Richmond is really situated in these ravines of the James, Shockoe, Gillies, and their connections. The profile marked A, Plate V, represents the section of the plateau