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By R. M. Sellwood

The No. 4 I.S.F. Smelter Complex at the Avonmouth Works of Imperial Smelting Corporation (N.S.C.) Limited commenced operation at the beginning of 1968. The furnace rating is 120,000 tons zinc and 40,000 tons lead per annum. Zinc and lead concentrates are unloaded onto a 1,000 tons per hour capacity conveyor belt and automatically weighed and sampled before receipt into a 48,000 ton capacity raw material store. Distribution is by a reversible boom stacker into 16 x 3,000 ton bays and recovery is by a front end loader. Materials are fed to 16 proportioning bins for feeding via continuous weigh feeders to a 132 square metre effective updraught area sinter machine with a material flow rate of 240 tons per hour over the machine. The required quantity of output lump sinter at up to 800ºC is fed to 2 x 600 ton storage bins on the I.S.F. plant. By-product SO2 rich gas is fed to a conventional wet gas single stream acid plant rated at 600 tons per day utilizing a dry N.T.P. gas volume of 100,000 cubic metres per hour. The hot sinter and preheated coke (800ºC) are automatically neighed and charged to a 27.3m2 shaft area I.S.F. fitted with 2 x 5.5 m. wide lead splash condensers. Grade 4 zinc is tapped and transferred to the zinc refinery. Conventional type lead bullion and slag are tapped from the bottom of the furnace through a separation forehearth. The refinery consists of 6 lead and 3 cadmium columns to produce some 52,000 tons per annum of S.H.G. metal. S.H.G. metal and Grade 4 metal is cast into various shapes as required.

Jan 1, 1970

By Richard I. Petritz

A brief review of today's processing of integvated circuits is given. The major trends in the development of advanced integvated electronics are identified as 1) the broadening of the integvated circuit concept to a large class of circuit function, 2) the processing of more complex circuits within relatively small chips of silicon, and 3) the processing of very large electronic functions on complete slices of silicon. This latter trend, called array technology, is then developed in detail. Emphasis is given to defining the key tech-nological problems. Current progress being made is illustrated. THIS paper will endeavor to identify the major trends in advanced integrated electronics technology. One of these, array technology, will be developed in some detail. The array technology discussion will identify the key problem areas. Since it is the scope of the entire meeting' to present specific progress in the science and technology of integrated electronics, we shall indicate general directions being explored rather than discuss comprehensively solutions to the problems. In order to set the stage for the discussion of future trends in integrated-electronics technology, let us briefly compare the processes by which circuits are fabricated through discrete-device technology with that of integrated circuits technology. The reader is referred to the December 1964 issue of Proceedings of IEEE2 for a comprehensive review of integrated electronics. The article3 by Jay Lathrop is an excellent discussion of integrated-circuits technology. A discussion of the history of semiconductor technology is contained in Ref. 4. A) Current Status of Integrated Electronics. Fig. 1 (top) shows the process by which circuits are constructed from discrete devices. Key points are: 1) Slices containing large numbers of transistors or diodes are processed separately. 2) The slices are scribed into small chips (on the order of 15 mils on a side is about as small as can be conveniently handled) each chip containing one transistor. 3) Each device is specified separately—circuit -function specs are derived largely from device specs. 4) Circuits are formed by connecting together the discrete devices. 5) The number of circuit connections required is approximately equal to the number of devices. 6) There are potentially many more discrete devices per inch2 of semiconductor—only our lack of ability to handle them in discrete form prevents us from going to several orders of magnitude higher density iin Fig. 1, 400,000 transistors are discussed at 1.5 mils on a side). The bottom part of Fig. 1 illustrates the integrated circuit process. Key points are: 1) On the same slice of silicon, transistors, diodes, and resistors are processed grouped to do a complete circuit function. 2) While still in slice form, the components are interconnected into circuit functions by an evaporation process, eliminating the need for separate interconnection steps later. Dramatic improvements in cost and reliability are realized. With a simple flash of metalization thousands of interconnections are reliably made. 3) The slices are scribed into chips which contain complete circuit functions. 4) The circuit functions are specified-not each component in the circuit. This important point was missed by some of the early opponents to integrated circuitry. They argued that, with device yields at x pct, integrated circuit yields would be pct, where n is the required number of devices to make a circuit. This argument leads to extremely low yields for integrated circuits. The fallacy of the argument is that in integrated circuits each device is not specified separately. Furthermore, since a device is forever integrated into a specific circuit function, it need meet only the requirements for that particular function. Discrete devices, on the other hand, are tightly specified so that they can be applied to a variety of circuit functions. 5) Extremely high packing densities are achievable because one need only make the basic devices as large as the circuit demands. Their size is not dictated by handling requirements. A current example

Jan 1, 1967

By A. A. Bauer, M. S. Farkas, F. A. Rough

An investigation of the d-phase relationships between the uranium-zirconium and uranium-molybdenum systems was conducted. A ternary cut joining U-31.5 at. pct Mo to U-74 at. pct Zr is presented on the basis of differential thermal analysis, metallographic and X-ray diffraction data. HyDothetical isothermal ternary sections, inferred from the determined d-phase relationships, are presented for the uraniztm-zirconium-molybdenum system. A ternary eutectoid, at 454ºC, was found in zirconium-rich alloys. Its composition, based on metallography and electron-beam micro-analysis, is estimated as U-61.7 at. pct Zr-7.1 at. pct Mo. URANIUM binary systems have been studied extensively in the past to supply basic information needed in reactor-fuel development. Alloys of uranium with zirconium, molybdenum, and titanium are of particular interest because, in these binaries, extensive or complete solid solubility between the body-centered-cubic forms of these elements and y uranium exists. In addition, an intermediate phase of limited solid solubility forms in each of these systems by transformation of the high-temperature ?-uranium phase. Previous investigation of the phase relationships existing between the intermediate 6 phases in the uranium-zirconium-titanium and the uranium-molyb- denum-titanium ternaries have already been reported.1,2 The results of an investigation of the phase relationships existing between the 6 phases in the uranium-zirconium-molybdenum system is reported here. The phase equilibria that occur in the solid-state portions of the pertinent binary systems are shown in Fig. 1. Phase nomenclature appearing throughout the report is as shown in these diagrams. The crystal structure of the phases in this system are given in Table I. EXPERIMENTAL PROCEDURES Alloys were cast and fabricated to 1/4-in.-diam rod. Specimens were heat treated and examined by metallographic and X-ray techniques. Thermal-analysis data were obtained.

Jan 1, 1960

By D. H. Bacon

Nearly all men are too busy with their own affairs to keep informed of the progress in other lines. From time to time we read statistics showing the development in some industry that astonish us; but the feeling of surprise soon fades: to be followed by others that likewise pass away. A short resume of what has been done in one line may be of interest. Down to late in the fifties the ore-product of Lake Superior mas handled over a mule-tram-road to Marquette; now the Duluth, South Shore and Atlantic, the Chicago and Northwestern, the Wisconsin Central, the Duluth, Superior and Western, the Duluth, Mesabi and Northern, the Duluth and Iron Range and the Lake Superior and Ishpeming railroads serve the shippers. Down to nearly 1870 a 700-ton ship was an enormous craft, the loading of which required two days; the unloading being seldom accomplished in that time. In 1871 the largest ore-barge carried 1050 toils and made twelve trips per season. Now the cargoes reach 5000 tons, the loading requiring less than three hours, and the unloading ten hours. Now the mines cover more land than was familiar to even the " timber-cruiser " when the Jackson mine was opened. The annual shipments have grown from a few thousand to 10,000,000 tons, and the ability of the mines to produce is not taxed. Lake-freights are at one-eighth, and rail-freights at one-quarter, of early prices. The deeper waterways, commodious locks and large ships of to-day are in a greater measure due to the movement of ore than to any other cause. Great savings have been made in each detail of each department. The only item of cost that has not been lessened, I am glad to say, is the money paid to men. Wages, measured by what they will buy, are as high

Jan 1, 1898

By J. G. Morlet, A. R. Troiano, H. H. Johnson

Delayed failure in steel occurs by controlled initiation and growth of a crack. The incubation period for crack initiation was measured. Crack initiation and Propagation are controlled by interaction between hydrogen concentration and triaxial stress state. The incubation period results from stress-induced diffusion of hydrogen to the point of crack initiation. THIS paper describes the phenomenon of delayed failureland the kinetics of crack initiation and propagation in uniformly hydrogenated steel. The investigation was prompted by service failures of high-strength-steel components at applied stresses far below the conventional yield strength, after the part had successfully sustained equal or higher stresses for an extended time interval. This delayed failure phenomenon, often termed static fatigue, is associated1 with the presence of hydrogen. This is not surprising, since the voluminous literature on flaking and hydrogen embrit-tlement demonstrates that hydrogen may exert a potent embrittling influence. Flakes, or internal hairline cracks in alloy-steel forgings, are related to the presence of hydrogen retained from the steel-making process.2 On the other hand, embrit-tlement arises from hydrogen introduced during surface treatments such as acid pickling or electroplating. Laboratory delayed failures have been induced in notch specimens of 4340 steel by electrolytic charging of the specimen surface with hydrogen and subsequent static stressing.l,4,5 Static fatigue was observed over a wide range of applied stresses; however, failure did not occur below a critical applied stress, designated as the static fatigue limit. In this instance the extended time for failure resulted primarily from the macroscopic redistribution of hydrogen. A crack formed to the depth of the hydrogen enriched "case* upon loading; further crack growth naturally awaited diffusion of hydrogen into the material ahead of the crack. The crack-propagation rate was therefore controlled primarily by the macroscopic diffusion of hydrogen into the specimen interior during the test. Thus, in this instance static fatigue was associated with the movement of a gross concentration gradient. However, delayed failure in steel of uniform hydrogen concentration is of greater fundamental interest, as well as commercial significance. With a homogeneous hydrogen distribution a different mode of delayed failure might be expected. As the heterogeneous hydrogen distribution became more uniform,4,5 the initial crack-propagation rate decreased markedly and, in fact, what appeared to be an incubation period for crack initiation was observed. However, the macroscopic concentration gradient precluded an accurate evaluation of these observations. Although the existence of an incubation period, up to this time, has not been established definitely, it is not amiss to point out some implications of the concept. It is of interest in all hydrogen-induced embrittlement phenomena, such as flaking, delayed failure, and hydrogen embrittlement. Much discussion has centered around the possibility of an

Jan 1, 1959

By Charles Luner

ALTHOUGH the kinetics of the atmospheric oxidation of tin have been studied,1-3 the kinetics in pure oxygen have not been reported. This note presents some results of the kinetics of the oxidation of tin foil in pure oxygen. The tin foil used in this investigation was 99.78 pct pure, the two major impurities being Pb (0.17 pct) and Sb (0.024 pct). The foil was degreased and air-dried prior to oxidation. The air-formed film was estimated by coulometric reduction4 of the surface oxides to be about 25A. The samples, which were in strip form and had a total geometric surface area of about 300 sq cm, were first evacuated at room temperature in an oxidation bulb to 1 X 10 -5 mm Hg and subsequently degassed for 1 hr at the temperature of the experiment. Spectroscopically pure oxygen was then introduced into the bulb. The rates of oxidation were measured by following the rate of pressure change due to oxygen consumption in a closed system, the volume of which was sufficiently large so that the pressure change during an experiment was 10 to 15 per cent of the total pressure. An oil-mercury manometer,5 with a sensitivity of 3 X x mm Hg (which corresponds approximately to 5 X 10 -7 gm of oxygen) was used to measure the pressure change. The oxidation bulb was heated by an oil-bath and controlled to within -10.3 C. The reproducibility of the rates was good, as determined by the coincidence of rates at 190oC for duplicate experiments. Fig. 1 shows the oxidation curves in the temperature range 168 to 211.5oC at 8 mm Hg pressure. The effect of pressure on the rate of oxidation at 190°C is also shown. The rate of oxidation was not markedly affected by changes in pressure in the range 4 to 9 mm Hg, except perhaps at the lowest pressure, 4 mm Hg, where after about 70 min there appeared to be a decline in the rate, as compared with the rate at the higher pressures. At the lower tem- perature, 168oC, and for short reaction times, it is difficult to distinguish between a linear relationship and a slight curvature in the oxidation rate. However, for longer times, there was a somewhat larger indication of curvature. The samples after oxidation were gold-colored in appearance. The oxide that was formed at 170°C was identified as a-SnO by reflection electron diffraction. This is in agreement with results obtained by other workers.6, 7 The rate data best fitted the logarithmic-oxidation rate law, w = K1n ln(1 + -t/to) [1] where w is the weight of oxygen consumed, t is the time, and K In, and to are constants. First estimates to were obtained according to the method of Taylor Thon8 and were then employed to obtain the best simuItaneous estimates of to and K In, that would fit the logarithmic expression. These estimates were found numerically, so that the residual variance could be minimized. The calculations were performed on an

Jan 1, 1961

By Robert Bosworth

THE liability for damages to the surface caused by subsidence is an ever present threat in all underground mining. In ordinary lode mining, this threat rarely materializes into an action, due to the method of mining metalliferous ores, the dip of the veins, and the nature of the ground itself. In the mining of coal, however, this threat is very real. The coal frequently lies close to the surface, in beds underlying large areas of land of which the surface is suitable for: agricultural or urban development. Furthermore, the coal is generally mined by the "room and pillar" method and when the pillars of coal are removed, the subjacent support is destroyed. This question of the duty of surface support has now become a very live one in Colorado. What was waste prairie land a few years ago has become valuable agricultural land dotted here and there with growing towns. Frequent references will' be made here to Colorado conditions and adjudicated cases, but those conditions and cases and the conclusions to be drawn therefrom are applicable to all coal-mining states. Briefly stated, the question is "Does the owner of the substrata or underlying mineral owe any duty of surface support to the owner of the superjacent strata or surface?" There is no absolute duty of support owed by the mineral owner and this assertion is made with full knowledge of numerous expressions to the contrary by courts of Pennsylvania, Illinois, Colorado and other coal-mining states. Whether or not any duty exists depends upon the circumstances surrounding each case, and since in the nature of things those circumstances are rarely identical, there can be no absolute rule.

Jan 1, 1928

By F. E. Gregory

MINING methods and customs in many districts of England are to this day strangely bound about by the records and traditions of the past. In some mining fields this is more apparent than in others, yet it is everywhere in evidence, for Cornwall with her mines under the sea, Wales with her famous quartzites, and Derbyshire with her remarkable cavern deposits, are all tinctured with quaint customs that have come out of the almost forgotten past. Here, modernism has never replaced tradition, and many of the laws are woven of the woof and warp of ancient custom. Indeed, these things exist because they have come to be part and parcel of the civil laws. And these laws are observed with meticulous care and accorded all the reverence due their venerable age. All activities pertaining to the mining of metals are hedged around by curious and ofttimes clumsy laws, each minute and trivial detail being covered by the civil code, and each petty law enforced by an ofttimes pompous official.

Jan 1, 1933

By A. S. Michaels, R. S. Timmins

A study of the effect upon oil recovery from an un-consolidated porous medium of chromatographic transport of selected reverse-wetting additives during water displacement is described. Flow tests were performed on hydrocarbon oil-saturated sand columns (containing connate water) into which small volumes of short-chain aliphatic amine solutions were introduced during water flooding. Concurrently, meusurements of oil-silica contact angles, oil-water interfacial tensions and oil-water distribution coefficients were measured us a function of additive concentration. Certain treatments were found to cause a slight reduction in oil recovery, while others produced a significant increase (up to 50 per cent of the normtzl irreducible rninimum oil saturation). Recovery eficiency was correlated most satisfactorily with the maximum degree of reverse wetting produced during additive transport; conditions which resulted in only mild oil wettability of the sand reduced recovery, while those favoring strong oil wetting increased recovery. A mechanism of reverse-wetting additive action during chromatographic transport is developed which ascribes the results to transient changes in oil-solid contact angle during flow, with consequent release of oil trapped by capillary forces. Implications of these observations with regard to improved waterflood efficiencies are discussed. INTRODUCTION The need for finding improved methods of oil production is amply illustrated by the large volume of oil considered economically unrecoverable by existing production practice. Water flooding has long been an excellent method of secondary recovery. However, even in those areas of a formation which are well swept by a water flood, 20 per cent or more of the oil remains trapped within the formation and is not recovered. This trapping of oil within the pores of the rock structure results primarily from interfacial forces. If these interfacial forces were altered, it is possible that the trapped oil could be released and recovered. The addition of surface-active agents to a water flood to alter the interfacial properties of the oil-water-solid system has received considerable attention as a method of increasing oil recovery. Studies of surfactant treatment have yielded varied and, in some cases, apparently conflicting results. Increased oil recovery using surface-active agents has been reported by a number of investigators. Others have found that use of surfactants in a water flood either has no effect upon oil recovery or decreases it. Since surface-active agents tend to alter the formation wettability and oil-water interfacial tension simultaneously, several investigators have tried to determine the role these two factors play in oil recovery. Data have been presented which indicate that the most desirable condition for the solid surface is strongly water-wet. Other results indicate that, although breakthrough recovery may be less, the greatest ultimate recovery is obtained when neutral wettability prevails.", " The desirability of low interfacial tension seems to depend upon the wettability of the formation. Reports of higher recoveries, when the interfacial tension is high in a water-wet system and low in an oil-wet system, are at odds with reports of increased recovery in water-wet systems when surfactants which decrease the interfacial tension are added to the water flood. A review of previous work studying the effects of using surface-active agents in a water flood shows that these agents produce widely different effects and that opinions as to the role of the various interfacial properties are diverse. The consensus, however, is that the interfacial properties are quite important in the displacement of oil from a porous medium by water. Even in those investigations where appreciable increases in oil recovery resulted from treatment with a surface-active agent, economic considerations generally made practical application of the treatment unattractive because surfactants tend to be adsorbed within the formation. This adsorption would necessitate using large quantities of surfactant if all of the flood water were treated to contain a given surfactant concentration, even if this concentration were quite low. Preston and Calhoun suggested that the principles of chromatography could be applied to the use of surface-active agents as a means of increasing oil recovery. A small volume of surface-active material is injec-

By A. M. Gaudin, A. F. Taggart

Flotation of ores is a practical utilization of the energy that resides in the surfaces of solids and liquids. The best known manifestation of this energy is called surface tension; an equally important, though less apparent, phenomenon is adsorption. This paper reviews some of the recent investigations of these phenomena, and gives the results of certain experiments performed by the authors. Surface tension is a manifestation of energy having its seat at the bounding surface between the adjacent phases of a multiphase system. Thus, at the interface between a liquid and a gas, or between two immiscible liquids, or between a solid and a gas or a liquid, there are forces capable of doing work, their magnitude depending on the nature of the adjacent phases and the extent of the bounding area. These surface forces are inappreciable when the ratio of surface to volume of the adjacent phases is small, but they become powerful when this ratio becomes large, as it does when one of the phases is highly dispersed. Froth flotation, which consists in buoying solids heavier than water to the surface of water by means of gas bubbles, utilizes the force of surface tension to attach the solid particles to the gas bubbles and again to maintain the floating mass of bubbles as a more or less persistent froth at the surface of a pulp for a sufficiently long time to allow its removal. It follows from the second law of thermodynamics that the potential energy of a system in equilibrium is a minimum. Therefore a multiphase system, tending toward equilibrium, will arrange itself in such a way that the total energy of the interfaces will be the least possible. This end can be accomplished in two ways: by a change in shape that will reduce the interfacial area; by a change in the nature of the surface layer in

Jan 1, 1923

By A. F. Taggart, A. M. Gaudin

Flotation of ores is a practical utilization of the energy that resides in the surfaces of solids and liquids. The best known manifestation of this energy is called surface tension; an equally important, though less apparent, phenomenon is adsorption. This paper reviews some of the recent investigations of these phenomena, and gives the results of certain experiments performed by the authors. Surface tension is a manifestation of energy having its seat at the bounding surface between the adjacent phases of a multiphase system. Thus, at the interface between a liquid and a gas, or between two immiscible liquids, or between a solid and a gas or a liquid, there are forces capable of doing work, their magnitude depending on the nature of the adjacent phases and the extent of the bounding area. These surface forces are inappreciable when the ratio of surface to volume of the adjacent phases is small, but they become powerful when this ratio becomes large, as it does when one of the phases is highly dispersed. Froth flotation, which consists in buoying solids heavier than water to the surface of water by means of gas bubbles, utilizes the force of surface tension to attach the solid particles to the gas bubbles and again to maintain the floating mass of bubbles as a more or less persistent froth at the surface of a pulp for a sufficiently long time to allow its removal. It follows from the second law of thermodynamics that the potential energy of a system in equilibrium is a minimum. Therefore a multiphase system, tending toward equilibrium, will arrange itself in such a way that the total energy of the interfaces will be the least possible. This end can be accomplished in two ways: by a change in shape that will reduce the interfacial area; by a change in the nature of the surface layer in

Jan 1, 1923

By T. A. Lang

For permanent structure underground, where rock is not competent, support usually consists of concrete or reinforced concrete. However, temporary supports in the form of timber or steel are often needed during construc-tion. Although the history of rock bolting is relatively short—50 years— their use has become widespread in general engineering construction as well as mining. This profusely illustrated and detailed study covers a broad range in the field of rock belting: from the behavior of rock and bolts including rock properties, masses, and structure; mathematical formulae for rock bolt applications; through analysis of various operations and descriptions of the bolts themselves. Rock construction is one of the oldest of the engineering arts and its origin is lost in antiquity. From the days when early man decided that he wanted to improve the natural caves which he was using for shelter and protection or made a river crossing by placing rocks to form a ford or causeway, we have had structures made of rock. It is not too much to say that rock in situ as a structural material forms part of every major engineering undertaking. Rock bolting is one means whereby the inherently good characteristics of rock in situ are preserved and used to the best advantage and the bad characteristics ameliorated. In many cases the latter are accentuated by construction processes used. Rock bolting, as with other rock construction techniques, is only just beginning to emerge from being an art. Consequently, its theory and practice is still more descriptive than mathematical. ROCK BOLTING In underground excavations, where the rock is not competent, support is provided. For the permanent structure, this generally consists of concrete or reinforced concrete. However, support may be needed during construction before the concrete can be placed, and conventionally this consists of timber or steel support in the form of ribs, struts, and lagging. Alternatively, rock bolts may be used. Although their use dates back over 50 years, it is only in recent years that rock bolts have become widely used, not only in mining but in general engineering construction. A rock bolt is a steel bar which is inserted in a hole drilled in rock. The end away from the rock face has a device which permits it to be firmly an- chored in the hole and the projecting end is fitted with a plate which bears against the rock surface. The bolt is placed in tension between the anchor and the plate, thereby exerting a compressive force on the rock. The essential feature of a rock bolt is that it is placed in tension. This distinguishes it from anchor bars which are grouted into holes in rock, but which are not prestressed. The difference between an anchor bar and a rock bolt when the rock bolt is grouted in is analogous to the difference between the reinforcement in ordinary reinforced concrete and in prestressed reinforced concrete. The view that rock bolts only pin or nail blocks or slabs of rock which are loose to the sounder rock behind them is erroneous. Rock bolts are useful for this purpose and have been so used for a long time. However, the term rock bolting, as used here, means the designed use of rock bolts to reinforce and develop the rock around an excavation into a structural entity which can competently play its part in a structure such as a powerhouse or a mine installation. Rock bolts behave quite differently than steel ribs. They can be installed at the working face directly after blasting and within a short space of time can be exerting a stabilizing pressure on the loosened rock surface. This early installation not only partially restores loosened blocks of rock to their original unloosened positions, but also it prevents the gradual relaxation or loosening of the decompression zone behind the new rock face. In contrast, steel ribs generally use timber blocks, wedges, and lagging between the ribs and the irregular rock surface. The timber is relatively compressible, and loosened blocks of rock must move outwards an appreciable distance before any load builds up on the steel ribs. Also, the ribs may settle as the foot blocks and foundation become compressed. Hence, it may take several days or weeks before the rock has moved sufficiently to make the steel ribs carry an effective load.

Jan 1, 1961

By R. E. Boni, G. Derge

SURFACE tensions of molten silicates are of metallurgical importance for many reasons. From a knowledge of their values, an insight into the problem of liquid slag structure can be gained. Also, such problems as separation of slag from metal, slag penetration of refractories, spreading of enamel coats on metals, bonding of cutting wheels, adsorption of gases, frothing of slags, and homogen-ization of slags are related to the surface tensions of the silicates. Because of the absence of a correlated review of the work that has been conducted in this field, the following survey is presented. It is not a complete summary of all the surface tension studies of silicates but only a review of the literature which is pertinent to metallurgical applications and research. Liquid Surface Tension The surface of a liquid differs from the interior in that its particles (ions, atoms, or molecules) are not

Jan 1, 1957

By H. H. Podgurski, J. C. M. Li, Y. T. Chou, F. N. Davis, R. A. Oriani

When an Fe-2 pct A1 alloy is nitrogemted at 500ºC with a gus tnixture (NH3-H2) in which the nitrogen activity has been kept Lou] enough to avoid the formation of iron nitride, a two-phase alloy is generuled which consists of AlN particles and a ferrite phase cotaining a heavy network of dislocations. The amount of nitrogen contained in such an alloy, when equilibrated with the nitrogenating atmosphere, far exceeds both that needed to satisfy the normal solution requirements of a Fe and that needed to convert all of the aluninuwi to AlN. This excess nitrogen is accounted for as being trapped on dislocations, adsorbed at the ferrite -AlN interface, and as an en-Iuznced lattice solubility in strained ferrite. This excessive uptake of nitrogen had previously been attribuled by other investigators to the formation of a nonstoichiornetric aluminum nitride. Isotope exchange experiments revealed various amomts of exchargeable N14 present in the originally nitrided samples that could not be removed by reduction with HS at 500ºC. This exchangeable nitrogen has been identified us that bound to the AlN -ferrite interface. Estimates of inter facial areas in alloys containing -3 pct by weight of A1N are as high as 10 sq m per g of alloy. ThE first1 of this series of papers described the experiments forming the basis for the elucidation of the mechanism of the formation of aluminum nitride particles within an Fe-A1 alloy. It was found that not only are dislocations necessary for the nucleation of the AlN particles but also the nitriding reaction in turn produces a dense network of dislocations in the ferrite matrix. It was also observed that nitrogen in excess of that needed for the formation of stoichiometric AIN is taken up by the alloy without the formation of an iron nitride. The present paper is an analysis of the excess nitrogen sorbed by the nitrided Fe-A1 alloy which considers the structure generated by the formation of the aluminum nitride particles. Because of the high density of dislocations, this system has proved to be quite useful in studying nitrogen-dislocation interactions. Wriedt and Darken2 have already reported such studies in a cold-worked ferritic steel. EXPERIMENTAL Nitrogen Sorption. The specimens of this alloy were cold worked (50 pct reduction) to 0.011 in. thickness and chemically cleaned in a 2:1 concentrated phosphoric acid-50 pct hydrogen peroxide solution before nitrogenation. The flowing nitrogenating atmosphere (11 pct NH3-89 pct H2) was established before the ni- trogenating temperature was reached. The same gravimetric and gas-flow equipment described in an earlier paper1 was also used in this investigation. Changes in nitrogen concentration were followed gravimetrically when establishing the isotherms. In the isotope exchange experiments, concentration changes were followed volumetrically. In some instances chemical analyses (Kjeldahl method) were used to check for material balances in both the gravimetric and volumetric procedures. Our objective was to obtain reversible nitrogen sorption isotherms for alloys equilibrated with NH3-H2 gas mixtures over a large range of nitrogen activity* and temperature. The *Defined as equal to PN H /P3/2 ,where P corresponds to partial pressure in atmospheres. Actually the nitrogen activity, aN, in the alloy equals K PNH3 /p3/2H2, where K is the equilibrium constant for the reaction NH3 = N + 3/2H2. upper limit for nitrogen activity was below that which would produce iron nitride; for reasons which will become apparent later, most of the sorption studies were made in the temperature range between 400" and 500'C. The alloy sample studied most extensively in this investigation was given a series of successive reductions (100 pct H2) and nitrogenating treatments at 500°C to attain a stabilized structure. Presumably some dislocations were lost during these treatments. Throughout most of the sorption studies, temperature was held at ± 1°C and the gas-phase composition was held to k0.2 pet NH3. Based upon the results of numerous diffusion experiments with this alloy* the 'Results to be published in a third paper of this series. times chosen for equilibration were considered more than adequate, Nitrogen Isotope Exchange. The first exchange experiments were carried out by circulating a measured quantity of H2 and NH3* (with a predetermined isotopic *The NH3 was synthesized over a synthetic ammonia iron catalyst using H2, and N2, enriched with N15. AS the NH3 was formed it was removed continuously from the gas phase by circulating the mixture through a refrigerated (78ºK) trap. When most of the nitrogen had been converted to NH3, it was distilled from the trap into a glass storage vessel. composition, N15/N14) over a nitrided specimen at 450°C in a closed glass system. Attempts to reach the exchange limit isothermally, i.e., an isotopic ratio (N15/N14) in the gas phase identical with the extractable nitrogen in the nitrided alloy, were futile. The exchange rate between the gas phase and the alloy was too slow, involving many days. To circumvent the slow exchange with the gas phase, measured amounts of N15 and N14 were introduced into the alloy by nitrogenating with an NH3-H2, mixture at 500°C containing an N15/N14 ratio of 7.76; the charged specimens were then sealed by allowing an oxide film to form over them in air, and in this final condition the specimens were subjected to 500°C in vacuum for various times during which isotope exchange was allowed to proceed within the specimen. It was estab-

Jan 1, 1970

By T. Egleston

The manufacture of charcoal in kilns was declared many years ago, after a series of experiments made in poorly constructed furnaces, to be unprofitable, and the subject is dismissed by most writers with the remark that in order to use the method economically the products of distillation, both liquid and gaseous, must be collected. It is asserted with truth that the number of kilns required for a large production of iron would be so great that it is doubtful whether any works would be justified in making the necessary outlay for their constructiou, but it can also be asserted with equal truth that for any such production in a given locality the use of charcoal as fuel would be eqnally unjustifiable. It appears to have been forgotten that there were other manufactures besides iron in which large amounts of charcoal were used, but these consumers seen] to have been guided entirely by the results of the experiments of the iron men, who necessarily made the largest qnantity of it. Some authors speak in a doubtful way of the quality of the charcoal produced, and a few concede that with great care good charcoal can he made in kilns, but that most of the workmen do not like kiln 'charcoal. This is the real secret of the opposition to this method of manufacture. Most of these objections were written when charcoal was the most important fuel used by the iron manufacturer, and when what was a largeproduction of iron for several furnaces was less than that produced by a single modern one, in localities where other fuels can be had. Almost all that has been written on the subject related to the use of the fuel for the manufacture of iron in the blast furnace, where very peculiar properties are required, and where the qnantity produced is limited by the height of the furnace, and this in turn by the crushing resistance of the charcoal. A large production was, therefore, only possible when the best and hardest woods were used. Of all these objections there is not a single one which is not eqnally applicable to any method of charcoal manufacture, whether it be meilers, pits, or furnaces. Until recently, therefore, the manufacturers of charcoal iron

Jan 1, 1880

[ ] DISCUSSION F A LORIA*-The method of testing gun steel for resistance to surface cracking described in this paper was restricted to the examination of small, rod-shaped specimens The writer would like to point out the importance of other factors in producing defects in forged and bored gun tubes which would not be apparent in this investigation because of the nature of )he test Actual section size would accentuate the possibility of internal wall (bore) defects arising from unequal expansion between the internal and external wall surfaces on firing, resulting in internal tearing Checks and tears on the inside walls arise from internal tensions and nonuniformity on cooling, but the internal tearing can be reduced by using alloys of low expansion and of good thermal conductivity so as to reduce the difference between the outer and inner wall surfaces Also, the possibility of the location of inclusion segregates within a machined gun tube becomes more likely than in a small test specimen The effect of these nonmetallics on gun life and performance is evident when one realizes that the inclusions are soft yet brittle They reduce the amount of plastic deformation which can take place before cohesive failure occurs Once localized fracture has occurred at the position of a chain of these inclusions, a sharp notch (crack) is formed which produces stress conditions more favorable to cohesive failure than to plastic deformation These cracks aid erosion by providing channelways for the explosive gases, eventually leading to the tearing out or spalling of blocks of metal Oxidation of the surface may be partly responsible for the change in the surface of gun steel during firing observed by the author The appearance of burn on the surface is an indication that high temperatures were reached on firing, resulting in a slight oxidation of the surface Since the color of the oxidized film depends on both temperature and time, a higher temperature is required for a given color to form when it is caused by explosive heat, which acts for only an extremely short time at a given spot, than when it is caused by ordinary tempering The cross section of the gun steel specimen, Fig 16, illustrates that the repeated firing temperatures were high enough to cause

Jan 1, 1948

By H. L. Marcus, P. W. Palmberg

As can be seen from the phase diagram A1-W1 the equilibrium solubility of tungsten in aluminum is practically nil at room temperature. By quenching from the liquid state (50,000°C per sec), Varic, Burov, and Kolesnicenko2 obtained A1-W solid solutions up to 0.15 at. pct W. The quenched alloys were in the form of foils, 0.2 to 0.3 mm thick. Considering the results of Duwez and Willens,3 it is obvious that this thickness, which makes impossible a sufficiently rapid quenching, was the main reason for the relatively low content of tungsten dissolved in aluminum found by Varic.2 he present note shows that the metastable solubility of tungsten in aluminum can be appreciably extended in aluminum-rich A1-W alloys. The quenching technique and the procedure employed for the preparation of the alloys have been described previously.475 The resulting quenched flakes varied in thickness from 1 to 20 µm from experiment to experiment. However, the measurements of the lattice parameters were carried out only with flakes thinner than 5 µm. The areas of quenched flakes were between 0.1 and 15 mm2. The quenched flakes were placed into a 0.3-mm glass capillary tube which was then mounted in a 114.6-mm-diam Debye-Scherrer camera. Straumanis asymmetric film position and nickel-filtered CuKa radiation were used. The lattice spacings were computed taking X(CuKa1) = 1.54050A for resolved and ?(CuKa) = 1.54178A for unresolved doublets. All specimens were rotated at room temperature, 26" +2°C. The lattice parameters were estimated from extrapolation against the Nelson-Riley function. It was estimated that the error in the lattice parameter of the measurements on a single film lies within +0.0004A for lower and about +0.001A for higher concentrations of tungsten. The lattice parameters of the metastable solid solutions A1-W are plotted vs the concentration of tungsten in Fig. 1 together with the parameters measured by previous investigators.' Each point of the present measurements represents a determination of the lattice spacing on different quenched flakes, for a given concentration of tungsten. With experimental accuracy, the lattice parameters of the metastable solid solutions fall on the straight line passing through the already known data.' As estimated from the uncertainties in the lattice spacings of the solid solutions, the alloys were homogeneous within 0.1 at. pct W. The solubility of tungsten in aluminum-rich A1-W solid solutions obtained by a very rapid quenching technique is increased to about 0.95 at. pct W. This value is 6 times greater than the amount known up to now. -he lattice parameters of the resultant aluminum solid solutions with higher concentrations of tungsten than 0.95 at. pct W did not remain constant AUGER electron spectroscopy has been used to clarify the role of impurities in the embrittlement of AISI 3340 steel. Analysis of fracture surfaces has shown that the embrittled condition is correlated with appreciable antimony segregation at grain boundaries. The low temperature (400" to 600°C) temper embrittlement of low alloy steels containing various combinations of Cr, Ni, Sb, Mn, P, Sn, and As has been examined extensively for many years. General reviews of the area have been made by McMahon1 in 1968, LOW' in 1959, woodfine3 in 1953, and Holloman4 in 1946. Recent work by Low, Stein, Turkalo, and LaForce5 has done much in separating the alloy and

Jan 1, 1970

By G. R. Love, M. L. Picklesirner

THE use of color adds a new beauty, power, and versatility to metallography. This has been amply demonstrated in a number of public exhibits and on the walls of corporate, government, and university metallographic laboratories around the world. Indeed, in a number of cases, the color not only is of esthetic value but is scientifically essential to the competent examination of particular samples and systems. Optical strain analysis,' determination of true grain size in U-A1 alloys: phase identification in Nb-base alloys,3 analysis of transformation rates in heat-treated Nb-Zr alloys,4 measurement of solidification segregation in cast Nb-Zr alloys,' study of the intermediate phases in Nb/Sn diffusion couples,6 investigation of the oxidation kinetics at various surface orientations in single crystals,7'8 and a number of other research efforts9'10 would have been vastly more difficult without the extra clarity and distinction introduced by color—either the colors resulting from particular polarized light techniques or the interference colors obtained by oxidation. It is unfortunate that the beauty of colored micro-structures cannot be shared more widely, but the economics of publishing a technical magazine apparently prohibits color plates except under extraordinary circumstances. It is doubly unfortunate that no convenient, general method exists for communicating the information available in colored microstructures to the scientific community. True, in some instances the color changes observed are dramatic enough that direct black and white photography is adequate. In photoelastic stress analysis, several orders of interference fringes may be produced and it is frequently desirable to suppress the color effects (use monochromatic light) to simplify interpretation. On the other hand, relatively minute color variations may be readily detectable by eye, be of considerable assistance in interpreting a structure, and yet be enormously difficult to reduce to an unambiguous black and white print. In order to illustrate a possible compromise or solution to the above problems, we wish to show three black and white photographs of the same region of an Nb/Sn diffusion couple whose interpretation depends heavily upon use of color techniques. These micro-structures were obtained from a section through a rod consisting of commercial-purity niobium tubing filled with 99.995 pct Sn (melt-filled in 10"6 Torr vacuum). The composite rod, measuring 500 mm long, was bent into a hairpin shape and inserted into water-cooled copper grips in a vacuum high-temperature furnace. The rod was outgassed for 2 hr at a furnace temperature of 800°C and was further heated by self-resistance using a 2.2-kva ac power supply. The rod was raised to 1910°C over a 4+-hr period, held for 15 min, slow-cooled to 1500°C over a -hr period, and free-cooled to room temperature (all temperatures were measured with W5Re/W26Re thermocouple). Throughout the heat treatment the ambient pressure was kept below 8 x lo-' Torr. Metallographic preparation of the sample was completely conventional except that it was necessary to extend the grinding steps to remove damage in the brittle NbsSn phase introduced by sectioning. No satisfactory chemical or electrochemical etch has been found for these diffusion couples; of those which have been tried, any that attack the niobium-rich phases at all attack the tin-rich phases disastrously. However, the final polishing steps did produce a slight relief effect and this, coupled with anodizing, yielded excellent clarity in the microstructures for direct observation. The anodizing voltage was chosen to give maximum change in color per unit change in composition. In this case, indeed normally, this maximum sensitivity occurred in the blue-to-red color range. The pure niobium tube wall anodized to a relatively bright blue

Jan 1, 1967

By Robert Henderson

SEVERAL very interesting articles have been written on the caving system of mining, but most of these papers have dealt separately with the slusher system or the chute and grizzly system. In this paper, a comparison will be made of the two methods, both of which are being used at the Climax mine. The mine is on the Continental Divide, in central Colorado, at an altitude of approximately 11,500 ft. above sea level. The long, cold winters, characteristic of the high Rockies, create a number of operating problems not usually found in other mining areas. THE ORE BODY The Climax ore body is just east of the Mosquito fault. This structural deformation has brought the granite on the east against the sedimentary rocks on the west. The ore occurs in an intensely altered granite and schist around a silicified granite core. The ore is in a highly fractured zone of moderate silicification. The principal mineral, molybdenite, is found in these fractures. Barren dikes of granite porphyry cut through the ore body and core with no apparent regularity. The grade of the ore is fairly uniform and gradually decreases toward the footwall core and also into the hanging-wall granite. The footwall and hanging wall are determined entirely by assays. The ore body is roughly dome-shaped, with the apex truncated at the surface. It is covered to varying depths with talus. A horizontal section of the ore body on the Phillipson level appears as an annular ellipse surrounding the footwall core. The ring of ore varies in width from 300 ft. to as much as 800 ft. The north-south axis of the core is about 1200 ft. and the east-west axis is about 1800 ft. In the ore zone, the rock is sufficiently strong to maintain reasonably large openings, and openings larger than haulage drifts usually have to be supported. The ore is cut by a great many fractures and shears and breaks into rather large blocks when caved, necessitating considerable secondary blasting. The waste that overlies the ore body breaks relatively fine in comparison with the size of the blocks of the caved ore and tends to run through the broken ore in the cave, causing dilution unless the draw is carefully controlled. MINING SYSTEMS For several years the ore was mined by the chute and grizzly system, a system that differs from that used in other caving mines only in the size of openings and equipment. In the chute and grizzly system, main haulage laterals were driven along the footwall core and also along the

Jan 1, 1944

By Charles S. Barrett

This paper is a progress report covering metallographic applications of the electron microscope that have been made during the past year at Carnegie Institute of Technology. An account is presented of the techniques that have been most satisfactory, the difficulties encountered, the resolution obtained, and the peculiarities that have been noted in the microstruc-tures. About 1200 exposures have been made during the year on the instrument, which is an RCA type B2 transmission microscope,' and a number of these have been selected to illustrate the results obtained. prints are also included showing the common types of falsities—to borrow a term from the biological field, the "artifacts." ln brief, the paper is a record of our attempt to determine the value of the electron microscope in the study of the structure of metals and alloys. In addition to comments on techniques and the quality of photomicrographs obtainable with them, the paper discusses the nature of the etch attack on a few metals, and the possible relation between the fine structure revealed by etching and the mosaic block structure of the grains, since numerous papers and reviews are available on the subject of imperfection in crystals, the comments here may be very brief; in fact, are restricted almost entirely to points having to do with recent theories relating the strength of metals to imperfections and to spacings of slip lines. Specimen Preparation and Photographs Mechanical polishing by hand was used throughout this work. Precautions that must be taken in microscopy at high magnification, which have been well explained by Vilella in his book on Metallographic Technique for Steel, are likewise important with the electron microscope. This applies particularly to the need for these polishing and etching (each successive polish becoming less severe and each etch lighter), since the fina1 etch should in general be no heavier than is used for oil-immersion optical microscopy and in many instances should be much lighter (compare Figs. 6a and 7a, 6d and 7b). An extremely light etch, of course, is incapable of cutting through a flowed layer of appreciable thickness. Unquestionably it would be very advantageous in each instance to compare the structures obtained by electrolytic polishing with those obtained by mechanical polishing, but difficulties with the electrolytic method have prevented this in the following collection of prints. The choice of etchant is important, of course; for example, picral proved superior to nital for tempered martensite. With the exception of Figs. Ib and 16, the replicas used were of silica, deposited upon polystyrene and floated from the polystyrene in ethyl bromide according to the method of Heidenreich and Peck.2 The samples were mounted in Bakelite, polished and etched, then the polished Bakelite

Jan 1, 1944