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By W. F. Chiao, R. B. Gordon

Tile sharp-yield point found in magnesium crystals in the solulion-treated and aged condition is studied by dislocation internal-friction experiments. The results show that the sharp yield is not file to the sudden release of pinned dislocations hut is movc likely due to the rapid multiplication of an initially small number of dislocations. Recovery or the dislocation internal friction after deformation is also studied. This yecovery results from the re-pinning of dislocations by a solute, presumably nitrogen, which moves with a relatively small activation energy. SHARP-yield points, when they occur, are a striking feature of the stress-strain curve generated during a tensile test. Although commonly associated with steel, sharp yielding has been found in a variety of metallic and nonmetallic crystalline materials. In particular, sharp-yield points have been found in zinc"' and cadmium3 containing nitrogen. With this background, Geiselman and Guy4 investigated the tensile properties of magnesium single crystals containing nitrogen to see if sharp yielding also occurs in this system. They found that sharp yields did indeed occur in solution-treated and aged specimens tested at elevated temperature but were not able to give conclusive proof that the sharp yield was caused by nitrogen, a yield drop being observed even in their purest crystals. Sharp-yield points have also been found in various polycrystalline magnesium alloys.7'8 In the study of the sharp-yield phenomenon it is desired to observe the behavior of dislocations in the earliest stages of the deformation process. Internal-friction experiments are useful for this purpose because dislocation damping is sensitive to the mobility of free-dislocation segments. At low strain amplitudes the damping, A, due to the the forced vibration of dislocation segments of average length L is ? =KAL4 [1] where A is the dislocation density and K, if the applied frequency is well below the resonant frequency of the dislocation segments? is a constant for the sample under observation.5 Dislocation damping, because of the fourth-power dependence on L, is particularly sensitive to the creation of free-dislocation segments during deformation. Since sharp yielding is associated with the sudden release of pinned-dislocation segments, marked changes in the dislocation damping are expected at the yield point.6 The use of the dislocation-damping observations to help elucidate the incompletely understood mechanism of yielding in magnesium is the primary objective of the experiments reported here. PROCEDURE Many investigations have shown that very marked and rapid changes occur in the dislocation damping of of a deformed material as soon as the straining is stopped.5 It was quite essential, then, for the purpose of this investigation, to make the damping measurements during the deformation of the samples. This can only be accomplished through the use of the ultrasonic-pulse method. In this method traveling sound-wave pulses are used and, in contrast to resonating-bar methods, only the sample ends are set in vibration. Thus, the sample can be gripped along its sides in the tensile-test machine without disturbing the damping measurements. In the pulse method, the decrease in the amplitude of a sound pulse is measured as it travels back and forth through the sample. If A is the amplitude after traversing a distance x and A. is the initial amplitude, A=Aoe-ax [2] and a is called the attenuation. It is commonly measured either in units of cm-I or as db per µ sec. The observed attenuation in a metal sample is due to a number of causes. These include scattering by grain boundaries and impurity particles, thermo-elastic damping, diffraction effects, stress-induced ordering of solute atoms, and dislocation damping. The total observed attenuation in a given sample usually cannot be resolved into these various components, but changes in a due solely to changes in dislocation damping can be accurately determined, provided the experiment is arranged so that all other sources of damping are held constant. It is desired to reduce the extraneous sources of attenuation to a minimum and for this reason the experiments are done on single crystals of high purity. Magnesium crystals offer the further advantage that, when properly oriented, only a single set of slip planes is active during deformation. Crystal Preparation. The method of sample preparation is similar to that of Geiselman and Guy.4 The starting material was high-purity, sublimed magnesium rod supplied by the Dow Chemical Co. Melting under Dow 310 flux was used to reduce the nitrogen content of the starting material: the fluxing was done under an argon atmosphere and the

Jan 1, 1965

By V.K. Zworykin

Throughout its development the science of electronics, like so many other branches of science and industry, has been indebted to the metallurgist. Metallurgy has provided the electronic engineer with conductors to furnish passage for electrons outside of his evacuated tubes: it has developed tungsten and tantalum wires for emitting electrons and various refractory metals and alloys suitable for electrodes, which receive them and guide them within the tube; finally it has supplied ferromagnetic materials both for shielding electronic apparatus from magnetic fields and for forming highly concentrated fields for deflecting electron . Today I hope to show you that electronics has not been altogether ungrateful for this assistance. More specifically, I wish to indicate the role that the electron microscope, a relatively recent product of electronic engineering, is playing even now in the study of metals. Every metallographer is aware that his standard metallographic microscope will not reveal structural detail involving separations smaller than a certain fraction —at the very best a tenth—of a micron. This limitation, he knows, is a consequence of the fact that the wave length of the light employed for forming the image has this order of magnitude. It is, thus, a property of all light microscopes. TO overcome it, a different imaging medium must be employed, The existence of such a medium became evident when it was demonstrated1 that electrons were affected by magnetic and electric fields with axial symmetry just as light is affected by glass lenses; these fields, or "electron lenses," curve the paths of electrons reaching them from an object located on the axis of symmetry in such a manner that, at some distance from the lens, a true image of the object is formed. Furthermore, although a wave length may . be ascribed to electron beams just as to light, this wave length is much shorter; for electrons accelerated through a difference of potential of 50 kilovolts, the wave length is only about one hundred-thousandth of that of visible light. Actually, the elcctron microscopes of today resolve detail one hundred times as fine as light microscopes; if the maximum useful magnification of the latter is taken to be a thousand, that of electron microscopes is one hundred thousand. The Electron Microscope Since electrons are readily scattered and absorbed by matter, specimens to be observed in the electron microscope must be prepared to be less than one micron in thickness; furthermore, the interior of the microscope must be carefully evacuated to prevent collisions between the clectrons and the molecules of the air. Finally, as already mentioned, the lenses are formed by axially symmetric magnetic or electric fields, and not by any material medium such as glass. Apart from these basic differences, the electron microscope closely

Jan 1, 1943

By V. K. Zworykin

Throughout its development the science of electronics, like so many other branches of science and industry, has been indebted to the metallurgist. Metallurgy has provided the electronic engineer with conductors to furnish passage for electrons outside of his evacuated tubes: it has developed tungsten and tantalum wires for emitting electrons and various refractory metals and alloys suitable for electrodes, which receive them and guide them within the tube; finally it has supplied ferromagnetic materials both for shielding electronic apparatus from magnetic fields and for forming highly concentrated fields for deflecting electron . Today I hope to show you that electronics has not been altogether ungrateful for this assistance. More specifically, I wish to indicate the role that the electron microscope, a relatively recent product of electronic engineering, is playing even now in the study of metals. Every metallographer is aware that his standard metallographic microscope will not reveal structural detail involving separations smaller than a certain fraction —at the very best a tenth—of a micron. This limitation, he knows, is a consequence of the fact that the wave length of the light employed for forming the image has this order of magnitude. It is, thus, a property of all light microscopes. TO overcome it, a different imaging medium must be employed, The existence of such a medium became evident when it was demonstrated1 that electrons were affected by magnetic and electric fields with axial symmetry just as light is affected by glass lenses; these fields, or "electron lenses," curve the paths of electrons reaching them from an object located on the axis of symmetry in such a manner that, at some distance from the lens, a true image of the object is formed. Furthermore, although a wave length may . be ascribed to electron beams just as to light, this wave length is much shorter; for electrons accelerated through a difference of potential of 50 kilovolts, the wave length is only about one hundred-thousandth of that of visible light. Actually, the elcctron microscopes of today resolve detail one hundred times as fine as light microscopes; if the maximum useful magnification of the latter is taken to be a thousand, that of electron microscopes is one hundred thousand. The Electron Microscope Since electrons are readily scattered and absorbed by matter, specimens to be observed in the electron microscope must be prepared to be less than one micron in thickness; furthermore, the interior of the microscope must be carefully evacuated to prevent collisions between the clectrons and the molecules of the air. Finally, as already mentioned, the lenses are formed by axially symmetric magnetic or electric fields, and not by any material medium such as glass. Apart from these basic differences, the electron microscope closely

Jan 1, 1943

By F. M. Sandoval, R. E. Ries, J. F. Power

Returning the original soil material to the surface of smoothed mine spoils is a practical means of restoring agricultural productivity. Research has established that high-sodium spoils in North Dakota: (1) must be covered with about 70 cm of soil material to achieve maximum production; (2) top-soil must be segregated and spread separately from subsoil; (3) potential production depends on the quality of the soil material returned; and (4) erosion and upward salt movement must be controlled for sustained production. Erosion is best controlled by reducing final grades as much as possible during the smoothing process followed by prompt establishment of vegetation.

Jan 12, 1979

By C. J. Chindgren

The Bureau of Mines investigated the technical problems involved in recovering commercial-grade vanadium products from alkaline solutions of low vanadium content. Conditions were defined for precipitating calcium vanadates from sodium vanadate solutions with calcium chloride and calcium hydroxide and for dissolving the precipitates with acid, sodium carbonate, and sodium bicarbonate to obtain vanadium-enriched solutions from which either red cake or ammonium metavanadate was recovered. Calcium vanadates with CaO:V205 mole ratios of 2, 3, and 4 were produced with recoveries of 93 to 100 percent. Optimum recovery of the low-lime variety of calcium vanadate was obtained by employing excess calcium chloride and adjusting the pH to a range of 8.0 to 8.5. High vanadium extractions were obtained in concentrated solutions by dissolving the calcium vanadate precipitates with any of the reagents tested. The resulting extracts contained 25 to 125 grams V205 per liter. Conventional procedures used to precipitate either red cake or ammonium metavanadate from the enriched solutions gave excellent vanadium recoveries.

Jan 1, 1967

By J. F. Smith, J. E. Davison

The heat capacity of CaMg2 was measured over the temperature interval, 4.8° to 287°K, by the technique of low-temperature adiabatic calorimetry. Heat content measurements were performed with a drop calorimeter over the temperature interval, 273" to 673°K. From these data the thermodynamic functions, (FT - H0)/T, ST - So, and & - Ho, were evaluated. A third-Law calculation of the standard entropy of formation of CaMg2 yields a value of -0.25 * 0.06 cal per (°K g-atom) , and the free-energy function derived from this study when combined with existing equilibria data yields a value for the standard enthalpy of formation which is in agreement with direct calorimetric enthalpy measurements. The accompanying paper' shows that the enthalpy of formation of CaMg2 has been determined with good precision by three different calorimetric techniques.'-= TWO independent determinations of the Gibbs free energy of formation of CaMg2 have also been made; both determinations were based on vapor pressure measurements, being in one case hydrogen vapor pressures over ternary Ca-Mg-H alloys4 and in the other case magnesium vapor pressures over binary Ca-Mg alloys.5 The present determination of heat capacity of CaMg2 below room temperature and of the heat content of CaMg2 above room temperature was undertaken to provide supplementary data. These data are useful in their own right but can in addition be used to evaluate an entropy of formation for CaMg2 which, because of the interrelation of free energy, enthalpy, and entropy, can be used as a check of the self-consistency of the composite of the presently available information. LOW-TEMPERATURE HEAT CAPACITY The heat capacity of CaMg2 was measured over the temperature interval 4.87° to 286.64°K in an adiabatic calorimeter. The physical details of the calorimeter and the experimental procedure for measuring the heat capacity of a specimen have been adequately described by Gerstein et a1.6 The source and purity of the calcium and magnesium are described together with the methods of sample preparation and chemical analyses in the accompanying paper.' Results of chemical analyses of the material which was used in the present investigation are shown in Table I. These analyses show that, on the basis of the published phase diagram,7 the heat capacity sample contained a slight excess of a calcium while the heat content sample contained a slight excess of magnesium. However, in both cases the excess was small, and X-ray diffraction patterns showed reflections which were without exception attributable to CaMg2. The sample which was used for heat capacity measurements weighed 69 g while the sample container and addenda weighed 132 g. The sample was in the form of annealed powder, 50 to 60 mesh, and was sealed into the sample container under 0.1 atm of helium. Copper fins inside the sample container facilitated thermal equilibrium of the powdered Sample. Time intervals of the order of 10 min were required for thermal equilibration, and such times are normal for this calorimeter regardless of the form of the sample. The observed heat capacities were corrected for the small excess of a calcium through use of the heat capacity values tabulated by Hultgren et a1.8 The corrected heat capacities are tabulated as a function of temperature in Table II. The free-energy function and the absolute entropy of CaMg2, which were calculated from the experimental heat capacity data, are listed in Table 111. A smooth curve was fitted to a plot of the experimental values of the heat capacity and in only two instances above 30°K did the plotted points deviate from the curve by more than 0.2 pct. Below 10°K the deviation of several of the points was as much as 50 pct. These large percentage deviations were attributed to the small value of the heat capacity and to the low sensitivity of the platinum resistance thermometer in this temperature range. The deviations in the region of 10°to 30°K were less than 5 pct. Although the percentage deviations of some of the low-temperature measurements are large, the actual value of these deviations is small since the magnitude of the heat capacity in that temperature range is small. The error in the value of the third-law entropy at 298.15°K was estimated to be less than 0.01 cal per (°K g-atom). A value of -0.25 ±0.06 cal per (°K g-atom) was obtained for the standard entropy of formation at 298.15°K from the relation:

Jan 1, 1969

By A Kondratiev, A E. Moiseev

Viscosity of oxide melts is one of the fundamental physicochemical properties that plays a crucial role in important technological and natural processes like slag flow, slag/metal separation, volcano eruptions etc. However, many oxides melt at extremely high temperatures and are highly corrosive in the liquid state, which makes experimental measurement of melt viscosity by traditional experimental techniques a difficult and expensive, if not unachievable, task. In this case it might be useful to employ other methods of viscosity determination such as modelling or simulation. In the present paper the shear viscosity coefficients of selected pure refractory oxides (CaO, MgO, Al2O3 and others) have been simulated at temperatures above their melting points via the classical molecular dynamics and compared to the available viscosity data (eg experimental viscosities, other model predictions) collected by the authors. The simulation has been carried out using the noncommercial molecular dynamics simulation package LAMMPS and the Born-Mayer-Huggins potential, which parameters for the selected oxides were taken from the literature. Several viscosity calculation techniques (the Stokes-Einstein and Green-Kubo equations, the so called Einstein relations, and the non-equilibrium molecular dynamics methods) have been applied to ensure a more reliable viscosity calculation. It has been demonstrated that the simulated viscosity of the selected melts agrees with the available experimental data. It has also been shown that the simulated viscosity of a number of the oxide melts investigated is close to that calculated by phenomenological viscosity models, which supports viscosity extrapolation from the corresponding binaries and ternaries, if no experimental data is present for unary systems. In general, it has been demonstrated that the molecular dynamics simulation could provide a reasonable estimation of viscosity if no other viscosity data is available.

Jun 19, 2024

By Charles A. Ashburner

' I. Natural-Gas Explorations. The rapid development of the natural-gas* industry in Western Pennsylvania, and the great economy which results from its use, both for manufacturing and domestic purposes, has led to an inquiry as to the occurrence of this gaseous mineral in all thickly populated and large manufacturing centers of the United States. Natural-gas springs are to be found in almost every State in the Union, and in many States gas has been obtained in wells sunk either for water, oil, or gas, or in search of solid mineral deposits. The occurrence of natural gas is, however, not dependent upon mere chance, as is popularly supposed, but upon the existence of special geological phenomena; this fact is now recognized by professional men and by many practical men concerned either in the exploration for or in the use of this gas. The desire among our leading manufacturers, to emulate Pittsburgh, has led to the sinking of many wells in many localities, in search of natural gas. Some of these wells are now being located and drilled under the direction of professional experts, but many more have been, and are still being located by "quack " explorers, who often depend upon spiritualistic communications, or the diviningrod, or by intelligent persons, who are ignorant, however, of the geological and physical conditions under which gas has already been found. My attention has recently been directed to a number of these exploring operations where holes have been drilled, and, after failing

Jan 1, 1887

By María Jesús Ojeda

El presente texto describe la aplicación de los principios de exploración geoquímica en un sector de la faja aurífera Nazca -Ocoña correspondiente a la mina "Las Agripiinas". El objetivo es determinar anomalías de oro en base a un muestreo sistemático de afloramientos y niveles ya en desarrollo y así ubicar nuevas áreas favorables para la realización de labores mineros que conduzcan a aumentar las reservas de la mina. La exploración por oro se realizó en rocas metamórficas esquistosas con vetas de cuarzo-pirita, intrusivos granodioríticos y volcánicos andesíticos caracterizados por procesos de dispersión primaría. La dispersión secundaria se determina en óxidos, producto de la alteración de los ferromagnesianos y sulfuros.

May 1, 1986

By Josef Intrater

A dilatometric determination of the a + ß region temperature limits was performed on vacuum melted Zircaloy-2. The temperature of transformation for a-a+ß and a+ß — ß on heating and cooling as a function of rate of heating and heat treating history was studied. The limits were found to be 815° to 830°C to 975° to 995°C on heating and from 960° to 930°C to 785° to 770°C on cooling. A 5° to 15°C increase was observed for a- a + ß with increased rate of heating and a 20° to 30°C decrease for ß - a + ß with increased rate of cooling. 1 HE transformation temperature for pure zirconium has been determined by many investigators1-5 using metallography, electrical resistivity measurements, and dilatometry. The effect of the rate of cooling on the transformation temperature of zirconium has been studied by Hayes and Kaufmann6 and Duwez,7 and the effect of alloying elements by pfei18 and McGeary.13 Since the development of Zircaloy-2, the limits of the a + ß region for that alloy have been also determined. The first reported temperature for the a — a + a transformation in Zircaloy-2 was 900°C and for a + ß - ß 1000C Subsequent studies by Picklesimer and damson" indicated the beginning of the transformation at 810°C, and the metallographic study by the Technology Group of the Special Materials Section at the Westinghouse Bettis plant1' suggested that 820°to 830°C is the temperature of transformation. The dilatometric investigation by the latter group yielded 830°C for the beginning of the transformation. Thomas and Forscher12 set the beginning of the transformation at 900 °C on heating and the end of the transformation at 870°C on cooling. The above investigators stated in their paper that the dilatometric curve exhibits features caused by a eutectoid reac-

Jan 1, 1962

By Taghi Sherizadeh, Kutay E. Karadeniz, Dogukan Guner, Samuel Nowak

Despite numerous empirical, numerical, and hybrid studies conducted on the subject of coal rib failure, mine fatalities related to rib failures continue to occur. To date, a standard methodology for the design of coal rib supports which can accommodate the wide range of unique conditions found in coal mines in the United States has not been developed, forcing mine operators to rely on the trial-and-error process or industrial legacy practices for the design of coal rib support patterns. In this study, to better understand the support systems' effectiveness, various rib bolting scenarios were investigated. A coal mass constitutive model is implemented to a Distinct Element Method (DEM) code, and rib factor-of-safety (RibFOS) analyses were performed by applying strength-reduction for the coal matrix and explicitly modeled face cleats. Ribs with various overburden depths and mining heights composed of solid Banded-Bright coal (BBC) were considered in this study. Different scenarios such as rib bolt length and the number of bolts were studied to quantify the effect of primary rib support density on rib stability. As a result of the unsupported coal rib analyses, a decaying exponential relationship is proposed between the mining height-overburden depth and the RibFOS. The developed coal rib models clearly show the coal-rib bolt interaction and illustrate how the addition of rib bolts restricts the movement of the coal rib. The results reveal that the strength reduction method in DEM code with the coal-mass model can aid in the development of practical primary support charts, which can help in the rib support design process. In addition, an unsupported RibFOS cutoff

By B. Strohmeier

An account is given of the use of a computer to control the performance of three ultra-high-powered electric-arc furnaces in Iscor 5 steelmaking plant at Vanderbijlpark, South Africa. Several of the reports and graphs printed by the computer are reproduced.

Jan 1, 1985

By John R. Green

ROTARY kilns, varying in construction, are used in a variety of processes. Products differ and operating conditions vary according to economic requirements. All of these variables influence the degree of instrumentation and type of control necessary or profitable to install. Products fired in rotary kilns are the results of combined temperature and time treatment and the interrelation of these two factors should be kept constantly in mind in the perusal of this paper. MEASUREMENTS OF KILN TEMPERATURE The securing of proper temperatures within the rotary kiln, either of the charge or of the kiln lining in the high fire zone, are basic objectives of kiln operation; therefore the measurement of these high-temperature conditions merits first consideration. For these measurements, radiation pyrometers, properly designed and protected, have proved adequate, particularly where records or automatic control are desired, while optical pyrometers may serve as portable indicators. Light-sensitive devices or photoelectric cells in this service are capable of producing records as well as certain forms of automatic control. High-temperature measuring devices for rotary-kiln work should have the measuring unit protected from dust, as a continued accumulation of deposit would lower the readings. Fig. I shows a typical application of radiation equipment to a rotary kiln, mounted far enough away from the sighting hole through the kiln hood to be protected from puffs or stingouts and with a sighting tube having a series of settling chambers, to prevent dust from reaching the lens. Although dust conditions inside the kiln itself usually fluctuate considerably and have their effect upon the readings at that moment, such effects are not cumulative and show as a continuous fluctuation in the temperature indicated, provided the radiation unit and recorder are responsive to such slight and rapid temperature fluctuations. The ambient temperature to which a measuring unit is subjected fluctuates from possibly 0° to over 200°F., therefore these changes should have no effect upon the final reading or upon the life of the measuring unit. A very narrow sighting angle is desirable, so that measurement of temperature may be made as far as possible into the high fire zone without effect of the flame temperature. There should be some sighting means on the measuring unit, so that the proper field may be viewed. Measurement of wall temperature taken at a point where the charge has just left the wall is less affected by dusting conditions than when taken elsewhere. Factors Influencing Temperature Table I gives an outline of the factors that produce kiln temperatures and comments on the possibility of measurement and control. Of greater number and of varied influence are the factors that control when, where and how the heat is delivered to the kiln, the type of flame and the rate of

Jan 1, 1941

By R. E. Shinkosk

This paper outlines the development of a program for increasing the life of woolen bags used for filtering Dwight-Lloyd gases by treating the bags and gases with hydrated lime. Methods and apparatus are described for determining alkalinity of dusts, acidity and breaking strength of bag cloth. Procedure and results, based on several years of operation, are presented. DURING 1939, additional facilities were constructed in the Dwight-Lloyd Blast Furnace and Baghouse departments at the Selby, California, Plant of the American Smelting and Refining Co. In order to handle adequately the increased volume of gases from the resultant increase in production, it was necessary to increase gradually the amount of water used for cooling gases ahead of the sinter machine baghouse. As a result of this increased water cooling, the average bag life dropped from 27 months in 1939 to 14 months in 1941. (Table I). This drop in life meant an increased. bag cost, as well as lower recovery of dust and some curtailment of operation. During 1941, it was found new bags showed as high as 0.3 pct acidity* after two weeks of opera- tion and as much as 2.0 pct acidity after some months of operation. This high acidity was present in spite of the fact that free oxide or relative alkalinity of the unburned dust ran from 5 to 6 pct. In view of these circumstances, a twofold program was started in Nov. 1941.t Part one of this program consisted of vigorously dipping all new bags in a weak lime solution, containing 50 lb of hydrated lime per 50 gal of water. Part two consisted of feeding fine, dry, hydrated lime into the gas stream intake of the sinter baghouse fan. Apparatus for feeding this lime is shown in fig. 1. All baghouse chambers are shaken in rotation about once each hour. On alternate hours, the baghouse operator places 50 lb of hydrated lime (one sack) into the lime feeder, starts feeder and immediately starts the bag shaking machinery. The rate at which lime is fed is set to coincide with the approximate time necessary to shake all sinter bag-house chambers, or about 15 min. It is felt this method of lime addition is most effective for getting lime into the woolen bag fabric. The amount of lime so fed averages about 600 lb per day. The amount of lime fed per day is varied to keep a minimum relative alkalinity of 9 pct in the unburned sinter dust. A daily dust sample is taken for alkalinity by allowing dust to accumulate in a sample pipe over a 24-hr period. This sample pipe, placed in any chamber cellar, is 2 in. in diam, 4 ft long, is sealed on the inner end, and capped on the outer end. It has a 1/2 in. slot cut for 18 in. along the tip end. This slot faces upward and allows the pipe to fill gradually with dust as bags are shaken. Breaking strength of bags has, in most cases, been the deciding factor in bag replacement. Bags that normally test 100 psi breaking strength when new are replaced when they test under 35 lb. The method for determining breaking strength is shown in the description accompanying fig. 2. Since the start of the liming program in 1941, bag life has increased from 14 months to an average of over 23 months, with a consequent material decrease in bag cost per year. Acidity, as per cent sulphuric acid, may be determined by means of a Beckman pH meter as follows: From a piece of bag cloth. which has been thoroughly cleaned of dust, a 5 g sample is weighed on a balance. Cut the sample into fine pieces and place in a 400 cc beaker. Add 100 cc (measured) of distilled water and stir vigorously. Filter on suction funnel, holding cloth pulp in beaker with a stirring rod. Wash cloth sample and filter wash water four additional times, each time with 20 cc distilled water, the last time squeezing cloth pulp over funnel. Discard pulp and rinse funnel and filter paper. Pour wash solution jnto measuring graduate and make up to exactly 300 cc with distilled water. Place into clean 600 cc beaker and measure the pH on meter. The per cent acid in bag cloth is read from the following table:—

Jan 1, 1951

By d&apos, L. Berenbaum, F. Heurle, R. Rosenberg

The structure of aluminum films obtained by evaporation was studied by electron microscopy, mostly by replica techniques and X-ray diffraction. The resistivities and stress conditions of the films were also determined. Film properties were studied as a function of source selection, substrate type, residual pressures of oxygen and water vapor, substrate temperature, and rate of growth. The formation of abnormal localized growths and whiskers resulting from annealing treatment subsequent to deposition was investigated. Films deposited onto single-crystal substrates were found to be epitaxially 0riented; for such films, relative orientations between films and substrates were determined. ALTHOUGH wide use has been made of evaporated aluminum films for the formation of conducting lines on semiconductor devices, relatively little has been reported concerning the structural characteristics of such films.1"9 The purpose of this study was to obtain an overall view of the dependence of these characteristics on film deposition and subsequent annealing conditions, which were similar to those used in silicon planar technology. Accordingly, most of this study was carried out using oxidized and bare silicon wafers as substrates, although some work was also done using alkali halide, magnesium oxide, and mica substrates. However, the main concern remained pragmatic. Emphasis was given to the study of the effects of deposition and annealing conditions on film characteristics such as structure, resistivity, and stress. I) EXPERIMENTAL PROCEDURES The films which were investigated in this study were deposited in 18-in.-diam glass chambers which were connected to the usual type of trapped diffusion pumps filled with silicon oil. Through the use of liquid-nitrogen-cooled Meisner traps and titanium sublimation pumps placed inside the deposition chambers, the pressure could be lowered to the lower portion of the 10- I Torr range and little increase in pressure would occur during the deposition cycle. Unless described otherwise, the substrates were 1-in.-diam p-type silicon wafers having a resistivity of 10 ohm-cm. The wafers were oxidized in wet oxygen at 975°C followed by a short dry-oxygen exposure at the same tempertture to a total oxide thickness of approximately 6000A. The wafers, backed by a layer of gallium, were mounted onto molybdenum discs brazed to a copper block.10 The latter was heated by imbedded commercial cartridge heaters. The substrate temperature could be maintained to within +10°C of a prescribed temperature during film deposition. The search for a satisfactory source for the controlled evaporation of aluminum has led to the use of 1-in.-diam crucibles" machined from rods of a commercially available, refractory composite* of Bn and

Jan 1, 1969

By P. L. Sibrell

Electrorefining of Ti in nonaqueous solvents has been studied by the U.S. Bureau of mines as a method for recycling impure scrap Ti. Electrochemical behavior of Ti species was investigated using cyclic voltammetry. Research results showed that Ti metal can be dissolved in polar solvents such as dimethylformamide or dimethyl sulfoxide. However, deposition of Ti from these solvents was not successful. Several solvent systems were investigated for electrodeposition of Ti but no deposits were obtained. Reduction of Ti4+ complexes to Ti3+ proved to be straightforward, but reduction to lower oxidation states could not be confirmed. In dimethylformamide solutions, cyclic voltammetry results demonstrated the reduction of Ti to an oxidation state of less than three, but no Ti metal was identified. In dimethyl sulfoxide solutions containing LiCl, it was possible to deposit Li metal. After adding Ti salts to the solution, electrolysis quickly passivated the electrode. Deposition of Ti was also investigated in solutions of dimethoxyethane and propylene carbonate but, again, no reduction of Ti to oxidation states of less than three occurred. Therefore, the prospects for a nonaqueous electrorefining system for Ti metal do not appear promising.

Jan 1, 2010

By J. S. Bowles

THE martensite transformation in lithium, dis- covered by Barrett,' has been studied extensively by X-ray techniques by Barrett and Trautz,² and Barrett and Clifton.V he present paper reports the results of an investigation into the metallographic characteristics of lithium martensite. Such an investigation has not been carried out before. The spontaneous transformation in lithium consists of a change from a body-centered cubic to a close-packed hexagonal structure with the hexagonal layers in imperfect stacking sequence." As far as is known at present, this transformation can be regarded as being crystallographically equivalent to the body-centered cubic to close-packed hexagonal transformation that occurs in zirconium,5 although stacking errors have not been reported in zirconium. From a study of the orientation relationships in zirconium, Burgers5 as proposed that the martensite transformation, b.c.c. to c.p.h., occurs by a heterogeneous shear on the system (112) [111]. The crystal-lographic principle underlying this proposal is that the configuration of atoms in the (112) plane of a b.c.c. structure is exactly the same as that in the (1010) plane of a close-packed hexagonal structure based on the same atomic radius. The pattern in 2v2 both these planes is a rectangle d X 2v2d where v3 d is the atomic diameter. Thus a close-packed hexagonal structure can be built up from a body-centered cubic structure by displacing the (112) planes relative to each other.* This mechanism leads to orientations that can be described by the relations: (110)b.c.e. // (0001)c,p.h.; [111]b.c.c. // [1120]c.p.h Observations confirm these relations. In zirconium, Burgers' measurements indicated an angle of 0" to 2" between the close-packed directions, while Barrett's measurements on lithium indicated an angle of 3". According to the Burgers' mechanism, the martensite habit plane for this transformation would be expected to be the (112)b.c.c. plane, for this plane would not be distorted by the transformation. One of the purposes of this investigation was to find out whether the observed lithium habit plane agrees with this prediction of the Burgers' mechanism. Experimental Procedure Materials: The lithium was from the same purified ingot used by Barrett and Trautz.² The Bridgman technique was used to produce single crystals. To maintain a temperature gradient in the melt, during the production of these crystals, it was necessary to use a steel mould with a wall thickness of only 0.015 in. Metallographic Techniques: Lithium specimens could be given an excellent metallographic polish by swabbing them gently with cold methyl or ethyl alcohol.? The best results were obtained with methyl alcohol saturated with the reaction product, lithium alcoholate. With higher alcohols the reaction became progressively slower and the attack became an etch pit attack rather than a polish attack. Butyl and amyl alcohols were used for macroetching. After polishing, it was necessary to remove all traces of alcohol from the specimens; otherwise, on subsequent quenching in liquid nitrogen, the alcohol froze to a glassy film. The alcohol was removed with dry benzene. The benzene in turn had to be removed before quenching, but since it does not react with lithium it could be allowed to evaporate. The specimens could then be quickly quenched before they began to tarnish. This operation could be carried out in air on all but excessively humid days when it was advisable to use an atmosphere of dry nitrogen or argon. For examinations at room temperature, the specimens could be transferred directly from the benzene bath into a bath of mineral oil. In mineral oil the specimens oxidized slowly by the diffusion of oxygen through the oil but the structure remained visible for about an hour. Lithium Martensite: Specimens prepared in the manner described above transformed spontaneously to martensite with an audible click when quenched into liquid nitrogen; i.e., M, was above the boiling point of nitrogen (77°K). The disparity between this result and the M, temperature of 71°K, found by Barrett and Trautz, is probably to be attributed to the large grain size and freedom from mechanical deformation of the specimens used in the present work. The relief effects produced by the transformation did not disappear when specimens were quenched from liquid nitrogen into mineral oil at room temperature. This permitted the microstructures to be studied at room temperature where, of course, the martensitic phase was no longer present. Typical micrographs of lithium "martensite" made at room temperature are reproduced in figs. 1, 2, and 3. As anticipated by Barrett and Trautz, the microstruc-

Jan 1, 1952

By C. G. Dunn

IT is well known that plastic deformation alters many of the properties of a metal and subsequent heat-treatment partially or completely restores these properties.1 In the deformed or strained state, the metal is unstable and tends to change toward a condition called a "strain-free state." The transformation occurs through recovery, recrystallization, and grain growth-processes that may take place singly or in combination. The distortion of the lattice of an individual grain of a metal in a state of strain may be rather complex in nature, because plastic deformation produces: (I) dislocations within mosaic blocks; (2) elastic variations of the lattice spacings; and (3) gross alterations throughout the lattice, especially along slip planes, along composition planes between a grain and its mechanical twins, and along boundaries of deformation bands. These gross alterations are of the nature of bent planes or rotated regions of the crystal lattice and are revealed by a spread in the orientation of the grain. Although we cannot describe these strains and their formation accurately because of insufficient knowledge, we can, nevertheless, use the information as well as possible to obtain a better understanding of recovery processes. In recovery, the lattice of a grain is not made anew as it is in recrystallization, but is improved or mended in such a way that the basic structure remains unaltered. Until recently observations were that recovery produced no marked changes in the shapes of spots in Laue diffraction patterns, whereas recrystallization did, but now it is known for silicon ferrite2 that Laue spots may become quite sharp entirely through recovery. Consequently, the shape of Laue spots alone would not be a suitable test to distinguish between recovery and recrystallization. There is considerable evidence that the micro- structure usually does not change visibly during recovery. Absence of a visible change in the microstructure, therefore, provides a sufficient test of recovery in many cases. However, including this observation in a definition of recovery as a necessary condition (this is usually done) is unfortunate, because recovery may, as will become evident later, produce new grain boundaries that are visible not only in the microstructure but also in the macrostructure. For the present, therefore, let us say that a necessary condition for a process to be one of recovery is that the principal orientation or orientations of a deformed grain be essentially unchanged throughout the transformation toward the strain-free state. Several transformations may occur that fulfill this condition, and the nature of the distortion in a grain indicates what these must be if the lattice is to be mended in part or fully. Consequently, it will be convenient as well as

Jan 1, 1946

By Tim Neil, O&apos

The coming years should see moderate growth in the US coal industry. That growth may come at the expense of the oil and natural gas industries. Conoco pegs coal growth at 2% a year, until the year 2000. During that same period, Conoco projects only 0.5% annual oil growth and "a flat or negative trendline" for natural gas. This is compounded by the fact that coal has a delivered cost per Btu that is only half as much as it is for natural gas and only a third as much as it is for oil. So said Ralph Bailey to many of the 2600 attending the opening session of the American Mining Congress Coal Convention, May 12-15, in Pittsburgh, PA. Bailey is chairman of the AMC. He is also chairman of Conoco. While coal's projected growth is not spectacular, "it is in fact almost an assured growth," Bailey said. Weak oil and gas prices will likely prevent faster growth for US coal. Most of coal's increased demand will come from the electric utility industry and expanded steam coal exports. Conoco's study projects that domestic coal demand will be strengthened in the 1990s. By then, the present surge of nuclear power plant constuction will be over. And there will be a lack of acceptably priced, large-scale generation alternatives for utilities. "It is not likely that any electric utility is going to be ordering new nuclear reactors," Bailey said. "And as oil and gas supplies become scarcer and more costly, it is only logical that coal is going to fill the gap." At the same time, Bailey believes the US coal industry must find ways to lower its costs. He said cost excesses can be found in "regulatory overkill, labor, and simply bad habits" hidden by years of high inflation. "Those costs have now been laid bare, because we are going through a pe¬riod of disinflation. We have to put our house in order, particularly if we are going to compete in world markets." Bailey also touched on coal research. "The industry certainly accepts the fact that we must find a way to burn coal as cleanly as possible. A lot of work in that regard is going on. I expect there will be some significant break-throughs." Bailey said the coal industry is being squeezed this year. Last year, coal customers accumulated inventories in anticipation of a major coal strike that never materialized. Now, many utility customers are working down these inventories. So they are not taking deliveries on their coal contracts. But coal use is up in 1985, compared with 1984, Bailey said. So increased coal use, along with supply drawdown, should strengthen the coal market before the year is out, he said. After Bailey's presentation, some 100 speakers addressed policy and technical topics at 15 sessions during the four-day meeting. It was the first time since 1977 that the AMC Coal Convention has been held in Pittsburgh. And this year's attendance was up 40% from the last AMC Coal Convention held two years ago in St. Louis, MO. This year's registrants included 228 companies, 225 manufacturers, and 106 associated members. The only negative was the David Lawrence Convention Center. It was less than ideal. By turns, meeting rooms were too small, too cramped, or too far from one another. The session on longwall mining was so crowded that the doors were propped open so conference delegates could peer in. A concurrent manufacturers' forum session needed 50 more chairs to accommodate those wanting to attend. However, on to summaries of some of the presentations. Coal transportation and export Since Congress approved the 1980 Staggers Rail Act, railroad rates for hauling coal have not been excessive. In fact, rail rates for coal have increased less than 0.5% a year, in real terms, since 1980. Moreover, the market oriented principles written into Staggers are contributing to the improved financial and operational health of the nation's railroads. But no railroad is earning excessive profits. That is the gist of a coal transportation study being completed by the US Department of Energy. William Vaughan is DOE's assistant secretary for fossil energy. He affirmed the thrust of the upcoming report. Vaughan did allow that Interstate Commerce Commission (ICC) regulations on rate reasonableness could permit the railroads to exploit their monopoly power on captive shippers. Luncheon comments later made by Don Hodel confirmed Vaughan's comments on railroad rate justification. Hodel is Secretary of the

Jan 7, 1985

By Jennifer Peirce Brandt

Project documents and the United States Army Corps of Engineers? permit for construction of the Stemmers Run Relief Wastewater Force Main across the Back River in Baltimore County, Maryland specified a minimal width, steel sheet pile cofferdam and a 12 feet wide, pile supported, timber decked, causeway trestle ? both approximately 1700 feet in length. Due to the impractical width of the causeway, the contractor desired to combine the cofferdam and the causeway structures in order to minimize wetland disturbance and maximize access for construction equipment. The resulting support structure was a steel sheet pile cofferdam, approximately 17 feet wide, internally braced, and capped with transverse timber deck mats to serve as the access and work trestle for the trench excavation, pipe bent construction, and trench backfill. Construction of this cofferdam/causeway progressed from the north shoreline toward the middle of the river. Then, working back toward the north shoreline, the contractor excavated, installed the 54 inch diameter pipe and H-pile support bents, and backfilled the trench in increments of approximately 60 linear feet. Excavation spoils from one section were used to backfill the preceding section. As the pipe installation progressed toward the north shore, the steel sheet piling and timber deck were removed. As sufficient sheet piling and deck mats were removed, the contractor began the process anew from the opposite shoreline using the reclaimed materials. The project was complicated by the presence of deep, very soft, weight of hammer, silts and organic clays and an unbalanced, hydrostatic head of 20.5 feet. In addition, concurrent pile driving, excavating, and backfilling in successive cofferdam sections required the use of heavy, long reach, hydraulic backhoes, and a 200 ton capacity crawler crane which controlled the design of the timber causeway deck and its supporting sheet piles.

Jan 1, 2008