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Papers in Classes A-Metal Mining, B-Milling and Concentration, H-Industrial Minerals, and I-Mining Geology are distributed in MINING TECHNOLOGY, which is issued every Other month. Papers in Classes C-Iron and Steel Division, D-Nonferrous Metallurgy and E-Institute Of Metals Division are distributed in METALS TECHNOLOGY, which is issued twice quarterly. Papers in Class G-Petroleum Division are distributed in PETROLEUM TECHNOLOGY, which is issued every Other month. TECHNICAL PUBLICATIONS in Classes F-Coal Division, J-Mineral Industry Education Division, K-Mining Administration, and L-Geophysics, are issued as separate pamphlets. Contributions are papers that when printed Or mimeographed are available, but Only On request. All the TECHNICAL PUBLICATIONS Of the F, J, K Or L classes, the TECHNOLOGYS and the CONTRIBUTIONS issued in 1945 are available at Institute headquarters, unless Otherwise noted. They are also On file in many public, university and technical libraries and, when so indicated in the list, the papers may be found in the TRANSACTIONS. An Institute member is entitled to One copy Of any TECHNOLOGY, TECHNICAL PUBLICATION Of the F, J, K Or L classes, Or printed Or mimeographed CONTRIBUTION. Copies Of TECHNOLOGYS and TECHNICAL PUBLICATIONS Of the F, J, K Or L classes listed have been mailed to members Of the Institute according to their registration by classes. CONTRIBUTIONS will he sent upon request. A member may purchase an additional copy Of a TECHNICAL PUBLICATION Of the F, J, K Or L classes, a paper in a TECHNOLOGY, Or a CONTRIBUTION at One cent a page; minimum charge, 25¢.

Jan 1, 1946

By Mary H. Brown

The heats of formation of oxalic acid and sodium, potassium oxalates, and lithium oxalates were related by solution calorimetry to the heat of formation of (COOH)2.2H20, a value believed to be reliable as reported in the literature. The following heats of formation were determined: (COOH)2(a), -198.1±0.1; (COOH)2(ß), -197.8±0.1; UAW,, -328.7±0.4; Na2C204 -316.2±0.1; K2C204, -321.9±0.2; and K2C204-H20, -393.5±0.2 kcal/mole. The heat of the crystalline transformation (COOH)2(a) ? (COOH)2(ß) was determined to be 0.30±0.02 kcal/mole at 298.15° K.

Jan 1, 1970

By A. J. Partos

One Liberty Place, at 315 m is the tallest building in Philadelphia, PA USA. It is supported on drilled piers socketed in heterogeneous rock. 3832 kN/m2 end bearing and 383 to 766 kN/m2 shaft resistances were selected. Design load distribution was 40% on the base and 60% by shaft resistance. The maximum compression on the corner core columns is supported by clusters of 3 drilled piers. In order to confirm load distributions along shaft and at the base, Drilled Pier G-10 supporting T13-A type outrigger column was instrumented. This column supports 53,849 kN compressive load which includes 13,440 kN windload. This paper reveals details about the process to select the final design for One Liberty Place together with pertinent Information about site geology, foundation construction, quality control, and methods of steel erection. It also presents detailed Information on the type of Instruments, their calibrations, field fabrication, and installation in the shaft of Pier G-10. Readings of concrete temperatures, computed loads, and load distributions are presented for a period from October 1985 through May 1988. The building was completed in 1987.

Jan 1, 1989

By N. A. Gokcen, S. Fujishiro

The dissociation pressure of Cr3C2 has been measured in the range of 1908" to 2237°K by means of graphite Knudsen effusion cells. It has been found that Cr3C2 vaporizes according to the following reaction: 1/3 Cr3C2 (s or 1) = 2/3 C (graph.) + Cr (g). The equilibrizcm pressure, P, of Cr (g) is found to be log Ps=- - (21,194/T) + 6.525 over solid Cr3C2 and estimated as log P, = - (19,535/T) + 5.76 over liquid Cr3C2. CARBIDES of chromium are of great importance in alloy steels and cemented carbides. The published data on their therm odynamic properties at high temperatures, however, are meager. The heat capacity and change in entropy of Cr3C2 were determined calorimetrically by Kelley and Moore1 in the range of approximately 50" to 300°K, and by Oriani and Murphy2 from 297" to 1188°K. The standard entropy of Cr3C2at 298.15°K, obtained by Kelley.7 was later confirmed by DeSorbo.4 Equilibrium in the reaction was investigated by Boericke.5 A recent tabular summary

Jan 1, 1962

By K. L. Ford, D. R. Lentz, J. H. Rickard, R. P. Taylor

Abstract - Coupled gamma-ray spectrometric and lithogeochemical studies throughout the Heath Steele Mines area, Bathurst Camp, New Brunswick, indicate that primary and secondary geochemical differences exist between the stratigraphic footwall and hangingwall crystal tuff units which host the massive sulfide deposits. Of particular interest is Th, and to a lesser extent, Zr and Y, which are more concentrated in the hangingwall than the footwall crystal tuffs, whereas the opposite is true for TiO2. This expands on earlier lithogeochemical-chemostratigraphic results concentrated in the eastern part of the Heath Steele belt that led to revision of the local stratigraphy, and necessitated a structural re-interpretation of the area with implications for exploration. Although K depletion (decreased K and K/Th) is typical of chloritized footwall zones of chloritization, these features were not fully apparent here due to the recessive nature of these altered zones. In situ radiometric analysis using a portable gamma-ray spectrometer is a rapid, inexpensive analytical technique for chemostratigraphic characterization of rock units within volcanogenic massive sulfide deposit settings, provided there is a contrast in the distribution of natural radioelements, particularly Th and K.

Jan 1, 1998

By A. S. Chekmarev, T. Z. Lygina, K. G. Egorova, A. V. Skvorcov

"We have conducted analytical and technological evaluation of sepiolite containing clay. The possible areas of application of the sepiolite have been investigated and complex methods of enrichment of natural sepiolite have been identified. It was determined that for preserving the structure of minerals after processing the most effective method of the natural agglomerates disintegration was the soft abrasion of the clay fraction up to 0,5 mm. Disintegration of sepiolite clay along with using high energy-stressed effects on the matrix can deteriorate the rheological properties of clay suspensions and reduce the yield of drilling mud and sorption properties. To improve the quality of clay powders we used combined gravity-modifying method of wet enrichment. After the wet enrichment the yield of drilling mud increased up to 12.7 m3/t, with the addition of MgO up to 20,3 m3/t. It was noted that drilling muds contenting more than 50% of sepiolite are stable in mineralized (salt) waters. Based on the studied activated sepiolite rocks we obtained the effective heat-insulating materials with relatively low thermal conductivity – 0,165 W/m·K, average strength – 7,29 MPa and water absorption-49,0%.INTRODUCTION The modern development of the Russian economy requires the implementation of scientific and technical tasks. The solutions of it involves a radical reduction in energy, heat losses and material consumption of products, rational and efficient using of all types of resources, as well as the using of new types of mineral raw materials and materials based on it. An example of a new type of mineral raw materials for Russia is sepiolite containing rocks, due to unconventional conditions for their soils accumulation in the climate of the Far North. Sepiolite is a unique type of nonmetallic mineral. It is formed in soils, marine and saline basins, occurs in carbonate and carbonate-clay rocks in the form of lenses and lens – shaped layers, rarely nodules, loose powdery masses, shell-like concretions. Sepiolite may have a soft porous macroscopic appearance or less often the structure of the fibrous mass. Color of sepiolite is from white to cream with gray, green, pink and even crimson shade depending on the degree of pollution. Sepiolite can be in two forms - a-sepiolite (parasepiolite), which occurs in the form of large packets of crystalline fibers and ß-sepiolite, which occurs in the form of amorphous aggregates or small flat rounded particles. The sepiolite fibers have a length of from 0.2 to 2 Å, width from 100 to 300 Å, the thickness from 50 to 100 Å (Geological dictionary, 1973)."

Jan 1, 2018

By H. J. Levinstein, H. J. Guggenheim

RbFeF3 is a transparent ferromagnet with a large faraday rotation which permits the direct observation of magnetic domain structures in bulk crystals. If the position of dislocations within the crystal were known a study of domain wall dislocation interactions would be possible. In this paper an etch pitting solution is described which gives a one-one correspondent between the etch pits and the dislocations intersecting the (100) surfaces of RbFeF3 crystals. In addition, RbFeF3 is shown to have sufficient plasticity so that known arrays of dislocaticms can be put into the crystal. It is concluded that RbFeF, is an ideal material for the investigation of domain wall dislocation interactions. THE influence of lattice defects on the motion of domain walls in ferromagnetic materials has been studied extensively both theoretically and experimentally.4 The experimental data obtained has been qualitative in nature due to the lack either of a quantitative knowledge of the magnetic domain array in the material or of the nature of the dislocation configuration in the material. At room temperature RbFeFJ has the cubic perovskite structure. It is ferromagnetic below 86°K.5,6 It is also transparent and has a large faraday rotation in the magnetic state.7 The domain structure of this material is observable in three dimensions in crystals which are millimeters in thickness.' Since RbFeF3 satisfies the requirements of having an easily visible three-dimensional magnetic domain structure, it was of interest to determine if the dislocation structure of the material could be determined and if the material was sufficiently plastic so that dislocations could be introduced into the as grown crystals. This is a report of the results of that investigation. EXPERIMENTAL PROCEDURE The crystals of RbFeFs used in this experiment were grown by a technique described elsewhere.5 In order to obtain flat strain-free surfaces, the samples were first cut to the crystal orientation desired and the surfaces were polished by employing standard metallographic techniques. The samples were then immersed in a solution of 1 to 3 g of KOH in 100 ml of water. This solution removes the damaged surface layers uniformly leaving a film on the surface of the sample. Etch pits are obtained by immersing the sample in an approximately 50-50 solution of 30 pct peroxide and concentrated acetic acid. The film formed during the KOH treatment turns deep red in color in the etching solution and flakes off the sample. The etching time required depends upon the pit size desired and

Jan 1, 1970

By P. G. Coombs

The kinetics of the cyclic oxidation and reduction processes for palladium powder were examined in the temperature range 848 to 923 K. The changes in oxidation behavior due to cycling are shown to result from the decrease in surface area. Sintering is found to occur only during the reduction process. Oxidation kinetics were found to follow a cubic law with time and yield a relation for the oxidation rate constant of k x = (1.05) 106 exp P74.0). 103 / RT] The kinetics of reduction are demonstrated to be first-order with the rate constant described by the expression: kr = (7.69) 1012 exp [-(208.0) 103 / RT] . In both expressions R is in J.mo1-1.K-1.

Jan 1, 1984

By Takao Mori

Novel rare earth boron icosahedral compounds are investigated as potential high temperature thermoelectric materials. REB50-type compounds and REB22C2N compounds were synthesized and the thermoelectric properties measured. Seebeck coefficients in excess of 200 V/K are observed at temperatures above 1000 K for the REB50-type compounds. Strikingly, n-type behavior was observed for REB22C2N. Up to now, non-doped B12 icosahedral compounds have all been p-type. The discovery of an n-type compound is extremely important in terms of the potential development of this class of compounds as viable thermoelectric materials. Low thermal conductivities of < 0.03 W/cm/K at room temperature was observed for these rare earth boron cluster compounds.

Jan 1, 2006

By Ray W. Carpenter, Ralph Hultgren, Raymond L. Orr

Heats of formation of Au-Zn alloys of compositions Au3Zn and AuZn were rneasured at several temperatures by liquid tin solution calorimetry. The data for Au3Zn show that much smaller heat and entropy effects are associated with the a2- a1 transformation than for the a1 - a transformation. This result is consistent with reported X-ray diffraction studies which indicate that the a1 and (a2 phases have ordered structures which only slightly differ, whereas the a phase is disordered. The heat of formation of AuZn(ß&apos;) does not change significantly between 322o and 8000 K, confirming that the ß&apos; alloy remains highly ordered to high temperatures. Not many measurements have been made of the energies of order-disorder transformations in alloy phases. In many cases these energies may be conveniently determined by measuring heats of formation as a function of temperature. Many alloy phases approximately obey Kopp&apos;s law of additivity of heat capacities; as a consequence their heats of formation do not change with temperature. In ordered alloys, however, a decrease in degree of order with increasing temperature will contribute an endothermic component to the heat of formation. Thus, for ordered phases where other anomalous contributions to heat capacity in the alloy or its pure components are absent, a measured change in the heat of formation may be attributed to the energy of disordering. A portion of the Au-Zn phase diagram1" is shown in Fig. 1. The composition AuZn(ß&apos;) has a well-ordered superlattice structure of the CsCl type at room temperature. The alloy is considered to remain ordered to its melting point,1 although, from X-ray diffraction data and electromotive force measurements of zinc activities, Terpilowski3 concluded that considerable disordering began at -673°K. The Au3Zn composition is a disordered fee solid solution (a) at high temperatures. Between 693o and 543oK, the ailoy orders to form the a1 phase, having a structure based on the L12(AuCu3) type, but with a regular distribution of ordering faults in the c direction, making it tetragonal. Below 543oK, the alloy orders further by means of slight atomic shifts, without diffusion, yielding a complex long-period orthorhom-bic superlattice structure, a2.4-7 Heats of formation of Au3Zn(a2) and AuZn(ß&apos;) were measured at 363°K by Biltz et al.8 by aqueous solution calorimetry. Heat capacities of several alloys between 14.9 and 38.4 at. pet Zn in the range from 373" to 723°K were measured by Iwasaki ef al.6 Stoichiometric Au3Zn, however, was not included in the alloys measured, the nearest composition being 26.1 at, pet Zn. Also, the heating rate used for the measurements, 2 deg per min, may not have permitted equilibrium to be reached in the neighborhood of the transformations. Heat contents of solid and liquid AuZn were measured between 488o and 1138°K by Kubaschewski.9 It was decided to determine the ordering energies of Au3Zn and to check on the possible disordering of AuZn by measuring the heats of formation of these alloys at several temperatures. The present paper reports measurements by liquid tin solution calorimetry of the heats of formation of the three phases of Au3Zn at temperatures within their regions of stability, and of AuZn at a low (322°K) and a high (800°K) temperature. EXPERIMENTAL Alloy Preparation and X-Ray Examination. Ten-gram ingots of Au3Zn and AuZn were prepared by melting weighed amounts of gold (99.95 pct Au) and zinc (99.99 pet Zn) together in sealed evacuated Vycor tubes at 1060°K, followed by rapid quenching. The resulting ingots were homogenized at 900°K for 10 days. The Au3Zn alloy lost no weight in preparation, the loss from the AuZn alloy was enough to introduce an uncertainty of only 0.1 at. pet in its composition. Filings for X-ray examination were taken from various parts of each ingot and strain-annealed at 723°K for 20 min in vacuo. The Au3Zn filings were quenched rapidly to retain the disordered phase. Diffraction patterns were determined with an X-ray dif-fractometer using copper Ka radiation.

Jan 1, 1968

By N. A. Gokcen, J. Chipman

A revised treatment of the authors&apos; published data eliminates the complex relation previously proposed between concentration of silicon and activity coefficient of oxygen in liquid iron. Revised values of the thermodynamic properties of the liquid solution are presented. IN a recent experimental study of the reaction SiO2 (s) = Si+ 2O; Kf, = [% Si] [% O]² [1] the authors&apos; found a substantially constant equilibrium product in liquid iron at 1600°C of 2.8x10-5 They also reported extensive data on the reactions: SiO2 (s) + 2H2 (8) = Si- + 2H2O (g); K&apos;2= [% Si] (H2O/H2 [2] and H, (g) + 0 = H2O (g); K&apos;3 =( H2 O [31 (H2) [%O] From the results on reaction 3 and earlier data of Dastur² on this same reaction in the absence of silicon, they determined the activity coefficient of oxygen, f0, on the basis of the definition K3 = (H2O)/ (H2)f0 [% 0] where K, is the equilibrium constant and f0, is taken as unity in the pure Fe-0 system. Similarly values of fsi were deduced from results on reaction 2. In a more recent study" of analogous reactions in the system Fe-A1-0, it was found impossible to reconcile the results on reaction 3 with Dastur&apos;s data; accordingly the latter were ignored and the equilibrium results were extrapolated to find a value of K, at zero concentration of aluminum. This procedure failed to locate the cause of the discrepancy but it did yield reasonable values of activity coefficients. It also avoided introduction of the complex empirical relation between the oxygen activity coefficient and the concentration of the added element. The same type of discrepancy exists for system Fe-Si-0.&apos; In the earlier paper an attempt was made to fit both sets of data by a single curved line (Fig. 6 of ref. l), the form of which is contrary to the theoretical requirement of a finite slope at infinite dilution. In the light of experience on the Fe-A1-0 system the discrepancy must be recognized as one which can be resolved only by more refined measurements. Accordingly Figs. 6 and 10 are retracted. It is pointed out also that until the discrepancy is resolved Figs. 7, 8, and 11 are subject to some uncertainty. Qualitatively the following conclusions still appear valid: 1—The activity coefficient of oxygen is reduced by addition of silicon. 2—In dilute solutions the activity coefficient of silicon increases with its concentration. 3—With respect to equilibrium in reaction 1, the above effects are approximately compensating. The discussion of K&apos;1 in the previous paper requires no revision. It was pointed out that the constancy of the product [% Si] [% 0]² ndicated a compensating effect of the activity coefficients of silicon and oxygen. Therefore, as a very good approximation, K1 = K&apos;1 and the following average values are suggested both for K, and K&apos;, at the temperatures 1550°, 1600°, and 1650", respectively, 1.0x10-", 2.8~10-" and 5.5 ~lo-&apos;. Revision of the thermodynamic treatment is necessitated by the recent appearance of new data, based on a combination of combustion and solution calorimetry,&apos; which yields for the heat of formation of low-cristobalite from the elements, the value —209,330 ±250 cal per mol at 25°C. This is about 4000 cal larger than the value previously accepted. The new value for cristobalite is used, together with Kelley&apos;s tables of high-temperature heat contents" and entropies and with Korber and Oelsen&apos;s&apos; heat of fusion of silicon to obtain the following equation for the standard free energy of cristobalite in the temperature range 1700" to 2000°K: Si (1) + 02 (g) = Si02 (crist.); ?F° = -217,700 + 47.OT [4] The free energy of solution of 0, in liquid iron is:8 O2 (g) = 20 (in Fe); AF° = -55,860 - 1.14T [5] and these two equations are combined to give: Si (1) + 20 = SiO, (crist.); AF° = -161,840 + 48.14T [6] ?F°1873 = -71,700 cal. From the experimental value of K, = 2.8x10-5, Si + 20 = SiO2 (crist.); ?F°1873 = -39,000 cal. [7] The combination of Eqs. 6 and 7 yields the free energy change when liquid silicon dissolves in iron to form the dilute solution of unit activity (1 pct). Si (1) = Si; ?F°1873 = -32,700 cal. [8] The heat effect in this process according to Korber and Oelsen&apos; is an evolution of 28,500 cal per gram

Jan 1, 1954

By F. R. Brotzen, L. D. Whitmire

Single crystals of high-purity molybdenum were de-formed at temperatures from 195°to 473°K, and the effect of deformation on the electrical resistivily was deler-mined. To separale the resislivity components of point and line defecls some cryslals were annealed at 473°K. The vale of resislivily increase wilh strain was nearly linear and was strongly dependent upon the deformation temperature. Point dejects are annealed out without any effect on the flow stress. At low temperatures the flow stress is a linear function of the square root of the resistivity increase attributable to dislocations. ELECTRICAL-resistivity measurements have been used successfully to gain information on structural changes in metallic materials. During plastic deformation the electrical resistivity rises because of electron scattering from newly created lattice defects. Such measurements lend themselves, therefore, to corroborating results from direct observation of lattice defects and, to a certain extent, to correlating defect densities and distribution with mechanical properties. Published information on research with single crystals of the bcc metals of Group VI, particularly molybdenum, is still limited. Yet, molybdenum single crystals of relatively high purity can be readily prepared by electron-beam-melting techniques. Furthermore, some valuable information on the defect structure of deformed crystals by direct observation is available. Lawley and Gaigher,1 for example, have examined dislocation configurations in deformed molybdenum crystals by means of transmission electron microscopy. Their results revealed that the dislocation density and distribution were strongly dependent upon the deformation temperature. These findings differed from those by Keh and weissmann,2 who found that the average dislocation density in polycrystalline iron deformed between 138° and 298°K depended only on the degree of strain and not on the deformation temperature. Martin3 and peiffer4 showed that point defects introduced in polycrystalline molybdenum by cold work can be eliminated by annealing at a relatively low tempera-ture. In view of their work it became apparent that resistivity measurements of suitably annealed crystals could disclose changes in their dislocation structure and contribute to the understanding of the work hardening of molybdenum crystals. EXPERIMENTAL PROCEDURE Crystals were grown by electron-beam zone melting5,6 of 0.062-in.-diam molybdenum rods (99.99 pct) supplied by General Electric Lamp and Wire Division, Dover, Ohio. The crystals, about 4 in. long, were prepared by using five zone-refining passes at a speed of about 6 mm per min in a vacuum of about 5 X l0-6 Torr. The resistivity ratio of the crystal, p(4.Z°K)/p(273°K), was generally near 10-3. These crystals were used as tensile specimens of uniform diameter in the "as-grown" condition. They were oriented for maximum shear on the (011)[111] slip system (Schmid factor >0.49). The specimens were held in spherically seated Templin-type grips so as to minimize bending. Samples were deformed on an Instron machine at a strain rate of about 5 X 10-5 sec-1 in an isopentane bath with dry ice at 195°K, in ice water at 273°K, and in a vegetable-oil thermostat at 373° and 473°K. The temperature in the latter was maintained constant within +2°K. Resistance measurements were carried out with a Kelvin double bridge. The resistance of the potential leads was kept low by using large-diameter wires outside the low-temperature bath. Many of the resistance data were checked by measurements made with an ac bridge. Current and potential leads were spot-welded to the specimens. The distance between the potential leads, about 3 in., was also considered to be the gage length for the strain measurements. Diameter and gage length of the samples were measured optically with an error of less than 2 pct. These measurements were used also to insure that the deformation had been uniform over the gage length of the specimen. Resistivity changes were then determined from the resistance measurements at 4.2°K assuming constancy of volume. In the course of a test, the crystal diameter, gage length, and resistance at 4.2°K were determined first in the initial state and subsequently for various amounts of elongation.

Jan 1, 1968

By Gearge C. Wallick

This paper describes experimental procedures for the calibration of capillary tubes to be employed as comparison standards in gas flow-rate measurements and considers several types of flow which were observed in the calibration of seven capillaries of varying diameter. It is shown that under certain experimental conditions deviations from Poiseuille flow are observed which may not be attributed to turbulence, and that this flow behavior may be described empirically by introducing the classical kinetic energy correction into the Poiseuille equation. INTRODUCTION Techniques have been developed for the measurement of the volume rate of flow of nitrogen through glass capillary tubes as a function both of the differential pressure applied and of the absolute gas pressure. Capillary tubes thus calibrated are frequently used to determine the rate of gas flow through a porous sample in the measurement of slip-corrected permeability. The purpose of this note is to describe the calibration procedure and to discuss some observed deviations from the ideal flow behavior predicted by the Poiseuille equation. EXPERIMENTAL PROCEDURE The volume flow rate of nitrogen as a function of the differential pressure was determined experimentally for a series of seven glass capillary tubes of varying diameter. As is shown in Table 1, the capillary radii in the series ranged from 0.004 cm for K1 to 0.07 cm for K7. The capillary tubes were cut from capillary tubing purchased on special order from several manufacturers and the bore radii were determined by microscopic measurement. The gas volume flow rate was measured for each capillary tube at a series of differential pressures in the range from 0 to 3 cm of mercury and at average absolute pressures of 1.0, 2.5, 4.0, and 6.0 atm. Experimental Procedure for Small Capillaries A schematic diagram of the apparatus used to calibrate the three smallest capillaries, Kl, K2, and K3, is shown in Fig. 1. By means of a standard Ruska Instrument Corp. volumetric pump (equipped with a synchronous motor drive, two stages of gear reduction, and a quick-change lathe gear box), nitrogen was displaced by mercury from a metal cell immersed in a constant-temperature bath. The pump, the line to the cell, and a part of the cell were filled with mercury. As mercury was forced into the cell, it displaced nitrogen which passed through the capillary tube being calibrated and into a large container with a volume of approximately 30 liters. Since the volume of this container was very large compared to the total volume change of the gas resulting from the action of the displacement pump, the absolute pressure of the system was essentially constant throughout any one run. Prior to any determination this pressure could be set at any desired level by means of an auxiliary nitrogen cylinder. The differential pressure across the capillary was measured with a Meriam Red Oil manometer and recorded together with the corresponding pump displacement rate which was equal to the gas flow rate. By repeating this process for a series of different displacement rates at each of the absolute pressures of interest, the data necessary for plotting the calibration curves for capillaries K1, K2, and K3 were obtained. All calibration measurements were made in a constant temperature room to minimize errors due to temperature fluctuations. In each run. the flow was maintained until equilibrium was established. Experimental Procedures for Large Capillaries The flow rates through Capillaries K4, K5, K6, and K7 required to obtain the pressure drops desired were larger than could be obtained from available constant displacement pumps, and it was thus necessary to employ an alternative calibration procedure. The arrangement of apparatus used in calibrating these capillaries at an average pressure of one atmosphere is shown in Fig. 2. Each capillary was calibrated by flowing nitrogen through the capillary and recording the differential pressure as a function of the flow rate. &apos;The differential pressure was measured with a Meriam Red Oil manometer and the flow rate was determined by collecting the effluent gas over water at constant pressure and recording the increase in volume per unit time after an equilibrium had been established. Appropriate corrections were made for the

Jan 1, 1953

By Elizabeth A. Johnson

The vaporization thermodynamics of the aluminum-silicon carbides Al4SiC4 and Al8SiC7 were studied by the Bureau of Mines over the temperature range of approximately 1,500 to 1,700 K. Vapor pressures were measured by a Knudsen effusion-mass spectrometry technique in which powdered samples were effused from graphite crucibles through small orifices. For each compound, a total of six orifice diameters was tested to verify equilibrium within the cell. Aluminum, mass number 27, was the only vapor species detected over the range 4 to 200 amu. Experimental results are based on the following equations for incongruent decomposition: A14SiC4(cr) - 4A1(g) + SiC(a,hex) + 3C(gr); Al8SiC7(cr) - 8A1(g) + SiC(a,hex) + 6C(gr). The observed vapor pressure-temperature relationships determined with a cell orifice area of 2.0 x 10-3 cm2 for Al4SiC4 and 1.81 x 10-3 cm2 for A18SiC7 are the following: Log P - (-18,682/T) + 12.476, for Al4SiC4 (1,550 to 1,643 K) and Log P = (-19,308/T) + 12.421, for Al8SiC7 (1,526 to 1,784 K), with P in pascals and T in kelvins. Third-law analysis of the data provided the following heats of formation: A14SiC4 ?H at 298.15 K - -50.0 kcal/mol and A18SiC7 ?H at 298.15 K - -92.1 kcal/mol.

Jan 1, 2011

By M. Abdellatif

"SynopsisCalcined basic nickel carbonate (BNC) concentrate was smelted in a pilotscale DC arc furnace to produce a nickel metal. The furnace was continuously operated for 12 days (24 hour/day), during which twelve different smelting conditions were investigated, with the major variables being reductant type and feed rate, flux composition and addition, and BNC feed rate.The 200 kW DC arc furnace was operated at power levels between 110 and 165 kW and at a total feed rate of 78 to 96 kg/h, resulting in an average slag and metal tapping temperature of about 1650°C. A total of 7.2 t of BNC were smelted, producing about 5.44 t of nickel metal and 2.94 t of slag. Nickel recoveries of 96.4% and higher were achieved, and the slag nickel content was as low as 0.1%. The major impurities in the metal were iron (mostly from oxygen lancing) and carbon. The calculated feed carry-over was less than 0.85% and the graphite electrode consumption was between 2.8–3.3 kg/MWh.IntroductionOne of the most distinctive advantages of DC open-arc smelting is the ability to process fine raw materials without any major issues with regard to the operability of the furnace, metal recovery, and metal quality. This has been demonstrated in Mintek’s DC arc pilot plant facilities over a period of about three decades (Curr et al., 1983). The materials that have been processed include laterite (Kotze, 2002), chromite fines (Curr et al., 1983), manganese fines (Lagendijk et al., 2010), PGM concentrates (Shaw et al., 2013), electric arc furnace (EAF) dust (Denton et al., 2005; Abdellatif, 2002a) and stainless steel (SS) dust (Denton et al., 2005; Abdellatif, 2002a; Goff and Denton, 2004), and petroleum fly ash (Abdellatif, 2002b). The top particle size of such materials can vary from a few millimetres (e.g. laterite) to micrometres (EAF and SS dust). Dusting, whether due to physical carryover of feed or to the arc side reactions, has been proven to be a non-issue. As such, the applications of DC open-arc furnaces have the potential to be extended to other raw materials such as particulate nickel oxide, which has a particle size much less than 100 µm.Nickel oxide is typically produced from laterite ore by sulphuric acid leaching, purification, and precipitation as basic nickel carbonate (BNC) (Rhamdhani, Jak, and Hayes, 2008) or as mixed hydroxide precipitate (MHP) (Mackenzie, Virnig, and Feather, 2006), and finally calcining at moderate temperatures (800–1200°C). The NiO product is very fine, with an average particle size in the range of 10–20 µm and a NiO content of more than 99%."

Jan 1, 2015

By L. B. Pankratz

High-temperature heat-content values of pure lutetium sesquioxide and dysprosium sesquioxide were measured over the temperature range from 298° to 1,800° K. Similar data for cerium sesquioxide were calculated from measurements of a mixture of cerium sesquioxide and dioxide and known values for cerium dioxide. The results for lutetium sesquioxide are regular. Dysprosium sesquioxide has a minor thermal anomaly near 1,590° K, the extra heat absorption being 220 cal/mole, Hexagonal cerium sesquioxide undergoes a transformation around 1,050° K, which is only slowly reversible; consequently results were obtained for both the low- and high-temperature varieties. The original heat-content data are reported, and smooth values of heat content and the corresponding entropy increments are tabulated. Equations were derived to represent the heat-content values.

Jan 1, 1963

By P. Chiotti, J. T. Mason

Metallographic, thermal, X-ray, and vapor-pressure data were employed in establishing the Ce-Zn phase diagram. Nine compounds and three eutectics were observed. The eutectic compositions in weight percent zinc and temperatures are 10 pct and 495"C, 37 pct and 795°C, and 56 pct and 810°C. Three of the compounds, CeZn, CeZnn, and CeZne.5, melt congru-ently at 825°, 87.505°, and 980°C, respectively; the other six compounds, CeZns, CeZns.67, CeZn4.5, CeZn5.25, CeZn,, and CeZnll, decompose peritectically at 820°, 840°, 870°, 885", 960°, and 795"C, respectively. The compound CeZn5.25 is an AB5 type with a small range of composition which lies on the zinc-rich side of the 1 to 5 stoichiometry. Zinc vapor-pressure data obtained by the dewpoint method were employed in calczilating the thermodynamic properties of both the liquid alloys and solid compounds. The data for the A critical review of the information available on the Ce-Zn system up to 1960 has been given by K. Gschneidner, Jr.&apos; Of particular interest is the work by J. schramm2 who investigated the region between 55 and 100 wt pct Zn and reported a CeZn,, compound which decomposes peritectically at 785"C, a CeZn, compound which melts congruently at 972"C, and five temperature horizontals at 79@, 817", 840", liquid alloys were fitted to the relation from which the relation was obtained by integration. In these relations F XS is the excess partial molal free energy, N is atom fraction, and the constants c and d have the values c = (-22,000 + 7.0T) and d = 6171,000 + 74.0T). Relations for the standard free energy of formation for the solid compounds were derived from the data. At 973°K the enthalpy in kilocalories per gram-atom z)aries from —11.3 for CeZnz to —8.21 for CeZn~l and the free energy in the same units varies from —7.1 joy CeZn, to -3.82 for CeZn11. and 942°C in the region between 55 and 75 wt pct Zn. No attempt was made to identify other features of the system. I. Johnson and R. yonko3 used a fused-salt cell to measure the electromotive force between pure cerium and an alloy consisting of zinc-rich liquid in equilibrium with CeZnll. Solubility data for cerium in zinc has been reported by J. Knighton et u1 .4 Johnson and Yonko give the following equa-. tions for the mole fraction of cerium in zinc and the standard free energy of formation of CeZnll:

Jan 1, 1965

By O. Schaaber

THE existence of isothermal martensite without the presence of the athermal form thus far has been established only in a 6 pct Mn, 0.6 pct C steel&apos; and a 23 pct Ni, 3.5 pct Mn-Fe alloy.&apos; " Theoretical calculations, moreover, predict this phenomenon to be observable only within narrow composition limits.&apos; In all other steels, it is generally considered that martensite inevitably forms upon cooling below the M, temperature. Even the possibility of isothermal martensite transformation has been questioned for the common steels, although Averbach and Cohen" showed that martensite formation does not stop when the cooling is arrested and that as much as 5 pct retained austenite may transform isothermally to martensite at room temperature. This note presents some observations made on a number of low alloy steels by dilatometric and inductive measurement of isothermal austenite transformation at various temperatures close to the Ms. In the dilatometer studies reported previously, austenitized specimens were immersed in a salt bath maintained at proper temperature and immediately inserted into the dilatometera8&apos; already at thermal equilibrium with the bath. The dilation was read on a dial gage divided into 0.001 mm intervals. Induction measurements were made with a separate excitation source and a test coil, sealed together in a salt-tight case. The increase in the induced voltage caused by the transformation products was recorded at a paper speed of 4 mm per sec. The steels studied are listed in Table I. Specimens prepared from steels 1 and 2 were in the form of hollow cylinders 60 mm long, 10 mm ID, 14 to 16 mm OD, while specimens of steels 3 and 4 were in the form of notched-bar impact test specimens, DVM type. Specimens of steel 5 were in the form of strip, 7x0.3 mm. In the bainitic range, curves representing the amount of transformation vs log time have a single step appearance, as is shown by the curve of isothermal transformation at 320°C in Fig. 1.Y ransformation proceeds in accordance with the Austin-Rickett equationo P -----------= k t" 100-P where P is the percentage of transformed austenite, t is time, and k and n are constants. Near the M, temperature, however, complex curves having two steps are observed. As shown in a previous papera for steel 3 isothermally transformed at 245"C, such complex curves can be separated into two separate transformations or reactions each following the Austin-Rickett equation. The values of n in the equation for a number of such two-step transformations are listed in Table 11 for steel 1. At transformation temperatures of 250" and 235"C, evidence of a second transformation is very

Jan 1, 1956

By H. Kreye, E. Hornbogen

An increase in electrical resistivity during aging or after quenching from high temperatures is known in a large number of alloys. Plastic deformation of alloys in this condition leads to a decrease in resistivity. This anomaly has been called the K effect. This effect has been reported in Ni-A1 alloys by several authors.&apos;-4 The nickel-rich solid solution y is in equilibrium with Ni,A1 (y&apos;) with CkAu structure. With this alloy it is therefore possible to produce a homogeneous solid solution as well as a coherent mixture of y and y. The changes in resistivity should be determined for these two conditions. In the present literature on the K effect no distinction is made between them, because of experimental difficulties to determine small coherent particles. In the present work transmission electron microscopy and image formation by (100) and (110) superlattice reflection of the y&apos; phase was employed for a detailed determination of the temperature dependence of solubility of aluminum in nickel and the resulting microstructures with alloys up to 15 at. pct Al. The solubility line follows the equation indicating a smaller solubility than given in the literature at temperatures below 700°C. X-ray scattering was used to get evidence for short-range ordering in the homogeneous solid solutions.5 Parallel to the determination of the microstructure electrical resistivity was measured as a function of aging tempera- ture, time, and aluminum content, which led to the following results: 1) Resistivity increases slightly during aging of a homogeneous solid solution which was quenched from a high temperature as a consequence of short-range order, Fig. 1, curve c,. 2) Resistivity shows a maximum during aging of all alloys which are heterogeneous according to the phase diagram, but which were obtained as a supersaturated solid solution by quenching, Fig. 1, curve c,. The increase in resistivity is mainly due to coherent precipitation of y&apos;. In Fig. 2 the effects due to short-range order pN and due to precipitation of particles APT are shown for an aging temperature of 450°C and different aluminum contents. 3) The increase in resistivity depends on the size !f the coherent particles. A critical diameter of 15 5A for the maximum was found for all alloys and aging treatments by extrapolating particle sizes determined by electron microscopy. 4) The maximum of resistivity of the heterogeneous conditions does not occur if particles, larger than the critical size, have formed already during quenching. 5) Plastic deformation destroys short-range order as well as small coherent particles. Therefore a decrease in resistivity is observed if the increase in resistivity caused originally by these phenomena is

Jan 1, 1967

By C. L. Magee, H. W. Paxton

PREVIOUS workersl&apos;% ave found that as-quenched ferrous martensites can be plastically deformed at low stresses. They have also found that the stress to obtain small strains can be significantly increased by aging at temperatures up to 150°C. This behavior has been interpreted in two ways: 1) that the deformation at low applied stress is due to internal stresses and thus the aging phenomenon is due to relaxation of the internal stresses;&apos; 2) that the microdeformation arises through the motion of unpinned dislocations and the aging process is the diffusion of carbon to the dislocations to pin them.293 In a recent paper,4 we have shown that under certain conditions the dominant microdeformation mechanism of as-quenched Fe-31Ni marten-site-austenite aggregates is the transformation of retained austenite. Our results on resistance changes during deformation and temperature dependence of the deformation also established that, at temperatures above 300° K, the microdeformation was not due to this transformation. The purpose of this note is to report results of experiments which indicate that explanation 1 is appropriate for this deformation. All results presented here are from conditions where transformation does not make a measurable contribution to the microplastic deformation, in Fe-31Ni-0.002C, or in Fe-29Ni-0.02C-0.25Ti. The experimental techniques that were used for measurement of the plastic deformation are described4 and analyzed5 elsewhere. Fig. 1 shows the microplastic response of 100 pct austenite at 300" and 350° K. The microplastic response of an austenite-martensite aggregate is also given in Fig. 1 and it is seen that, after formation of martensite, the initial plastic deformation occurs at lower stresses. Thus, the softness is not entirely due to retained austenite—the quenched structure can be deformed at lower stresses despite the fact that the macroscopic strength is significantly higher. A result which allows a distinction to be drawn between the alternative explanations for this behavior is derived from aging experiments on the low-carbon alloy containing titanium. We have previously shown4 that the presence of titanium in this alloy reduced the free carbon to a sufficiently low level that thermal stabilization of the austenite-martensite transformation was not detected. Despite this, Fig. 2 shows that the microplastic response is decreased by aging treatments. A similar aging effect in Fe-ZONi, with some titanium, has previously been reported by . Thus, carbon is not necessary for the aging process and explanation 2 is at best incomplete. Since internal stress relief can occur independently of carbon (any temperature dependence of the flow stress can result in decreased internal

Jan 1, 1969