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By Leonard R. Weisberg

HE procedure of directional freezing by the Bridgman technique1 is frequently used in crystal preparation. On those occasions where the crystal is regrown, it can be advantageous to Crop part of the ingot before regrowth to achieve purification. This note describes some simple, yet interesting, observations concerning the effects of cropping an ingot between successive freezes. First, it is not effective to Crop the front end of an ingot, whether or not the distribution coefficient, k , of the impurities is greater or less than unity. This can be shown as follows. The concentration C, of an impurity in a directionally frozen ingot of length d with a uniform cross section is given by where x is the distance along the ingot, and C0 is the initial concentration per unit length. It is assumed in deriving this equation that diffusion is negligible in the solid, is complete in the melt, and that k is constant. Consider that a section of the ingot Ad is removed from the front end. Then the average impurity concentration in the remaining (d- Ad) section of the ingot can be shown by integration to be given by When the ingot is remelted and refrozen, the new impurity distribution is given by where xl is the distance along the refrozen ingot. Substituting the value of c into Eq. [3], one finds This is identical to Eq. [11 when x = (x, Ad), which represents the original impurity distribution in the (d - Ad) section of the ingot after the first directional freeze. Therefore, the cropping and re-freezing accomplished nothing. This can also be seen physically by realizing that the average impurity content in the melt after the first Ad section is frozen, is identical to that after the resulting ingot has been cropped and remelted. Hence, it is assumed in the following sections that only the tail end of the ingot is cropped. However, it must be realized that for impurities with k greater than one, the pieces cropped from the tail end are purer, and are therefore saved. After cropping an amount Ad from the tail end of an ingot, the average impurity concentration of impurities in the remaining portion of the ingot is given by wheref= d/d. For the case of k < 1, the purification is defined as c,/c. It is obvious from Eq. [5] that the purification increases asf increases, but the increase in purification is not large. For example, iff is doubled from 0.1 to 0.2, the purification increases by only 10 pct for k = 0.5, by only 24 pct for k = 0.1, and by 32 pct for k =0.01. Much smaller values off than 0.1 are not desirable since insufficient purification is achieved. These figures indicate that much larger values off do not lead to substantial improvement, especially considering that much of the original ingot is lost. Therefore, it is generally useful to Crop about 1/10 of the ingot to achieve purification. As compared to doubling the value off, it is much more helpful to remelt, refreeze, and crop the ingot twice. Using Eq. [51 reiteratively, and assuming f= 0.1, it is found that the purification after this process is found to be increased over the purification after a single freeze and cropping by 33 pct for k= 0.5, 450 pct for k = 0.1, and 4100 pct for k = 0.01. This indicates that considerable purification can be obtained by this procedure. However, if purification is the main goal, one should resort to zone refining,3

Jan 1, 1962

By R. H. Jacoby, M. J. Rzasa

Experimental equilibrium vaporization ratios (K values) were obtained for nitrogen, methane, carbon dioxide, ethane and hydrogen sulfide in two natural gas-absorber oil mixtures and in two natural gas-Elk Basin crude oil mixtures. For each mixture of constant over-all composition, data were obtained at 100°, 150° and 200°F and at various pressures in the range 200 to 5,000 psia. Some effects of composition on the K values were obtained to serve as a guide in choosing K&apos;s for engineering calculations on other mixtures. The pressure cell used to obtain the data is a new type and is described here for the first time. INTRODUCTION The phase equilibria of complex hydrocarbon mixtures such as natural gases, crude oils and their mixtures have been studied previously for the purpose of finding equilibrium vaporization ratios for the hydrocarbon constitutents. In a few cases, such non-hydrocarbon.: as nitrogen, carbon dioxide, and hydrogen sulfide were included in the mixture. studied because they occur. in the fluids obtained from petroleum reservoirs. The increasing occurrerce. of these non-liydrocarbon.; antl their growing economic importance. make it necessary to account for them more accurately in engineering calculation.: than is now possible using the meager published data. The available data for non-hydrocarbons may he classified into two groups: namely, binary mixtures of a hydrocarbon and a non-hydrocarbon. and mixtures containing three or more components, only one of which is a non-hydrocarbon. Amon: the former. phase analyses are available for two nitrogen-HC mixtures, tve carbon dioxide-HC mixtures and three hydrogen sulfide-HC mixtures. Data for more complex mixtures are available as follows: Nitrogen-Methane-Pentane&apos;; Nitrogen-Methane-Hexane,&apos;; Nitrogen-Methane-Heptane&apos;; Carbon dioxide-Natural Gas-Natural Gasorline": Carbon dioxide-Natural Gas-Crude Oil". These data have been used generally lor engineering calculations, often with little regard for their precise applicability because data for the non-hydrocarbons in the complex mixtures being dealt with were not available. The use of K values from binary data for calculation:; involving complex mixtures is open to criticism because such K&apos;s are not a function of composition and very often show large differences from the K&apos;s for the same components in a complex mixture. Thus the effects of composition must be evaluated when obtaining K&apos;s for components in complex mixtures. Poettmann and Katz " varied the carbon dioxide content of their mixture.; from about five to ten mol per cent and found substantially no effect on the K values due to this change. This was not surprising since one might expect that changing a minor com-ponent by * three mol per cent would have little effect. It is more important to find the composition change which have the largest effect on the K values. For example. varying the methane or heptanes — plus compositions over a wide rangr may have a large effect on the K&apos;. of all components in the mixture. Interesting data to this effect were obtained by Eilerts and Smith." It was toward these problems that the experimental data presented here were directed. EQUIPMENT The pressure cell used to obtain the data i:. somewhat dif-ferent from those which have been described in the past. Photographs of the equipment are shown in Figs. 1 and 2. Fig. 1 Shows. the front panel: from a .rated position at the right the

Jan 1, 1952

By C. M. Wayman, R. Bullough

The selection rules fir twinning in fcc, bcc, and hcp lattices as established in Part I are used to predict the positions, relative to the matrix (untwinned) reciprocal lattice, of reflections due to double diffraction from the twins. These doubly diffracted reciprocal lattice points, which often coincide with ordinary matrix reciprocal lattice points, are deduced from kinematical considerations. 1. INTRODUCTION. A Bragg diffracted beam under certain conditions may be rediffracted to produce a third beam i .e., the incident beam, the first diffracted beam, and the rediffracted beam). In such a case an initial incident beam is diffracted by a set of planes; the diffracted beam may then be rediffracted by a second set of crystallographically different planes. The initially diffracted beam acts as an incident beam for the second set of planes, thus resulting in a twice-diffracted beam. This twice-diffracted beam may be regarded as a singly diffracted beam from a set of lattice planes whose structure factor is zero. In order to find the reciprocal lattice point corresponding to the doubly diffracted beam, it is customary1,2 to combine vectorially the component reciprocal lattice vectors which head to the extra reflections. For example, hcp metals may exhibit the forbidden (0001) reflections.* As Fig. 1 shows, the (0001) reciprocal lattice point results from: (1010) + (1011) = (0001) Similarly, combination of the beams (1011) and (1010) gives rise to: (1011)- (1010) = (0001) As Pashley and stowell2 have pointed out, even if in fact the double diffraction points lie on the Ewald sphere, they may not actually represent observed doubly diffracted beams because the initially diffracted primary beam, i.e., the source, must also correspond to a reciprocal lattice point which lies on the sphere of reflection; however, the reciprocal lattice point corresponding to the planes causing the rediffraction need not lie on the sphere. A little consideration of the Ewald construction in Fig. 2 makes this argument clear. In Fig. 2 the incident beam is represented by the wave vector ko. This beam is initially diffracted by the lattice planes (hkl) which are represented by the reciprocal lattice vector r(hk1) The reciprocal lattice point (hkl) of course lies on the Ewald sphere in order that the Bragg condition be satisfied. The initially diffracted beam is represented by the wave vector kl. If now kl is rediffracted by a second set of planes (h&apos;k&apos;l&apos;) resulting in k2 the lattice point (h"k"l") must lie on the Ewald sphere if the double diffracted beam k2 is to be observed. It is clear that (h"k"l") is the vector sum of (hkl) and (h&apos;k&apos;l&apos;), and that (h&apos;k&apos;l&apos;) need not in fact lie on the Ewald sphere. In the usual1,2 analysis the origin (000) of the reciprocal lattice is shifted to the point (hkl). However the translation (000)— (hkl) automatically shifts the point (h&apos;k&apos;l&apos;) to the Ewald sphere, i.e., (h&apos;k&apos;l&apos;)— (h"k"1"). It is to be seen that (hkl), the source reflection, must lie on the Ewald sphere; if it does not the translation (000) — (hkl) places the "new" origin off the sphere, not satisfying the Ewald construction and hence the Bragg condition. The point (h"k"1") of course must lie on the sphere if it corresponds to an observed doubly diffracted beam. It is to be noted that crystals having the hcp structure, as just discussed, are intrinsically capable (i.e., without lattice defects such as twins) of double diffraction, as contrasted to fcc and bcc crystals which are extrinsically capable (requiring lattice defects or reoriented lattice regions). The "allowed" bcc reciprocal lattice points (which comprise an fcc lattice) are (110), (2001, (211), (220), (310), (2221, (321), (4001, and so forth. The combination

Jan 1, 1967

By Y. K. Rao

In the carbonyl process for the refining of crude nickel CO(g) reacts with nickel in the 310-370K range producing nickel tetracarbonyl, Ni(C0)4(g). Iron and cobalt impurities also form gaseous carbonyls but their partial pressures are low. The carbonyl is led to a decomposer plant wherein the gas disproportionates in the 500-600K range depositing pure metal on nickel pellets that move countercurrent to the gas-flow. This system serves to illustrate the fundamental principles involved in the vapor phase mass transport of elements, against temperature-gradient, under the influence of chemical potential gradient. Unlike in the crystal growth, the source is at a lower temperature (say 350K) whereas the seed is in the hot-zone (say 550K) of the closed ampoule-type reactor. By assuming virtual gas-solid equilibria in the end zones, with diffusion of gaseous species between them acting as a slight perturbation, the quasi-steady- state mass-transport rates are computed for a range of CO-pressures and temperatures.

Jan 1, 1993

By Haotian Xue

A new process to extracted antimony directly from stibnite concentrate by reductive sulfur-fixation smelting in sodium molten salt has been presented. The influences of sodium salt content and composition, ferric oxide addition, temperature and time was investigated, respectively. The optimum conditions was determined as follows: W????: ??concentrate=40%, W??alt: ????concentrate =88.75%, WFe2O3 :Wconcentrate =55.13%, W??aCl: ????alt=40%, 1123K, 1h. Under above-mentioned optimum conditions, the average direct recovery ratio of antimony can reach 91.48%, and the main chemical composition of obtained crude antimony is Sb 94.31%, Fe 4.436%, Pb 0.502%, Au 0.0236%. In comparison to traditional antimony pyrometallurgical process, the smelting temperature of present process is reduced from 1423~1473K to 1123~1173K. During the smelting operation, SO2 emision can be avoided completely due to sulfur-fixation as FeS. Furthermore , S0 can be obtained when the molten slag is handled by water leaching with conditions of 323K, L/S=5/1, 2h.

Jan 1, 2014

By M. Arlandi-Rodríguez, and A. García-Berrocal, A. Alonso-Jiménez, C. Lopez-Jimeno

Spain is a major producer of dimension stone, which is one of the most important industrial sectors in the northwest of Spain. This justifies the maintenance of these industries, although the technical and environmental requirements for their continuity are increasingly demanding. The main target of this paper is to present a new methodology in order to obtain k-ratio stress values on the basis of flat jack measurements and finite element numerical back- analysis with Rocscience© RS2 software. Continuous iterations were performed to try to find a relationship between the k₀ and the measured stress in the tunnel roof and sidewalls. It focuses on technical aspects of the method for designing mine chambers in the slate industry that were previously mined by open pit methods. The size of the chambers impacts the operating cost, and the dimensioning of a correct support ensures better efficiency and safety. Correct knowledge of the k₀ therefore is critical for the design of the support. The proposed new method entails a simplification of the classical procedure for estimating the k-ratio.

Sep 1, 2022

By Do-Hyeong Kim, Tae-Jung Kim, Seung-Yeon Won, Jong-Jin Pak, Min-Kyu Paek

Liquid iron alloys containing V, Mo, and Ni can be produced by the carbothermic reduction of spent catalysts used in petrochemical industry. Thermodynamics of carbon in these alloy melts is important for refining these alloys. In the present study, the carbon solubility in Fe-V, Fe-Mo, Fe-Ni, Fe-V-Mo, Fe-V-Ni, Fe-Mo-Ni and Fe-V-Mo-Ni alloy melts of various compositions was measured at 1873 K. The temperature dependency of vanadium effect on carbon solubility in liquid iron was also measured in the temperature range from 1823K to 1923K. The additions of vanadium and molybdenum significantly increased the carbon solubility in liquid iron alloys while nickel decreased the solubility. The experimental results were thermodynamically analyzed using Lupis’ relation at constant activity to determine the first- and the second-order interaction parameters of vanadium, nickel and molybdenum on carbon at carbon saturated condition. Using thermodynamic parameters determined in the present study, the carbon solubility in Fe-V-Mo-Ni alloy melts of various composition were accurately predicted and verified experimentally at 1873 K.

Jan 1, 2014

By Raphaella Hermont Fonseca Murta

O ensaio não destrutivo por ultrassom é amplamente utilizado para detectar e dimensionar descontinuidades no interior do material. A técnica TOFD (Time Of Flight Diffraction [do inglês]) foi a técnica ultrassônica utilizada. Entretanto, a classificação do tipo de descontinuidade, a partir dos sinais ultrassônicos obtidos durante uma inspeção requer um profissional altamente capacitado. Esta tarefa pode ser realizada por algoritmos de reconhecimento de padrões, capazes de processar rapidamente uma grande quantidade de dados. Nesse trabalho, foram simulados três tipos de descontinuidades em juntas soldadas: falta de penetração, poro e trinca, utilizando-se o Método dos Volumes Finitos (MVF). Em seguida, foi aplicado o método de reconhecimento de padrões K-vizinhos mais próximos (K-NN – K-nearest neighbors [do inglês]), para verificar como esses dados são separados. Esse trabalho é um passo inicial para o emprego de simulação numérica do ensaio ultrassônico para produzir sinais simulados e utilizá-los no treinamento de ferramentas de reconhecimento de padrão, a serem futuramente testados com sinais ultrassônicos experimentais. O K-NN classificou bem os sinais simulados. Conseguindo uma taxa média de acerto de aproximadamente 84%.

Oct 30, 2017

By William Gleason

Despite a global slowdown in most mining sectors, Caterpillar, the world?s largest mining equipment maker continues to forge ahead with new, and improved offerings to the global mining industry. On Nov. 10, as part of its Loading and Hauling Mining Focus Session at its Tinaja Hills proving grounds south of Tucson, AZ, Caterpillar unveiled to customers and media its two latest mining products, the 994K wheel loader and 6020B hydraulic shovel. The Caterpillar 994K wheel loader builds on a nearly 25-year history of the 994 model but with one noticeable difference ? the 994K is bigger ? much bigger. Weighing in at 239,142 kg (527,218 lb) the 994 K is up to 20 percent larger and comes with up to 30 percent increase in payload capacity. This behemoth of a machine is currently being tested at Caterpillar?s Tucson Proving Grounds, Anglo Gold Ashanti?s Cripple Creek and Victor gold mine in Colorado and Taseko?s Gibraltor copper and molybdenum mine in British Columbia, Canada.

By R. E. Wagner

Consistent increase has been the mark of North American potassium (K) consumption. In 23 of the last 25 years there was upward progress The pace of usage has quickened in the past three or four years This, together with a predicted accelerated future demand, has created unprecedented interest -and activity in the potash industry. Potassium enjoyed a ninefold increase in consumption from 1940 to the present time in North America (Figure 1). Since 1950, it increased from just over a million tons of potash (K20) annually to nearly three million tons in 1964. World-wide usage exclusive of mainland China is now about 10 million metric tons. Some predictions call for another doubling in consumption in the next 10 to 15 years, About 20 percent of the four million tons of K20 produced in North America is now exported overseas and this percentage is likely to increase in the years ahead. Ten years ago, exports represented only 3-1/2 percent of total K2O production from this continent.

Jan 1, 1966

By G. E. Walden

The Bureau of Mines is currently engaged in a continuing investigation of the thermodynamic properties of certain inorganic compounds. As a part of this investigation, the heat contents of bismuth and cerous chlorides were measured throughout the temperature ranges of 370° to 630° K. and 370° to 1,200° K., respectively. Equations representing heat contents as a function of temperature were derived from the data by the method of least squares. These equations were used to calculate heat contents at selected temperature intervals ranging from the ice point to 650° K. for bismuth chloride and to 1,200° K. for cerous chloride; also, the heats of fusion of both compounds were calculated at their respective melting points. EXPERIMENTAL Materials The cerous chloride used in this investigation was supplied by the National Carbon Company of Cleveland, Ohio. A chemical analysis indicated Ce 56.57 percent and Cl 43.39 percent. No attempt was made to purify the compound or identify impurities since the analysis showed only about 0.04 percent total impurities. Reagent grade bismuth chloride was used without additional purification.

Jan 1, 1961

By J. S. Browning

The Bureau of Mines investigated the concentration characteristics of high-clay sylvinite ores from potash companies operating in the Permian basin near Carlsbad, N. Mex. These ores, containing 14 to 19 percent K20 and 3 to 5 percent clay slimes, cannot be effectively processed by current commercial flotation methods because of their high clay content. A solution to this problem was shown to be the use of two-stage moderate scrubbing conditions for clay disaggregation and removal as opposed to strenuous attritioning. Bench-scale beneficiation techniques for recovering potash minerals by flotation from the scrubbed material resulted in acceptable product grades and recoveries. By using a coarse grind, emphasis was placed on production of premium granular and coarse products. Flotation results showed that concentrates of 59.6 to 60.4 percent K.0 values can be obtained. Continuous pilot plant beneficiation techniques for recovering potash minerals by flotation resulted in concentrates containing 58.8 to 59.8 percent K20 with recoveries of 69.7 to 81.4 percent of the K20.

Jan 1, 1975

By K. O. Bennington

The thermodynamic properites of petalite (Li2A12Si8O20) were determined by the Bureau of Mines. The enthalpy of formation was determined by hydro-fluoric acid solution calorimetry. The values from the elements and from the oxides are ?Hf°298.15 = 2,335.8 ± 3.0 kcal/mole and ?H°295 (from oxides) = -50.60 ± 1.20 kcal/mole. Low-temperature heat capacities were determined by adiabatic calorimetry from 10.69 to 302.11 K. The derived standard entropy is S°298.15 = 111.0 ± 1 cal/deg-mole. Enthalpy increments above 298 K were measured by copper block calorimetry from 298 K to 1,193.6 K. The various experimental data were combined with other data from the literature to calculate the Gibbs energies of formation and equilibrium constants of formation over the temperature range of the measurements. Tables of enthalpies of formation and Gibbs energies of formation are given as a function of temperature from the elements and constituent oxides. The Gibbs energy of formation is ?G°f298.15 = 2,203.8 kcal/mole.

Jan 1, 1980

By Hong Yong Sohn

A thermodynamic and experimental investigation has been performed to develop a new process for converting sulfur dioxide to elemental sulfur by a cyclic process. The most promising new process is a cyclic reaction scheme involving calcium sulfide and calcium sulfate. In this process, the reaction between sulfur dioxide and calcium sulfide produces elemental sulfur vapor and solid calcium sulfate. The latter is reduced by a suitable reductant such as hydrogen to regenerate calcium sulfide. &apos;Experimental results showed that up to 60 % of calcium sulfide powder was converted to calcium sulfate in 10 min at 1153 K under a sulfur dioxide partial pressure of 25.8 kPa. More than 95 % of nickel-catalyzed calcium sulfate powder was converted to calcium sulfide in 20 min at 1123 K under a hydrogen partial pressure of 86.1 kPa, water vapor being the only gaseous product. Sulfur dioxide-containing streams from certain new sulfide smelting plants contain much higher partial pressures of SO2. The rate of the first reaction is expected to be accordingly higher than in the test conditions reported in this paper.

Jan 1, 2002

By Peter Beardmore, Michael B. Bever

The effects of the temperature of deformation and the degvee of deformation on the annealing spectrum of a Au-Ag alloy have been determined by vesistance measurements. Specimens were deformed in torsion at 4°, 78K and room temperature up to strains nd/l of about 1.0 and were isochronally annealed. Discrete annealing stages similar to those found for pure metals were observed. Stage A occurred below room temperature; the decrease in reszstance associated with this stage increased as the temperature of deformation was lowered or the strain was increased. Stage B manifested itself as an increase in resistance; this is attributed to the restoration of short-range order promoted by vacancy or vacancy aggregate migration. At temperatures above 48S0K, recrystallization or Stage C occurred. Stages A, B, and C in the annealzng curves of this alloy may be considered to correspond to Stages II, Ill, and V, respectively, in the terminology used to describe the annealing spectrum of pure metals. ThE annealing behavior after deformation below room temperature has been thoroughly investigated on pure metals, in particular gold and copper. The occurrence of several discrete stages in the annealing spectrum of these metals has been established, but the interpretation of some of these stages in terms of specific mechanisms is still controversial.&apos; The annealing of alloys deformed below room temperature has been the subject of only a few investigations. In the investigation reported here, a Au-Ag alloy was annealed after deformation at and below room temperature. This continues a research program on the deformation and annealing behavior of Au-Ag alloys.2-8s EXPERIMENTAL PROCEDURE An alloy rod of composition 82.6 wt pct Au-17.4 pct Ag was reduced to wire, 0.0428 in. diam, by swaging and drawing. After a recrystallization treatment, the grain size was 0.031 mm, as obtained from the average linear intercept.7 The ends of wires about 6 in. long were flattened and sealed into short brass tubes with cold setting cement to form the grips of the torsion specimens. The equipment used for deformation has been described elsewhere.6 The specimens were deformed at room temperature, 78", and 4°K to various strains nd/l, where n is the number of turns, d the diameter of the specimen, and 1 its length between grips. The strain rate ?max was 0.1 min-&apos; at the sur- face of the specimen except where noted otherwise. The specimens were annealed isochronally for 30 min at intervals of approximately 30°K from the temperature of deformation to approximately 800°K, except that after deformation at 4°K the lowest annealing temperature was 78°K. A potentiometric method was used to measure the resistance: all measurements were made at 78°K with the exception of some measurements at 4°K mentioned below. Data obtained with a single specimen yielded a complete annealing curve: in several cases duplicate specimens were used to confirm the reproducibility of the curves. Since the surfaces of the specimens were rough after deformation, their diameters could not be measured accurately. The resistance increments after deformation and annealing are therefore reported as percentages of the resistance of the same specimen measured after completion of the annealing, that is, after full recrystallization. The corresponding resistivity values can be calculated by obtaining the effective diameter of a deformed specimen from the ratio of its resistance after recrystallization to the true resistivity, which was determined with a smooth specimen of known dimensions. This method of calculation was used to obtain data shown in several of the figures. RESULTS AND DISCUSSION The isochronal annealing curves after deformation to various strains at 4", 78K, and room temperature are shown in Figs. 1, 2, and 3, respectively. The resistance increment of the as-deformed specimens as a function of strain is shown in Fig. 4. For the specimens deformed at 4°K. values measured at 78°K are plotted with the exception of those for the as-deformed

Jan 1, 1970

By C. J. Guntner, R. P. Reed

A commercial 18Cr-8Ni iron alloy (AISI 304L) was examined in tension at 300°, 76°, 20°, and 4°K. Continuous stress-strain recordings were made, X-ray analyses at periodic stress (strain) intervals were obtained, and the magnetic measurements were taken. From this data the percentage of martensitic products [bcc(a) and hcp (E)] was computed as a function of stress (strain). It was found thatup to 15 pct E phase forms at low temperntures. The amount of E formed increases to a maximum at about 5 pct strain, then decreases. This decrease indicates the additional transformation of E to a&apos;. The total amount of E and a&apos; was suppressed at constant stress (strain) at 4°K as compared to 76°K. It is proposed that the suppression of E and a&apos; is associated with the decreased mobility of extended dislocations at very low temperatures. The yield strength decreased as the temperature was depressed below room temperature and then increased rapidly near 4°K. SOME ferrous alloys which are austenitic (fcc ?) at room temperature appear to be unique in that two martensitic products (hcp e and bcc a&apos;) may form on cooling to lower temperatures or on application of mechanical stress. The most common room-temperature austenitic ferrous alloys are 18Cr, 8Ni stainless steels. Most aspects of the spontaneous transformations have been previously described for these steels.&apos; Several previous papers have described special aspects of the stress-induced transformations at low temperatures for the stainless steels, such as the existence of the hcp phase (c) after straining at 76oK,2-7 the morphology after straining using electron microscopy,7 and the decrease in E at higher strains at 76oK.4 However, for a complete representation, one must know the stress-strain characteristics and the dependence of both martensitic products on applied stress and temperature. It is the intention of this paper to provide that documentation. To accomplish this, continuous stress vs strain recordings were made at four temperatures: 300°, 76", 20°, and 4°K for annealed AISI 304L (a commercial 18Cr-8Ni alloy). At periodic stress intervals at each temperature the integrated X-ray line intensity of a selected peak for each phase (y, E, and a&apos;) was measured. In addition, photomicrographs of the strained surfaces were taken and magnetic measurements were made. The magnetic readings can be directly converted into percent a&apos;.&apos;,e With these measurements the percentage of each phase may be plotted as a function of stress (or strain) and test temperature. It was found that up to 15 pct E phase forms upon stressing the AISI 304L alloy at low temperatures. The E percentage increases abruptly after the alloy yields, but then decreases gradually at higher stresses. The rapid increase in e at 76°K is associated with an "easy-glide" portion of the stress-strain curve. The total amount of a&apos; + .G is suppressed below 76°K at a constant stress or strain. The yield strength decreases down to 76°K but increases rapidly below 20°K. EXPERIMENTAL PROCEDURE Tensile test specimens were cut parallel to the rolling direction from 0.1-in.-thick sheet. Continuous stress vs strain recordings were obtained at each test temperature (300°, 76o, 20°, and 4°K) using equipment and methods described elsewhere.&apos; The specimens which were used in the X-ray analysis were stressed to successive increments of strain at each temperature, analyzed at room temperature, then restressed at the test temperature. This procedure was repeated until approximately ten X-ray analyses had been performed with approximately 1.0 pct strain increments. The specimens had a reduced section 1 in. long, 1.2 in. wide, and 0.1 in. thick. They were electro polished prior to testing and after each strain increment. Table I lists the chemical composition, grain size, and hardness for the alloy which was used. This is the same alloy for which extensive mechanical-property tests3 and morphological studies of the spontaneous transformations&apos; have previously been made. For the low-temperature tests (76o and 4°K) below the Ms temperature the specimens were initially cooled to the test temperature, held for 1/2 hr, then warmed and X-rayed at room temperature. The results are listed in Table 11. From earlier work8 it was known that additional transformation on the second cycle would be considerably less (-0.1 pct

Jan 1, 1964

By D. G. Westlake

The electrical resistance of a series of V-H alloys (0 to 3.5 at. pct H) has been measured over the temperature range G° to 360°. Interstitial impurities made contributions to the residual resistivity, but not the ideal resistivity. The contribution of hydrogen in solid solution is expressed by Ap = 1.12 microhm-cm per at. pct H; but the contribution of precipitated hydride was negligible. A portion of the so1vu.s for the V-H phase diagram is presented. The solubility limit is given by In N (at. pct H) = (5.828 i 0.009) - (2933 i 44)/RT. Comparison of critical temperatures joy hydride precipitation and published critical temperatures for hydrogen embrittlement suggests the two are related. ThiS study was initiated as part of an investigation of the mechanism by which small concentrations of hydrogen embrittle the hydride-forming metals at low temperatures. It has already been shown that, in the case of hcp zirconium, a reduction in ductility accompanies the strengthening resulting from precipitation of a finely dispersed hydride phase.&apos;&apos;&apos; Our attempts to detect a similar precipitation of a second phase at low temperatures in V-H alloys by transmission electron microscopy have been thwarted because we have been unable to prepare thin foils that are representative of the bulk material with respect to hydrogen concentrati~n.~&apos;~ The present investigation establishes the solvus of the V-H system at subambient temperatures. Subsequently, we hope to be able to determine whether the embrittlement temperature is related to the critical temperature for precipitation of the hydride in a given V-H alloy. veleckis5 has proposed a partial phase diagram for the V-H system based on extrapolations of the pressure-composition relations he measured at higher temperatures. Kofstad and wallace&apos; conducted a similar study of single-phase alloys but did not attempt to establish the phase diagram. Zanowick and wallace&apos; and ~aeland&apos; have studied a portion of the phase diagram by X-ray diffraction, but they investigated no alloys in the hydrogen concentration range 0 to 3 at. pct, the range of interest to us. EXPERIMENTAL PROCEDURE The vanadium was obtained from the Bureau of Mines, Boulder City, Nev., in the form of electrolytic crystals. The analyses supplied with them listed 230 ppm by weight metallic impurities, 20 ppm C, 100 ppm N, and 290 ppm 0. The crystals were electron-beam-melted into an ingot that was rolled to 0.64 mm. Strips, 60 mm long and 4.2 mm wide, were cut from the sheet, and both rolled surfaces were ground on wet 600-grit Sic paper to produce specimens 0.4 mm thick. They were wrapped in molybdenum foil, vacuum-encapsulated in quartz, and annealed 4 hr at 1273°K. The specimens were annealed in a dynamic vacuum of 2X lo-&apos; Torr for 30 min at 1073°K for dehydrogenation, and charged with the desired quantity of hydrogen by allowing reaction with hydrogen gas at 1073°K for 2 hr and cooling at 100°K per hr. Purified hydrogen was obtained by thermal decomposition of UH3. Sixteen specimens were studied: two contained no hydrogen and the others had hydrogen concentrations between 0.5 and 3.5 at. pct (hydrogen analyses were done by vacuum extraction at 1073°K). Electrical resistances were measured by the four-terminal-resistor method on an apparatus similar to the one described by Horak.~ The specimen holder was designed so that both current and potential leads made spring-loaded mechanical contact with the specimen. The potential leads were 30 mm apart, and the current leads were 55 mm apart. The current was 0.10000 amp. We used the following baths for the indicated temperature ranges: liquid nitrogen, 77°K; Freon 12, 120" to 230°K; Freon 11, 230" to 290°K; and ethanol, 290" to 340°K. Temperatures lower than 77°K were achieved by allowing the specimen to warm up after removal from liquid helium. Temperatures above 77°K were measured by a calibrated copper-constantan thermocouple (soldered to the specimen holder) and below 77°K by a calibrated carbon resistor. The temperature of the bath changed less than 0.l0K between duplicate measurements of the resistance. RESULTS AND DISCUSSION Typical plots of resistivity p vs temperature T are shown in Fig. 1. In the interest of clarity, only five curves are presented and the data points have been

Jan 1, 1968

By K. K. Kelley, W. W. Weller

Heat capacity measurements of akermanite ( Ca,MgSiO ) , cordierite (Mg2A14 Sig018 ) , gehlenite ( Ca₂Al₂ SiO ) , and merwinite ( Ca ,MgSiO ) were conducted over the temperature range from 50 ° to 298.15 ° K. The entropies at 298.15 K ( expressed in cal / deg mole ) were evaluated as follows : Akermanite , 50.0 ± 0.5 ; cordierite , 97.3 ± 0.9 ; gehlenite , 47.4 ± 0.4 ; and merwinite , 60.5 ± 0.5 . All four compounds have positive entropies of formation from their constituent oxides at 298.15 ° K ; the values range from 4.6 cal /deg mole for akermanite to 10.1 cal / deg mole for cordierite .

Jan 1, 1963

By John C. Edwards, F. Friel, John J. Opferman, Robert A. Franks

A series of diesel fuel fire experiments were conducted in the Pittsburgh Research Center&apos;s Safety Research Coal Mine (SRCM) to determine products-of combustion (POC) spread rates along a single entry under zero imposed airflow conditions. Six experiments with an average fire intensity of 330 kW and three experiments with an average fire intensity of 30 kW were con- ducted in a 180 m long entry which had an average 2 m height and 4 m width. POC spread rates were measured by the response time of diffusion type CO detectors, positioned at 30 m intervals, to CO concentrations 5 ppm above ambient. For the 330 kW fires, average POC spread rates of 0.22, 0.1 3, and 0.06 m/s were determined at 30, 60, and 90 m distances from the fire. For the 30 kW fires these average spread rates were reduced to 0.08, 0.04, and 0.04 m/s. The measured maximum roof layer temperature 30 m from two of the 330 kW fire was 30 and 36"C, which is less than the 57°C alarm point of a typical mine thermal sensor. It was determined that smoke detectors can be more effective for mine fire detection than CO detectors. The experimentally determined POC spread rates can be used to provide guidance for specification of sensor spacing to improve early fire detection at zero or very low air flows.

Jan 1, 1997

By John C. Edwards, Gene F. Friel, John J. Opferman, Robert A. Franks

A series of diesel fuel fire experiments were conducted in the Pittsburgh Research Center&apos;s Safety Research Coal Mine (SRCM) to determine products-of-combustion (POC) spread rates along a single entry under zero imposed airflow conditions. Six experiments with an average fire intensity of 330 kW and three experiments with an average fire intensity of 30 kW were conducted in a 1 80 m long entry which had an average 2 m height and 4 m width. POC spread rates were measured by the response time of diffusion type CO detectors, positioned at 30 m intervals, to CO concentrations 5 ppm above ambient. For the 330 kW fires, average POC spread rates of 0.22, 0.13, and 0.06 m/s were determined at 30.60, and 90 m distances from the fire. For the 30 kW fires these average spread rates were reduced to 0.08, 0.04, and 0.04 m/s. The measured maximum roof layer temperature 30 m from two of the 330 kW fire was 30 and 36"C, which is less than the 57°C alarm point of a typical mine thermal sensor. It was determined that smoke detectors can be more effective for mine fire detection than CO detectors. The experimentally determined POC spread rates can be used to provide guidance for specification of sensor spacing to improve early fire detection at zero or very low air flows.