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By Regis M. N. Pelloux, N. J. Grant

Five or six alloys each in the systems Ni-C.v, Ni-Mo, and NL-W, spaced to cover the single phase areas as well as a part of the adjacent two-phase field, were prepared as uacuum-melted alloys. Tensile tests at room temperature and stress rupture tests at 1200° and 1500°F we.ve run for time periods to give fracture in 0.1 to 500 hr. Observations mere made of solid-solution and second-phase strengthening or uleakening, coupled with studies of ductility and the role of structure on the noted behavior patterns. THE development of stable creep-resistant alloys while broad and systematic is also highly empirical. A number of simple rules have been suggestedL-" but these are based on scant data. Whereas rules for low-temperature alloy strengthening can be applied with some success in more simple systems, the extension to behavior at high temperatures (greater than about 0.4 of the absolute melting temperature) is very poorly understood and has encountered important exceptions and deviations in terms of atom size or valency effects. In particular, the occurrence of both solid-solution weakening4,5 and second-phase weakening2 at high temperatures is of interest. MATERIALS AND PROCEDURE Nickel was chosen as the base material because of its important role in current high-temperature alloy applications, because of its freedom from a phase transformation, and because of wide solubilities for many elements of interest. The selected alloys were single- and two-phase structures in the Ni-Cr,6 Ni-Mo,7 and Ni-w 8 systems. The alloys were vacuum melted and cast, utilizing high-purity raw materials, in the form of 15 lb ingots. They were readily forged into 1/2-in. bar stock (except the two highest chromium alloys). The alloy compositions are shown in Table I. Typical impurity values are: Carbon: Max 0.03 pct (except for 30 and 35 pct Cr alloys which had 0.07) Nitrogen: Max 0.005 pct (except for two of the Cr alloys which had 0.05) Sulfur: Max 0.004 pct Silicon: Max 0.05 pct Each alloy was solution treated (air quenched) to produce comparable grain size. The two-phase alloys were then overaged in an effort to produce a stable structure for testing at 1200° and 1500°F, The results are summarized in Table 11. Following the heat treatments outlined in Table 11, the bars were machined to a gage section of 1.25-in. long by 0.250-in. diam. In addition to room-temperature tensile tests, stress-rupture tests were run at 1200" and 1500°F for time periods from 0.1 to about 500 hr. RESULTS Room-Temperature Mechanical Properties—The ultimate tensile strength, total elongation, and reduction of area values for all the alloys are plotted vs atomic percent of the solute element in Fig. 1. It can be seen that for the same amount of solute element the ultimate tensile strength increases in the order chromium, molybdenum, tungsten. Elongation increases (reduction of area decreases) with increasing amounts of solute for all the solid solution alloys, the values ranging from 50 to 70 pct. The ultimate tensile strength values for the two-

Jan 1, 1961

By S. F. Reiter, You-Chao Liu, W. R. Hibbard

Cyril Stanley Smith in his classic 1948 Institute of Metals Lecture&apos; noted in the case of annealing twins that: "It is well known that approximately the same number of twins per grain and the same general geometry are maintained in large grains as in small ones, a fact that certainly suggests a mechanism such as the above where boundaries and twins grow proportionately together. If this view is correct, a spherical grain should have no mechanism for keeping its twins." Such a constancy of twins per grain would be of particular interest as a tool for the study of the origin of annealing twins. It has been proposed by Mathewson2 and later by Barrett3 that in face-centered cubic metals slip occurs in the {111} Plane by <112> shears which combine in pairs to produce the macroscopically observed <110> movement. This proposal is schematically inviting since <112> slip permits the atoms of one plane to move along the interatomic valleys of its neighbor rather than up the hills across the atom sites. There is strong experimental evidence? that annealing twins result from the growth of nuclei in the form of "twin faults" produced by single <112> shears. It is possible that more twin faults would form at low deformation temperatures than at high ones, because the more rigid lattice may increase the tendency to "freeze" the twin faults and prevent their dissipation in slip. This is suggested by (1) the greater resistance to slip at low temperatures and (2) greater tendency toward mechanical type twinning at low temperatures (a summary of these factors is presented by Seigle and Brick5). These considerations would suggest the following: a. Constant twin/grain ratio for specimens deformed constant amounts at a constant temperature, but annealed at various temperatures above the recrystalliza-tion temperature. b. Larger twin/grain ratios for re-crystallized specimens previously deformed constant amounts at lower temperatures. The purpose of this investigation is to test these considerations. One half in. rods of phosphorous deoxidized electrolytic copper and 70-30 alpha brass (68.36 pct Cu, 0.005 pct Pb, 0.01 pct Fe, 31.62 pct Zn remainder) were rolled to a thickness of 0.350 in., milled to specimens 0.350 X 0.437 X 2 in., and annealed at 700°C to an average grain size of 0.065 and 0.090 mm, respectively. These specimens of each metal were then rolled 50 pct reduction in thickness and annealed one hour under conditions which were all combinations of the following: Rolling Annealing Temperatures. Temperatures. °C °C -70 400 25 500 200 600 Standard metallographic techniques&apos; were used to prepare specimens. By the method of lineal analysis7 using a minimum of ten samples of fifty grains each for each specimen, the ratios of twins* per total grains, twins per twinned grain, twin families* per total grains and twins per twin family were determined. Recrystallized grain size was determined by A.S.T.M. comparison methods.8 All observations were made on the rolling plane. The results are tabulated in Table 1.

Jan 1, 1950

By T. W. Healy, P. Somasundaran, D. W. Fuerstenau

The flotation behavior of quartz in the presence of alkyl ammonium acetates as a function of alkyl chain length has been interpreted in terms of hemi-micelle formation at the solid-liquid interface. The van der Waals cohesive free energy that is responsible for hemi-micelle formation has been found from these results to be 1.0 kT per CH2 group. This is in excellent agreement with literature values obtained from research on the properties of micelles in bulk systems. Collectors of the type CH3(CH2)n-2CH2-P, where P is a polar group and n is the number of carbon atoms in the straight alkyl chain, will induce flotation of an appropriate mineral at lower concentrations as n increases. This reduction in collector concentration with increasing n has been reported for such systems as xanthates on sulfides1,2 and amines on quartz.&apos; The effect of chain length of alkyl surfactants on such solution properties as conductivity,&apos; surface tension,&apos; and solubility6 and such interfacial properties of solids as contact angle7 and electrokinetic potential8 have received considerable attention, but only limited quantitative descriptions of the effects have been given. The electrokinetic studies of alkyl amine salts on quartz indicated that the solution concentration of collector at which the marked change in electrokinetic potential of quartz occurs decreases systematically as the length of the alkyl chain increases. The aim of the present work was to obtain a quantitative description in terms of current theories of flotation of the effect of the hydrocarbon chain of alkyl ammonium acetates on the flotation behavior of quartz. BASIC PRINCIPLES The marked changes in electrokinetic potentials of quartz in dodecylammonium acetate (DAA) solutions were postulated to result from the association of adsorbed collector ions into two-dimensional aggregates, called hemi-micelles.9 Subsequently, the rapid increase in flotation rate of quartz was shown to coincide with hemi-micelle formation." We would like to discuss briefly the concept of hemi-micelles in terms of recent interpretations of micelles in bulk solution. Micelle hypothesis: In dilute solutions, alkyl ammonium and related salts behave as ordinary strong electrolytes, but at a certain concentration there is a marked change in physical properties of the solutions, e.g., in equivalent conductance, transport number, freezing point lowering and viscosity. To account for these phenomena, McBainl1 introduced the concept of micelles, which are aggregates of long-chain ions. It is believed that the ionic heads of the constituent ions of the micelle are in contact with water, whereas the nonpolar groups turn away from it and are in contact with each other. Work must be done to bring these charged polar groups together, but energy is gained (i.e., so called van der Waals cohesive energy) when hydrocarbon chains are expelled from the water and allowed to associate. For a given polar group, the tendency to form micelles will therefore strongly depend on the hydrocarbon chain length. Theoretical treatments of micelle formation by Shinoda12 and Phillips13 and others lead to the following expression for the concentration at which micelles form (the critical micelle concentration or cmc) in aqueous solutions of long- chain electrolytes

Jan 1, 1964

By J. W. Freeman, D. N. Frey

Fundamental reasons for the improvement in creep resistance of an austenitic alloy by cold working were investigated mainly by X-ray diffraction. The creep resistance was found to be improved by the internal stresses in the lattice of the alloy induced by the cold work. THIS investigation was concerned with the fundamental reasons for improvement in creep resistance of an austenitic alloy as a result of cold working. Also, the investigation was carried out to elucidate the conditions under which cold working could be expected to improve the creep resistance. To achieve these ends, creep resistance and internal structure were correlated for a variety of cold-worked conditions. Since the aim of the investigation was not to obtain specific and extensive information on any one alloy, creep testing was done with a single stress at 1200°F. Structural studies were carried out primarily with X-ray diffraction characteristics. The alloy used, low carbon N-155, was selected on the basis of being representative of at least some of the alloys used in gas turbines. Low carbon N-155 alloy in the form of %-in. sq bar stock was used in this investigation. The chemical composition, in percent, was: C, 0.13; Mn, 1.43; Si, 0.34; Cr, 20.73; Ni, 18.92; Co, 19.65; Mo, 3.05; W, 1.98; Cb, 0.98; N, 0.14; and Fe, balance. The bar stock was produced from a 13-in. sq billet, finished to 7/s in. round cornered square between 2060" and 1910°F. Prior to use in this particular investigation, the bar stock was solution-treated 1 hr at 2200°F and water quenched. This procedure was used in order to put the stock in a condition where effects of prior processing were minimized. Experimental Procedure The specific approach to the problem was twofold. First, the influence of cold working, under various conditions, on the creep rate under a single stress at 1200°F and on the internal structure was in part determined. Second, the effect of annealing at various times and temperatures on the creep rate and internal structure of the cold-worked samples was in part evaluated. The first step was basic to the investigation—creep resistance and structure were to be correlated. The second step was taken to see if the annealed samples showed some internal changes which could also be correlated with changes in creep resistance. This it was felt would facilitate solution of the basic problem. The creep and structural studies were carried out on samples reduced approximately 5, 15, and 40 pct at room temperature and 15 pct at temperatures up to 2200 °F. Annealing of various of the samples was done at 1200°, 1400°, 1600°, and 1800°F for time periods up to 1000 hr. Studies of the annealed samples were concentrated on materials rolled approximately 5, 15, and 40 pct at room temperature and 15 pct at 1400°F. The creep tests were carried out at 1200°F under 40,000 psi, the latter being approximately the 1000 hr rupture stress of the material

Jan 1, 1952

By F. Kurata, A. F. Bertuzzi, P. C. Davis, T. L. Gore

The phase and volumetric properties of 10 very volatile mixtures are presented for temperatures from — 200°F to above the critical points. These mixtures consisted of natural gases and of mixtures of natural gases with methane and nitrogen. Existing correlations of compressibility factors have been extended to apply to these mixtures. Existing correlations of critical pressures and temperatures do not apply to these mixtures. Methods have been developed for estimating critical temperatures of these mixtures to ± 4°F and critical pressures to 2 5 per cent. These methods apply to other volatile and very volatile mixtures. The results of this work are particularly applicable to the separation of nitrogen from hydrocarbons by low-temperature distillation. INTRODUCTION Knowledge of the low-temperature phase and volumetric properties of natural gases and of other mixtures of the light hydrocarbons is becoming increasingly important as interest in low-temperature separation processes increases. Low-temperature distillation has been used to separate ethane and ethylene from natural gas and from refinery gases for petrochemical uses. Removal of nitrogen from natural gas by low-temperature distillation has been proposed 7,20 as a means of increasing the capacity of existing gas transmission lines and of improving the marketability of the gas. Further application of low-temperature separation processes has been retarded by lack of data on the phase and volumetric behavior of mixtures at low-temperatures and at high pressures. This paper presents the results of determination of the phase and volumetric properties of 10 very volatile mixtures at temperatures from - 200 °F to above the critical point. These mixtures consisted of natural gases with methane and nitrogen. Generalized methods are presented for estimating the critical temperatures, critical pressures, and the densities of such mixtures. EXPERIMENTAL APPARATUS AND PROCEDURES The apparatus and the experimental procedures have been described in an earlier paper13. The method consists of displacing the mixture from a reservoir which is maintained at constant temperature and pressure into an agitated glass equilibrium cell which is maintained at constant temperature. The liquid level within the glass equilibrium cell was visually observed, and the pressure was measured to within & 3 psi with a calibrated Bourdon gage. COMPOSITIONS OF MIXTURES STUDIED The compositions of the mixtures studied are summarized in Table 1. The measured properties included in Table 1 will be discussed later in this paper. The sources of these gases are described below: Gas "A-1&apos;&apos; was obtained from the Phillips Petroleum Co. Its composition was reported in connection with earlier work." The properties of this gas were reported in an earlier paper.13 Gases "A-2, A-3, A-4" were prepared by mixing nitrogen with gas "A-1." Gas "AB-1" was prepared by mixing methane with gas "A-1." The properties of this gas were reported in an earlier paper.&apos;" Gases "AB-2" and "AB-3" were prepared by mixing nitrogen with gas "AB-1." Gas "B" was obtained by W. W. Bodle of J, F. Pritchard & Co. from the primary separator of a well in western Kansas. Gas "C" was obtained from a Cities Service Co. pipeline at Lawrence, Kans. Gas "D" was prepared by mixing gas "AB" with gas "C."

Jan 1, 1955

By E. A. Has, E. Mcl. Tittmann

Double roasting of sinter carrying a high percentage of lead concentrates, gave rise to the problem of removing the sheets of metallic lead formed in the wind boxes. The solution of the problem has been found in the water sealed wind boxes. The metallic lead is granulated and can be removed without seriously interfering with the operation of the machine and eliminates necessity of men going in wind boxes with air guns. THE practice of double sintering the charge for lead blast furnaces, which is now standard throughout the lead smelting industry, has introduced the rather difficult problem of cleaning the wind boxes on sintering machines used for the final pass. Two factors have more recently accentuated this problem: (1) the growing demand of workmen for better working conditions and less arduous labor, and (2) the growing dearth of crude lead ores and the improved grade of lead concentrates demand a charge carrying the maximum percentage of lead. One to 2 pct of such high lead charges (30 to 40) when processed on machines in reasonably good condition will pass through the grates and report in the wind boxes. One-half to three-quarters of this material will be metallic lead reduced by the coke breeze or other fuel mixed with the charge. This lead forms large cakes or chunks which are hard to remove and which substantially increase the time the machine is out of operation for cleaning the wind boxes. A high lead fall can reduce the operating time 30 pct. As a specific example, a 30 ft machine having 63 in. pallets, and equipped with three conventional wind boxes, requires 3 to 4 hr per day for removing the accumulation in the wind boxes when operated as a final pass machine. This same machine when operated on raw charge requires less than an hour per day for cleaning. To eliminate formation of large chunks of lead in the wind boxes of the final pass machines and time lost in cleaning the boxes, R. C. Rutherford of the Chihuahua smelter of the American Smelting and Refining Co., devised and patented* a wind box having a water bath to granulate the lead as it falls from the grate bars. Later, C. H. Harris of the San Luis plant made and patentedt an improvement on Rutherford&apos;s device in which the water bath seals the wind box in a manner permitting the latter to be readily cleaned without destroying the vacuum. The first machine to our knowledge to use the water bath box was at the Chihuahua plant along the lines of the Rutherford patent. In 1942, a machine was placed in operation at the El Paso plant which incorporated the features of both Rutherford and Harris. This machine is 40 ft long equipped with pallets 63 x 24 in., and having 4 wind boxes 10 ft 4 in. x 7 ft 2 in. x 51 ft 3 in. in size (fig. 1). The air from the fourth box is returned to the first three, and the gas from the first three discharged to a baghouse. The machine has conventional drive, discharge hopper,

Jan 1, 1951

By J. M. Oblak, R. F. Hehemann, R. H. Goodenow

STUDIES of surface relief and growth kinetics have lead to the concept that widmanstatten ferrite along with upper and lower bainite constitute a continuous series of decomposition products.1-4 Current models4 propose that these products form as plates with a coherent or semicoherent leading edge which propagates at a rate controlled by diffusion of carbon into the surrounding austenite. There are, however, important crystallographic and morphological differences between these products—particularly between upper and lower bainite. For example, upper bainite appears to exhibit a (11lIy orientation habit, whereas lower bainite develops with a more irrational habit near {2251y.5-7 Many of the morphological features of these decomposition products are not yet well-documented. Recent studiess have demonstrated that low-carbon martensites form as sheets of closely spaced needles on {lllly planes while higher-carbon martensites form as plates with {225}? or other orientation habits. The similarity in the crystallography of these two modifications of martensite with upper and lower bainite is striking. Therefore, a study of the morphology of bainite in a series of hypoeutec-toid alloy steels has been initiated to explore these relationships further. The question of immediate interest is whether upper and lower bainite form as plates or needles. A two-surface (approximately perpendicular) metallographic method was employed to study the morphology of bainite in a variety of low and medium alloy steels. Compositions of these steels have been reported elewhere. The behavior of 4340 and 4370 was typical and will be described here. Austenitizing treatments involved 20 min at 2350°F for 4340 and at 2000°F for 4370. Isothermal transformation was conducted in molten-salt baths. Upper bainite was produced at 925°F in the 4340 steel and lower bainite at 575°F in 4370 with transformation times adjusted to produce 10 to 15 pct of the decomposition product. Many of the morphological features of upper bainite have been catalogued in the recent literature.&apos;&apos; The two principal variants observed in the present investigation are illustrated in Fig. l(a). One form appears as long, thin plates or needles and the other as small, frequently irregularly shaped particles. Both variants may occur as isolated forms but more frequently appear in groups as demonstrated in Fig. l(a). Two-surface analysis reveals that these two variants constitute different sections through a single morphological form. To demonstrate this, a number of sections perpendicular to the plane of Fig. l(a) were prepared at various positions along the length of the elongated particles. A section taken at position 1 in Fig. l(a) is presented in Fig. l(b). Here, the dark line represents the edge of the sample and the left-hand portion of this photomicrograph is that from the surface perpendicular to the original plane of polish. Since it was necessary to repolish the original surface after each sectioning, the shape of the bainite particles on this surface, right hand side of Fig. l(b), changes with each sectioning. The disappearance of plate A, Fig. l(a), in Fig. l(b) emphasizes the small cross section of these structures. The group of particles in the lower left-hand

Jan 1, 1964

By J. P. Heller, H. B. Bradley, A. S. Odeh

It is an accepted procedure to represent oil field displacement problems in which the pressure is relatively constant by a potentiometric model. Variations in reservoir permeability thickness product are represented in the model by proportional variations in electrolyte depth. It is shown that significant errors are present wherever these variations are of such magnitude that the consequent differences in the electrolyte depth in the model or any regions therein are appreciable in comparison with their respective horizontal dimensions. To demonstrate the order of magnitude of this error, a hypothetical linear oil field in which permeability varies linearly with distance was treated both analytic.ally and by potentiometric model. The results obtained from the model are compared with the exact solution for various configurations of linear geometry. Deviations in flow times up to 11 per cent were observed. It is confirmed that these discrepancies can be reduced by increasing the areal scale and/or decreasing the vertical scale of the model. It is the purpose of this work to assist in the design of potentiometric models by indicating the relationship between this error and the chosen scale factors. INTRODUCTION The fundamental geometrical criterion which determines whether the pressure distribution in an oil or gas reservoir may be simulated in a conventional potentiometric model is the requirement that all reservoir parameters be constant along any vertical line between its upper and lower boundaries. This situation never obtains exactly; nevertheless, it is usually assumed that there is no permeability stratification within the section of interest, that all wells completely penetrate the sand, that there are no gravitational effects, and that variations in thickness of the sand are small compared to the horizontal extent of the field. In these ways the reservoir problem is reduced to two dimensions in which there is no variation of pressure in the vertical direction within the limits of the sand. Variations in sand thickness and/or horizontal pesmeability may be taken into account as described by Muskat, by considering the fluid conductivity of the reservoir in its horizontal plane to be proportional to the product of permeability and sand thickness. If the variations in sand thickness are small compared to the horizontal dimensions of the reservoir, then it is a good approximation to consider the reservoir problem to be essentially two dimensional. The same approximation, however, is made in the simulation of the assumed two-dimensional reservoir by the electrolytic model. The model, if it is to take into account variations of permeability-thickness product, must of necessity be made in three dimensions, that is, with variable depth. Most potentiometric model studies and theoretical treatments reported in the literature to date2,3,4,5,6,7,8 are those in which either an average permeability was used or a constant permeability was assumed. This is understandable since detailed permeability data are not usually available for the majority of reservoirs. Many investigators have recognized that the failure to incorporate permeability variations within a reservoir in model studies leads to serious error in predictions made

Jan 1, 1957

By J. P. Heller, H. B. Bradley, A. S. Odeh

A potentiometric model technique is presented for determining the areal sweep efficiency of a five-spot well pattern, at and beyond breakthrough. A sharp interface between displaced and displacing fluids is assumed. Although the prototype svstem is referred to as a waterflood operation, obvious changes in the notation and computations will adapt the results to other displacement processes. The results of the study include the following. 1. Areal sweep efficiencies for a five-spot well pattern, at and beyond breakthrough, for mobility ratios (displacing to displaced fluid) of 4:1, 2:1, 1:1 and 1:4. 2. Extension of potentiometric analysis to the investigation of the areal sweep efficiency beyond breakthrough in a five-spot pattern by the application of conformal mapping and conductive-solid models. 3. The use of layers of conductive fabric in representing mobility ratio changes in potentiometric models. 4. The development of a probe mechanism for probing conductive solids. The results obtained by conductive-cloth models agree with earlier areal sweep efficiencies at breakthrough obtained by Aronofsky and Ramey 1 on the potentiometric analyzer using electrolytic-tank models. Results beyond breakthrough differ from those obtained by the X-Ray Shadowgraph technique. Data from this study show that, for mobility ratios greater than one, water cut rises rapidly as fluid is produced after breakthrough. However, for mobility ratios smaller than one, a large increase in area swept resulted with only a small increase in water cut. INTRODUCTION In calculating reservoir performance of waterflood-ing operations and other fluid-injection programs, it is necesssary to estimate the areal sweep efficiency * before and after injected-fluid breakthrough into production wells. Influence of mobility ratio on oil-production history, before and after breakthrough for a five-spot well pattern, has been studied by X-Ray Shadowgraph techniques 2-5 and by gelatin models.6 In none of these investigations was the transition zone controlled experimentally. Steady-state anaiog techniques assume that a vertical and discrete interface exists between the displacing and displaced phase. Thus, when using a potentiometric analysis, it is assumed that no transition zone exists. To determine the areal sweep efficiency beyond breakthrough for a five-spot well pattern using the potentiometric analyzer, four principal problems had to be resolved. These were the following. 1. The laborious method of representing changes in mobility ratio in electrolytic tanks by means of contoured wooden blocks. 2. Vapcrization of the electrolyte solution during the study causing concentration changes and, thereby, variable conductivity. 3. The scale-limitation problem 7 that is accentuated by abrupt eiectrolyte depth changes. 4. A wellbore geometry problem. EXPERIhlENTAL EQUIPMENT AND PROCEDURES CONDUCTIVE-SOLID MODEL The theory, equipment and procedural techniques of the electrolytic-tank potentiometric model have been treaced excellently by Lee8 and by Muskat.9 By the use of a conductive solid to represent the fluid conductivity of the porous media, the need for contouring wooden blocks to represent mobility ratio was eliminated. It was found that a carbon-black coated fabric, Uskon D-16,** could be employed as a fairly uniform conductive media. This material, when stacked in appropriate layers and pressed together, can be used to represent changes in mo-

By T. P. Papazoglou, N. A. D. Parlee, W. C. Phelps

HE high vapor pressures of metals such as lead, calcium, lithium, bismuth, and magnesium at steel-making temperatures present experimental problems which have thus far rendered it almost impossible to obtain really reliable data for their solubilities in liquid iron. Many investigators have attempted to equilibrate liquid iron in the same crucible with the undissolved liquid phase of such volatile metals. The published results,l-6 although useful, are often questionable on the grounds of not being obtained under true equilibrium conditions. Such information is not always of practical value in any case since the equilibrium vapor pressure is often several atmospheres and steel is not currently made at these pressures. Solubility measurements at lower partial pressures (< 1 atm) appeared to be more practical and easier to make. These data could be used to calculate solubilities at other pressures where Henry&apos;s Law is obeyed, and to estimate solubilities under other conditions of temperature and pressure with useful accuracy. This note outlines the development of a general technique for the measurement of solubilities in systems of this kind. The method involves equilibration of the high-boiling metal at known temperatures with the vapors of a low-boiling metal at known partial pressures. Analyses of quenched samples provide vapor pressure-solubility data and make calculations of alloy thermodynamics possible. The principle involved is similar to the closed-system diffusion-transport method which is difficult to apply with most high-melting liquid metals like iron, due to closure problems. A two-zone horizontal (molybdenum wire element) tube furnace, Fig. 1, provides two constant-temperature zones in a reaction tuve (3/4 in. ID by 1 in. OD by 36 in.). A high-boiling metal sample, 9, introduced in the higher-temperature zone, is maintained at temperature T1, and a volatile metal sample, 7, in the lower-temperature zone, is held at T2. A stream of argon with 10 pct hydrogen is passed via flowmeters, 1, and mixing-drying towers, 2 and 3. through the reaction tube at a favorable flowrate and acts as a carrier gas which entrains vapor from the volatile liquid metal at a specific constant partial pressure. The gas mixture passes through a system of constrictions, 6 and 8, to the higher-temperature zone, establishes intimate contact with the high-boiling liquid sample, 9, and exits through a small condenser tube. The entire system is at (nearly) atmospheric pressure and the volume of carrier gas passed is measured with a wet gas meter. When the high-boiling sample attains equilibrium with the vapor phase, both samples are removed and quenched. Analysis of the high-boiling sample for solute content reveals its solubility for the low-boiling metal at a vapor pressure calculated from carrier-gas volume and either a) weight loss of volatile metal or 6) weight gain of high-boiling sample plus condenser (which collects the undissolved vapors). To test the capabilities of the method, liquid silver at 1403&apos;C was equilibrated with lead vapor at various partial pressures. The relatively simple Pb-Ag system was particularly suitable for uncovering experimental problems and providing the first step toward investigations with more volatile metals and more difficult combinations.

Jan 1, 1965

By Bernt Ellingsaeter, Terkel Rosenqvist

IN the silicothermic reduction of magnesia, burned dolomite is treated with high grade ferrosilicon in an evacuated steel retort at temperatures between 1150° and 1200°C. The following reaction is assumed to occur MgO + CaO + 1/2 Si (Fe) - Mg(g) +- & Ca,SiO, + Fe with the equilibrium constant on the basis of thermodynamic data for the substances involved and assuming unit activity for all solid constituents, Kubaschewski and Evans&apos; calculated the magnesium pressure as a function of temperature logp,, (mmHg) = 15.06-1.61 T- log T- 13,16O/T. Pidgeon and King," who measured the magnesium pressure by means of a flow method, found values about three times the calculated ones. This may be caused by uncertainties in the thermodynamic data, but may also be caused by the formation of other reaction products, such as Ca,SiO,, which is known to be the stable silicate in equilibrium with lime. Whatever the exact reaction may be, it is evident that as long as all other factors are maintained constant the magnesium pressure will vary with the silicon activity, viz: p,, = &,. (p,,) ", where (p,,)" is the magnesium pressure by the reduction with silicon of unit activity. In the present investigation, p,,, was therefore measured for various grades of ferrosilicon and their silicon activities were calculated. The experimental method was similar to that used by Pidgeon and King. Briquettes of burned dolomite and Fe-Si alloys were placed in a 1 in. heat resistant steel tube and were heated to 1200°C. By means of a flow of purified hydrogen, the magnesium vapor was swept into a condenser filled with steel wool. From the amounts of hydrogen used and magnesium condensed the magnesium partial pressure was calculated. First a tube of 28 pct Cr steel, and later a tube of Kanthal D (a ferrous alloy with 22.6 pct Cr, 2 pct Co, and 4.5 pct Al), was used as a heat resistant tube. The latter tube showed the best heat resistance. The dolomite used had the following composition: 43.6 pct MgO, 55.5 pct CaO, 0.2 pct K,O + NalO, 0.2 pct Fe,O,, and 0.3 pct insoluble. The ferrosilicons were prepared from 98 pct Si of technical grade (0.7 pct Al, 0.3 pct Ca, and 1 pct Fe) by melting with various amounts of electrolytic iron of high purity. The alloys thus obtained were analyzed on their iron and silicon contents, which added up to between 99 and 100 pct. The amounts of reactants were chosen so that there would always be an excess of the oxides, and the average decrease in silicon content during the experiments would be about 1 pct. Most of the reaction occurred in the part of the reaction mixture facing the gas flow. The change in the silicon concentration in the part facing the condenser was, therefore, negligible. To facilitate the reaction, about 1 pct fluorspar was added to the briquette mixture. Fluorspar does not enter the reaction, but is known to act as a

Jan 1, 1957

By R. D. Pehlke, J. V. Gluck, R. L. Louvet

A study has been made of the effect of small additions of bismuth on the activity of zinc in dilute solution in molten tin. Free-energy interactions have previously been determined between zinc and various third elements where the solvents were molten bismuth or molten lead.&apos;-4 In both of these solvents, the activity of zinc exhibits a strong positive deviation from ideal behavior (at 550°C y° for zinc in lead is 11.4 and for zinc in bismuth is 3.0). The present work, using tin as the solvent, is an extension to a case where the positive deviation is considerably diminished (y°Zn at 550°C is 1.63). Several previous investigators have studied the Zn-Sn binary system; however, little data is available in the range below 0.1 mole fraction zinc.5= Previous high-temperature galvanic cell studies in the Sn-Zn-Bi ternary system included the determination by Gluck and Pehlke of interactions in the bismuth-rich corner1 and separate investigations of the central region by Oleari and Fioriani6 and by Ptak and Moser.7 Yokokowa et al.8 conducted Knudsen effusion studies in the central region; however, their experiments at 625°K were conducted somewhat below the present experimental temperature range. Their results indicated an increase in zinc activity with the addition of bismuth. The present series of experiments was conducted in galvanic cells represented as follows: Zn Zn++ in LiCI-KC1 eutectic Zn + Bi in Sn (pure reference (fused salt electrolyte) (molten alloy) standard) The experimental apparatus. a multi-electrode system employing alumina crucibles and contained in a Vycor tube under a helium atmosphere, has been described previously, as have been the experimental procedures, precautions, and the methods of data reduction.1-4,- The experimental measurements were made over the range from 450° to 650°C. Between thirty and forty measurements were made in each run. The linearity of the electromotive force vs temperature relations was verified by linear regression techniques. The correlation coefficients exceeded 0.99. The experimental results summarized in Table I include the interpolated electromotive force at 550°C and the temperature dependence of electromotive force. Only results from stable and consistent cells containing more than 0.025 mole fraction zinc are reported. Attempts to run cells at 0.01 or 0.02 mole fraction zinc were not satisfactory. This is attributed to the closeness of the free energies of formation of the chlorides of tin and zinc. Calculations employing Wagner and Werner&apos;s criteria for displacement reactions10 indicated that reduction of the zinc content to 0.01 mole fraction places the cell near the borderline concentration for a 1 pct error in measured potential. The compositions shown in Table I are the actual weighed-in amounts. Previous experience has indicated that compositional changes during the running of a stable cell are negligible.&apos; Over the range of compositions studied for the binary alloys, the activity coefficient of zinc was essentially constant indicating that Henry&apos;s law is followed to 0.05 mole fraction zinc. The temperature, OK, de-

Jan 1, 1969

By W. C. Hagel, J. H. Westbrook

THERE has been a recent revival of interest in the intermetallic compound AgMg as an experimental material for study of the physical and chemical properties of simple ordered structures. Studies of mechanical behaviors,1-4 diffusion,5,6 and thermo-dynamic properties7&apos;8 have been reported. In several of these studies, heat treatments have been carried out in argon-filled silica capsules at temperatures as high as 750°C with no apparent adverse effects. The present authors were, therefore, startled to discover in the course of some yet unpublished work, that gross melting of near-stoichio-metric AgMg compositions occurred in such samples more than 100 deg below their melting point of about 800°C. This note is to report a brief series of experiments carried out to establish the reason for this behavior. Gross errors in sample composition and failure of furnace temperature controls were quickly eliminated as causes of melting. The first tangible lead came from chemical analysis of an AgMg sample which had melted during treatment at 750°C. A silicon content of 3.3 wt pct was found. Since satisfactory analyses had been obtained on the original as-cast ingot, contamination by diffusion and/or reaction with the fused silica capsule seemed a distinct possibility. A perplexing fact, however, was the apparently capricious incidence of the effect. Not only was it previously unknown, even in the experience of the present authors; but, in the early part of the present study, melting sometimes occurred and sometimes not with specimens treated under constant conditions. Indeed, one sample successfully survived a 750°C heat treatment and yet melted completely during the course of a subsequent anneal in an identical capsule at a lower temperature. To obtain evidence that silicon contamination could lower the melting point to the extent observed, the following experiment was performed. A series of ternary alloys was made up with a stoichiometric AgMg base and containing 0.1, 0.2, 0.4, 1, 2, and 4 wt pct Si. Melting was done in MgO crucibles under a cover of argon gas. After holding 10 to 20 min in the temperature range 850° to 900°C, the alloys were allowed to solidify in the crucible and the temperature during cooling automatically recorded with a Pt/Pt-10 Rh thermocouple. Results from the cooling curves are shown in Fig. 1. Checks within 2 to 5C° were obtained upon repeated melting, cooling, and freezing. The whole series of cooling curves as well as metallographic examination of the melted alloys established that the AgMg rich portion of the AgMg-Si quasibinary is an eutectic-type system. The melting point of AgMg is lowered from approximately 820°C in the pure stoichiometric binary9 to about 710°C in the saturated intermetallic phase. Since second phase was observed in all samples on cooling to room temperature, the solid solubility of AgMg for silicon evidently falls rapidly with decreasing temperature as indicated schematically by the dashed solvus in Fig. 1. It is thus established that a silicon content

Jan 1, 1963

By E. T. Stephenson

Wert and Marx1 pointed out that a straight-line relationship exists between the activation energy of a relaxation process and the temperature at which the maximum relaxation occurs. The data available at the time indicated that this relationship held for a number of Snoek peaks, several grain boundary peaks, and pair relaxation in a brass. Theoretical justification for the observed relationship was found in the following equation, which Wert and Marx derived from the theory of interstitial atomic diffusion coefficients:&apos; where AH is activation energy, R is the gas constant, T is the internal friction peak temperature, v is the interstitial atomic frequency, f is the frequency of the applied stress, S is entropy of activation. More accurate internal-friction data on interstitial diffusion in bcc metals have become available since Wert and Marx&apos;s paper. Table I gives activation energies calculated by several authors from a combination of elastic aftereffect data and the peak temperatures at several frequencies of measurement. (In the case of Fe-C and Fe-N, the referenced authors5&apos;7&apos;8&apos;10 also used high-temperature diffusion data.) However, diffusion experiments at 150°C and above1&apos;-13—rather than anelastic techniques—were used to determine the activation energy of hydrogen diffusion in Fe-H. In order to plot this recent data as a AH vs T graph we calculated the peak temperatures of the systems listed in Table I (with the exception of Fe-C, Fe-N, and Fe-H) by using published values3&apos;&apos; of AH and Do. These calculated peak temperatures varied by only a few degrees from experimentally determined peak temperatures. The calculated values were felt to represent the better average. A number of investigators have found the peak temperatures in Fe-C and Fe-N to be 38 to 40°C and 20° to 24°C, respectively. The values of 39" and 22°C (312° and 295°K in Table I) were determined by carefully executed experiments.6&apos;8 The hydrogen peak temperature has been measured at 1 cps,12 20 cps,14 and 35,000 cps.15 All hydrogen peak temperatures were adjusted to 1 cps for Table I using AH = 3000 cal per mole. As Fig. 1 shows, the data of Table I fit a straight line at least as well as the earlier data used by Wert and Marx. Linear-regression analysis was applied to the data in Table I. The Fe-H data was omitted because the activation energy has not been experimentally determined in the temperature range of the peak. The analysis yields the equation: with a standard error of 860 cal per mole. The agreement of the data in Table I with the Wert-Marx equation is excellent. Strict application of Eq. [I] forces the linear regression analysis through the origin. In this case, the analysis gives a slope of 62.1 cal per mole per deg, and a standard error of *890 cal per mole. With this value, it follows from internal-friction theory that Hence, Do varies by only 30 pct among these bcc-interstitial systems. Thus, a concept suggested originally by Wert and Marx1 is confirmed by recently published data. The

Jan 1, 1965

By J. S. Dodge, I. M. Krieger

The laminarturbulent transition was studied for monodisperse rigid polymer latices as functions of particle diameter and concentration at several tube diameters. Breaks in the graph of friction factor US Reynolds number were used to characterize the transition; rates of shear were sufficiently high so that Newtonian behavior at the high shear limiting viscosity could be assumed. No abnormal behavior was noted at concentrations below 30 volume percent. At higher concentrations, suppression of turbulence was observed with critical Reynolds numbers rising to as high as 5,500 at 50 volume percent. No definite effect on the transition was noted due to variation of particle size or tube diameter. The type of surfactant used to stabilize the latex was found to have an important influence on the critical Reynolds number. INTRODUCTION For some polymer solutions and solid-in-liquid suspensions, the transition from laminar behavior to turbulence in pipeline flow has been reported to take place at unusually low1-5 and in some cases at higher than normal6,7 critical Reynolds numbers. Extreme values of critical Reynolds numbers (NRe*) have been found to range from 1 to 6,000, as opposed to the values of 2,000 to 3,500 which are obtained for ordinary liquids. Observations have also been reported of drag reduction in fully developed turbulent flow, i.e., a decreased value of the friction factor in the Reynolds number-friction factor plot6*10-14 in colloidal and polymeric fluids. In some cases, turbulence suppression (unusually large values of Nre*) was noted to occur preceding the drag reduction,6 while a normal transition was noted in other cases of drag reduction.14 To relate the occurrence of turbulence suppression and drag reduction to the molecular or particulate structure of the fluid, it is desirable to characterize the structural variables with some precision. For most colloidal dispersions and polymeric fluids, this is very difficult; particle sizes, shapes and stiffnesses may vary over wide ranges in the same sample. Recently, however, a colloidal fluid has become available which consists of rigid spherical particles of highly uniform diameter dispersed in a simple Newtonian liquid. These are monodisperse polymer latices, prepared by carefully controlled emulsion polymerization reactions. The purpose of this research was to study the transition to turbulence in these well-characterized colloidal fluids as a function of concentration, particle diameter and tube diameter. Typical flow curves of latices of high solids content are shown in Fig. 1. While these curves were obtained with monodisperse latices, the general shape of the curve is also typical of a polydisperse latex. It is observed that a shear-thinning region occurs for low to moderate rates of shear. At sufficiently high shearing rates a limiting Newtonian viscosity is reached. The viscosity µ diminishes with decreasing volume fraction 4 at all shear rates. For 4 less than 0.25, latices are Newtonian at all rates of shear.15 An increase in average particle size (at a given extends the Newtonian viscosity region to lower rates of shear. A third factor which influences the

By S. I. Liu

THE effects of strain histories, consisting of several prestrains in opposite directions, on the flow and fracturing characteristics of metals determined in a final test have been investigated previously.&apos;" Such strain histories vary from a single prestrain in tension or compression to the number of strain cycles leading to fatigue failure.&apos; Between these two limits, various strain histories could be visualized and some can be attained readily. One such example is a strain history consisting of a first prestrain in tension of various magnitudes and a second prestrain in compression also of various mag-nitude. In this investigation the strain history was extended to the combination of these two limits, i.e., a single prestrain in tension or compression followed by balanced strain cycles of a selected magnitude e, = k0.12. It was found in this case that only compressive initial prestrains could be investigated with sufficient accuracy.* Such strain histories can be considered also as (low cycle) fatigue tests of a metal subjected to various amounts of cold working. It appears from previous publications that cold working within a wide range of reductions usually raises the un-notched fatigue strength of many metals.&apos;-&apos; This effect, however, has been found to be inconsistent and sometimes reversed for other metals?.7 Furthermore, Ludwik reports that the yield strength of cold-worked specimens may be reduced by cyclic strains, while that of materials without cold work is generally increased in the initial cycles." " In addition to the above tests, a study was made of the effect of intermediate re-solution heat treatment on low cycle fatigue behavior. Such anneals should eliminate the strain hardening induced by the cyclic strains. As far as their effect on the fracture characteristics is concerned, a few previous tests seemed to indicate that the damage resulting from cyclic strains is retained only partially after heat treatment." A further investigation was made in which one specimen was subjected to repeated unbalanced tension cycles in which the strain interval was approximately $ 0.013. This repetition of plastic tension damages the material slightly. This result appears to confirm Ludwik&apos;s observations." " Commercial 3/4-in. rod of the aluminum alloy 24ST4 was selected for this investigation. The material was subjected to the following treatments before machining: 1—Re-solution treatment at 920" ± 10°F for 45 min, 2—water quench at room temperature, and 3—aging for four days at room tem-perature.? The treated material then was machined to desired specimen contour and tested. A coolant was used during machining to minimize any artificial aging effects of heating during machining. In some cases the 24ST4 specimens were reheat treated after having been strained. In these cases, the heat treatment was the same as the re-solution heat treatment described above. Procedure As shown in Fig. 1, threaded end specimens with a minimum diameter of 0.266 in. and a contour radius of 2 in. were used for prestraining to an axial compressive strain ranging from 6, = —0.10 to E, = —0.48. For large prestrains, two consecutive corn-

Jan 1, 1952

By Robert C. Linares

Cubic zinc sulfide has been grown from molten salt solutions substantially below the hexagonal-cubic phase transition of 1020°C. Crystals free of birefringence have been grown from molten lead chloride at temperatures from 500° to 800°C. Factors affecting the optical transmission and the birefringence are discussed. CUBIC zinc sulfide is of interest for electrooptic devices and as an optical coating material. However, it cannot readily be produced as large crystals which are free of birefringence. The birefringence arises from the fact that the cubic ZnS is usually grown as the high-temperature hexagonal phase and is transformed to the lower cubic phase by annealing.&apos; This results in stacking faults, stress, and birefringence. A requirement for the growth of cubic ZnS is that it be grown below the phase transition of 1020°C.2 Crystals of cubic ZnS have been grown below 1020°C by the hydrothermal,3 flux,4 and vapor transport5 techniques. However, these all appear to have limitations in size or quality of material produced. It was felt that a new flux method might have a good chance of overcoming some of the previous problems. Mita6 reported the growth of hexagonal ZnS from molten NaCl and wilke7 reported the growth of iron sulfides from molten lead chloride solution, indicating that molten chlorides make good solvents for sulfides. An investigation of a number of possible molten chlorides as solvents showed that molten PbCl2 has an appreciable solubility for zinc sulfide and that crystals can be grown at temperatures from 500° to 800°C. EXPERIMENTAL Crystal growth was performed in open or sealed Vycor or fused silica tubes, in an argon atmosphere or vacuum. There were no deleterious effects due to using vacuum; however, a sealed essentially isothermal system must be used to prevent vapor transport mechanisms from dominating. This will be discussed later in detail. Noble metal containers were not usable as they were severely attacked by these melts. The materials used were: reagent-grade PbC12, reagent-grade ZnS, optical-coating-grade ZnS, and Irtran 2 (ZnS). Crystal growth was accomplished by both slow cooling techniques and gradient growth techniques. In the slow cooling techniques, 15 g of ZnS and 100 g of PbCl2 were used. The components were placed in the silica tube, heated at 800°C for 2 hr, and then slowly cooled (l° to 10° C per hr) to 500°C. The furnace was constructed so that the tube could be inverted, thus allowing the liquid to drain off the crystals at the end of the run. The gradient runs were made by placing the above mixtures in a silica tube at 550° to 600°c, Fig. 1. A temperature gradient was maintained such that the floating mass of undissolved sulfide was 10° to 50°C warmer than the bottom of the tube. Growth occurred on spontaneously nucleated sites at the cooler bottom. RESULTS When using high cooling rates (5° to 10°C per hr), crystals form in thin sheets perpendicular to the {111} face. Crystals 5 by 5 by 1.2 mm, Fig. 2, have been ob-

Jan 1, 1969

By M. K. Yen, W. R. Hibbard

Previous studies of plastic deformation of metals have emphasized the important role of bending and constraints during strain under relatively pure stresses.1"5 Some new phenomena such as early conjugate slip6 and polygonization7 are intimately concerned with the relief of bending stresses, the former by slip and the latter by a process analogous to re-crystallization. However, few analyses of the bending deformation of single crystals were found in the literature, and those8,9 are sufficiently previous to the modern interpretations of slip to invite further investigation in this area. The transverse bending mode of testing, using the two-point loading method, was selected because the center portion of the specimen may be considered as under a theoretically pure bending stress with a uniform bending moment. Considerable attention was given to both the lattice distortion and flow characteristics of the crystals during deformation. Experimental Proeedare A specimen under the action of equal and opposite couples at both ends is said to undergo pure bending. The shear and moment diagrams of a specimen under the two-point loading method of transverse bending are shown in Fig 1. The moment over the middle-third of the span is equal to PL/6, and the vertical shear is zero. Fig 2 (A) illustrates the stress distribution in the elastic range on a plane across the middle of the specimen. It can be seen that the normal stress has a maximum value at the extreme surfaces on the tension and compression sides, and decreases proportionately to zero as it approaches the neutral plane. However, when the plastic range is reached, the stress distribution is no longer a straight line relation, but changes in a manner which can be best illustrated as shown in Fig 2(B). The following calculation and stress analysis are mainly in accordance with the works reported by Timoshenkol0 and Kochendörfer.9 From the simple beam formula, the maximum normal stress will occur at the surface of the specimen. For a round specimen with a radius r and for a rectangular specimen with a height 2h and width 2b, the maximum normal stress, Sp, will be given by the following formulas: For round specimen: 2PL Sp = 3pr3 [1] For rectangular specimen: Sn = 8bh2 [2] Since it is reasonable to consider that slip takes place under the same conditions as in uniaxial loading, the resolved shear stress S?, along the operative slip direction will be as follows: For round specimen: 2PL sin x cos ? Sp = 3pr3 sin x cos ? [3] For rectangular specimen: PL S8 = 8bh2 sin x cos ? [4] where X is the angle between the specimen axis and the slip direction and X, the angle between the specimen axis and the major axis of the glide ellipse. It was also reported by Kochenclorfer9 that the critical bending moment, that is, the bending moment exerted on the specimen to initiate slip, should be higher than the value given by the equations stated above. Based

Jan 1, 1950

By W. M. Lehrer

RECENT development of high-temperature brazing alloys has required information regarding the eutec-tic temperature and composition of the Pd-rich section of the Pd-B system.. Literature on this subject was found to be scanty with no complete system yet determined. Buddery and welch1 report an inter-metallic compound occurring in the Pd-B system at 6.33 wt pct B (PdsBz). Another source, Sieverts and Bruning,2 indicates that after annealing at 700°C, a 1.6 and a 2.0 wt pct B alloy were two phase whereas a 0.75 pct B alloy was single phase. Recent work3 using a hot-stage microscope has proposed a eutectic temperature of 743OC. This method utilized the observation of the onset of incipient melting at grain boundaries. The eutectic composition, however, was not determined. METHODS AND PR0CEDURES Five alloys were prepared by triple inert arc-melting high-purity palladium (95.98 pct) with additions of 2 to 6 pct purified amorphous boron. The alloys were crushed within a hardened steel mortar with a steel pestle. The 2 pct alloy, however, was too tough to be crushed in the above manner so was crushed by successive reductions through a rolling mill. Approximately 17 to 18 g of the crushed alloy was used in the thermal analysis. The alloys were melted in pure quartz crucibles. The thermocouple protection tubes were also of quartz and fused along the inside wall of crucibles to prevent floating of the thermocouple. This was an expediency as centering of the thermocouple in the melt would have been preferable. Melting was done in a tube furnace with a slow flow of tank helium maintained as a protective atmosphere. Heating and cooling rates were maintained at 3.5OC per min through the critical temperature ranges by means of a synchronous motor hook-up to a furnace controller. All specimens were heated to 100°C over the indicated liquidus on heating prior to reversing to the cooling cycle. Specimens emerged from the furnace with mirrorlike brightness attesting to the protective quality of the helium atmosphere. Thermal arrests were detected by the differential thermocouple technique using chrome l-alumel couples and nickel as the reference specimen. Arrests were recorded on a Leeds-Northrup automatic X-Y recorder. The specimen temperature and temperature difference were read to + 7.5OC and ± 1.5OC, respectively. These readings were well within the sensitivity of the instrument amplifier. Chromel-alumel couples were used in lieu of Pt-Rh as very few arrests were contemplated in excess of 1200" to 1300°C, the approach of instability. No standardization was performed on these thermocouples subsequent to their use. RESULTS The thermal arrest temperatures obtained are plotted in Fig. 1 as a function of wt pct B. The composition function was obtained by chemical analysis of portions of the specimens after the thermal analysis was completed. The 2 to 6 pct nominal alloys were found to have 1.80, 2.35, 3.65, 4.18 and 5.90

Jan 1, 1960

By Whitman E. Brown, Louis J. Erck

The installation in 1948 of a Hum-phrey~ spiral concentrator section at the Hill-Trumbull plant of The Cleve-land-Cliffs Iron Co. is the latest commercial method on the Mesabi Range being used for the recovery of fine iron ore. In two stages of concentration 84 spirals treat approximately 120 long tons per hour of minus ? in. ore. These spirals augment the production of the heavy-density plant which recovers the plus 36 in. iron from the plant crude ore. Structure of the ore is such that, when crushed, about 50 pct of the plant crude is minus ? in. size. After de-sliming in a 66 in. Akins classifier, grinding the classifier product in a ball mill and again desliming in a 78 in. Akins classifier about 15 pct of the crude ore remains to be treated in the spiral plant. Overall recovery of the ball mill feed in the Hill-Trumbull spiral plant during the 1948 season was about 53 pct of the weight and 66 pct of the total iron content. Of the actual feed delivered to the spirals from the 78 in. classifier 64.9 pct of the weight was recovered containing 73.7 pct of the total iron. The average analysis of the spiral concentrate is 55.05 pct Fe and 14.83 pct SiO2. An average of mill assays during the 1948 season is given in Table 1. The Hill-Trumbull plants treat both wash ore and jig-type ore. During the 1948 season spirals were used only on the fine sizes of jig-type ore. At times the deslimed minus ? in. size is of sufficient grade to warrant bypassing the spirals but in the main the fine size is delivered to the 48 first stage spirals and thence to the 36 cleaner or second stage spirals. In the past several years numerous Mesabi Range ores in the fine size cate- gory have been tested by a wide variety of beneficiating equipment. The prodigious amount of research devoted to the recovery of values in the fine ore reflects the dire need of the iron industry to squeeze the last possible unit of iron from the mined ore and to develop suitable equipment and processes to satisfactorily concentrate the leaner horizons as they are encountered in the process of mining. Large governmental and private appropriations have been allotted, new laboratories built, research and technical staffs increased, and operator-manufacturer cooperative agreements applied to hasten the solution of the problem. The University of Minnesota, at its Eighth Annual Mining Symposium in January 1947, dedicated as its objective the bringing to light of technological developments in iron ore beneficiation. Papers were given at that time relating to processes being developed. Specifically, these papers reviewed flotation, Baum jig, selective media concentrator, Hardinge concentrator, Dorrco sizer, heavy media concentration, Hydrotator, and the Humphreys spiral. The Cleveland-Cliffs Iron Co., after encouraging results from tests in a small pilot plant using one full size spiral, made the first commercial installation of Humphreys spirals on the Mesabi Range at their Hill-Trumbull mine, Taconite, Minn. This company

Jan 1, 1950