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By A. Vignes, J. P. Sabatier

A study of ternary diffusion at 1315°C in the Fe-Co-Ni system covering the entire ternary phase diagram has been carried out. Experimental values of the four interdiffusion coefficients DFeNico,DFeCoCo, DFeCoNi were computed at 33 points of the ternary diagram. The limiting values of these coefficients on the three sides of the ternary diizgram have also been determined. This set of data is presented as a contour map on the ternary isotherm for each of the four coefficients. Assuming that the Fe-Co-Ni system can be considered as ideal, the phenomenological coefficients Lk ij (with k = Fe) have been computed and the Onsager reciprocal relutions verified. It is shown that, in the Fe-Co-Ni system, the diffusion process can also be described by only two interdiffusion coefficients DFeFe and DCoNiFe, the second cross diffusion coefficient DCoFeNi being equal to zero and the second direct difusion coefficient being given by The values of the cross interdiffusion coefficients and of the Onsager coefficients are explained in terms of atomic mobilities of the three components with the help of a kinetic calculation due to Lane and Kirkaldy.8 It is shown that all the results are explained if the tracer difusion coefficients of the three components are such that DFe > DNi ~ DCo in complete agreement with experimental data on the three binary systems. DIFFUSION in a ternary alloy system is basically and significantly different from diffusion in binary alloys. In binary diffusion, there is just one independent composition variable and only one coefficient Dij is needed to describe the interdiffusion process. In ternary diffusion, we must allow for cross interaction between two independent species, and four interdiffusion coefficients are necessary to describe the transport process. Kirkaldy et al.1,2 have determined interdiffusion coefficients in the systems, Cu-Mn-A1 and Zn-Cu-Al. Guy and Leroy4 have reported intrinsic diffusion coefficients for the r phase at 1300°C of Co-Ni-Cr alloys as a function of composition using the analysis of Philibert and Guy.3 Interdiffusion coefficients were measured at three different compositions at 850°C in the single phase copper-rich corner of the Cu-Zn-Mn system by Dayananda and race.5 Zie-bold and Ogilvie6 have determined interdiffusion coefficients in the single-phase field of the Cu-Ag-Au system at 725°C. Preliminary results on diffusion at 1136°C in the system Fe-Co-Ni have been reported.7 In this study, data are reported on a more complete determination of interdiffusion coefficients in the Fe-Co-Ni system in the entire ternary at 1315°C. There is complete solid solubility with the fcc structures at 1315ºC, and this system can be considered as nearly ideal. This approximation allows the computation of the Onsager phenomenological coefficients. These values can then be used to test a kinetic calculation of the Onsager L coefficients in ternary substitutional solid solutions due to Lane and Kirkaldy.8

Jan 1, 1970

By C. E. Westley, R. R. Beebe

Recent works by Plaksh et al.,1,2 Glembotsky,3 and others have renewed interest in the effects of oxidation on the surface activity of the sulfides. Since considerable supporting data are available on galena-potassium ethyl xanthate, this system is being studied at South Dakota School of Mines and Technology by contact angle measurement, using the technique of McGlashan and McLeod.4 The contact-angle method is well adapted to investigation of the influence of small amounts of oxygen on the establishment of a stable contact angle on galena in potassium ethyl xanthate solution. Samples of massive galena containing less than 0.001 pct Cu, 0.001 pct Ag, and 0.01 pct Zn are mounted in castable plastic and ground and polished manually in a glove box containing the desired proportions of oxygen and purified nitrogen. Oxygen and nitrogen contents of the test atmosphere are determined with an Orsatt analyzer. In this way a reproducible surface is created in contact with whatever oxygen concentration is desired. Water and all reagents are prepared and stored in the test atmosphere. An absorbent is used to control carbon dioxide that might be present. Final polishing is done with levigated alumina on a glass plate. The prepared sample is placed in the test solution and transferred to the contact angle apparatus in a sealed box, and the test is conducted while both sample and solution are maintained under a slight positive pressure of the test atmosphere. Table I gives the results of contact angle measurements made at various 02-Nz concentrations.5 Each value of contact angle is the average of at least six individual measurements made with different bubbles at different locations on the sample surface. A period of 20 to 25 min has been found by preliminary tests to be sufficient to permit develop- ment of maximum angle, and all measurements are made after at least this much time has elapsed. Exposure of prepared samples to pure water under the test atmosphere before exposure to the xanthate results in a small but measureable and consistent reduction in contact angle. This is particularly true in the oxygen-deficient atmospheres; for example, at 2.2 pct O2 such water contact reduces the average angle about 8" from that obtained by immediate testing in xanthate. The general trend of increasing contact angle with increasing oxygen concentration corresponds to the results of Plaksin et a12 The absence of diminish-ment of contact angle at very high oxygen concentration has been attributed to the high concentration of xanthate per unit of galena surface: At oxygen concentrations below 1 pct (the limit of accuracy of the Orsatt analyzer), no contact angle is obtained. Furthermore, no contact angle is obtained at any oxygen concentration in the absence of xanthate. This result seems to be in disagreement with those cited by Plaksin.1 Further work on the interaction of galena and potassium ethyl xanthate or a similar collector as influenced by oxygen is contemplated. The true nature of the interrelation is as yet unknown. For example, it is not known whether the governing oxygen reaction is with the mineral, with the reagent, or with both.

Jan 1, 1961

By Arch J. Alexander

COAL is produced, in commercial quantities, in thirty-five of the sty-five counties of West Virginia. Oil and gas are produced, commercially, in forty-two counties. So, you may readily see that coal, oil and gas are closely related as to production areas. Many of the West Virginia coal mines are studded with oil and gas wells, as drilling has been done in thirty-two of the coal bearing counties. When the drilling of oil and gas wells was placed under the regulatory control of the Department of Mines on June I, 1929, it was estimated, by the State Geological Survey, that 64,000 wells had been drilled in West Virginia and that 34,mo wells were then being operated as oil and gas producers. No records of many of these remaining 30,000 abandoned wells exist and some of them remain a standing menace to safety as our coal extraction continues. Of a total of 13,100 new wells drilled since June 1929, approximately 5,200 have been drilled through coal measures. Approximately 7,000 wells, which were drilled through coal measures, have been abandoned in the same period of time. Many of these wells were drilled prior to the enactment of the oil and gas laws. Prior to the enactment of the Oil and Gas Law, which established the Oil and Gas Division of the Department of Mines in 1929, there had been several mine explosions attributable to cutting into un- charted wells and the improper plugging of other wells. The most serious explosion was that of Mines No. 47 and No. 49 of the Consolidation Coal Co. in Marion Co., when one of the so-called plugged wells leaked or seeped through some 80 ft of strata to the coal bed elevation, filling the mine with gas, the gas being ignited, killing a good many men and wrecking two coal mines. Legislation, to combat well hazards to coal mines, was slow in coming. In 1928, R. M. Lambie, then Chief of the Dept. of Mines, got sufficient support from coal, oil and gas interests to get the legislature to pass our present oil and gas laws. These statutes not only protected the coal industry but went a long way toward conserving the oil and gas resources of our state. Before drilling for oil or gas on any tract of land, known to be underlaid with one or more workable seams of coal, the well operator is required to submit a map of the area showing the location of the proposed well, and to send a copy to the Dept. of Mines and a copy to the coal operator. If no objections to the location of the proposed well are made by the coal operator within ten days, a drilling permit and a number for the well are then issued and work may proceed. If, however, the location of the proposed well is objected to by the coal operator, on the grounds that the location of the well will interfere with present mine operations, projected workings, or other- wise Cause a dangerous condition, the operator may file a written objection with the Dept. of Mines.

Jan 1, 1948

By L. A. Rapport, J. R. McCord, W. P. Drews, K. H. Coats

Water movement about an oil or gas reservoir can be predicted provided an aquifer influence function is known. This function is generally determined from an electric analyzer study or by fitting an idealized mathematical model to field data. A prohlem arises in determining that influence function which best reproduces field data and satisfies certain smoothness requirements, without making any idealizations concerning aquifer geometry and heterogeneity. This study shows the problem to be solvable through the linear programming technique and presents applications to one oil reservoir and two gas storage reservoirs. In addition, a theorem is stated and proven which confirms influence junction smoothness requirements heretofore accepted on physical intuition and establishes additiotzal smoothness constraints formerly not recognized. INTRODUCTION The pressure decline accompanying production results in water encroachment into oil and gas reservoirs situated adjacent to aquifers. The importance of this water movement derives from the significant dependence of production rate upon reservoir pressure and of pressure, in turn, upon water encroachment. Pressure and rate of water movement are uniquely related through an "influence" function which may be in the form of reservoir pressure response to a unit water encroachment rate or of water movement caused by a unit reservoir pressure drop. This influence function reflects the heterogeneity and geometry of the aquifer and is therefore particular to each reservoir. If the influence function is known, then reservoir pressure may be predicted from a production rate schedule, or vice-versa, with the aid of the material balance equation which relates water influx to reservoir production and pressure. The problem of determining this influence function for a given reservoir has been approached in three different ways. Van Everdingen and Hurst calculated and tabulated certain influence functions pertinent to idealized mathematical models which satisfy simplifying assumptions such as aquifer homogeneity and elementary reservoir-aquifer geometries.' Other studies developed additional tables for a variety of elementary reservoir-aquifer geometrical con- figurations and demonstrated their validity and utility.:' Hicks, et al. described the use of an electrical network to determine an influence function giving "best" match of field history and allowing prediction of future performance.' Finally, Hutchinson and Sikora5 and Katz, Tek and Jones attempted to develop a calculation method for deriving the influence function directly from field data with no idealizing assumptions concerning aquifer geometry and homogeneity. They encountered difficulties with inaccuracies in field data and with satisfaction of well-known smoothness requirements of the influence function. This study is concerned with the determination of influence functions from field data and, more specifically, treats the following problem: given field pressure-production data of arbitrary accuracy, how does one determine the influence function which, subject to satisfaction of known smoothness requirements, gives best agreement with field history? A rigorous solution to this problem is ohtained through linear programming as described below. Example applications to one oil and two gas storage reservoirs are presented. In addition, a theorem is proved which confirms influence function smoothness requirements heretofore accepted on physical intuition and establishes additional smoothness requirements formerly not recognized.

Jan 1, 1965

By Rex E. Cheek, Donald E. Menzie

The fluid mapper, a model relatively new to the petroleum industry, was used to study the effect of various mobility ratios on the areal sweepout efficiency for two typical spacing patterns. The experiments indicated the areal sweepout for the five-spot pattern varied from 51.8 per cent at a mobility ratio of 0.093 to 89.1 per cent for a ratio of 24.4. In the direct line-drive pattern, the areal sweepout varied from 58.7 per cent at a mobility ratio of 0.089 to 92.0 per cent at a ratio of 24.8. The fluid mapper may prove useful to determine quickly the effective areal sweepout for any well spacing. INTRODUCTION The effect of the mobility ratio on the areal sweepout efficiency during primary depletion of a water drive reservoir and during secondary recovery operations has recently become more widely recognized The mobility ratio, M, is defined as: _ kjp (displaced fluid) k/u (displacing fluid) where k = effective permeability u = viscosity When the displacing fluid is miscible with the displaced fluid, the permeabilities are equal and the mobility ratio may be expressed as a ratio of viscosities: u (displacing fluid) u (displaced fluid) The mathematical analysis for calculating the areal sweepout efficiency with mobility ratio other than unity is quite tedious.5,11 An experimental method by using a potentiometric model2 in a step-wise manner and in using an X-ray shadowgraph model3,12 with continuous fluid flow has been published. Several types of models have been used to study oil and gas reservoir performance. These models may be classified as physical, electrolytic, potentiometric, X-ray shadowgraph, and fluid mapper. The X-ray shadowgraph and fluid mapper are models relatively new to petroleum engineering and have not been used extensively for specific applications. The theory of the fluid mapper indicates it may be adapted to a study of areal sweepout efficiencies for various mobility ratios as well as other complex problems in petroleum engineering. The use of the model and results obtained when using displacing and displaced fluids of equal densities but different viscosities are discussed. FLUID MAPPER DEVELOPMENT H. S. Hele-ShawV eveloped a fluid mapper model based on the hydrodynamic theory. This theory is that in the steady flow of a viscous fluid between horizontal parallel plates spaced a very small distance apart, the effect of viscous shear is of such magnitude in the vertical plane that the motion in the horizontal plane is practically undisbrted streamline flow. Techniques developed by Hele-Shaw were not expanded and no additional developments in fluid mapper models were forthcoming until A. D. Moore, University of Michigan, published a series of papers starting in 1949, which describe the construction of a flexible and inexpensive model'h nd the fluid mapper technique for the solution of certain problems.' The essential components of the fluid mapper as developed by Moore are::.ln 1. A base slab. made of dental stone (calcium sulphate and water). which is shaped to represent the prototype. 2. Plate glass slightly larger than the slab and spaced

Jan 1, 1956

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 B. M. Larsen, T. E. Brower

In two previous paperslJ dealing with the carbon-oxygcn reaction, and the simultaneous content of each, in liquid steel in the furnace, we have made use of the quantity A[O], defined as the excess oxygen beyond what would be in equilibrium with carbon then present if the pressure of carbon monoxide were I atm.; that is, if [C] X [O] is taken as 0.00222, A[O] = [O] - 0.0022[C] where [O] is the percentage of oxygen by weight as measured by the method described earlier.3 This quantity ?[O] proves to be substantially independent of carbon content over the range 0.08 to I,z per cent, as well as of the basicity of the slag, and is nearly always within the limits o.o15 to o.oz5 per cent when the bath is boiling normally and is in what we have termed a steady state, Apparently it must be at least about 0.014 per cent before boiling occurs; but this threshold value seems to depend upon the ease of bubble formation at the metal-hearth interface, hence upon the condition of the surface of the hearth. In any case, ~(01, on the average, changes considerably following any disturbance of the bath, as by addition of ore. The present paper deals with the average changes in A[O] level following addition of spiegel or crop ends, or after procedures to promote stirring, or by tapping of the steel from the furnace. The observations were made on a large number of commercial heats, and consequently are subject to the influence of various disturbing factors; the results have the compensating merit of showing the consistency obtainable under the limitations imposed by practical operation. Variability of Excess Oxygen in Normal Open-hearth Operation The preceding genera' statements refer to the average value of A[0] particularly in heats that are boiling actively; on individual heats, which are less active, there may be a variable time lag between the disturbance and its effect, which complicates the interpretation of what is going on. For instance, if in the normal refining process boiling is sluggish, the slag usually is gaining Oxygen from the gas phase above it, Or from added Ore$ faster than it is losing oxygen to the metal; Yet when the bath starts to boil vigorously, the opposite condition may prevail for Some time. The consequence of this lag is a variation of A[o], the interpretation of which in a sing1e heat may not be immediately obvious. This condition is illustrated in Figs. I and 2. In Fig. 1, A[0] at the beginning of the test period was near the lower limit of its usual range (dashed lines) in the steady state as a consequence of the lime boil, which had ended about as indicated. The bath is now cold, carbon drop is slow, and the first small orc feed causes only a small rise in A[O]; as the temperature rises and as lime dissolves in the slag, and the bath becomes more active, the

Jan 1, 1948

By John McGhee, Jack Newcombe, M. J. Rzasa

A series of water floods was made on laboratory prepared unconsoli-dated sand columns to study the effects on oil recovery of the solid-water-oil contact angle, the oil-water interfacial tension, flood rate, and oil viscosity. A procedure was developed for treating silica sand with silicone polymer to produce surfaces of varying degrees of wettability as evaluated by measuring the contact angle on a flat silica plate that had been simultaneously treated with the sand. Fluid interfacial tensions were changed by the use of surface active agents in the flood water. Water-wet, oil-wet, and intermediate wettability systems were studied at high and at low values of interfacial tension, at several flood rates, and with oils of different viscosities. For both oil-wet and water-wet systems and a low viscosity oil, recoveries were functions of the oil-water interfacial tension; also, increase in flood rate resulted in increased oil recoveries. High interfacial tension floods were more efi- cient than low interfacial tension floods on water-wet systems, while low interfacial tension floods were more eficient on oil-wet systems. Intermediate or neutral wettability systems were less sensitive to rate of flood advance and interfacial tension than either oil-wet or water-wet systems. The eflects of surface forces on oil recovery for high viscosity oils were not so well defined as for low viscosity oils. INTRODUCTION Reservoir rock surfaces vary in their wettability1, some being water-wet while others are apparently oil-wet. The factor of wettability enters into reservoir performance in both primary and secondary recovery, and into laboratory measurements of capillary pressure, connate water saturation, and relative permeabilities.' In theory, the degree of wettability is measured by the contact angle for the system solid-water-oil. A water-wet system is defined as one in which the advancing water contact angle is less than 90". An oil-wet system is one in which the advancing water contact angle is greater than 90°.3 The surface forces in a solid-water-oil system are related by the Young-Dupree equation as follows4: These surface forces are commonly expressed as the difference in adhesion tension, or the product of the water-oil interfacial tension and the contact angle. If the contact angle is less than 90°, the adhesion tension difference is positive and oil displacement by water from a solid surface will be spontaneous and favored by a high oil-water interfacial tension. If the angle is greater than 90" the displacement will not be spontaneous but will require less energy the lower the oil-water interfacial tension. The contact angle and interfacial tension also appear in the capillary pressure equation5: PC = 2ocosejr .... (2) The quantity cos was used by Rapoport and Leas6 s a factor in the generalized form of their "sealing coefficient." Warren and Cal-houn' presented the results of cos on oil recovery in oil-wet systems and correlated their data using a "scaling coefficient" suggested by Jones-Parra and Calhoun.8 The "sealing coefficients" were advanced to help correlate the effects of the variables influencing oil recovery by

Jan 1, 1956

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'' 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.'" 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 Kenneth M. Ritchie

Mineral wool is a term applied to man-made fibers of silicate glass with useful properties resulting from their fibrous nature. In contrast with crystalline fibrous minerals such as asbestos, mineral wool fibers are amorphous, solid filaments produced by drawing from molten liquid and subsequent cooling. Chemically they are silicate glass with varying percentages of metallic oxides, especially those of aluminum, calcium, magnesium, iron, and in glass wool, sodium, potassium and boron. Other elements such as manganese, titanium, sulfur, etc., result from their presence in the raw materials used and are not purposely added. In the United States, mineral wool is a generic term and may be applied to rock, slag or glass wool. In Europe, glass silk and silicate cotton are products in the same category, but the term mineral wool is less commonly used. Current usage is to ignore the actual source and to differentiate products on a composition basis; thus rock and slag wools have about 35-45 pct of silica, while glass wool has 54 to 60 pct. Much mineral wool of slag origin is called "rock wool," and this practice is increasing, although wool made of slag from lead or copper refining is often referred to as "lead slag wool." Its greenish-gray to greenish-black dark color, due to 5-25 pct Fe (reported as FeO), distinguishes it from "white" wools made from iron, blast furnace slag containing only 1-2 pct FeO or Fe203. Most mineral wool is used for thermal insulation against heat and cold; sound absorption and isolation are probably the next most important uses. Both its thermal and acoustic values result primarily from the physical structure of the heterogeneous mixture of fibers and air which is the form in which the fibers are first obtained and handled. For this reason, within fairly wide limits, differences in chemical composition are relatively unimportant, and for most conventional applications all types are competitive in properties and value. Mineral wool intended for extreme conditions of high temperature, acid resistance and special purposes must have a chemical composition which will insure the desired properties. This may differ greatly from that of ordinary wools; for example one product approximately 98 pct Si02 and another consisting of 50 pct A1203 and 50 pct Si02 are produced and sold for high temperature service up to 2000°F or more. These are considerably more expensive to manufacture and their cost limits their use. Historical The manufacture of mineral wool consists fundamentally of a process which subjects molten material to shear and/or tensile forces that draw them into fibers. The liquids are cooled at a rate which solidifies them quickly. As a solid glass they are technically super-cooled liquids since they have no true melting point. The drawing out of glass into thin rods, filaments and tubes was known from very early times, and present day continuous production of glass filament for textiles was evolved gradually by adapting hand methods to automatic machinery. Rock and slag wool manufacture had a somewhat different development. Early explorers reported finding filamentous material

Jan 1, 1960

By D. J. Carney, E. C. Rudolphy

Large macroscopic nonmetallic inclusions were related to altered fireclay refractories by chemical and microscopic means. Pouring refractories are discussed as a source of these large inclusions. Nozzles and wells are major contributors. Use of alkali and titania contents as tracers is described. Recommendations are offered to minimize the sources of inclusions from pouring refractories. IN any attempt to improve the cleanliness of plain carbon and alloy steels, consideration must be given not only to the proper deoxidation practice to minimize inclusions, but also to sources of inclusions from pouring refractories. In some cases, the inclusions resulting from deoxidation may be minor in amount, yet a relatively dirty steel may be produced as a result of improper care in the pouring practices for the steel. The number of studies of inclusions resulting from pouring refractories has increased recently and some excellent reports on this subject have already been published.'4 Some of these reports were reviewed briefly in a companion paper by M. P. Fedock.5 Mr. Fedock's contribution is a fine addition to the studies necessary to improve steel cleanliness for the ultimate benefit of all steel producers and consumers. In the interest of constantly improving cleanliness, the authors have been actively engaged for the past two years in experimentation to determine more closely the sources of inclusions in steel. One phase of this work was associated with efforts to define more closely the sources of macroscopic inclusions which have been experienced on occasional heats. The term "macroscopic inclusions" is defined in general as those inclusions which are visible to the naked eye or at low magnifications of the order of less than X25. These inclusions sometimes can be seen in the macro-etch tests of billets and slabs. This report summarizes a few of the field experiments and laboratory studies conducted at the South Works of the United States Steel Corp., which were made regarding nozzles, wells, and ingot scums, as well as inclusions occurring in steel products. The data in the present study, together with the data of Mr. Fedock concerning ladle erosion, should be of value in regard to future studies of inclusions arising from pouring refractories. The knowledge gained as a result of data collected thus far at South Works has been helpful in improving the cleanliness of the products and in pointing the way toward further improvements. Similarity of Large Inclusions to Refractories and Altered Refractories In the routine inspection of billet etch tests, occasional inclusions visible to the naked eye have been observed. These large inclusions most frequently occur near the top of the ingot and near the billet surface. When such material was encountered, careful examinations were made in an attempt to determine the origin of these inclusions. In a relatively few cases, examination revealed that the material was unaltered fireclay refractory of a type similar to that used for hot-top material, with only the surface of the inclusions having an altered appearance under the microscope. However, the great majority of these inclusions were completely altered-refractory material. The term "altered refractory" is defined

Jan 1, 1955

By B. M. Larsen, T. E. Brower

In two previous paperslJ dealing with the carbon-oxygcn reaction, and the simultaneous content of each, in liquid steel in the furnace, we have made use of the quantity A[O], defined as the excess oxygen beyond what would be in equilibrium with carbon then present if the pressure of carbon monoxide were I atm.; that is, if [C] X [O] is taken as 0.00222, A[O] = [O] - 0.0022[C] where [O] is the percentage of oxygen by weight as measured by the method described earlier.3 This quantity ?[O] proves to be substantially independent of carbon content over the range 0.08 to I,z per cent, as well as of the basicity of the slag, and is nearly always within the limits o.o15 to o.oz5 per cent when the bath is boiling normally and is in what we have termed a steady state, Apparently it must be at least about 0.014 per cent before boiling occurs; but this threshold value seems to depend upon the ease of bubble formation at the metal-hearth interface, hence upon the condition of the surface of the hearth. In any case, ~(01, on the average, changes considerably following any disturbance of the bath, as by addition of ore. The present paper deals with the average changes in A[O] level following addition of spiegel or crop ends, or after procedures to promote stirring, or by tapping of the steel from the furnace. The observations were made on a large number of commercial heats, and consequently are subject to the influence of various disturbing factors; the results have the compensating merit of showing the consistency obtainable under the limitations imposed by practical operation. Variability of Excess Oxygen in Normal Open-hearth Operation The preceding genera' statements refer to the average value of A[0] particularly in heats that are boiling actively; on individual heats, which are less active, there may be a variable time lag between the disturbance and its effect, which complicates the interpretation of what is going on. For instance, if in the normal refining process boiling is sluggish, the slag usually is gaining Oxygen from the gas phase above it, Or from added Ore$ faster than it is losing oxygen to the metal; Yet when the bath starts to boil vigorously, the opposite condition may prevail for Some time. The consequence of this lag is a variation of A[o], the interpretation of which in a sing1e heat may not be immediately obvious. This condition is illustrated in Figs. I and 2. In Fig. 1, A[0] at the beginning of the test period was near the lower limit of its usual range (dashed lines) in the steady state as a consequence of the lime boil, which had ended about as indicated. The bath is now cold, carbon drop is slow, and the first small orc feed causes only a small rise in A[O]; as the temperature rises and as lime dissolves in the slag, and the bath becomes more active, the

Jan 1, 1948

By T. K. Prentice

The January-February number of the Journal of the Chemical Metallurgical and Mining Society of South Africa, 1943, is made up entirely of a discussion of Ball Wear in Cylindrical Mills. Following the principal paper by T. K. Prentice are several remarkably pertinent and carefully prepared discussions. Few persons in this country would be likely to see this publication, and since the information presented is new and of current interest, it seems desirable to abstract and review this publication for the benefit of the members of the A.I.M.E. The purpose of the investigation is stated in the first two paragraphs of Prentice's paper, as follows: Early in 1941, The Chamber of Mines Steel Products, Limited, initiated a series of tests under semi-working scale conditions to determine, if possible, those physical and chemical properties of a ball which make it resistant to wear when used in a cylindrical mill as a grinding medium, with the primary object of incorporating those beneficial qualities in the balls being produced at their works. This paper describes the tests carried out and discusses the results obtained. From these results it was possible to formulate a new theory relating to ball wear in cylindrical mills. This theory is presented in the second portion of this paper. Practical Ball-mill Tests in a Cylindrical Mill Part I of the paper begins with a discussion of the methods used for the manu- facture of grinding balls in South Africa. The following paragraph is of particular interest. The cast steel ingots, 4¼ in. square by 3 ft. 6 in. long, are re-heated in a gas-fired sloping stationary-hearth furnace and then rolled in a six-pass continuous mill into 25/8 in. round billets. Some of these billets are then removed and cut into suitable lengths for forging into 4 in., 3¼ in. , 3 in. or 2½ in. balls by means of three Drop and two Beche hammers, but the greater number, whilst still at about 1,000, pass directly into a set of scroll rolls which produce, in an ingenious manner, finished 3 in. balls direct from the 25/8 in. billets. Except in special cases, all balls are allowed to cool in the atmosphere and are not water quenched. Details of the Tests In order to enable the reader to evaluate properly the results and conclusions in the rest of the paper and in the discussions following the paper, most of the information presented by the author under this heading is quoted: The testing unit was a nominal 30 in. diameter and 18 in. long centre discharge Denver Ball Mill. The ore pulp to the ball mill comprised a small portion of the normal feed to one of the fourteen City Deep 5 ft. 6 in. X 22 ft. tube mills, and the grinding media consisted of the balls under test plus other balls to give the desired load. The running time of the test-mill was divided into approximately equal periods of five days 13½ hours each. The usual procedure was to examine and make up the load

Jan 1, 1947

By T. K. Prentice

The January-February number of the Journal of the Chemical Metallurgical and Mining Society of South Africa, 1943, is made up entirely of a discussion of Ball Wear in Cylindrical Mills. Following the principal paper by T. K. Prentice are several remarkably pertinent and carefully prepared discussions. Few persons in this country would be likely to see this publication, and since the information presented is new and of current interest, it seems desirable to abstract and review this publication for the benefit of the members of the A.I.M.E. The purpose of the investigation is stated in the first two paragraphs of Prentice's paper, as follows: Early in 1941, The Chamber of Mines Steel Products, Limited, initiated a series of tests under semi-working scale conditions to determine, if possible, those physical and chemical properties of a ball which make it resistant to wear when used in a cylindrical mill as a grinding medium, with the primary object of incorporating those beneficial qualities in the balls being produced at their works. This paper describes the tests carried out and discusses the results obtained. From these results it was possible to formulate a new theory relating to ball wear in cylindrical mills. This theory is presented in the second portion of this paper. Practical Ball-mill Tests in a Cylindrical Mill Part I of the paper begins with a discussion of the methods used for the manu- facture of grinding balls in South Africa. The following paragraph is of particular interest. The cast steel ingots, 4¼ in. square by 3 ft. 6 in. long, are re-heated in a gas-fired sloping stationary-hearth furnace and then rolled in a six-pass continuous mill into 25/8 in. round billets. Some of these billets are then removed and cut into suitable lengths for forging into 4 in., 3¼ in. , 3 in. or 2½ in. balls by means of three Drop and two Beche hammers, but the greater number, whilst still at about 1,000, pass directly into a set of scroll rolls which produce, in an ingenious manner, finished 3 in. balls direct from the 25/8 in. billets. Except in special cases, all balls are allowed to cool in the atmosphere and are not water quenched. Details of the Tests In order to enable the reader to evaluate properly the results and conclusions in the rest of the paper and in the discussions following the paper, most of the information presented by the author under this heading is quoted: The testing unit was a nominal 30 in. diameter and 18 in. long centre discharge Denver Ball Mill. The ore pulp to the ball mill comprised a small portion of the normal feed to one of the fourteen City Deep 5 ft. 6 in. X 22 ft. tube mills, and the grinding media consisted of the balls under test plus other balls to give the desired load. The running time of the test-mill was divided into approximately equal periods of five days 13½ hours each. The usual procedure was to examine and make up the load

Jan 1, 1947

By P. Hudock

Thin films of PbS and CdS have been deposited on insulutiug- sapphire substrates by euzploying a subliwzation technique rising near-equilibriurum conditions in ultrahigh vacuum. Oriented polycrystalline PbS and CdS films on sapphire have mobilities approachitzg values characteristic of bulk crystals. In the case of CdS, special purification procedures were crucial in obtaining high-mobility films. By performing the depositiotz of a compound within a small chamber heated to a UNiform temperature within a Vacuum systerrz, it is possible to approach equiilibrium cod-tions r.~litl~irs the chamber. In this way; the sublimation and condensation proceed under near equilibrium co?zditions, and it was found that the properties of dePosited corrzpounds were similar to those of the source material. Oriented PbS films on sapphire have a roor?l- temperature unobility of 700 sq cm per v sec and a T-5/2 temperature dependence characteristic of bulk crrystnls. CdS layers on sapphive Izazse a resistivity ~uhich is corrlpamble to the resistivity of the souvce crystals over a range of four ordem of rrlagnitude. Irz contrast, Ihe resistivity of CdS films prepared by conventional evaporation depends largely upon the substrate terrzperat~ire and postheating treatrrletlt, vather than upon the properties of' the solirce rrraterial. In the case oj the CdS films the achievment of high carrier mobility required the cargful exclusion of cont~~~~ii~unts from the films. The steps taken to accomplish this included presublimation of the source material, performance of the deposition at a backg-m~ozd pressure less than 10-8 Torr, and a solvent extraction with liquid cadminum, similar to that described by Aven and woodbury. The deposition of ,films under near-equilibrium conditions is being op-plied to other classes oj COmpounds. II should he of 1:allce ,tor llle deposition of nny matevial that decomposes in the vapor state. THIN films of PbS and CdS have been deposited on insulating sapphire substrates by employing a sublimation technique using near-equilibrium conditions in ultrahigh vacuum. Oriented polycrystalline PbS and CdS films on sapphire have Hall mobilities approaching values characteristic of bulk crystals. In the case of CdS, special purification procedures were crucial in obtaining high-mobility films. Depositions were performed in a small quartz sublimation cell shown in Fig. 1 that contained the compound and the single-crystal sapphire substrate. The substrates were etched in tapered solutions of hot phosphoric acid, rinsed in deionized water, dried, and transferred to the cell under dry nitrogen. Graphite crucibles and substrates were used in experiments where it was necessary to provide an inert test vehicle for the analytical determination of impurities in the source crystals and deposited films. The crucibles and substrates were machined out of spectrographic-grade graphite having less than 1 ppm of impurities. A quartz mask was sometimes used to define a pattern which could be used for Hall and resistivity measurements. Close spacing between the compound and substrate was maintained to insure better transport of each component from the source material.

Jan 1, 1968

By R. J. Wasilewski

The variation of elastic modulus with terrzperature between -150° and 600°C has been investigated. Compounds close to equiatomic cornposition exhibit very low modulus values and very high damping near room temperature. The modulus rises steeply with both decreasing and increasing temperature. The modulus minimum and the high damping are believed to be connected with a martensitic transformation of TiNi. In bulk material this transition takes place slightly above room temperature quite rapidly and reversibly, with a hysteresis of some 30°C, depending on the Ti:Ni ratio. Oxygen impurity affects the reaction time. THE inter metallic compound TiNi has been reported to exist in an ordered CsCl (B2) structure,l-6 the homogeneity range varying rather markedly with temperature.7 Some investigators reported this compound to decompose peritectoidally to Ti2Ni and TiNi, between 650° and 800°C,3 or below,',g the latter workers also suggesting the decomposition to be strain-sensitive. Purdy and Parr were the first to report a structural transformation to a new, possibly hexagonal, structure at 36°C,7 a temperature indubitably too low to allow the significant amount of diffusion necessary for a peritectoid reaction. Mechanical-property investigations of compositions close to TiNi just above room temperature have qualitatively shown remarkable anomalies, particularly with respect to clamping,' and to a "memory" effect, that is, plastically deformed material returning to its original shape on being heated through the "decomposition" temperature.9 The original explanation of this effect—based on the apparent experimental observation of Ti2Ni or TiNi, formation in the material subjected to tensile or compressive stresses, respectivelp—does not appear plausible. It appeared more probable that the change involved may be a martensitic, diffusionless structural transformation, similar to those observed in other B2 structures such as 0 brass,'' AuCd,ll and AuZn.12 The existence of such transformation has been established recently,', although the symmetry of the low-temperature structure is not yet known. The present paper describes the elastic modulus and damping behavior of polycrystalline TiNi in both structures. EXPERIMENTAL METHOD 1) Specimens. All the specimens to be investigated were prepared from premelted electrolytic nickel and iodide titanium by nonconsumable arc melting and casting in a water-cooled copper mold. The cast billets were canned in mild steel, extruded, and swaged to approximately 0.375 in. diam. The cans were then removed by pickling or machining. Preliminary material balance checks indicated no significant weight losses on melting (less than 5 mg on a 50-g button); hence nominal compositions have been used throughout. In agreement with previously reported observations7 no single-phase material was obtained at—or close to—Ti 1.00 Ni1.00 a small amount of finely divided second phase always being present. It was found that most of the oxygen impurity was associated with this minor phase, which was identified as oxygen-bearing Ti2Ni—possibly Ti,Ni,O. The amount of this phase—at any given Ti:Ni composi-

Jan 1, 1965

By D. E. Peacock, B. Harris

Thermal-expansion and electrical-resistivity measurements have been carried out below 400°K on niobium and two niobium alloys containing tungsten. For anonaly in the expansion us temperature curve below aboct 300°K. This reslt is consistent with an earlier obsercation that Young's modilus joy Cb-132 lms an unusiully strong -tenperati-e dependence below roon temperature. No anonulous behavior was observed in the resistiuity vs temperature curve for either alloy or in the magnetic susceptibility us tenperature curve for Cb-132. These results are disclssed in terms of various electronic and bonding theories of the transition metals and their alloys, but it has not been possible to reach any definite conclusion as to the cause of the results obtained. ALONG with investigations of the low-temperature mechanical behavior of niobium and its alloys, some of the physical properties of these materials have also been studied. In the work described here, thermal expansion and electrical resistivity were measured below 400°K for niobium and two of its alloys, Cb-132 and D-43. In addition, the magnetic susceptibility of Cb-132 was measured over the same temperature range. The alloys are representative of two distinct tion-hardened alloy such as might find service as a turbine blade, while D-43 (Nb, 5.3 at. pct W, 1.1 at. pct Zr. and 0.08 at. pct C) is a solution- and dispersion-hardened alloy, of considerably lower strength than Cb-132. which is a potential vane material. Their significant common feature is the presence of tungsten as the principal source of solution hardening. EXPERIMENTAL TECHNIQUES Thermal-expansion measurements were made with a quartz-tube dilatometer using baths of liquid nitrogen, liquid bromoethane, and a liquid polyalkylene glycol derivative to cover the range 80 to 400 K. Results are recorded as expansion relative to that of quartz, and the probable maximum error in any value of relative expansion. All, is about il pct. The metallurgical condition of the specimens, which were in rod form. will be discussed in the section dealing with experimental results. Resistivity was measured on recrystallized wires 0.030 in. in diam using a potentiometric technique. The same baths were used for temperatures between 80' and 400°K as were used for the expansion measurements. and in addition the resistance of D-43 and Cb-132 was measured at 4.2 K by immersion in liquid helium. The maximum expected experimental error in any resistivity value is about 3 pct and that in any change in resistivity about i0.05 pct. Temperatures in both sets of experiments were measured with liquid-in-glass thermometers with an accuracy usually better than 1°K. EXPERIMENTAL RESULTS 1) Thermal Expansion. In Fig. 1 is shown the relative linear expansion of recrystallized niobium. D-43. and Cb-132. The curve for Cb-132 is composed of results from several runs on three different samples. Two of the samples were annealed for an hour at 1500°C to cause recrystallization and the third was annealed for an hour at 2000'C to remove some mi-crosegregation of tungsten which was known to be present in the wrought alloy received from the manu-

Jan 1, 1967

By W. J. Tait, A. E. Craig, E. P. McCurdy

The Circuitron herein described applies current from the classifier motor circuit and energy from the sound of grinding media to move an oscillating disc. The disc through a photoelectric cell controls the speed of the ore feeder and consequently the amount of ore delivered to the mill. THE Telluride Mines, Inc. at Telluride, Colo., is operating a flotation concentrator recovering lead, zinc, and copper with some gold and silver. The nominal capacity is 500 tons per 24 hr. The ore, which comes from several different mines, is characteristic of the district, changing from extremely tough rhodonite to soft gouge. The ore is crushed and washed, recrushed, and delivered to the mill bin at about % in. to serve as ball mill feed. Details of Grinding Circuit The material from the fine-ore bin is carried over a belt feeder driven by a Reeves vari-speed device. The belt discharges to a No. 86 Marcy ball mill, which operates in closed circuit, with jigs and a 6-ft Dorr classifier. A Massco density controller holds the density of the classifier overflow at a predetermined point. The overflow, which contains about 5 pct + 48 mesh, goes to the flotation section. Manual Operation Before the adoption of automatic control for the grinding circuit, this work was all done manually by the operator. The bin gate was set to deliver 40 to 50 lb of ore per lineal foot of belt, and the speed of the belt was adjusted by the operator to deliver at the rate of about 500 tons per 24 hr. As the ore changed in hardness, specific gravity, or in the amount of moisture, or, as the size of the feed changed due to bin segregation, crusher setting, or other causes, the operator made corresponding changes in the rate of feed by manipulation of the Reeves control. Sometimes these changes occurred so rapidly that they caused sharp, pronounced surges, which created very considerable unbalance from normal conditions in the grinding circuit and, more critically, in the flotation section. Since it is not possible for the operator to anticipate or follow such changes closely, a very considerable unbalance from normal conditions may occur, which will require a drastic change in the rate of feed. These surges upset the fineness of grind and interfere radically with the balance between tonnage and reagent control. All of this tends to reduce the grade of concentrates, increase the loss in the tailing, and thus decrease the recovery of values. The Circuitron Some years ago, The Mine and Smelter Supply Co., in conjunction with the operators at the Telluride Mill, undertook to build a device that would give close control of the rate of feed from the ore bin and to coordinate with this a related device that would regulate the amount of sand load on the classifier rakes. Emphasis was strongly laid on the fact that such a control must apply to the entire grinding circuit and must include the feed to the ball mill, the classifier sand return, and the density of the classifier overflow. If this could be done successfully, we felt that the circuit could be operated under best possible conditions, with compensations

Jan 1, 1951

By G. B. Craig, H. E. Rosinger, W. J. Bratina

NUMEROUS studies have been reported on how the mechanical properties of a bcc metal are affected by interstitial solute atoms in the temperature range where appreciable diffusion occurs in finite time. Only recently, though, has work on an "interstitial-free" iron been reported, this by Leslie and sober,' on an Fe-0.15 pct Ti alloy. The data was limited to a maximum temperature of 296°K. This work presents a systematic study of the flow stress and the activation volume of a similar material as a function of plastic deformation over the temperature range 253" to 473°K. The material studied was Ferrovac E iron containing 0.01 wt pct C and 0.0002 wt pct N annealed at 870°C for 1 hr, and the same iron with an addition of 0.15 wt pct Ti annealed at 870°C for 80 hr; cooling rates being 75°C per hr. In the latter alloy depletion of interstitials in the a-iron matrix associated with the second phase formation was expected. The temperature dependence of the flow stress was measured at 6 = 3.33 x 10-5 sec-1 from 253" to 473°K as a function of the deformation in 0.01 intervals from 0.03 to 0.12 strain. Results for two strains, 0.03 and 0.09 are shown in Fig. 1. The flow stress increased and reached a maximum in the Ferrovac E iron with increasing temperature, but showed a consistent gradual decrease in the Ferrovac E-0.15 pct Ti alloy. A yield point and Luders region, observed in Ferrovac E, was absent in the Ferrovac E-0.15 pct Ti alloy. Also, the Ferrovac E exhibited a serrated stress-strain behavior in the temperature range 330" to 400°K; dynamic strain-aging characteristics were absent for the titanium alloy. The activation volume was determined over the same temperature range by the method of stress relaxation at constant strain. Results are shown in Fig. 2. At the temperatures of serrated stress-strain behavior in Ferrovac E the activation volume was found to increase toward infinity and, as the temperature rose, to decrease, to about 100 to 200 v/b3. By contrast, the activation volume for the Ferrovac E-0.15 pct Ti alloy tended to increase continuously from the initial value of approximately 300 at 300°K to more than 800 at 473°K. Above 400°K, then, the corresponding activation volume values of Ferrovac E were less than that of the Ferrovac E-0.15 pct Ti alloy. The activation volumes, Fig. 2, appear to depend on dislocation-interstitial interaction in Ferrovac E and on dislocation-dislocation interaction in Ferrovac E-0.15 pct Ti alloy. The gradual increase in the latter metal is associated with thermally activated motion of dislocation segments.' The decrease of the activation volume in Ferrovac E above 400°K is probably related to the diminishing effect of interstitials on dislocations. Here, the interstitials can be moved along with a dislocation without appreciable drag. As indicated in Fig. 1, removal of interstitials

Jan 1, 1970

By C. S. Smith, K. K. Ikeuye

In an earlier paper1 one of the authors called attention to the significance of the relative free energies of grain boundaries and interphase boundaries in alloys in determining the shape and distribution of micro-constituents. The ratio of the interphase and inter-crystalline boundary energies (that is, —?12, where ?12 is the energy of the interface between a crystal of phase 1 and a crystal of phase 2, and ?11 is the energy of the boundary between two crystals of phase 1) will be denoted by F. It is this ratio that determines, by the simple triangle of forces relation, the dihedral angle, ?, of phase 2 where it adjoins a boundary between two grains of phase 1. On a metallographic sample various angles are actually obtained because of the random orientation of the plane of observation, but the statistically most frequent angle is the true one. These basic principles were discussed in detail in the earlier paper. The experiments described below show the effect of both composition and temperature on ? and T for some alloys containing a liquid phase, and provide data on the rate of approach to the equilibrium angles in both solid and liquid phases. All the alloys were melted in a graphite crucible and cast into ingots 3/4 by 11/8 in. cross-section. Some of the aluminum alloys consisted of two immiscible liquids from which uniform castings could not be obtained. The amount of liquid phase varied locally to a considerable extent and the analyses were meaningless. Nevertheless, the composition of the liquid would not differ from that in an alloy of the intended gross composition, and the synthetic composition of the alloys was therefore used in considering the surface energy results. The ingots were given initial deformation by cold-rolling to 50 pct reduction, annealed, and given a second 50 pct reduction prior to cutting into small samples for heat treatment at the times and temperatures subsequently reported. The resulting micro-samples were carefully prepared metallographically and examined at magnifications of 650, 1280, or 2500. The objectives used were 21X, 0.40 NA (dry); 41X, 0.65 NA (dry); and 80X, 1.40 NA (oil emulsion). The appropriate angles were measured by rotation of the stage of a Bausch and Lomb metallograph to align the appropriate boundaries successively with a cross-hair in a micrometer eyepiece. About 250 angles were measured on each phase. Though the angles were read to 1°, the accuracy is probably not above 3°, because of uncertainty in setting the cross-hair tangent to the sometimes curved boundary. The corners of very small particles, particularly in early stages of adjustment after cold-rolling, were difficult to measure and the results were slightly dependent on the magnification used (compare Fig 1-C and 1-D). With particles of larger size and more nearly equilibrium shape, magnification made no difference (vide Fig 1-F and 1-G). The measured angles were grouped in 10° intervals (5° if ? was less than 20°) and plotted in bar

Jan 1, 1950