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By R. T. Hukki

The purpose of this paper is to present an analysis of the unit operation of grinding and the circulating load, of the unit operation of classification and the circulating load, and of the two superimposed into one operation to clarify the overall trend of events relating the circulating load to the capacity of the closed circuit grinding system, to the specific surface area of the final fine product, and to the energy consumption in the closed circuit grinding process. The capacity of the closed circuit is frequently, if not always, determined by the classifier, not by the mill." With these words a startling idea was expressed in 1934 by Dorr and Anable.1 Today, some 30 years later, grinding in closed circuit is universally accepted. The basic curve presenting the capacity factor versus circulating load by Dorr and Anable has obviously been so convincing that not a single authoritative investigation regarding its validity seems to have been conducted. The only major subject of discussion appears to have been the relative merits of the 'high' and 'low' circulating loads. It seems to be universally agreed that much still remains to be hoped for regarding sharpness of classification. BASIC CURVES FOR CONSTANT MILL LOADING Fig. 1 presents a series of basic curves for constant mill loadings in function of new feed rate and circulating load. The mill loading indicated by each curve is the sum of hourly tonnages of new feed and circulating load. For example, at point 0 where the new feed rate is 100 t/h and the circulating load 300%, or 300 t/h, the mill loading is 400 t/h. In closed circuit grinding, the new feed rate corresponds to the rate of finished classified material produced. Although at this stage the effect of classification is excluded in construction of the basic curves, the trend indicated by these curves is strongly in favor of closed circuit operation under relatively small circulating loads. A study of the curves reveals that, e.g., a mill operating under a load of 200 t/h at point P where the new feed rate is 50 t/h and the circulating load 300% will also operate under the same total load at point Q where the new feed rate is 100 t/h and the circulating load 100%. In other words, a reduction of circulating load from 300% to 100% would lead to doubling of the new feed rate and doubling of the rate of production of finished material, without a change in the total mill loading. The obvious question is, is it also possible by a reduction of the circulating load in a closed industrial grinding circuit to increase the production of finished classified material and, if so, how and to what extent? GRINDING TESTS BY DORR AND ANABLE In a series of open circuit grinding tests reported by Dorr and Anable1 limestone was ground at various feed rates in a 3-ft ball mill. The original data are reproduced in Table I. It can be seen that with the increased feed rate production of -65-mesh material increased and the energy consumption per unit weight of the -65-mesh product decreased in the reverse ratio. The data shown in Table I have been reproduced for our purposes in Table II for a scale corresponding to grinding in a large industrial mill. This reproduction

Jan 1, 1968

By Paul A. Flinn, Jean-Marie Robert Genin

The MCssbauer effect was used to study the distribution of carbon in Fe-C alloys of high carbon content during room-temperature aging. In freshly formed rnartensite the carbon distribution is approximately random; carbon clustering occurs dun'ng aging. In the retained austete the carbon atoms are isolated, suggesting an efiective repulsion; and no rearrangement during room-temperature aging is evident. The kinetics of the carbon clustering in martensite has been studied in detail at 0" . 10". and 20°C. The time and temperature dependence observed is sinzilar to that reported for a variety of other aging effects, such as resistance change, hardness increase, and recovery of internal friction. The stabilization of the martensite kransformation also appears to be related to the clustering effect. DESPITE extensive efforts since the early days of Reaumur, the mechanism which provides the strengthening of steel remains controversial in many cases for several reasons: 1) The structure of as-quenched martensite is not well-determined. 2) Experimental methods capable of distinguishing between various hardening mechanisms are not well-developed. 3) The temperature of formation of many low-alloy martensites is so high that the martensite formed during quenching may be already tempered to some extent before any observation. Among all the hardening phenomena, the most puzzling one occurs at room temperature, where no structural changes have been detected by the usual methods of X-ray diffraction or electron microscopy. However, a new and more sensitive technique became available with the discovery of the MBssbauer effect. This effect makes possible the detection of changes in the local environment of iron atoms in solid solution. It has been extensively used in the study of substitutional alloy systems, for example, Fe-Al,1 Fe-Si,2,3 Fe-Rh,4 and Fe-Ni.5 Making use of the possibility of obtaining new structural information, we undertook an investigation of the aging of high-carbon Fe-C martensite to follow the structural changes involved in the aging at room temperature. Preliminary results6 showed that a clustering of the carbon atoms occurs with time. A systematic study of the kinetics of the process showed a striking similarity to the kinetics of stabilization of the marten-sitic transformation, thus suggesting further investigation of the relationship. EXPERIMENTAL TECHNIQUE To eliminate difficulties with the aging of martensite prior to the first experimental measurements, we needed an alloy with an M, temperature not above room temperature. Other investigators7 were misled by results obtained on alloys which transformed above room temperature and underwent structural changes prior to the first Mossbauer measurements. Winchell and cohen8 dealt with this difficulty by using a third element, nickel, to depress the MS below room temperature. The presence of nickel did not seriously interfere with hardness or resistivity measurements, but it would complicate the interpretation of the Mossbauer data by increasing the variety of iron environments. We chose, therefore, to obtain the necessary lowering of the M, simply by increasing the carbon content. After the first quench to room temperature, our specimens are retained austenite, which we later quench into liquid nitrogen. The martensitic transformation takes place suddenly, so that the as-quenched condition of the samples is retained, since the temperature is low enough to prevent any carbon diffusion. A Massbauer spectrum at 77°K can be taken and analyzed; after an appropriate up-quenching to the aging temperature, a new Mossbauer measurement at 77°K can be made. Fig. 1 shows a typical cycle of experiments. The samples were foils 25 p thick of high-purity

Jan 1, 1969

By F. Paredes, W. R. Holman, R. W. Crawford

The diffusion coefficient for hydrogen in the ß titanium alloy containing 13 pct V, 11 pct CY, and 3 pct A1 was measured over the temperature range 20° to 500°C. Results fit the expression: D= 1.58 x lgs exp-------==-----) cm2,sec THE diffusion coefficient for hydrogen in the metastable ß-phase titanium alloy containing 13 pct V, 11 pct Cr, and 3 pct A1 was measured as part of an investigation of the effects of hydrogen on the mechanical properties of titanium alloys. Several theories on the mechanisms of hydrogen embrittle-ment include diffusion of hydrogen at ambient temperature as an important step in the embrittling process.'-5 In hydrogen-contaminated a-ß titanium alloys, it has been postulated that the rate-controlling step may be the rate at which hydrogen diffuses from the ß phase to stress- or strain-nucleated brittle hydride platelets at the a-ß interface.' However, embrittlement of the all-ß alloy investigated in this work may proceed by a different mechanism, since this alloy can be embrittled without the formation of detectable hydride platelets.6 Troiano has suggested that in this case the mechanism of delayed failure or embrittlement is similar to that proposed for high-strength steel, i.e., repeated crack initiation caused by a decrease in bonding energy as hydrogen diffuses to points of high tri-axial stress at the root of a notch. In both types of alloy the rate of embrittlement is believed to be controlled by diffusion of hydrogen in the ß phase. Accurate hydrogen-diffusion data in the vicinity of room temperature should therefore be of some assistance in understanding the mechanisms of embrittlement in these two classes of titanium alloys. Diffusion of hydrogen in pure titanium has been studied by Wasilewski and Kehl7 at temperatures above 500°C. Their measurements on diffusion in the ß phase were extended below the ß-a transformation temperature (882°C) to approximately 600°C. This was possible because of the 8 stabilizing effect of hydrogen. No results at lower temperatures have been published and there are no data in the literature on hydrogen diffusion in the ß -phase alloy used in this program. Hydrogen diffusion in metals is generally investigated by measuring the rate of transport of hydrogen past a solid-gas interface, i.e., by absorption, permeation, or degassing-rate measurements. These methods produce accurate diffusion data when bulk diffusion is the rate-determining step in the over-all process. However, at the lower temperatures of interest in hydrogen-embrittlement studies or under conditions where surface films are present, the measured rates may be surface-controlled and the calculated diffusion coefficients will be in error. Surface effects were eliminated in the present work by using a modification of the common welded-couple technique m which two bars with uniform but different compositions are joined before the diffusion anneal." The same type of step change in the initial concentration vs distance curve was produced by electrolytically hydrogenating thin-strip specimens which had been electrically insulated over half of their length. Concentration vs distance curves were determined, after appropriate diffusion-annealing treatments, by vacuum-extraction analyses of transverse samples sheared from the strips. Diffusion coefficients were calculated by the methods of Grube.M This technique was feasible because of the large concentrations of hydrogen which can be charged into p -phase alloys without the formation of hydrides15'16 and because of the extremely low degassing rates observed when hydrogenated titanium alloys are heated in air. EXPERIMENTAL WORK The diffusion couples were cut from a 0.022-in.-thick mi ll-annealed sheet.* Strips 8 in. long by 1/2

Jan 1, 1965

By R. S. Shoemaker, D. L. Harris

PST investigations into the possibility of concentrating the low-grade iron ores of the Gogebic Range in Wisconsin have been hampered by the complex association of the constituent minerals. In part the problem arises from the fact that the iron occurs essentially as two minerals, hematite and goethite, having nearly the same chemical composition but exhibiting different physical properties. Individual grains of these minerals are usually so small that the ore must be ground to a size finer than 325 mesh if substantial liberation of the minerals is to be secured. Appraisal of beneficiation tests on this iron ore requires, therefore, some method of determining quantitatively the contents of constituent minerals in the various products of the beneficiation. Because of the chemical similarity of the two iron minerals, chemical analyses do not provide a means of differentiation. Although the minerals are different physically, they are both opaque and friable, and as the ore must be ground to a very fine size for liberation to be secured, quantitative microscopic methods of analysis are extremely difficult at best. In an effort to overcome these analytical problems, a quantitative X-ray diffraction analysis method has been developed at the University of Wisconsin for the research program on iron ore beneficiation. The X-ray diffraction analysis of chemical compounds of crystalline form has proved of inestimable value for structure studies and rapid qualitative analytical purposes in a number of fields.' In some cases X-ray diffraction analysis has been found suitable for quantitative determinations. H. P. Klug2 found that quantitative procedures for quartz powders when mixed with calcium fluoride were reproducible within ±1.0 pct. Talvenheimo and White3 reported quantitative analyses of clay minerals to be accurate within 10 pct and also detected 1 pct of bentonite in 99 pct illite. In other investigations,'" powders of quartz and mica have been analyzed quantitatively with accuracies from 1 to 5 pct. A powder of tungsten carbide was analyzed similarly by Redmond7 and Rooksby8 reported the determination of small amounts (0.11 pct) of calcium oxide in magnesium oxide. In the most generally practiced use of X-ray diffraction, traces of the diffracted beam are recorded as lines on a film much as lines of elements are recorded on an optical spectrograph film. As with the spectrograph, the darkness of the lines denotes the amount of the constituent in the sample. If the film is replaced by a Geiger tube assembly and a graphic recorder or a scaling unit, the intensity of the diffracted beam can be registered as a peak on a chart or energy impulses per unit of time on the scaler. Several methods of quantitative measurement have been investigated and reported in literature. Klug2 used manual operation of the goniometer and a counting technique to determine the difference in counting rates at the diffracted angle and for the background. In another case3 the area under the recorded diffracted peak was the basis for the determination. In other instances the height of the recorded diffraction peak above background, measured while the goniometer was moving, has been the basis for the measurement. The sizes of particles most suitable for diffraction techniques are reported in the literature as follows: for tungsten carbide a maximum of 40 microns7 and for quartz a maximum of 5 microns.' Very fine sizes of crystals are known to cause a broadening of the diffused beams; hence some workers have set a lower limit of 0.1 micron for quantitative results. Guinier10 has indicated that broadening of the diffracted X-ray beam is not appreciable for crystallites larger than 0.02 to 0.03

Jan 1, 1956

By S. C. Sircar, D. R. Wiles

The rate has been studied of the hydrogen reduction of nickel ions in acetate -buffered solutions, using a nickel catalyst. At temperatures between 130°and 160°C, the rate is found to be proportional to the catalyst area, the nickel ion concentration, and the hydrogen pressure. The effect of hydrogen ions is to reduce the observed rate, likely by causing the reverse reaction (dissolution) to proceed. The experimental activation energy was found to be 25 kcal per mole. THE precipitation of metals and lower oxides from solution by hydrogen reduction has been quite actively investigated during the past few years.1 In the case of nickel, the kinetics of the precipitation have been studied in ammonia solution2 but extension of this study to acid solutions has not attracted much interest, largely because of the unfavorable thermodynamics at all but the lowest acidities. For example, Schaufelberger foundg that only 10 pct reduction of nickel could be effected in sulphate solutions. One kinetic study of the reduction of Ni++ has been reported by Knacke, Pawlek, and Sussmuth,4 in which the order of the reaction was found to be one in nickel ion and one-half in hydrogen pressure. No mention was made as to the part played by the nickel catalyst, or by the pH of the solution. Moreover, the activation energy reported (4 .12 kcal per mole) is so low as to lead to some question as to whether diffusion might be playing a major role in determining the kinetics. We have recently completed a study5 of the kinetics of the hydrogen precipitation of nickel from acetate-buffered acidic solutions whose results confirm and amplify those of Knacke et al. EXPERIMENTAL PROCEDURES The work was done in a high-pressure autoclavee by the usual technique of removing small samples of the solution for analysis. Nickel analysis was done colorimetrically by the dimethylglyoxime method.' The catalyst used was carbonyl nickel powder (Standard A powder of the Mond Nickel Co., Ltd.) which was found to be composed of spheres of less than 350 mesh. The surface area of the powder was determined in this laboratory by the B. E. T. method to be 1.85 sq m (m2) per g. The catalyst was added to the solution only after the proper temperature and pressure had been reached. Agitation of the baffled system was by a turbine-type impeller, rotated at speeds between 400 and 750 rpm. The reduction rate was found to be independent of the stirring rate, so it was assumed that diffusion in the liquid does not limit the rate. In typical experiments, the nickel concentration was unchanged during an induction period of variable length. The concentration then decreased sharply, and gradually levelled off to approach the final equilibrium value. In some cases, notably at high stirring rates, the nickel concentration was found to increase considerably during the induction period, and then to decrease. In all cases, the rate was determined from the slope of the tangent to the rate curve as the concentration first decreased below the initial value. This is seen in Fig. 1. The rate measurements were found to be reproducible to within about 5 and to be quite independent of the nature or duration of the induction period. The range of conditions used is given in Table I.

Jan 1, 1961

By E. R. Morgan, J. C. Shyne, V. F. Zackay

NITROGEN used as an alloying element in steel has received increased attention in recent years. Its merit as an austenite stabilizer and hot strengthener has long been recojinized, particularly by European investigators.' Recent work' indicates that nitrogen contents of 1/2 pet or more allow the addition of several percent of ferrite-forming hot strengtheners, such as molybdenum, without subsequent austenite decomposition at elevated temperatures. The room temperature properties of such alloys are characterized by high yield and tensile strengths with excellent ductility, even after cold working, as shown in Tables I and 11. The 1350°F creep-rupture properties of Cr-Mn-Mo-N steels are comparable to those of commercial alloys such as Timken's 16-25-6, containing 16 pct Cr, 25 pct Ni, and 6 pct Mo, as shown in Table 111. Cr-Mn steel containing 1/2 pet N must be made under pressure if ingot gassing is to be avoided. However, there are difficulties attendant to this practice. Pressure melting restricts the ingot size, and the equipment required is costlier and more complicated than comparable air melting facilities. An effort was made, therefore, to determine more economical methods of adding nitrogen. The pressures generated in centrifugal casting usually range from 5 to 10 atm and are sufficient to prevent the gassing of high nitrogen Cr-Mn steels. A centrifugal casting was made of an alloy containing 16 pct Cr, 18 pct Mn, 2 pct Mo, and 0.73 pct N. A risk, 8 in. diam and 11/2 in. thick, was cast at 1000 rpm. It has been calculated that a pressure of 9 atm was developed at the periphery of the disk at this speed. Metallographic inspection of specimens taken from the disk revealed no gas holes or other defects. The elevated temperature properties of radial and circumferential specimens taken from this casting are given in Table IV. The creep-rupture life of this cast nickel-free austenitic steel was equivalent to that of the wrought Cr-Mn-Mo-N steels. Although centrifugal casting appears to lend itself to the manufacture of high nitrogen austenitic steels, its applicability is limited to relatively small sizes. A process applicable to the production of large ingots of high nitrogen steels is suggested by low carbon rimming steel practice. Gas holes formed during ingot solidification are not detrimental so long as they weld shut during hot rolling. An economic advantage of gassing ingots is the increased ingot-to-slab yield, especially if the ingots are mechanically capped. Also, it is probable that higher nitrogen levels can be achieved with mechanically capped ingots than with hot-topped ingots. A series of gassy heats was made under both atmospheric and higher pressures, as indicated in Table V. Several of the air melted ingots were mechanically capped by chilling the molten ingot tops with a steel plate. The ingots were allowed to freeze in steel molds without hot-tops unless otherwise indicated. A comparison of Table 111 with Table V shows no significant difference in the creep-rupture properties of the gassy and the nongassy ingots after hot work- ing nor between the gassy ingots produced under different conditions. References 1 F. Rapatz: Application of Stainless and Heat Resisting Steels Alloyed with Nitrogen. Sinhl and Eisen ( 1941) 61, pp. 1073-1078. 'V. I?. Zackay, J. F. Carlson, and P. L. Jackson: High Nitrogen Austenltlc Cr-Mn Steels. Trans. ASM 119551 48, PP. 509-523.

Jan 1, 1957

By P. E. Arnold, G. S. Ansell

RELAXATION in metals has been studied in detail by many workers in recent years.1-5 These studies have shown that there is an energy-loss peak observed in a metal placed in mechanical resonance at low frequencies which may be correlated with various metallurgical processes. These experiments have been largely used to study single-phase materials. In order to study the effect of a finely dispersed second phase in a metal matrix upon this phenomenon, the relaxation behavior of an aluminum-aluminum oxide SAP-Type alloy in both the fine-grained as-extruded and coarse-grained recrystallized conditions was investigated by the use of internal-friction measurements. The alloys studied, designated MD 2100, consist of a matrix of commercial-purity aluminum containing a finely dispersed second phase of aluminum oxide. The aluminum oxide is present in this alloy in the form of fine platelets approximately 130A units thick and several microns on edge. The mean free path betwen dispersed platelets is approximately 0.5 p. The grain size of this alloy is extremely stable at temperatures as high as the melting temperature of the aluminum matrix. In the as-extruded condition the grain diameter is several microns, while in the recrystallized condition it is several millimeters in diameter. The damping characteristics of the alloy samples were determined using a torsional-pendulum device. The internal-friction constant was determined for this alloy in both the fine-grained as-extruded and coarse-grained recrystallized conditions over the temperature range from 343" to 923°K at frequencies of 0.9, 1.3, and 1.8 cycles per sec. An internal-friction peak was observed in testing the fine-grained alloys which was not observed for the coarse-grained alloys. This peak, which might be associated with a type of grain-boundary relaxation, was observed at each of the three different test frequencies for the fine-grained sample. The temperature at which the relaxation peak occurred for each of the three different frequencies is shown in Table I. From these data an activation energy of relaxation for each pair of frequencies was determined by comparing the temperature shift of the relaxation peak with frequency between each of the test frequencies, assuming that an Arrhenius-type rate equation is applicable. The activation energy of relaxation determined from these data is also shown in Table I. The mean value of the activation energy was about 6 kcal per mole. The activation energy for the relaxation process determined in this investigation indicates that the relaxation associated with the grain boundaries in this aluminum-aluminum oxide SAP-Type alloy is quite a different process than grain boundary relaxation in single-phase aluminum alloys. In these latter alloys, the activation energy for relaxation has been found to be the activation energy for self-diffusion, approximately 36 kcal per mole1,2 Where the activation energy is the same as the activation energy for self diffusion, it has been proposed that the relaxation phenomena is dependent upon vacancy formation and motion. It is apparent therefore, that, in this aluminum-aluminum oxide SAP-Type alloy, the relaxation must be due to another type of atom transport. It has been shown previously in studies of the high-temperature, low-stress, steady-state creep behavior of as-extruded aluminum SAP-Type alloys, that the activation energy for steady-state creep is one that may be characterized by the nucleation of dislocations from the grain boundaries. It is proposed that the relaxation behavior observed here is due to a similar effect. In this case, the internal-friction peak is a resonance behavior due to the time-dependent nucleation of dislocations from grain boundaries in the sample. A process of this type would have an activation energy which is undoubtedly stress-dependent and of the form Q = Q, + (dQ/du)u

Jan 1, 1962

By R. G. Weavind, R. S. Young, I. Wolf

ONE of the most important fields of investigation at the Diamond Research Laboratory in Johannesburg is concerned with improvements in metallurgical practices for the diamond mining companies, with particular reference to increased recoveries of the smaller industrial stones. Considerable work has been done on the possible application of flotation processes to the diamond industry. From the viewpoint of recovery processes, diamonds in their natural state may be grouped into two classes, the water-repellent diamonds, which adhere to a grease surface, and the water-avid diamonds, which, because of their wettability, will not adhere to a grease surface and must be recovered by means other than the grease tables used for water-repellent diamonds. Experiments in the flotation of small diamonds from both kimberlite and alluvial deposits indicate the following conclusions: Water-repellent diamonds: Satisfactory flotation of —16 mesh diamonds, which are naturally water-repellent, may be accomplished using either Aero-float 25 together with cresylic acid, or Du Pont B23 as frother together with kerosine as auxiliary oily conditioner or froth stiffener. The quantities of reagents required are of the order of 0.15 lb per ton Aerofloat and 0.18 lb per ton cresylic acid. The use of acid circuits is detrimental, and for best results a pH between 7 and 9 should be maintained. R. G. WEAVIND and I. WOLF are with the Diamond Research Laboratory, Johannesburg, South Africa, and R. S. YOUNG, Member AIME, is Director of Research, Diamond Research Laboratory. TN 76B. Manuscript, March 23, 1951. A flotation period of 5 to 10 min is necessary to insure that all floatable diamonds are removed. Diamonds larger than 16 mesh cannot be recovered satisfactorily by flotation. Xanthates do not act as collectors for diamonds, and this is probably associated with their inability to impart a water-repellent surface to this mineral. Water-repellent diamonds smaller than 28 mesh can be floated quite well by the addition of a frother alone, such as pine oil or Du Pont B23. Water-avid diamonds: Partial flotation of the smaller sizes of wettable diamonds can be achieved by preconditioning with fatty acid soaps, cationic amines, and similar reagents, which will impart a water-repellent film to diamonds. Washing to remove excess reagent, followed by flotation, will result in a fair recovery, but the latter is much lower than for water-repellent diamonds. Crushed boart: Recovery of crushed boart from the waste products of industrial uses is best accomplished by first conditioning the diamonds present in the mixture with fatty acids, cationic amines, etc., removing the conditioning agent by washing, and floating in a cell of the pneumatic type. Flotation reagents found to be most suitable are Du Pont B23, and Aerofloat 25 together with cresylic acid. The optimum quantities are 1.2 g Du Pont B23, and 0.55 g Aerofloat plus 1.4 g cresylic acid, per liter of pulp in the cell. A solids-to-water ratio of 1 to 4 is found to be the most suitable, and alkaline circuits are necessary for best results. Diamonds larger than 28 mesh are not recovered satisfactorily by this procedure, but for finer sizes flotation offers an excellent procedure for the reclamation of this strategic industrial material.

Jan 1, 1952

By T. R. Ingraham

When aluminum sulfate was decomposed in an evacuated apparatus and the sample cooled, Q alumina was found. The thermodynamics of the decomposition reaction were resolved by measurements of the total pressure of SO3, SO2, and O2 generated over the sample at various temperatures. The results were correlated with other published data to calculate the rmges of thermodynamic stability of the various compounds involved. The thermal decomposition of aluminum sulfate was studied by Wijhler, Pluddeman, and Wöhler1 and by Warner and Ingraham.2 The results of both studies were critically reviewed by Kellogg,3 who observed that "each set of data shows considerable scatter and strong curvature on a plot of log pso3 vs 1/T".3 He agreed with Warner and Ingraham2 that both the discrepancy in the two sets of results and their curvature may arise from the indefinite properties of the particular form of A12O3 which is formed during the decomposition. While studying the thermal stability of other sulfate systems, we had noted the presence of nonequilibrium oxide properties in both the cobalt4 and manganese5 systems, but neither had shown any appreciable curvature on a logPSO, vs 1/T relationship, and the data from both systems agreed reasonably well with prior work. It therefore seemed reasonable to reexamine the technique which had been used in our earlier work on aluminum sulfate.2 The principal difference was that a tightly compacted pellet had been used for the earlier aluminum sulfate work, whereas a loose powder, contained in a platinum boat, was used for our work on other sulfate systems. In addition, a better technique had been developed for dehydrating the samples. From work done on the nickel system,6 we had become aware of the highly protective nature of some sulfate layers on their oxjdes, and hence of the necessity of providing a large surface area of P3e sample when equilibrium was to be attained in a reasonable time. That observation suggested that perhaps a steady state, rather than equilibrium, had been reached in the earlier work on aluminum sulfate. This paper reports a repetition of the experimental work with large, finely divided samples of anhydrous aluminum sulfate. APPARATUS AND PROCEDURE The apparatus used in the experimental work was described in earlier papers.2,7 The source material was Anachemia reagent-grade Al2(sO4)3 - 18H2O which was first partly dehydrated by heating at 400°C for 48 hr and then completely dehydrated by repeated baking of an aluminum sulfate-oleum slush to dryness at 450°C. ? Alas was prepared by decomposing some of the sulfate in a muffle furnace at 800° C overnight. Approximately equal amounts of the 7) alumina and aluminum sulfate were used in the experiments. The finely divided samples were handled under dry box conditions, and in addition some of the aluminum sulfate was decomposed in the apparatus while it was under vacuum, to ensure its complete dehydration prior to sealing the apparatus. The samples were heated to a series of constant temperatures on both increasing- and decreasing-tem-perature programs. Two to three days were required to obtain steady readings of the total decomposition pressure on an increasing-temperature program, and 5 to 6 days on a decreasing-temperature program. Three samples were examined on both programs. Within experimental error, the results for each sample and each program could not be distinguished.

Jan 1, 1969

By James Kemp

PostScript to a paper presented at the New York meeting, February, 1915, and printed in Bulletin No. 98, February, 1915, pp. 129 to 154. The writer looked over the quarry with care in the search for fossils, having in mind shells or corals of fairly large size. In the brilliant summer sunshine, none were observed on the glaring white ledges. The impression was gained that none were present and the statement to this effect was made in the edition of this paper published in the Bulletin' of the Institute for February, 1915, p. 136. On closer examination in the laboratory it has been discovered that the limestone itself is made up of minute organisms, which are clearly revealed by microscopic examination of thin sections. The principal component of the rock is a small foraminifer, 0.1 to 0.3 in. (2.5 to 7 mm.), of the genus Orbitoides, presumably an Oligocenic form. Figs. 1 and 2. illustrate it. The accompanying description has been kindly summarized by Marjorie O'Connell, M. A., Curator in Paleontology in Columbia University, who first detected the evidences of organisms in the rock. Orbitoides kempi O'CONNELL N. SP.1 The foraminiferan which makes up the Seboruco limestone is an Orbitoides of a Species new to North America. The only Orbitoides heretofore described from this country is 0. mantelli from the lower Oligocenic of the Gulf States. This form from Cuba, then, so different in all of its characteristics from the 0. mantelli, is of great interest as perhaps forming a basis of correlation over wide areas. The most closely related Species is 0. dispansa Sowerby, which occurs in the Nummulite limestone of the Eocenic of the Bavarian . Alps, in the Priabona beds of the lower Oligocenic of Massano, and elsewhere in Italy, as described by Gümbel.2 The age of the limestone in Cuba would thus Seem to be of upper Eocenic or lower Oligocenic age, probably the latter. The fossil has the form of a sphere Surrounded by a wavy rim of horizontal extent, the whole resembling two flat-brimmed, round-crowned hats placed base to base. The total extent of the Shell ranges up to 7+ mm., while the thickness of the central sphere is 2.5 mm. in one of the largest individuals. Like all of the other Species of Orbitoides, this form begins with a Single layer of chambers which multiply in one plane and assume a circular outline; but it is in the subsequent growth that the distinguishing specific characters appear, for the chambers at the central portion of the shell increase more rapidly than do those near the periphery and in consequence a Swelling is produced which finally gives the Spherical form which is so characteristic. The rim, on the other hand, shows little chamber-increase and remains thin. This is clearly Shown in the sections figured, where the central row of larger chambers forms the equatorial zone. Radiating from this row, in section, there appear, a number of solid cones alternating with broad reticulated ones. The solid cones mark the more dense structure forming the walls surrounding the reticulated or chambered cones. These appear upon the Surface as distinct pits, whereas the solid part appears as raised walls.

Jan 7, 1915

By M. E. Learmont, R. J. Lipp, I. Iwasaki

In the selective flocculation of iron ores, the concentration of alkaline earth ions in pulp solutions plays a critical role. Sodium silicate, alone or with sodium tripolyphosphate, has been used as a dispersant. When Ca+ + concentration exceeds 15 to 20 ppm, however, only a strong complexing agent, such as ethylenediaminetetraacetate (EDTA) was found to be effective (Heerema, Lipp, and Iwasaki, 1979). Some iron ores release Ca+ + in excess of 20 ppm. With ores that contain gypsum, the Ca+ + concentration may reach several hundred ppm. The purpose of this investigation was to compare the effectiveness of EDTA with nitrilotriacetate (NTA) in countering the adverse effects of Ca+ +, particularly at high Ca+ + concentrations. Emphasis was placed on the use of NTA since it is more cost-effective than EDTA. It is also used in detergents in some countries (Malaiyandi, Williams, and O'Grady, 1979). NTA, like EDTA, forms a soluble complex with Ca+ + with a 1:1 molar ratio. Its structure and the value of log Kca are given below together with EDTA (Shibata, 1963). [ ] For experimental materials, an equal weight mixture of Lac Jeannine hematite and a high-purity quartzite from Thompson, MN, both ground to - 30 µm (- 560 mesh) was used. Selective flocculation test conditions and procedures were identical to those used in previous investigations (Heerema, Lipp, and Iwasaki, 1979). The optimum level of starch addition for the above mixture was determined to be at 300 g/t (0.6 lb per st). Initially, a series of selective flocculation tests were performed on the mixture pulped with 10-3M CaC12 (40 ppm Ca + +) at pH 11. With no NTA present, flocculation of the entire suspension resulted. The selectivities achieved in tests with 90, 100, and 150% of the stoichiometric amount of NTA were virtually identical to each other and also to the selectivity of separation obtained in the absence of Ca+ + Such an observation could have been expected since Ca+ + concentrations up to a few ppm may be tolerated in selective flocculation (Krishnan and Iwasaki, 1982). A similar series of tests were performed at 10-2M CaC12 (400 ppm Ca+ +). The results are shown in Fig. 1 as grade¬recovery curves. For comparison, the results obtained in the absence of Ca++ are included. At 90% of the stoichiometric amount of NTA, a large enough concentration of uncomplexed Ca+ + was left in solution to cause indiscriminate flocculation. Note in this figure that NTA is capable of countering the adverse effect of Ca+ + even at this high concentration when it is used in excess of stoichiometric amounts. The free Ca+ + concentrations at 100 and 150% are calculated to be 2.5 and 0 ppm, respectively. [ ] The relative effectiveness of NTA and EDTA was then compared at 100% of the stoichiometric amount using 10-2M and 10-3M CaCI2 (Fig. 2). EDTA appears to be slightly more effective than NTA. The free Ca++ of 0.02 ppm in 10-2M CaC12 with EDTA compared to 2.5 ppm free Ca+ + with NTA might account for the difference. As evident, prohibitively high additions of EDTA and NTA were required to complex high concentrations of calcium ion. The use of both of these agents would result in the accumulation of complexed Ca+ + in recycle water.

Jan 1, 1985

* Kennecott Copper Corp. gets Charles R. Cox as president on Jan. 1. Mr. Cox is resigning his position as president of Carnegie-Illinois to take the new post with Kennecott, left vacant by the death of Mr. Stannard in September. •The ECA signed a contract in December to advance X3,600,000 to Newmont Mining Corp. to aid development of lead and zinc mines in French Morocco. The funds are to be repaid in lead and zinc for the United States' stockpile over a period of seven years. The mines are owned by the Societe des Mines de Zellidja, with which organization Newmont is associated. • Under the direction of John M. Brooks, Jr., general manager, the Matahambra mine in Cuba, will probably produce sufficient tonnage to make 4 million lb of copper per month during 1950. The grade is presently running between 7 and 10 pet. •S. H. Ash reports that the fatality rate per million-man-hr for the anthracite industry for 1949, through November, is 0.78. This is 15 pct better than that achieved during 1948, which was the lowest fatal injury rate in coal mining history. The first full year on record without a major disaster was recorded in 1949 (p. 34). •The Atomic Energy Commission has authorized the production of 200 lb of uranium metal for use under AEC license in non-Commission research projects. •A national survey of projected 1950 purchases of new machine tools, machine tool accessories, materials handling equipment, etc., just completed by the American Society of Tool Engineers reveals that, of the companies reporting, 80 pct state that they plan to buy either more equipment or the same amount as in 1948. • Armour Research Foundation is conducting investigations for the use of clay and shale deposits to make lightweight aggregates. The material is heated until it expands and forms material suitable for mixing with cement which it is hoped will be lighter, stronger, have better insulating qualities and will lower the cost of concrete. •In the first six months of 1949 the bituminous coal miners' average hourly earnings were $1.94 -as compared with X1.392_ national average for all manufacturing. Average annual earnings of full-time employees in the bituminous coal mines in 1948 were $3387 as compared with $2809 for all industry. •LaSalle Business Bulletin reports: "year ends on a rising trend in industry and trade ... nearly record-breaking demand from almost all sources keeps business high... most indicators but little below postwar peak... forces keeping activity high arestill powerful--changes in general business conditions likely to be slow and moderate." •Office of Internal Trade of the Commerce Department requests that technical data significant to the national security which is to be sent outside of the United States be submitted to it for an official opinion on the desirability of transmitting such information. This voluntary compliance program is part of our national security control. • Blast furnace slag reduced to 12 to 16 mesh is being used for sanding track at the Mont Coal mines of Armco. The slag replaces silica sand which caused silicosis. It has proved so effective and cheap that tests are being made to use the slag for rock dusting.

Jan 1, 1950

By B. Trafton, H. L. Hartman

An earlier paper1 introduced a rapid solution for mine ventilation network problems, employing the digital computer. In this paper, refinements and additions to the computer program which expand its scope of application and a solution to a ventilation network having a coal-mine configuration are presented. The revised program-written in FORTRAN for the IBM 7074 computer in Penn State's Computation Center-is applicable to any mine ventilation network employing natural splitting and having its fan located externally. It accomplishes the following: 1) Distributes an assumed total quantity of air flow among all airways of the network, performing iterations until an acceptable level of error is attained and the flow in each airway is known. 2) Computes the pressure drop (head loss) in all airways and the overall network and mine head losses. 3) Determines the operating point for the mine and a given fan, adjusting all air flows and head losses to the actual values. The basis of analysis used is the Hardy Cross method of successive approximation for solution of any fluid network, explained in detail in the earlier article. In brief, corrections to assumed air flows are computed for all the loops of a network; following distribution to the airways of each loop, the process is repeated until acceptable accuracy is attained. When a hand or desk-calculator solution is used, there is advantage to close approximation of the actual flows in the original assumption of air-flow distribution in the network. Since publication of the previous paper, in which assumption of initial quantities was also necessary in the computer solution, the program has been modified to make the first distribution itself, assigning the total quantity to one specified path in a split and then proceeding to correct the flows. The number of iterations required for a high-accuracy solution is little affected, at least in networks of few loops, 10 to 15 being sufficient to reduce the error to 1 pct or less. The principal limitation of the original program was that it contained no provision for handling a fan. Further, it did not determine the overall head loss in the network and was not designed for multiple parallel openings, such as occur in coal mines. The revised program was written to overcome these disadvantages and also to print out the adjusted flows for all airways, corrected for the system operating point. At the present time, the program can handle only an external fan. The procedure employed in solving a ventilation network is now as follows: 1) Input data consisting of airway characteristics and loop designation along with assumed direction of flow, for each branch of the network and any trunk airways, are fed into the computer. 2) Employing the resistance relationship, where R is resistance, K is friction factor, P is perimeter, L is length, A is area, and n is number of airways (where multiple intakes and returns are employed); values are computed for all airways. 3) An arbitrary, continuous route of flow through the circuit—from beginning to end—is selected and the path identified by airway numbers and read in. 4) Based on a total assumed quantity of flow Q (usually 100,000 cfm.) the computer employs the procedure described in the previous article in distributing quantities of flow among all the airways until a satisfactory level of accuracy has been attained (in the current program, the machine is turned off when the cumulative corrective error in cfm, is reduced to five times the number of airways). 5) Airway head losses H are calculated by the relation H = R Q2 and cumulated along the original designated flow route to find the overall head loss for the network. Trunk airways are then included to obtain the mine head.

Jan 1, 1964

By B. H. Caudle, W. J. Bernard

Factors which influence the success or failure of a waterflood can seldom be determined in the laboratory. For this reason pilot waterfloods are initiated in a repreventative portion of the oil reservoir in question. For a pilot flood to predict quantitatively the recovery to be expected in a field-wide waterflood operation, the pilot area must behave as though it were confined (surrounded by similar areas). In this study, laboratory fluid-flow models were used to determine the simplest pilot pattern, for particular conditions of mobility ratio and initial gas saturation, that would behave as though it were confined. Pilot patterns studied ranged in complexity from a single inverted five-spot to a grouping of nine regular five-spots. Only the innermost producing well in each pattern was studied. Model results showed that the optimum number of wells in the pattern depends upon the oil-water mobility ratio and the expected oil-bank size. Unfavorable mobility ratios will, in general, require more wells in the pilot pattern than will favorable mobility ratios. Pilot patterns in reservoirs which contain a dispersed, flowable, free gas saturation will require fewer wells than for the under-saturated case. The single inverted five-spot pattern was found to be unsatisfactory for predicting behavior of fully developed waterfloods. In particular, it is possible that, in reservoirs which contain a flowable, dispersed gas phase, the oil bank will never be observed at the producers due to the large amounts of free gas which continue to be produced with the oil. INTRODUCTION One method which has been used to predict the performance of a waterflood is the pilot flood. The pilot waterflood is a flood which involves only a small cluster of the reservoir wells and is located in a small, representative portion of the reservoir. The object is that oil produced from the pilot can, in some way, be related to the oil recovery to be expected from a field-wide expansion of the waterflood. However, these field pilot waterfloods have often been unreliable in the prediction of oil recovery in a fully developed waterflood. This unreliability has also been demonstrated in several laboratory studies of pilot floods. Some of the investigators have shown that there are situations in which the pilot flood oil production is far too optimistic with respect to the oil recovery in the fully de- veloped flood. Others4-G have shown that the pilot results can also be pessimistic, especially if the pilot waterflood is initiated in an oil reservoir which has been depleted by primary recovery and is at very low pressure. The major reason for this unreliability of pilot water-floods is the migration of fluids into or out of the pilot area. By the well-known method of images, if straight lines can be drawn to represent vertical planes of symmetry in a porous medium which contains pressure sources and sinks (injectors and producers), then these lines are invariant streamlines, or lines across which there is no potential gradient, and therefore no flow. In an actual reservoir, these lines of symmetry can never be established exactly because of reservoir inhomogeneities and irregular reservoir boundaries. However, if the reservoir is relatively large and contains wells in repetitive patterns, these lines of symmetry are commonly assumed to exist for the pattern units sufficiently far removed from the reservoir boundary. Lines of symmetry for the five-spot injection pattern are shown in Fig. 1. Each five-spot unit in this figure can be considered confined with respect to flow across its boundary. In pilot floods this is not the case. The lines of symmetry for the pilot patterns investigated in this study are shown in Fig. 2. It is obvious that the fluid within these pilots is not confined and is therefore able to migrate into or out of the pilot area. Intuitively, one can see that, if more wells are added to the pilot, the innermost unit tends to behave more and more like the confined pattern. However, there is a practical limit to the number of wells which should be placed in the pilot. This limit is usually determined by economic factors. It was the purpose of this study to use laboratory fluid-flow models to determine which of the previously mentioned pilot patterns will force the innermost producing well to behave as it would in a fully developed waterflood. Since fluid migration is influenced by initial saturation conditions and the mobility ratio, these factors were included in the study. The ultimate objective of this study was to develop data which would allow the operator to choose a pilot pattern and operating conditions that will yield a production history which can be applied directly as an estimate of the performance of each production well of the fully developed waterflood. BASIS FOR THE STUDY The basic problem of field pilot floods is the migration of the reservoir fluids into or out of the pilot area. This problem has been the subject of previously reported model studies on pilot floods. These studies have been concerned mainly with the development of arbitrary "correction factors" to be applied to the simple, unconfined pilot systems such as the single five-spot. The correction factors were intended to adjust the production history of the un-

• As part of $850,000 granted by the House Appropriations Committee for development of manganese in the U.S., the Bureau of Mines will build a pilot plant at Artillery Peak, Ariz., for development of low grade manganese ores. • The historic Argo tunnel and mill in Idaho Springs, Colo., will reopen shortly for the mining of uranium. The Uranium Co. of America has acquired control of the tunnel and mill and 12 nearby mining properties. J. H. Rodgers and G. C. Ridland will manage the operation. •The opening of a new 4000-ton per day coal mine in Washington Co., Pa., and the reopening of another mine of the same capacity in Fayette Co. has been announced by the H. C. Frick Coke Co. They'll help meet added war demands. •A 7000 bbl per day commercial synthetic liquid fuel plant, making gasoline from natural gas at Brownsville, Texas is being operated by the Carthage Hydro-col Corp., a Texaco subsidiary. The gasoline is produced by the Hydrocol process, chemically similar to the Fischer Tropsch process, but differing mechanically in several ways. To operate the process it has been necessary to build an oxygen plant producing 95 pct pure oxygen in quantities equal to U. S. production of commercial oxygen in 1946. •Over 96 pct of the class of 1950 at Montana School of Mines are now employed,, in industry, and they're scattered from MIT to the island of Cuba., • Cobalt, heretofore almost entirely imported, will soon be produced in Idaho. The Calera Mining Co. is building a 600-ton mill in which a cobalt and copper concentrate will be obtained from Idaho ores. •Plans for mining iron ore on the Conarky Peninsula in French Guinea, (an ECA project) call for equipment purchases as follows: 8 wagon drills, electric shovel for mining, conveyor for the port, 8 trucks, wrecker, 2 tractors, as well as miscellaneous accessories and spare parts. •A low-grade lead-zinc mineralization, located east of any known ore bodies in Utah's East Tintic district, has been located by a 2000-ft wildcat USGS drill hole. * Higher-than-going rates have been authorized by the Munitions Board for its stockpile program, where domestic production of scarce materials is low or uneconomical. Payment in excess of 25 pct over the foreign price is now permitted. •A new self-centering conveyor roll, developed by Carnegie-Illinois Steel, is expected to revolutionize materials handling. It completely eliminates the necessity for sideguides to keep materials on a conveyor. See P. 1028. •Great Britain's socialized coal industry employs twice as many miners, but produces less than half as much coal as America's coal industry. last year, British mines produced 28 million fewer tons of coal than the output of the same ,mines in 1939. Absenteeism amounted to a big 12 pot of working time. • Labor market conditions have tightened on almost a country-wide scale. Only 4 out of 143 major labor market areas have a substantial surplus -- less than half the total for May. Growing scarcities of skilled labor are in evidence.

Jan 10, 1950

By H. K. Martin

IN September 1954 the Lavender pit concentrator at Lowell, Ariz., began treating low grade porphyry copper ore from the nearby Lavender mine. Nominal capacity of the mill is 12,000 tpd, but production now averages 16,226 tpd. Plant design was somewhat affected by the re-use of old equipment and the substantial re-use of old buildings. A breaking-in period between June 24 and Sept. 1, 1954, was devoted to training operators and making minor changes in launders, chutes, and piping. From Sept. 1, 1954, to July 1, 1956, the mill treated 8,598,105 dry tons of ore, from which 556,541 tons of concentrate were produced, containing an indicated 144,055,185 lb of copper.

Jan 11, 1957

By J. P. Timmons, J. H. Moran, G. K. Miller, M. A. Coufleau

A prototype equipment has been designed and built for the digital recording of well logs on magnetic tape at the same time that the regular film recording is made. The format of the digital tape produced is such that it can be used directly at the input of the ZBM 704, 7090 or other models of ZBM computers which accept digital magnetic tape. This apparatus has been used for the experimental field recording of dipmeter tape logs which were subsequently computed by means of an ZBM 704 or 7090. In this paper the equipment and the digital tape are described briefly, and their application to the computer-interpretation of dipmeter data is discussed. A principal element in the interpretation of the dipmeter log is the correlation of the three microresirtivity dipmeter curves to determine the depth displacements between them. Several correlation methods for computer use are considered, with particular attention to their sensitivity to error and their consumption of computer time. The tape data were used to compute information content of the dipmeter microresistivity curves in terms of their frequency spectra. The results show that the sampling rate used in recording the digital information is quite adequate and illustrate a use of the digital tape in evaluating the characteristics of new tools. Some examples of field results are shown. It can be foreseen that, when digital tape recording becomes available for general field use, a whole new realm of possibilities will be opened up for the processing of other well logs through computations, which hitherto were not feasible because they were too laborious and time-con.sunzing. INTRODUCTION The last few years have seen a revolution in the design and production of data-processing equipment. Stored-pro-gram digital computers have progressed from a research curiosity to the basis of a major industry. There are now hundreds of such machines in daily use in the United States. With the acceptance of a technique that was, in fact, already clearly described by John von Neumann in 1945, the last decade has seen great strides in the development'of components, reliability, programming systems and, most spectacularly, in the sheer number of machines built and in use. In 1957 there were enough digital computers available to the oil industry to justify the suggestion that it would be worthwhile to investigate the possibility of using these machines in processing well log data.' The first result of this investigation was the appearance of what may be referred to as the input-output bottleneck. Well logs are customarily recorded on film. To get these data into a machine required then (and still does): a time-consuming semi-automatic reading of the film; conversion of the log data to digital form; and recording these digital data in some medium acceptable for computer input, such as cards, magnetic tape, or punched paper tape. However, the recording, reading, and re-recording could only result in deterioration of the data. Therefore, it was concluded that the fist step should be the development of a new, more direct recording technique supplemental to the film recording, which would provide easy access to the digital computer. There are many solutions to the problem of recording log data in an easily recoverable form. After careful consideration it was decided to adopt the boldest solution which, it was felt, was also the most elegant. It was decided to record well logs directly, in the field, on magnetic tape in such a way that this tape could be used without further modification as an input to the IBM 704 or 7090 computer. To realize practical field recording of magnetic tape logs, it became necessary to develop in a rather small package, an analog-to-digital converter, a tape recorder, and the necessary multiplexing and control circuits to allow the simultaneous recording of a multiplicity of logging signals. The magnetic tape recording was to be made simultaneously with the conventional logging operation in such a way as not to interfere with it. Along with the development of hardware, it was necessary to begin development of interpretation techniques and machine programs that would exploit the power of the digital computer. Here, again, there is a long list of possible applications. After much consideration it was decided to concentrate on the interpretation of the dipmeter log as a first application. It is the object of this paper to describe in some detail the developments sketched in the last three paragraphs.

By Victor A. Phillips

A series of strips of a Ni-12.7 at. pct A1 alloy were Prepared containing cubical y'(NisAl) precipitates with edge lengths from 60 to 500A. A particle-free solution-tveated strip was included for cornparison. They weve cold-rolled 95 pct and the effects of particle size on the isochronal (1/2 hr) annealing behavior between 300° and 950°C studied (by hardness and light and electron microscopy). It ulas inferred that the particles deformed with the lnatvix becoming lamellae which remained coherent. Comparison with published data fov pure nickel showed that aluminum greatly re-tavded softening and recrystallization, but it made little difference whether or not particles were present. The presence of pakticles led to a heterogeneous distribution of precipitates after annealing at 700" to 750°C. Recovery was not detected. Recrystallization occurred by the growth of new grains into unrecrys-tallized material. In a previous study by the author,' the growth of Ll2-type ordered yl(Ni3Al) precipitates was followed in Ni-12.7 at. pct A1 alloy as a function of aging at 600" and 700°C. The particles were showo to be cubical in shape in all sizes from 50 to 3000A and remained coherent. This work was used as a guide in preparing the starting structures for the present study of the effect of these particles on the annealing behavior of heavily cold-rolled strip. Another question of present interest was whether dislocation and particle hardening were additive, since the structures before rolling ranged from solution-treated to peak-aged to overaged. Also, precipitation might occur on annealing after cold-rolling. Reference may be made to other papers2"5 for previous work in this relatively unexplored field and only some recent work will be mentioned her:. phillips2 studied the effect of deformable 0 to 590A-diam cobalt particles on a Cu-3.23 pct Co alloy rolled 95 pct and found that the particles, which rolled out into thin lamellae, impeded softening and recrystallization. Tanner and servi3 likewise studied the annealing of cold-swaged Cu-2 pct Co alloy containing 150A-diam particles and found impeding effects. Haessner et a1.,4 on the other hand, found that incoherent 2-p-diam non-deformable particles of B4C (0.04 vol pct) tended to increase the rate of recrystallization of copper rolled up to 95 pct reduction. They attributed this to the formation of new grains at the particle interfaces. Humphreys and artin' found that nondeformable silica particles in copper rolled to 30 pct reduction accelerated recrystallization if the particle spacing was large and retarded it if the spacing was smaller. Haessner et a1 4 also studied a rolled Ni-Cr-A1 alloy; however, the particles of y'(Ni3Al)-type precipitate were not put in before rolling, but separated during the isothermal annealing at 750°C. No previous work appears to have been carried out on the effect of y' (Ni3A1) particles on the annealing of Ni-A1 alloy. Hornbogen and ICreye7 redetermined the solubility c of aluminum in nickel as a function of temperature T and showed that it was given by c = 32.6 exp(-1940/RT). This relation gives aluminum solubilities of 15.1, 14.2, 12.0, and 10.7 at. pct at 1000°, 900°, 700°, and 600°C, respectively. The phase precipitated from the nickel-rich solid solution is fcc y1 (Ni3A1) which has a Cu3Au -type ordered structure8 and remains ordered up to 1000°C.B EXPERIMENTAL PROCEDURE The alloy used was identical with that used before. Chemical analysis showed 6.27 wt pct (12.71 at. pct) Al, the principle impurities being 0.065 pct Fe, 0.022 pct Co, 0.020 pct Cu, and 0.004 pct C. Bar stock of 1 in. diam was cold-swaged to % in. diam, cold-rolled to 0.300-in.-thick strip, and annealed at 900°C in dry hydrogen. It was cold-rolled to 0.100-in. thickness and solution-treated for 1 hr at 1000°C while sealed in a quartz tube in argon, quenching in iced brine with the aid of a device to snap off the nose of the tube. Lineal analysis gave an average grain size of 0.055 mm. Pieces of strip were aged at 700°C in vacuo for 30 min, 51/4 hr, and 1 week to produce nominal average particle widths of 60, 150, and 500A, respectively, as known from the previous work.' The average diamond pyramid hardness was determined. The heat-treated strips were rolled from 0.100 to 0.005 in., a reduction of 95 pct, and the rolled strips stored at about -5°C. Small pieces were annealed within 1 week for 30 min at temperatures from 300° to 950° ±2°C in a horizontal vacuum furnace. Strips were withdrawn into a cooling zone, giving an estimated initial cooling rate from 950°C of about 50°C per sec. Average diamond pyramid hardnesses were determined on a lightly electropolished spot on the surface of each strip using 300-g load. Each point on the softening curves represents a separate annealed specimen. Sections containing the rolling direction were examined by optical metallography. Selected specimens were electrothinned to the center plane' and examined by transmission at 100 kv in a Siemens Elmiskop I electron microscope. It is well-known that changes in the structure tend to occur when a deformed strip is electrothinned below a thickness of a few hundred angstroms, although this is less serious with a material such as nickel which has a high melting point, and also is apt to be less serious when particles are present. Observations were nevertheless confined to thicker regions of the foils with estimated thicknesses over 1000A. No changes were observed due to beam exposure.

Jan 1, 1968

Jan 1, 1945

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Jan 1, 1938