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By Jack White

This paper gives details of the results of careful testing carried out on two types of ball mills, conical trunnion overflow and cylindrical grate discharge, on identical ore. The object of the test work was to determine which ball mill was the most economical to install for future extensions to the Mufulira concentrator.

Jan 1, 1950

The following is a report of the papers submitted to the Papers 'and Publications Committee during 1928: The Committee held nine regular meetings during the year 1928. During that period there were presented to the Institute 214 papers which were acted upon as follows: Accepted as Technical Pub1ications............................ 85 Declined for publication...................................... 16 Action pending, Dec. 31...................................... 25 Manuscripts held for annual volumes, Dec. 31................... 7 Withdrawn temporarily...................................... 1 Accepted as Preprints........................................ 20 Printed for first time in volumes.............................. 35 Published in Mining and Metallurgy........................ 12 Papers in Technical Publication No. 156 (Coal Classification) and not accounted for elsewhere in this table..................... 10 Mimeographed only*................................... 3 Total.................................................. 214 * A considerable number of papers were mimeographed for the annual meeting. Of the 85 papers accepted as Technical Publications 8 were reprinted in the Transactions, 7 in Proceedings of the Institute of Metals Division (1928), 7 in Iron and Steel Technology in 1928, 13 in Geophysical Prospecting, and 50 were in Technical Publication form on Dec. 31. Of the 20 papers accepted as Preprints 1 was reprinted in the Transactions, 13 in Petroleum Development and Technology in 1927, 2 in Geophysical Prospecting, and 4 were in Preprint form on Dec. 31. Of the 35 papers printed for the first time in the various volumes 8 were included in the Transactions, 2 in Proceedings of the Institute of Metals Division (1928), 1 in Iron and Steel Technology in 1928, and 24 in Petroleum Development and Technology in 1927. Of the 12 papers accepted for Mining and Metallurgy 1 was, accepted for Geophysical Prospecting and 1 for the Transactions. There were published in 1928 113 Technical Publications containing a total of 1928 pages, as against 88 in 1927, totaling 1528 pages. The Technical Publications published in 1928 were classified as follows: Group A, Metal Mining, 17 papers (361 pages); B, Milling and Concentration, 4 papers (39 pages); C, Iron and Steel, 15 papers (256 pages); D, Non-ferrous Metallurgy, 13 papers (191 pages); E, Institute of Metals, 36 papers (588 pages); F, Coal and Coke, 15 papers (392 pages); G, Petroleum and Gas, 10 papers (246 pages); H, Non-metallic Minerals, 3 papers (33 pages); I, Mining Geology, 18 papers (356 pages); K, Mining Administration, etc., 3 papers (47 pages); L, Geophysical Prospecting, 21 papers (430 pages).

Jan 1, 1929

By J. J. Luchessa

HAULAGE was one of the many problems to be solved in the successful handling of the Miami Copper Company's low-grade orebody. The ore extracted had to be increased from 1000 to 18,000 tons per 24 hours over the existing track-age and haulage way. This called for increased speed, longer trains, in¬creased car capacity, and a block signal system so as to maintain a fixed schedule and headway. The motive power in service at the time of this transition consisted of Baldwin-Westinghouse 6-ton trolley locomotives. (See Fig. 3.) These locomotives were purchased to handle twenty inverted-V-bottom side-dump cars of 60 cu. ft. capacity. Dimensions were limited as to height on account of ore chutes, width on account of short radius curves, and length of 12 ft. from bumper to bumper- so that the locomotives could be handled on the man and material hoist which has a cage length of 121/ ft. The limited length made it possible to bring the locomotives to the surface for periodic overhauling and major repairs such as changing wheel tires, gears, and

Jan 1, 1934

This excellent, concise paper by Dr. Iwasaki on the principles of selective flocculation for iron ores discusses many of the principles and problems which have occurred in our bench and pilot plant test-work. The use of sodium tripolyphosphate in combination with sodium silicate as a dispersant is very effective. However, this may cause a problem with the environmental groups as phosphorous is a nutrient. We have also established that the lower the Ca level in the pulp solutions the greater the dispersion. We have found that ores from the same geological strata, having the same general mineralogy and iron content will sometimes have widely different degrees of dispersion. There was-no difference in the gross mineralogy but the solubility of the Ca and SO ions was much less in the ores most easily dispersed. Research efforts should be directed towards a more practical means which would more easily enable one to predict the amount of dispersant required for the various ores. With regard to water quality we have found that waters having higher contents of SO4 and C1 ions hinder dispersion. This could be a method of controlling too much dispersion by the addition of sulfate or chloride ions. This would require further investigation. We have had no trouble with agitation speeds of up to 925 rpm in conditioning starch with the dispersed pulp prior to selective flocculation. We have found about 0.3Lb/LT of starch to be sufficient for selective flocculation on our ores. The increasing of the starch to 1.25Lb/LT has had no effect on the metallurgy of the selective floccula-

Jan 1, 1979

By G. E. McElroy

MUCH attention has been directed to mine-air flow in recent years, more especially in Great Britian where there is frequent reference to a theory of fluid flow developed by English engineers. Briefly stated, this theory is that for similar passages of the same relative roughness, in which fluid flow occurs, the conditions of flow are exactly the same for equal values of the product W D V/ µ, where W = density of the fluid, D = diameter of the passage through which flow occurs, V = mean velocity of flow, and µ = absolute viscosity of the fluid flowing. This, the "Reynolds Criterion" of fluid flow, had its origin in the work of Prof. Osborne Reynolds' more than 40 years ago. Later, Lord Rayleigh amplified the theory2 which has been conclusively proved for small pipes by the experiments of Stanton and Pannel3 over a large flow range, and by Lacey4 over a somewhat more limited range. Concordant results on small pipes have also been obtained by numerous other investigators with single fluids over more or less limited ranges of flow. According to this theory results in one medium, such as water, are immediately applicable to another, such as air; and experimental results on models are (theoretically, at least) applicable to full-scale designs. This is of great importance in aeronautics and can be of considerable value in mine ventilation research. Hodgson, in a recent paper,5 has outlined the application of this theory to mine-air flow and recent English experiments" on the resistance of a timbered mine airway have been expressed in this form.

Jan 10, 1926

By G. E. McElroy

Much attention has been directed to mine-air flow in recent years, more especially in Great Britian where there is frequent reference to a theory of fluid flow developed by English engineers. Briefly stated, this theory is that for similar passages of the same relative roughness, in which fluid flow occurs, the conditions of flow are exactly the same for W D V equal values of the product where W = density of the fluid, D = diameter of the passage through which flow occurs, V = mean velocity of flow, and p = absolute viscosity of the fluid flowing. This, the "Reynolds Criterion" of fluid flow, had its origin in the work of Reynolds1 more than 40 years ago. Later, Rayleigh2 amplified the theory which has been conclusively proved for small pipes by the experiments of Stanton and Panne13 over a large flow range, and by Lacey4 over a somewhat more limited range. Concordant results on small pipes have also been obtained by numerous other investigators with single fluids over more or less limited ranges of flow. According to this theory, results in one medium, such as water, are immediately applicable to another, such as air; and experimental results on models are (theoretically, at least) applicable to full-scale designs. This is of great importance in aeronautics and can be of considerable value in mine ventilation research. Hodgson, in a recent paper,6 has outlined the application of this theory to mine-air flow and recent English experiments6 on the resistance of a timbered mine airway have been expressed in this form.

Jan 1, 1927

By Martin Mayers

IT has long been recognized that it would be highly desirable to be able to predict the temperatures at various points in a burning fuel bed and their variations with changes of the properties of the fuel and the rate of air supply. Experimental investigations of fuel-bed tempera-tures1-4 have not been lacking, but the absence of any theoretical back-ground has made it impossible to use the results of these tests as a basis for prediction, except in a very general way. A mathematical analysis5, based on a somewhat simplified theory of the distribution of heat in a, fuel bed, has recently been completed by the author. Even though numerical values of some of the coefficients are not. known, the calcula-tions result in some conclusions of general significance. Thus, for example, it appears that when the temperatures throughout the fuel bed can be calculated, the rate at which ignition of the fuel by underfeed action can be maintained can also be calculated. The uncertainty concerning the values of the coefficients referred to above is a serious limitation on the use of that method. The following paper presents a discussion of these coefficients and includes estimates of their values based on the data now available. A brief description of the theory on which the analysis is based, and some results of the calculations showing their degree of agreement with experimental results, are presented by way of introduction to the discussion of, the coefficients. For a more extended discussion of the theory, see the A.S.M.E. paper5.

Jan 1, 1937

By W.G. Harbert, C. Upthegrove

DURing the past year considerable work dealing with physical properties of cartridge brass was done at the University of Michigan in cooperation with the Ordnance Department of the U. S. Army. This paper gives some of the data bearing on the effect of the anneal, previous to the final reduction-or rolling, on the physical properties, particularly the hardness. Various phases of the subject of physical properties of cartridge brass have been presented by different investigators. Mathewson and Phillips1 refer to the work of Grard, in 1909, as the first systematic presentation of the relation between temperature and time of anneal, changing of physical properties and microstructure, and the previous reduction by cold rolling. They discuss the relation between time and temperature of annealand the previous reduction by cold rolling; also the relation between physical properties and grain size of annealed brass. The degree of deformation previous to the annealing was found to determine the temperature at which recrystallization and corresponding changes in physical Properties would take place. relation between grain size and Brinell hardness, found the hardness for low-temperature annealing to be dependent on the previous degree of reduction, while for anneals above a certain temperature the hardness after the anneal was independent of the degree of reduction. Actual differences in hardness, due to the degree of reduction, disappear only on annealing at 600" C. or above; though the differences for metal subjected to different degrees of reduction and annealed at temperatures between 350" and 600" C. were found to be relatively small. In their determination of the relationship of grain size to Brinell hardness, Bassett

Jan 1, 1923

By W. G. Harbert, C. Upthegrove

DURing the past year considerable work dealing with physical properties of cartridge brass was done at the University of Michigan in cooperation with the Ordnance Department of the U. S. Army. This paper gives some of the data bearing on the effect of the anneal, previous to the final reduction-or rolling, on the physical properties, particularly the hardness. Various phases of the subject of physical properties of cartridge brass have been presented by different investigators. Mathewson and Phillips1 refer to the work of Grard, in 1909, as the first systematic presentation of the relation between temperature and time of anneal, changing of physical properties and microstructure, and the previous reduction by cold rolling. They discuss the relation between time and temperature of annealand the previous reduction by cold rolling; also the relation between physical properties and grain size of annealed brass. The degree of deformation previous to the annealing was found to determine the temperature at which recrystallization and corresponding changes in physical Properties would take place. relation between grain size and Brinell hardness, found the hardness for low-temperature annealing to be dependent on the previous degree of reduction, while for anneals above a certain temperature the hardness after the anneal was independent of the degree of reduction. Actual differences in hardness, due to the degree of reduction, disappear only on annealing at 600" C. or above; though the differences for metal subjected to different degrees of reduction and annealed at temperatures between 350" and 600" C. were found to be relatively small. In their determination of the relationship of grain size to Brinell hardness, Bassett

Jan 1, 1923

By J. S. Harris

AS a result of the study of social problems to which so much thought has been given in this country and Europe in the last half century, many employers of labor have come to think that some provision should be made for their workingmen in case of injury. There has been a growing tendency so to administer the laws governing industrial pursuits in these countries as to add self-interest on the part of capitalists, to the plea urged by humanity, that every possible care should be taken to guard the workers from accident; but as no care can guarantee immunity, there is a necessity to supplement these precautions by some method of providing pecuniary aid that shall be available when disabling accidents do occur. It was once a favorite idea of theorists on political economy, that in the ideal state of society every man should take care of himself, and that the less care or control there was assumed by any man over others' private affairs, the better; but this gospel of selfishness has had its day, and it is now generally recognized that in the existing state of affairs the stronger and richer cannot escape the duty of being to some extent, the keepers of their less fortunate brethren ; and, on the other hand, that an assumption of care for them involving to some extent an exercise of authority, is not a thing to he necessarily and always resisted. Out of these convictions, many efforts for the amelioration of the condition of workingmen have grown—which or one result have produced various plans which combine the con-

Jan 1, 1884

By C. Upthegrove

DURING the past year considerable work dealing with physical properties of cartridge brass was done at the University of Michigan in cooperation with the Ordnance Department of the U. S. Army. This paper gives some of the data bearing on the effect of the anneal, previous to the final reduction or rolling, on the physical properties, particularly the hardness. Various phases of the subject of physical properties of cartridge brass have been presented by different investigators. Mathewson and Phillips1 refer to the work of Grard, in 1909, as the first systematic presentation of the relation between temperature-and time of anneal; changing of physical properties and microstructure, and the previous reduction by cold rolling. They discuss the relation between time and temperature of anneal and the previous reduction by cold rolling also; the relation between physical properties and grain size of annealed brass. The degree of deformation previous to the annealing was found to determine the temperature at which recrystallization and corresponding changes in physical properties would take place. Bassett and Davis,2 in establishing the relation between grain size and Brinell hardness; found the hardness for low-temperature annealing to be dependent on the previous degree of reduction, while for anneals above a certain temperature the hardness after the anneal was independent of the degree of reduction. Actual differences in hardness, due to the degree of reduction, disappear only on annealing at 600° C. or above; though the differences for metal subjected to different degrees of reduction and annealed at temperatures between 350° and 600° C. were found to be relatively small. In their determination of the relationship of grain size to Brinell hardness, Bassett

Jan 5, 1922

By James S. Browning

For the past several years, USBM has conducted laboratory and continuous process development work on the weathered mica pegmatites ores of Alabama, Georgia, and North Carolina to determine the feasibility of recovering commercial-grade mica concentrates by flotation. The research has resulted in the development of two processes for flotation of mica: 1) an acid-cationic method for recovery of coarse mica and 2) an alkaline-anionic-cationic method for recovery of fine mica. The research indicated that the two processes may be effectively utilized separately or in combination for flotation of mica from weathered pegmatite ores. This report summarizes the process development work, and demonstrates the feasibility of producing commercial-grade concentrates with a high recovery of the contained mica. Mica mining in the United States is confined largely to pegmatites and schists in a few well-defined areas. The largest region extends from central Virginia southward through western North and South Carolina, northern Georgia, and east-central Alabama.'" Whereas in western North Carolina, these pegmatite dikes are weathered to only a shallow depth, they are deeply weathered in the Carolina Piedmont and in Georgia and Alabama. Particularly in Georgia and Alabama, mica is found in the decomposed slates and schists adjacent to the pegmatites, and in deeply weathered granites. Most flake mica is obtained as the major marketable product by crushing and milling pegmatites4 To a lesser extent, mica is produced as a byproduct of feldspar" and spodumene. Past research by U.S. Bureau of Mines (USBM) has developed two methods for mica flotation. One method utilizes acid-cationic flotation for recovery of mica.' This method requires thorough desliming of the ore with consequent fine mica losses. The other utilizes an alkaline-anionic-cationic process for recovering fine-size mica from pegmatite ores after desliming sufficiently to remove clay materials but not so drastically as to remove the fine mica.8-18 The latter process has also been successfully applied to a micaceous schist ore from California.' This report summarizes the results of these research studies. Both of the flotation processes developed by USBM have been adopted by the mica industry and are being commercially utilized separately and in combination for flotation of mica from weathered pegmatite ores. Description of Ores The weathered mica pegmatite ores used in the investigations were obtained from commercial mica operations in Alabama, Georgia, and North Carolina. The

Jan 1, 1971

By J. H. Swisher

The rate of internal sulfidation of austenitic Fe-Ti alloys in H2S-H2 gas mixtures is controlled primarily by sulfur diffusion, with counterdiffusion of titanium playing a minor role. At temperatures below 1100°C, enhanced diffusion along grain boundaries becomes important. The rate of internal sulfidation at 1300°C is approximately equal to the rate computed from the sulfur diffusion coefficient. The diffusion coefficient of titanium in y iron has been determined from electron microprobe traces in the base alloy near the subscale interface. The solubility of sulfur in Fe-Ti alloys has been measured in the temperature range from 1150° to 1300°C. The equilibrium sulfur content is found to increase with titanium content, due to the large effect of titanium on the activity coefficient of sulfur. The Ti-S interaction becomes stronger as the temperature decreases. TITANIUM as an alloying element in stainless steels is an effective scavenger for interstitial impurities, carbon in particular. Titanium is known to form stable sulfides; however extensive thermodynamic data on the Ti-S system are not available. Schindlerova and Buzek1 have shown that the Ti-S interaction in liquid iron is moderately strong. There have been no previous studies of the Ti-S interaction in solid iron. Internal sulfidation of Fe-Mn alloys was the subject of a recent investigation by Herrnstein.2 He found the rate of internal sulfidation to be an order of magnitude greater than predicted from available solubility and diffusivity data. A satisfactory explanation for the discrepancy could not be given. In the present study, the solubility of sulfur in austenitic Fe-Ti alloys was measured using a standard gas equilibration technique. Fe-Ti alloy specimens were also internally sulfidized. The rate of internal sulfidation was measured as a function of temperature and alloy composition. Supplementary electron micro-probe measurements were made to provide additional information on the nature of the internal sulfidation process. EXPERIMENTAL The starting materials were alloys containing 0.12, 0.24, 0.38, and 0.54 wt pct Ti. The alloys were made in an induction furnace by adding titanium to electrolytic iron that previously had been vacuum-carbon-deoxidized. The major impurity in the alloys as determined by chemical analysis was carbon. The carbon content of the alloys averaged about 100 ppm; metallic impurities were presented in concentrations of 50 ppm or less. Specimens were made in the form of flat plates, 0.03 by 2 by 4 cm for the equilibrium measurements and 0.5 by 1.5 by 3 cm for the rate measurements. The experiments were performed in a vertical resistance furnace wound with molybdenum wire and containing a recrystallized alumina reaction tube. In the gas train, flow rates of the reacting gases were measured using capillary flow meters. The source of H2S was a mixture of approximately 2 pct H2S in H2, which was obtained in cylinders from the Matheson Co. A chemical analysis was provided with each cylinder. The H2-H2S mixture was diluted with additional hydrogen to obtain the desired ratio of H2S to H2, and the resulting mixture was diluted with 30 pct Ar to minimize thermal segregation of H2S in the furnace. Argon was purified by passage over copper chips at 350°C and subsequently over anhydrone. Hydrogen was purified by passage over platinized asbestos at 450°C and then over anhydrone. The H2-H2S mixture was purified by passage over platinized asbestos and then over Pas. The samples used in the solubility measurements were analyzed for sulfur by combustion and iodometric titration. The subscale thickness in the internally sulfidized samples was measured on a polished cross section, using a microscope with a micrometer stage. Electron microprobe traces for titanium in solution were made on several samples that had been internally sulfidized. A Cambridge microanalyzer was used, and the known titanium content at the center of the specimen was used as a calibration standard. The procedure for the microprobe measurements will be described further when the results are presented. RESULTS AND DISCUSSION Equilibrium Data. Fig. 1 shows the sulfur concentration as a function of gas composition for three alloys equilibrated at 1300°C. The dashed line is based on data published by Turkdogan, Ignatowicz, and pearson3 for pure iron. The breaks in the curves are the saturation points for the alloys. The fact that the initial slope decreases with increasing titanium content indicates that titanium interacts strongly with sulfur in solution. To obtain information on the composition of the precipitating sulfide phase, the measurements described in Fig. 1 were extended to higher sulfur partial pressures. These results are shown in Fig. 2. (The initial portions of the curves are reproduced from Fig. 1.) The highest PH2s /pH2 ratio used is believed to be below the ratio required for the formation of a liquid sulfide phase. Time series experiments were used to study the approach to equilibrium in the samples. It was found that equilibrium with the gas phase was reached in less than 4 hr at 1300°C.

Jan 1, 1969

By D. S. Gleason, D. E. Severson, D. R. Skidmore

Pittsburg and Midway Coal Co. has modified the German Pott-Broche process, on which patents date back to 1927, to produce on a bench scale liquid products by solution hydrogenation of coal. A continuing program of lignite solution-hydro gena-tion experiments is directed toward investigating coal solution reactions, determining favorable conditions for the solution refining of lignite by the Pott-Broche process, and investigating some of the uses for the de-ashed product obtained from lignite The German Pott-Broche process1" on which patents date back to 1927, has been modified by the Pittsburg and Midway Coal Co., a Gulf Oil subsidiary, to produce on a bench scale liquid products by solution -hydrogena-tion of coal." The objectives of the present effort are to investigate coal solution reactions, to determine favorable conditions for the solution refining of lignite by the Pott-Broche process, and to investigate some of the uses for the de-ashed product obtained from lignite. This paper is a summary of results to date in a continuing program of lignite solution-hydrogenation experiments. The coal solution reaction program has several principal aims. The first of these is to determine whether lignite can be successfully dissolved in solvents that might be practical for commercial development. The second object is to determine whether the solvents function after successive cycles of use, recovery, and reuse. It seems necessary to the economics of a potential commercial process that the solvent be recycled. Third, it is desired to learn something about the distribution of the ash constituents between cake and filtrate. The extent of ash removal is important. The nature and quantity of mineral matter passing through the filter may determine end-use marketability. For certain use applications, trace quantities of certain minerals can be objectionable, e.g., titanium and vanadium must be very low in electrode carbon for aluminum production. The Solution Reaction The coal solution Process involves an extremely complex system of chemical reactions. An initial solvent such as anthracene oil is a mixture of hundreds of different compounds with a boiling range of roughly 500" to 750°F at atmospheric pressure. The coal macro-molecule is broken down by thermal decomposition and solvent action into myriads of different compounds, some the same as those comprising the solvent. This similarity in structures opens up the possibility of production and subsequent recovery of solvent. Some solvent is inevitably lost by reaction. Regeneration of solvent was not a problem in the early German Pott-Broche plant. The coal refinery was an integral part of a petroleum refinery complex and replacement solvent was readily available. A coal refinery using lignite, however, might be isolated from other hydrocarbon processing facilities and the regenerability of solvent could be vital to the economic success of the venture. Several structural features of the solvent molecules have been cited as important to the coal solution process.'. The first of these is aromaticity of the material, the second, ability to transfer hydrogen to another molecule, as for example the ability of tetralin to transfer hydrogen and be converted to naphthalene. Finally, the presence of hydroxyl groups on aromatic rings within the molecule, i.e., phenolic character, seems beneficial. Mixtures of pure compounds have been tried by various investigators. Mixtures of o-cresol, a phenolic substance, and tetralin were found to dissolve bituminous coal better than either substance alone.3 This maximum solubility was not found with lignite." Hydrogen contributes to the reaction by hydro-genolysis and by combining with free radicals and molecular "loose ends" to stabilize the compounds formed in coal depolymerization. High boiling point, and correspondingly high molecular weight, seems to be a property which improves solution potential for coal with a given type of compound.' The maceral components of the coal appear to have an important bearing on its ease of solution. The fusain portion is quite inert to solvent action, but the an-thraxylon material dissolves quite readily.3 The hydrogenation reaction can be improved by the use of a catalyst; commercial hydrogenation catalysts having been found effective. Although cost is involved in the use of catalyst and catalyst recovery, the resulting saving in time and perhaps lowered temperature or pressure might justify their use in the solution refining process and decrease the total process costs. Apparatus and Procedure The coal solution runs were made in a 1-gal stainless steel stirred autoclave. The autoclave was provided with thermocouple wells and a transducer to permit continuous recording of temperature and pressure. The autoclave stirrer was magnetically driven, eliminating the leakage inherent with a rotating pressure seal. For runs in which a catalyst was used, the catalyst in the form of beads was placed in a wire mesh container mounted on the stirrer shaft. A control system programmed the heatup and reaction cycle. The permissible heating rate was 5°F per min because of the need to minimize thermal stress in the autoclave body. The temperature was raised at that rate until the reaction temperature was attained and then the temperature was held constant for the desired length of time. The maximum temperature seldom exceeded the average run temperature by more than 15°F.

Jan 1, 1971

By P. L. Rittenhouse, M. L. Picklesimer

A rapid and seniquantitative method of determining prefered orientation on large numbers of. Zircaloy-2 specimens was desired. knoop microhardness measurerrzetzls were irvestigated as a solldtion to this pro6lem. The variation of Knoop microhardness measurerlerzts on selected planes as a function of 'irzdenle axis relutilje lo cryslallograplzic or fabrication divectals were used to corzstrrcl a polar coordinate hardness contour map. With use of an empirical relationslip between the single-crystal hardnesses and those of the polycrystalline material conentional pole figures could be constructed which compare favorably also obtained. To determine preferred oriention qualitatively from hardness data requires a minimum of twelve measurements per plane on three, preferattention to grain size, specimen prepartion, and in-rreinetzt, and analjlsis is of the order of- 45 to 60 rrin. THE design of structures from Zr alloys requires consideration of preferred orientation and the resulting anisotropy of mechanical properties. Rapid and semi-quantitative methods of evaluating anisotropy and of determining preferred orientation are needed for quality control and for examining the large number of test specimens required in development programs. The variation of Knoop microhardness with indenter orientation has been studied in single crystals of several hcp metals including titanium.' beryllium,' magneium, and zinc.4 The maximum hardness observed on any crystallographic plane other than the basal plane invariably occurred when the long axis of the Knoop indenter was either parallel or perpendicular to the projection of the [ OOOI.] direction on the plane of examination. When the major slip mode was (0001)(i2i0j the maximum hardness occurred at the parallel positio! but when the operating slip system was {10i0) (i210) the hardness was a maximum perpendicular to the [0001] projection. A minimum hardness was always observed at a rotation of 90 deg from the maximum. It follows that the orientation of the projection of the [0001] can be determined on any non-basal plane by making hardness measurements at a number of indenter orientations. The determination of the orientation of the [0001] projection on two non-parallel, preferably orthogonal, surfaces of the specimen will allow location of the [0001] direction in the specimen. It seems possible that such measurements could be used to examine, at least qualitatively, the preferred orientation existing in polycrystalline hcp materials. An investigation of the microhardness anisotropy in Zircaloy-2 was undertaken to ascertain whether these measurements could be used for this task. EXPERIMENTAL PROCEDURE Single crystals of Zircaloy-2 were grown by an a-8-a annealing sequence using electron-beam heating.= The orientation of the crystals was determined by a conventional back-reflection Laue technique. The crystals were then mounted on a goniometer head and the desired crystallographic faces were milled and chemically polished. Polycrystalline Zircaloy-2 specimens were prepared from fabricated sheets or plates. Inverse pole figures for these materials were obtained using the X-ray diffraction techniaue described by Jetter, McHargue, and illiams.' A Wolpert-Greis Micro-Reflex hardness-testing machine was used to make the Knoop microhardness measurements. The single-crystal and polycrystalline specimens were loaded to 0.5 and 2.0 kg, respectively. Determination of the scatter of hardness numbers as a function of applied load for several indenter orientations on several specimen surfaces showed that the loads selected were the lightest consistent with minimum scatter. Heavier loads did not appreciably decrease the scatter and produced hardness impressions too large to be conveniently measured with the equipment used. Seven crystallographic planes of the single crystals were examined, while six planes of examination were used in studying Zircaloy-2 polycrystals. The specimens were rotated 10 to 15 deg after each measurement and from four to eight impressions were made at each angle of rotation. RESULTS The two angles which were used to relate crystallographic directions and planes in the hcp cell to the planes of examination of the single crystals are shown in Fig. 1. 8 is the angle between the c axis. [0001]. and the normal, N, to the plane of examination. a is the angle between the long diagonal of the Knoop indenter and the projection of the c axis on the plane of examination. For exampIe, if P = 90 deg and a = 0 deg, the plane of examination is of the family

Jan 1, 1967

By P. M. Robinson, M. B. Bever

THE heats of formation at 273°K of the compounds InBi, In2Bi, and TIBi2 have been determined by metal solution calorimetry with bismuth as solvent. The published information on the thermody-namic properties of these compounds is limited. The structure of the compound InBi (mp, 383°K) is tetragonal of the PbO (B10) type.1 The compounds In2Bi (mp, 362°K) and TIBi2 (mp of highest-melting composition, 486°K) are now believed to have structures of the NizIn (B8) type273 and not the A1B2 (C32) structures reported earlier.4, 5 The compounds In2Bi and TIBi2 have limited homogeneity ranges at room temperature, while the compound InBi has no detectable homogeneity range.' Samples of the compounds were prepared from 99.99 pet Bi (Mallinckrodt Chemical Works), 99.999 pet in (American Smelting and Refining Co.), and 99.99 pet Tl (Amend Drug and Chemical Co.) by melting the components in sealed, evacuated Vycor tubes. The compounds InBi and in2Bi were of the stoichiometric compositions. The compound TIBi2 contained 40 pet T1; this composition was chosen because at room temperature the alloy of stoichiometric composition does not lie within the homogeneity range.' The melts were held approximately 50°C above the liquidus for 8 hr and then quenched into iced brine. The samples were homogenized for 48 hr at temperatures 20°C below the temperature of complete solidification. Metallographic examination of sections taken from the center and the ends of the ingots did not reveal second phases or segregation . The heats of formation were determined as the difference in the heat effects on solution of a compound and of a mechanical mixture of its components added from the reference temperature of 273°K to liquid bismuth at 623°K. The details of the calori-metric procedure and method of calculation have been described elsewhere? The calorimeter was calibrated by adding bismuth at 273°K to the bismuth bath at 623°K. The calculated values of the heats of formation of the compounds, listed in Table I, are based on a value of 4.96 keal per g-atom for the difference between the heat contents of bismuth at 273" and 623oK7 No published values are available for the heats of formation of the compounds InBi and In2Bi. Hultgren et a1.7 have calculated a value of -0.50 i 0.10 keal per g-atom for the heat of formation at 423°K of the compound TIBi2 containing 40 at. pet T1 from heat-content measurements in the range from 398" to 700°K and the heats of formation of the liquid alloy. The difference between this value and the value of -0.66 * 0.01 keal per g-atom at 273°K is too large to be attributed to a difference between the heat capacities of the compound and the components over the temperature range 273o to 423oK7 However, the direct determination of the heat of formation by a calorimetric method should give a more accurate value. The heats of formation at 273°K of the compounds InBi and In2Bi lie on a straight line when plotted as a function of composition, Fig. 1. The compound In2Bi, therefore, appears to be barely stable with respect to its neighboring phases. In order for the free energy vs composition curve to be concave towards the composition axis, the entropy change on formation of In2Bi must be more positive than that on formation of InBi. As the compounds are ordered,2, 3, 8 there is no configurational entropy change on formation. The difference between the entropy changes on formation of the two compounds, therefore, is probably associated with the vibrational entropies. In view of the low heats of formation, the changes in vibrational entropy, due to changes in bond strength on formation of the two compounds, are likely to be small. Owing to the volume contractions on formation of the two compounds,5 the vibrational entropies probably decrease slightly but the decrease of the vibrational entropy of InBi is expected to be larger than that of In2Bi.

Jan 1, 1965

By P. Lelong, P. Lacombe, J. Herenguel

IN previous studies on the effect of orientation on the rate of anodic oxidation of A1-3 pct Mg mono-crystals of high purity, certain anomalies were observed on the cold-worked metal. These anomalies were shown to correspond to regions of changed orientation within the grains resulting from plastic deformation.' In fact, they are deformation bands revealed by differences in rate of oxidation and produced by more or less continuous bending of the lattice about a [Ill] axis common to the original crystal and the band.2,3 Preliminary observations made after relatively large degrees of cold working revealed an approximate twin relationship between the bands and the surrounding crystal. Fig. 1 shows the etch figures formed on such a band and on the original monocrystal after a 67 pct rolling reduction. It is evidently not a true twinning, since there is a broad transition zone between the two systems, however the two extreme orientations are nearly in a twin relationship. It was decided to investigate these preliminary observations by progressive rolling-reductions on monocrystals of varied initial orientation. From these studies, which form the subject of the present article, it became apparent that the initial observation of an approximate twin relation between the bands and the monocrystal was simply a special case. Our experiments show that deformation in rolling proceeds by a mechanism analogous to those which have already been observed in the simpler cases of tension and compression. Micrography—in particular, the formation of etch figures—has been applied to the quantitative study of these orientations. In addition, observations have been made of slip lines, of thin oxide films yielding interference colors, of thick films in polarized light, and of etchants giving "engraving." These micrographic methods for studying orientation have established the orientation relationship without any ambiguity, whereas X-ray methods would have given only a statistical result because we were often dealing with thin bands (2 to 100 microns) and even narrower connecting zones covering a maximum of 20 microns. Specimen Preparation and Methods The Al-3 pct Mg alloy was prepared from 99.95 pct A1 and is of the type used industrially in France for brilliant anodized finishes under the name of Brillalumag. This material combines the normal commercial properties with an enduring brilliance due to the protection of a thick, but perfectly transparent, film of alumina.' The monocrystals were prepared by the method of critical deformation followed by prolonged annealing. Great care was taken to insure perfect homogeneity of composition, to eliminate included crystals,6,7 and to avoid the formation of undulations during oxidation. The critical deformation for this alloy is about 1.2 pct (1-l0/10x100) and the subsequent annealing was for one week at 500 °C after gradual increase of temperature (35°C per hr). The crystals thus prepared had a section of 10x5 mm and a length of 20 to 40 mm. Each of these crystals was polished electrolytically and etched for the formation of etch-figures with the classical reagent.' The orientation was then calculated from their angles, as measured with a goniometer microscope.

Jan 1, 1954

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

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

Jan 1, 1964

By Wilbur H. Somerton

In order to evaluate the quantitative determination of porosity by various neutron logging systems, four test wells were constructed to simulate some of the possible variab1e.r found in field logging conditions. All of the test holes contain sections of limestone with one section of sandstone included in one well. Each well has a representative section of high, medium, and low porosity. Three borehole sizes are represented by three of the test wells, all containing fresh water. One test well contains saturated brine. Statistical and tune constant checks are made for each system evaluated. Runs and repeat runs are made with the sonde centered and eccentric. Factors evaluated are the effect of borehole size, sonde position, salinity, chemical composition of rock, and statistical variation. A semi-quantitative method of evaluation of these effects is used giving the average maximum per cent error possible for each. Drift and calibration procedures are also discussed. The effect of the various factors appears to be largely a function of the phenomena detected as well as the means of detection. Graphic illustrations of some of these effects are presented. It is concluded, that for accurate log interpretation, the hole size and sonde position should be known. INTRODUCTION The use of neutron logs for the derivation of porosity has become an accepted practice in many areas. In recent years, many different neutron logging systems have been offered to the industry. The neutron sources presently available are of the radium-beryllium or polonium -beryllium type. Detector types used are ionization chambers, Geiger-Mueller-type counters, proportional counters, or scintillation detectors used to detect or measure gamma rays, thermal neutrons, epithermal neutrons, fast neutrons or combinations of these. It is well-known that all systems do not respond alike in all environments. As a result, testing facilities and an evaluation method were developed for use in evaluating the porosity discriminating ability of neutron logging systems using conditions simulating those normally encountered in the field. With such an evaluation, the suitability of a logging system can be determined lor selected field conditions. TEST FACILITIES The testing facilities consist of wells containing rocks of various porosities, constructed to include as many parameters as practicable. Three pits were drilled to a depth of 20 ft and the fourth to a depth of 9 ft, all having 48-in. diameters. Rat holes were dug to a depth of 6 ft in the center of each pit and fitted with sections of pipe having appropriate diameters. The top of this pipe was located approximately 8 in. above the pit bottom. A 6-in, layer of cement was then poured on the bottom and while still wet, 42-in. OD corrugated, galvanized culvert pipe was set on bottom and centered in place. This pipe extends approximately 1 ft above the surface of the ground. The annulus around the culvert pipe was then filled with cement to the top. A 1- or 2-in. layer of sand was placed on the cement bottom to provide an adjustable bed on which to place the series of rocks set in each hole. A cross section of a typical test well containing the porous rocks is shown in Fig. 1.

By P. A. Beck, S. Kohara, M. N. Parthasarathi

IT has been shown1,3 that many observed phenomena related to annealing textures in f.c.c. metals can be adequately accounted for, at least in a qualitative way, by considering the orientation dependence of the boundary mobility, without any hypotheses concerning preferred orientation of nuclei. It was noted1 that this approach is particularly successful in the common cases of primary recrystallization in highly cold-worked polycrys-talline metals, where nuclei occur in great abundance, and that in the other extreme case, where the number of nuclei is very limited, or even only a single crystal is grown, the orientation dependence of boundary mobility has only a small effect, or none at all, on the orientations resulting from annealing. Recently Dunn described examples3-6 where observed secondary recrystallization textures apparently cannot be accounted for on the basis of oriented growth alone, but also require oriented nuclei, or at least the absence of nuclei in certain orientation ranges. In general, the great difficulty in correlating the preferred orientation of recrystallized grains with that of nuclei is inherent in the fact that nuclei are by nature very small, and that they are usually identifiable as "nuclei" only after growth, i.e., after they have already been subject to growth selectivity. An investigation was carried out by Liebmann and Lücke,' and also a very similar one by Graham and Cahn,' to obtain quantitative information on the orientation depend- ence of boundary migration rates in the recrystallization of slightly deformed aluminum single-crystal rods or plates, in which artificially nucleated recrystallized grains of predetermined orientation were grown. Liebmann and Lücke foupd maximum boundary mobility for boundaries across which the misorientation corresponded to a rotation of 40 deg around a common [Ill] axis, in accordance with earlier conclusions.9,1 Also, they confirmed that such an orientation relationship predominates among crystals growing into slightly extended single crystals from presumably random artificial nuclei. On the other hand, Graham and Cahn found no preferred orientation among crystals grown in a similar manner. It is not as yet known how these observations may be reconciled with each other. The view has been expressed in various papers5'10,21 that selective growth based on the orientation dependence of boundary mobility is not in itself sufficient to account for the formation of sharp re-crystallization textures, such as those often observed in highly deformed polycrystalline metals after annealing. The present work was undertaken to ascertain whether or not it is possible to obtain a sharp re-crystallization texture in a case where random nuclei are assuredly present in large numbers. It was previously found1' that high-purity aluminum crystals rolled 80 pct on the (110) plane in the [1T2] direction, when suitable precautions are taken, may be annealed for periods of about 1000 sec at 350°C without recrystallization. It was also found that the reluctance to recrystallize in this case is due to the scarcity of material in sufficiently deviating orientations to serve as nuclei. By using such a matrix,

Jan 1, 1959