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By C. G. Dunn, E. F. Koch, K. T. Aust

Strain-induced grain boundary migration was studied in a series of silicon-iron (3% pct Si) bicrystals of controlled orientations. Each bicrystal was given a 7 pct cold-rolling strain rind annealed at 1100°C. The direction of boundary migration was found to depend on orientation; results for several orientations related by a common [110] axis are given. Analysis of the micrographic and X-ray data is made in terms of the residual strain-energy densities within the crystals (energy per unit volurne) and a driving force on the boundary due to an energy density difference across the boundary. Relative strain energies were obtained for the various orientations investigated. A CHROME-acetic acid electroetching method for revealing dislocation sites in silicon iron was previously applied to clarify the structural features and the energetics involved in strain-induced grain boundary migration.',' The present paper is a continuation of this study, but is primarily concerned with the influence of crystal orientation. Sperry, as reported by Beck,3 attempted to determine the factors that influence the preferred growth of one grain over another in aluminum due to strain-induced boundary migration. He found that the particular grain of a pair which work hardened more was invaded, although exceptions to this correlation were noted. The index of work hardening was determined from microhardness measurements of each grain before and after cold-rolling. In the present study, orientation itself was taken as a useful variable for studying the behavior of individual grains in a bicrystal and the direction of boundary migration, since the extent of work hardening is orientation dePendent." The effect of strain on boundary migration is evident from a consideration of driving forces. Thus, in the absence of inclusions, the driving force (per unit area of boundary) for growth of grain A into grain B when a bicrystal is strained and annealed may be expressed as follows:2

Jan 1, 1960

By E. C. Harder

INTRODUCTION THE situation in the United States, at the present time, regarding the supply of manganese ores and alloys of manganese is one of great seriousness and is likely to become increasingly so while the European war continues. The two principal iron-manganese alloys, ferromanganese and spiegeleisen, are indispensable in steel manufacture, being used extensively in the Bessemer and openhearth processes.. Spiegeleisen, the lower alloy, contains between 15 and 25 per cent., and ferromanganese, the higher alloy, between 60 and 80 per cent., of manganese. Besides manganese the alloys contain iron and carbon. On the market ferromanganese is usually quoted on the basis of 80 per cent. manganese, and spiegeleisen on the basis of 20 per cent. manganese. The consumption of ferromanganese has been increasing during recent years at the expense of spiegeleisen, because larger quantities of the latter must be used to ac-complish the same purpose with the result that the amount of carbon introduced with it into the molten metal is frequently injuriously great. Manganese ore proper, in the form of manganese dioxide, is used extensively in many chemical industries, especially for oxidizing purposes. It is also used for the manufacture of both wet and dry electric cells and in the manufacture of paints and dyes. The manganese ore used in this country has been derived hitherto from three principal sources:. Southern Russia, Southern British India and East Central Brazil. The following tables show the quantity of manganese ore imported from these countries, and (for comparison) the domestic production, during 1912, 1913 and 1914. The imported manganese ore has been used largely in the manufacture of iron-manganese alloys and in addition large quantities of the alloys themselves have been imported, chiefly. from Great Britain, Germany and other European countries.

Jan 5, 1916

By A. F. Meston

Centrifugal force has been used for centuries for separating liquids but machines for doing this are a comparatively recent development. The use of these machines is being extended into many industries but this paper is confined to their use in the oil industry. The centrifugal machine is found at the well where "cut oil" is dehydrated for acceptance by pipe lines; and in the refinery and byproduct plant. In fact, wherever finely divided suspended particles should be removed from an oil, there is a possible use for a centrifugal machine, if the particles have, or can be made to have, a specific gravity different from that of the oil. Centrifugal machines are also used for cleaning fuel and lubricating oils and dehydrating transformer oils. Applications and Results When oil comes from the well mixed with water, it is spoken of as cut oil. Settling often does not remove sufficient water for the oil to be accepted by pipe lines, thus necessitating chemical or other treatment. Centrifuging alone, or following chemical treatment, effectively prepares such oil for pipe lines, as is shown by the following data: WateR, Etc. Wat~R. Etc. Temperature, Oil to Pipe Line, aT StUt at Finish Degrees F. Bel. Per HouR PIE Cent. PEECent Oklahoma lease.... 160 10 10 0.25 Kansas lease....... 125 4 20 0.25 to 2 On the Oklahoma lease, the machine was cleaned of solid material once in 12 hr. At first, it was thought that chemical treatment was necessary to start separation and 1 qt. of prepared compound was added to each 100 bbl. of the cut oil before centrifuging. Later it was found that

Jan 1, 1924

By P. W. Rainier

THE Chivor emerald field is situated on the eastern slope of the Andes in the Department of Boyacá, at an elevation of about 8000 ft. above sea level. It overlooks the Llanos (plains) of the Orinoco and is watered by many streams flowing into the Rio Meta, the Orinoco's largest tributary. The Rio Meta is navigable from the Orinoco to a point within about 50 miles of the Chivor district and may eventually prove to be the reasonable outlet for the future development of this part of the country. The topography of the district is extremely rugged and mountainous (Fig. 1), the difference in elevation between two points on a mining claim 1 km. square being sometimes as much as 4000 ft. The ground is covered with dense forest growth and the available timber is suitable and sufficient for mining purposes, but it is becoming gradually depleted by Indian clearings as the country around the mines becomes settled. The many streams combined with the rough topography give good possi-bilities for hydroelectric power. The center of population nearest to Chivor is Bogota, the capital of the republic and a city of some 300,000 inhabitants; the distance is two and one-half days' travel. The first stage of the journey from Bogota, is accomplished by rail to Chocontá, some 4 hr. travel. From Chocontá the journey is made in the saddle, one night being spent in Guateque. The latter is a small town and the nearest post office to the mines, being some 10 hr. ride distant. The roads are mere bridle paths, in parts hazardous and almost impassable in the wet season. All supplies brought to the mines, other than those produced locally, are carried by pack mule; mule freight from Chocontá costs 3 centavos1 per pound. The climate of the Chivor district is healthful and bracing. The wet season begins in March and concludes in November, the remaining months being dry. The annual precipitation is about 150 in. The temperature throughout the year is nearly constant, varying from about 45° F. to about 65° F. shade temperature. The rains are cold and unpleasant, and for the greater part of each day in the wet season the country is shrouded in dense mist. A fire can with comfort be kept burning in a living room all the year round. There are a few slight

Jan 1, 1929

By D. T. Peterson, T. Carnahan

The diffusion coejTicients of carbon, nitrogen, and oxyget were determined in $ thorium over the tempernilcre range 1440" io 1715°C. The diffusion coyfiicir?zls are given by: D = 0.022 exp (-27,000/RT) jor carbo)~, D = 0,0032 exp(-l7,00Q/RTj for nitrogen, and D = u.0013 expt(-11,UOU/RT) for oxygen. Cavl~orz was found to increase the hardness of thoriunz nearly linearly with concentration over the range 100 to 1000Ppm carbon. ThORIUM has a fcc structure up to 1365°C and a bcc structure from this temperature to its melting point at 1740°C. Diffusion of carbon, oxygen, and nitrogen in bcc thorium was of interest in connection with the purification of thorium by electrotransport.' In addition, it was possible to measure the diffusion of all three of these interstitial solutes in the same bcc metal. Only in niobium, tantalum, vanadium, and a iron have all three interstitial diffusion coefficients been measured in a given bcc metal. Diffusion coefficients have been measured for carbon and oxygen in a thorium by Peterson2, 3 and for nitrogen by Gerds and Mallett.4 Activation energies for diffusion are reported by the above authors to be 38 kcal per mole for carbon, 22.5 kcal per mole for nitrogen, and 49 kcal per mole for oxygen. Values of the diffusion coefficients of carbon and nitrogen in 3 thorium have been reported by Peterson et al.' However, these were secondary results of their investigation of electrotransport phenomena in thorium and it was hoped that the present study could provide more precise data. EXPERIMENTAL PROCEDURE The specimens used in this study were the well-known pair of semi-infinite bar type. The couple was formed by resistance butt welding two 0.54-cm-diam by 3.0-cm-long bars of thorium together under pure helium, the concentration of the solute being greater in one cylinder than that in the other. The finished couple then contained a concentration step at the weld interface and diffusion proceeded only along the axis of the rod. The thorium used in this study was prepared by the magnesium intermediate alloy method.5 The total impurity content was less than 400 ppm. The major impurities were: carbon, 100 ppm: nitrogen, 50 ppm; and oxygen. 85 ppm. The total metallic impurity content was less than 150 ppm. The high solute concentration portions of the diffusion couples were prepared by adding the solute to the high-purity thorium in a non-consumable electrode arc melting procedure. Carbon and nitrogen were added in the form of spectroscopic graphite and nitrogen gas while a Tho2 layer was dissolved by arc melting to add oxygen. High-purity thorium formed the low concentration portions in the carbon and nitrogen couples. The low oxygen portions were obtained by deoxidizing high-purity thorium with calcium for 3 weeks at 1000°C according to a method reported by Peterson.3 The high C-Th contained 400 ppm C, the high N-Th contained 400 ppm N, the high 0-Th contained 220 ppm 0, and the low 0-Th contained 25 ppm O. The high O-Th was brine-quenched from 1500°C to retain most of the oxygen in solution at room temperature. These concentration levels were all below the solubility limits in 0 thorium at 1400°C. A resistance-heated high-vacuum furnace was used to heat the couples. The samples were mounted horizontally on a tantalum support which had small grooves near each end. Spacer rods of thorium, 0.4 cm in diam, were placed in these grooves to prevent contact between the sample and the tantalum support. This arrangement should have prevented contamination of the sample by contact with the support. In further effort to reduce contamination, the oxygen diffusion couples were sealed inside evacuated outgassed tantalum cylinders lined with thorium foil. Thorium rings around each end of the samples acted as spacers in this case. Pressure during diffusion runs was about 10-6 torr after an initial outgassing stage. Temperature measurements were made by sighting on black body holes in the sample support adjacent to the samples with a Leeds and Northrup disappearing-filament optical pyrometer. Temperatures were constant during a diffusion anneal to ±5C. The observed temperatures were corrected for sight glass absorption after each diffusion run. The pyrometer was checked against a calibrated electronic optical pyrometer and a calibrated tungsten strip lamp with the electronic pyrometer being taken as the standard. All temperature readings agreed to within ±3C over the temperature range 1450" to 1690°C. Time corrections due to diffusion during heating and cooling were necessary because of the short diffusion times. The diffusion times ranged from 6 min for the oxygen sample run at 1690°C to 90 min for the carbon sample run at 1500°C. A series of temperature vs time plots were made for heating and cooling of the samples to the various diffusion temperatures. This data was then used in a method according to shewmon6 to determine the time corrections. The corrections amounted to

Jan 1, 1970

By D. A. Summers, C. J. Haas, G. B. Clark, J. W. Brown

While significant advances have been made in excavation of rock, largely in improvements in drilling, blasting, loading, and haulage, conventional operations have been improved until little feasible increase in efficiency or rate of advance appears possible. Tunnel-boring machines have been developed which will excavate at rapid rates in soft to medium- hard rock. Hypervelocity impact is being intensively investigated as a possible means of cutting and breaking rock, as well as lasers, electric current, explosive drilling, high frequency vibration, etc. The current development and use of high-velocity small-diameter water jets, metallic jets, and projectiles of various materials involve ultra-high-pressure phenomena of fundamental interest. Rock disintegration by water jets has been investigated in the USSR for over a decade. Large-diameter jets of low velocity are used to mine coal, and high-velocity capillary jets will cut and break rocks under laboratory conditions. Velocity ranges for breaking and cutting are dependent upon rock and jet properties, and pulsed jets break some rocks more easily than continuous jets. Spectacular laboratory results have been reported for breakage of unconfined blocks of some types of rocks. Compressors, pressure multipliers, gas explosion chambers, and water cannons have been used to generate jets. Jet properties, such as continuity, unit pressure, total pressure, and stability have been measured. Results agree with theory, although the latter has been established only for relatively low-velocity flow. Diameter, speed of traversing, and frequency of pulsed jets affect rock response. Investigations in Britain have only recently begun consideration of harder rocks and higher velocities, although water jet cores have been found to be more continuous at lower velocities than previously believed. Lower limits of jet velocity for rock cutting were established for the rocks investigated.

Jan 1, 1970

By G. S. Tint, M. Herman, V. V. Damiano

Dislocation arrays and substructures were studied in cadmium doped zinc crystals using a newly devised etching technique. Cadmium precipitates delineating the dislocations were revealed by etching a surface closely parallel to the (0001) slip plane. Cinephotomicrography of the continuous etching process revealed the three-dimensional aspects of dislocations in the bulk crystal. Dislocation etch patterns were studied in both deformed and annealed crystals after suitable aging at room temperature. The effect of annealing was evidenced by a rearrangement of the dislocations into low-angle boundaries and hexagonal networks. ETCH pit techniques have been used extensively to study dislocations in both deformed and annealed bulk metal crystals. Ideally one hopes to obtain a one-to-one correspondence between the etch pits and the points of emergence of the dislocations at the surface. One then attempts to deduce the way in which dislocations are arranged in the bulk crystal from the arrangement of etch pits on the surface. It is clear that one can obtain only limited information of the dislocation configurations inside the crystal from etch pit studies of single surfaces. Considerably more information is obtained if one is able to follow the course of the dislocations through the crystal using progressive etching technique. Techniques of this sort were used by Gilmanl to study dislocations on the slip planes of NaCl crystals and by Damiano and Tint2 to study dislocation arrangement in zinc crystals grown from the melt. The present paper makes use of a technique first described by Tint and Damiano3 to observe and continuously record the dislocation structures which appear while a crystal surface was being progressively etched. Studies were made on cleaved (0001) surfaces to reveal the dislocations along their length on the surface closely parallel to the slip plane. The technique for revealing segments of dislocations along their length by etching is well known. Wilsdorf and Kuhlmann-wilsdorf4 revealed disloca- tions along their length in aluminum containing a few percent copper, when precipitates segregated along the dislocations. The technique was used by Low and Guard5 to study dislocation configurations on the slip plane in Fe-Si alloys containing carbon. In the present work the technique was applied to zinc containing cadmium since it was shown by Gil-man6 that a cadmium-rich phase could be made to precipitate from supersaturated solutions along dislocations in zinc. Segments of dislocations delineated by the precipitates were revealed by etching a surface prepared by cleaving the crystal. The three-dimensional nature of dislocations and substructures was thus studied from the cinephotomicro-graphic record of the continuous etching process. EXPERIMENTAL Single crystals of zinc containing the order of 0.1 pct Cd were prepared by slowly lowering a graphite crucible containing the melt through a temperature gradient of 15°C per cm at a rate of 1.5 X 10-3 cm per sec. "As grown" crystals were aged for periods of 1 month at room temperature, then cleaved in liquid nitrogen, and etched according to the procedure used by Gilman.' The etchant containing 32 g of CrO3, 6 g of hydrated Na2SO3 in 100 ml of water behaved as a chemical polish for zinc and etch pits were produced at the site of precipitates or inclusions. After the precipitates or inclusions were removed from the surface, the etch pits left behind were eventually polished smooth. This behavior enabled one to continuously observe the surface while the specimen was immersed in the etchant. Best results were obtained when the specimen surface was vertical and the reaction products of polishing were continuously removed by gravitational convection. Some crystals were heavily deformed in excess of 25 pct strain, others were lightly deformed the order of a few pct by compression such that the deformation occurred essentially by basal glide. Some crystals were etched immediately after deformation, others were allowed to age at room temperature for several weeks prior to etching. Heavily deformed crystals were annealed at various temperatures and etched on the cleavage plane immediately after annealing, others were allowed to age at room temperature for several weeks prior to etching. The etched structures of deformed and annealed structures were studied. Similar experiments were conducted on 99.9999 pct pure zone refined Tadanac zinc crystals which

Jan 1, 1963

By R. E. Zimmerman

THE separation of fine sizes of coal from its impurities by means of various flotation methods has become of increasing importance in the coal industry. This, no doubt, will be even more so in the future as the quantity of high grade coal is depleted, particularly that used for metallurgical purposes. The purpose of this paper is to describe and report the results of research work done under the auspices of the Pittsburgh Coal Co. to determine the amenability of their bituminous fine sizes of coal to flotation, to investigate the value of various reagents and factors affecting their use, and compare the results between froth flotation and bulk oil flotation. Compared with the preferential flotation of complex minerals, or ores, the flotation of coal is comparatively easy. However, this statement should not lull one into the feeling that there are no special problems involved. For instance, the separation of coal from pyrite in high sulphur coals is still far from being 100 pct successful. Size consist has considerable effect on reagent consumption and recovery. Other factors will be described and finally it must be remembered that in the flotation of coal a low priced material is being treated and thus economic considerations govern more closely its application than is generally the case in treating other minerals. As a result of the research work done by the Pittsburgh Coal Co. on the flotation of coal, it was concluded that it was practical to clean the -48-mesh coal commercially by froth flotation and after several different types of flotation units and circuits were investigated by means of pilot plants, large scale units were installed at their Champion Nos. 1, 4 and 5 Preparation Plants for the cleaning of -48-mesh slurries. These large scale operations have been recently described by D. H. Davis. 1 C. P. Proctor and C. B. Carlson2 in their chapter on Froth Flotation of Coal in the AIME Seeley W. Mudd series book on Coal Preparation describe some of the practical applications of our Pittsburgh Coal Co. laboratory work in actual plant practice as well as summarizing part of the investigational work. The author presents this paper, however, as a supplement to their reports, and records the basic research accomplished in the laboratory investigational work as well as the results of experi¬ments using bulk oil flotation. In presenting this work the author wishes to state much more work must be done in applying the principles of flotation to cleaning coal, especially in view of recent studies and practices in other mineral beneficiation fields. METHODS OF CONDUCTING LABORATORY TESTS The bulk of the research work was conducted in the laboratory of the Champion No. r Preparation Plant. This plant has elaborate facilities for sampling and analyzing coal and proved to be an admirable location

Jan 1, 1948

By D. L. Sikarskie, B. Paul

A theory is presented for the static penetration of a single rigid wedge into brittle material. The material considered is one which exhibits both crushing and chipping phases in the penetration process. If the wedge angle and three parameters are specified, the theory predicts forces and associated penetrations during both the crushing and chipping phases. For certain ranges of the parameters agreement with the limited experimental data available is promising, except for the initial phase of the penetration process where refinements on the proposed theory are required. The theory also predicts that for certain values of the wedge angle and other known parameters, the chipping process does not occur and penetration is due entirely to crushing. When viewed in detail, the drilling of rock by percussive means involves, among other things, system dynamics, actuating forces, dynamic stress levels and the actual penetration mechanism of the bit into rock. If rock drills are to be significantly improved, a thorough understanding of the entire system would be highly desirable. In this paper, one aspect of the system, namely the mechanism of penetration of the bit, will be studied in detail. It has been found1 that for the velocities encountered in percussive drilling (of the order of 20 fps) a static analysis adequately describes the penetration process, at least for some rocks. Hence, we will only be concerned with describing analytically the static penetration of a single wedge shaped tool. It will further be assumed that the wedge is long enough to permit a two-dimensional analysis. Numerous authors have studied the static penetration of a wedge into rock. The following papers give some of this work and provide additional references to other work. Cheatham2,3 has assumed the rock to behave plastically and has obtained force-penetration equations for both Coulomb-Mohr and parabolic yield criteria. Evans and Murrell4 have studied the penetration of two types of coal and have found equations relating the penetration characteristic (P/dSc) to wedge angle for the various strength coals tested. race' attempted to find a correlation between hardness as determined by indenting the material and other mechanical properties and concluded that the results of such a test are generally inconclusive. His paper however contains a very extensive bibliography on the indenting of many different materials. Gnirk6 also has a fairly complete literature review on the static penetration of rock, of which he makes use in his indexing studies. A wide range of behavior is found in the wedge penetration of different rocks under different external conditions. For example, a rock that is essentially elastic-brittle at standard pressure may become elastic-plastic at a high confining pressure.7 It has also been observed4. " that some rocks will merely be crushed and indented by a wedge, whereas others will crack and form chips, furthermore the existence or non-existence of chips depends in great measure on the geometry of the indentor, type of rock and the depth of penetration. Hence, to attempt a theory which embraces all possible behavior is not practical at present. We, therefore, confine our attention to predicting the force-penetration characteristic and volume removal behavior for a type of rock which exhibits both crushing and chipping phases in the penetration process. Such behavior is characteristic of the harder rocks such as granites and represents a more difficult problem than the behavior of softer rocks such as coal and certain sandstones. In this preliminary study an attempt will be made to describe only the essential features of this complex penetration process. A qualitative description of these essential features is obtained with the aid of Fig. 1.1, where a wedge of vertex angle 28 is shown at some intermediate stage of the penetration process. As the wedge advances, the rock is fragmented (i.e. crushed) in some local region surrounding the wedge, the shape of this region being unknown. Simultaneous with the fragmentation in this local region, essentially elastic stresses are assumed to be building up in the surrounding rock. When a certain penetration level, di+1, is reached, the stresses along some surface are sufficient to cause failure and a chip is thus formed. The process now repeats, i.e., a crushing phase followed by the formation of a chip.

Jan 1, 1965

By J. J. Kramer, K. Foster

The orientation distribution of surface-energy -induced secondary recrystallized grains was determined. This work was conducted on thin sheets of a 3 pct Si-Fe alloy annealed under environmental conditions that furor grouth of grains with a (100) plane in the surface of the sheet. The texture was found to be extremely sharp and almost independent of sheet thickness. The distribution varied exponentially with the angular deviation from the {100} plane. It was possible to relate the distribution to the nu-cleation rate of the secondary rains as influenced by the surface-energy difference. THE role of surface energy in the secondary grain growth of cube-oriented grains (grains with a (100) plane in the plane of the sheet) in thin Si-Fe sheets has been previously discussed.1-4 In high-purity sheet material normal grain growth usually occurs until the grains have extended through the sheet. Further grain growth is inhibited by the thermal grooving of the boundaries at the sheet surface. However, additional growth of cube grains can occur by a secondary grain growth process under conditions where the (100) plane has a lower surface energy than other orientations. Apparently for these alloys, cusps exist in the polar plot5 of surface free energy with the lowest cusp energy occurring at the (100) orientations. This has been reported to be the result of preferential adsorption of sulfur on the (100) planes.6 As a result of this process, a distribution of orientations could arise from two possible mechanisms. First, when a cusp is present in the polar plot of surface free energy, there are orientations inside the cusp that have a lower surface energy than elsewhere on the polar plot. Also, at sufficiently high temperatures, flat surfaces whose orientations are inside or just outside the cusp (depending on its shape) can often thermally etch, yielding a microscopically stepped surface of even lower surface energy. As a result, grains oriented close to cube would also have a lower surface free energy, either because of the cusp shape or by thermal etching, and could possibly grow as secondary grains by the surface-energy phenomenon. One should thus observe a distribution in the surface orientation of the cube grains comprising the secondary structure. It is the purpose of this paper to investigate this orientation distribution experimentally and to discuss the factors involved in its formation. For this purpose, the surface orientations of a large number of secondary grains in various sheet thickness were determined by means of the Laue back-reflection X-ray technique. PROCEDURE A vacuum-melted 3 pct Si-Fe alloy containing a nominal impurity content of 0.005 wt pct was processed into strip. A single cold-rolling step of 90 pct reduction was used for each strip regardless of the final sheet thickness. Final strip thicknesses of 0.60, 0.30, 0.15, and 0.075 mm were used. Care was taken to insure that the final strip surface was smooth and flat. All strips of a given thickness were annealed together at 1200°C in dry hydrogen (dew point -70°C) to develop the desired secondary structure and to insure identical environmental annealing conditions. The annealing time was selected to develop a complete secondary structure in the thinner sheets but to permit the thicker sheets (0.60 mm) to have residual primary grains remaining. This was necessary to determine whether growth impingement could lead to one secondary grain consuming another at a greater angular deviation. For the X-ray determination of the surface orientation of the secondary grains, a special specimen holder was used. The camera and holder arrangement could be aligned by X-raying a grain in three positions rotated 180 deg to each other. Thus, with a small beam X-ray focus (1 mm), the surface orientation of any grain could be determined to within one-half a degree. The surface orientations of one hundred cube secondary grains were determined for each sheet thickness. The criteria of a secondary grain were its size relative to the sheet thickness and the number of sides of the grain observed in the sheet surface. (A primary recrystallized grain extending through a sheet will generally have six edges visible in the plane of the sheet, whereas a secondary grain will have many more when growing entirely into primary grains.) Grains were selected as randomly as possible by X-raying every secondary grain found along a line drawn on the strip. No attempt was made to determine the exact orientation of the planes of the surface, as many strips from randomly selected sheets were used. On1y the angular deviation of the surface plane from {100} was measured. In order to assess the volume distribution in the

Jan 1, 1965

By H. J. O’Donnell, B. C. Parks

IN 1930 the late Dr. Reinhardt Thiessen set up a method of microscopic analysis and type classification of coal that has since been followed as standard practice in the coal-petrography laboratory of the Bureau of Mines. Thiessen's terminology which designated the constituent parts of coal in terms of botanical origin was introduced in 1920.l The technique, however, of preparing a completely representative series of thin sections from a column sample of coal for use in making quantitative determinations of coal components with a microscope was developed about 10 years later by Thiessen and coworkers G. C. Sprunk and H. J. O'Donnell.2 Complete thin-section analyses subsequently have been made of 126 column samples of various ranks and types of American coals. The data and information were assembled from these thin-section studies and published in a large number of reports dealing chiefly with investigations of the coking and hydrogenation properties of certain American coals. In the years following adoption of Thiessen's method, a considerable amount of work was done in collecting column samples of many coals, making routine thin-section analyses of these, interpreting the results, and finding practical application for the information in other fields of coal research. The many reports and papers covering the work in coal petrography, however, offer very little discussion that can be considered as critical appraisal of the technique. Criticism outside the Bureau most often has voiced questioning opinions concerning the accuracy of the method used of measuring coal components microscopically and classifying the coal into arbitrary types on the basis of the quantitative determinations. The principal purpose of this paper is to discuss in some detail and present data showing the results of certain investigative work done in the petrography laboratory on the accuracy of the Bureau's method of microscopic measurement of components in coal thin sections. Data from microscopic analyses on file made by G. C. Sprunk and H. J. O'Donnell were freely used in the investigation, and a table of columnar analyses from an unpublished manuscript by Sprunk is included in this paper for reference. In the course of the experimental work a method was developed for measuring instrumentally with a planimeter the components shown in micrographs of selected thin sections. Measuring coal components with a planimeter furnished useful information for studying the accuracy of microscopically measuring the same components in thin sections. PETROGRAPHIC COMPONENTS AND TYPE CLASSIFICATION OF COAL Thiessen considered coal to be composed of two visibly different major components present in various types of coal in greatly varying proportions. He named

Jan 1, 1948

By L. A. Weitzenkamp, N. M. Bashara

A study of the electrical conductivity of gold films less than 200 in thickness indicates a negative temperature coefficient of resistance and a thermal actiuatlon energy of less than 0.25 ev. The films consist of discrete metal islands of linear dimensions from a few angstroms to 1000A. Films were able to withstand applied fields up to 60,000 v per cm before breakdown occurred. A model for the conduction mechanism is proposed which involtes a Potential barrier due to work junction, irriage forces , and an electrostatic potential arising from separating an electron from a neutral island leaving behind a positively charged metal island. Activation energies of less than 0.25 ev ave consistent with this model, which includes a tunneling andor Thermal mechanism for conduction between the separate metal islands. An apparent satuvation effect in conductivity at high fields is observed experimentally. The saturation effect may be explained by the influence of the electrostatic contribution to the potential barriers for the transition through several islands adjacent to the original island which was activated to give up an electron. The proposed model gives Poor quantitative agyeement for the intermal electrical field between islands. ThIS paper will relate the structure of discontinuous metal films to the electrical properties and will emphasize the following topics: 1) the relation of the conduction mechanism to particle size and a comparison of particle size from electrical measurements with electron-microscope studies; 2) the saturation of the conductivity at high electric fields; and finally, 3) a comparison between the external field applied and the apparent field between particles. che- latter comparison points to a need for a modification in the model for the conduction mechanism first proposed by orter' and expanded by Neugebauer and webb2 which will be dealt with in the discussion. The paper is based on results on gold films on glass microscope slides. The clms were vacuum-evaporated and were about lOOA thick, thickness being measured by interferometry. It has been observed that metal films of this thickness do not exhibit bulk metallic conduction. Films thinner than some critical thiclmess, depending upon substrate temperature and other factors, have conductivities which increase with increasing temperature with thermal activation energies of less than 0.25 ev. Electron-microscope studies3 have shown that these films consist of discrete metal islands having linear dimnsions from a few angstroms to approximately 1000A. When the metal is being vacuum-deposited on the substrate, islands on the order of a few angstroms appear first. As the deposition continues the islands may tend to agglomerate into larger particles and may eventually grow together into a continuous film,3''' In our tests the conductivity of the gold films was found to be about ten orders of magnitude less than the bulk conductivity of gold. When oxygen was introduced into the test chamber the conductivity decreased by a factor of about one-third. This can be related to an increase in work function for gold caused by adsorption of oxygen, as reported by Oullet and Rideal.s Exposure to an atmosphere of water vapor caused an increase in conductivity by a factor of 2 or 3 when a low field was applied. When the films were exposed to water vapor under a high field the conductivity increased by as much as two orders of magnitude. The activation energies measured were much less than the work function for gold, 0.25 ev or less, with the smaller activation energies observed for thicker films. It will be shown that the activation energy is a function of particle size and spacing. In general the model for the potential between metal islands would include the effective work function, the image force, the applied field, and an electrostatic term. The electrostatic contribution arises from the potential required to separate an electron from a conducting sphere. According to Neugebauer and webb2 the maximum potential due to the field and the electrostatic term only is

Jan 1, 1967

By G. H. Bruce, C. E. Williams

The trend toward deeper drilling, together with the attcndant increase in power requirements for circulation of the drilling fluid, has emphasized the need for a critical examination of the factors affecting the removal of bit cuttings from the hole by the drilling fluid. The ability of drilling fluids to lift cuttings is called their carrying capacity. A series of laboratory and field experiments has been conducted to determine the minimrim annular velocity necessary to remove cuttings, and to investigate the effects of properties of drilling fluids on their carrying capacities. Consideration of the results of these experiments led to the following conclusions: 1. Turbulent flow in the well annulus is most desirable from the standpoint of cutting removal. 2. Low viscosity and low gel are advantageous in removing cuttings. 3. Increase in mud weight is effective in increasing carrying capacity. 4. The carrying capacity is higher when the pipe is rotated than when it is not. 5. If turbulent flow can be maintained, an annular velocity slightly higher than the slip velocity of the largest cuttings to be transported should keep the bore hole clean. This implies velocities of 100 to 125 ft per minute rather than the presently used 175 to 225 ft per minute. INTRODUCTION Power Savings by Reduction of Annular Velocities A large portion of the power expended in drilling operations is consumed in circulating the drilling fluid. An important factor in establishing the rate of mud circulation is the minimum velocity in the annulus necessary to remove bit cuttings. Empirically, it has been found that average annular mud velocities of about 200 ft per minute will remove cuttings. It was not definitely known, however, whether annular velocities of about 200 ft per minute were just above the minimum necessary to remove cuttings, or whether such velocities could be materially reduced without sacrifice of the ability of the mud to remove cuttings. It is apparent that if annular velocities could be reduced without impairment of cutting removal, a considerable saving in power requirements would result. Need for Research on Carrying Capacity The ability of a drilling fluid to transport cuttings is called its carrying capacity. Although it has been recognized that the carrying capacity of a mud is affected by mud properties such as viscosity and density1,2,3,4 there have been various views in the industry as to the effects of these mud properties on carrying capacity. The economic importance of the problem of carrying capacity and the scarcity of information on the subject indicated that research on the problem was needed. THE FACTORS AFFECTING CARRYING CAPACITY Qualitative Determination of Factors The mechanism of cutting transport is closely related to that involved in the separation of material by settling processes. A considerable amount of research has been done on settling problems, and discussions of sedimentation theory can be found in standard texts.5,6 Consideration of the information available from these sources, together with consideration of the mechanism of cutting transport, leads to the conclusion that the factors affecting carrying capacity are the dimensions of the system, the physical properties of the cuttings. and the physical properties of the drilling fluid. system Dimensions and Their Effect The dimensions of the fluid circulating system of importance to carrying capacity are the bore hole size, drill pipe size, pump capacity, and pump speed. These dimensions determine the annular velocity of the drilling fluid. Physical Properties and Their Effects The physical properties involved in the interaction between mud and cuttings are the density and shape of the cuttings and the density, viscosity and gel strength of the drilling fluid. The effect of the density factor on carrying capacity is fairly obvious; high density difference between cuttings and fluid results in a low buoyant force and therefore decreases carrying capacity. The effect of cutting shape is less obvious. Although

Jan 1, 1951

By C. E. Williams, G. H. Bruce

The trend toward deeper drilling, together with the attcndant increase in power requirements for circulation of the drilling fluid, has emphasized the need for a critical examination of the factors affecting the removal of bit cuttings from the hole by the drilling fluid. The ability of drilling fluids to lift cuttings is called their carrying capacity. A series of laboratory and field experiments has been conducted to determine the minimrim annular velocity necessary to remove cuttings, and to investigate the effects of properties of drilling fluids on their carrying capacities. Consideration of the results of these experiments led to the following conclusions: 1. Turbulent flow in the well annulus is most desirable from the standpoint of cutting removal. 2. Low viscosity and low gel are advantageous in removing cuttings. 3. Increase in mud weight is effective in increasing carrying capacity. 4. The carrying capacity is higher when the pipe is rotated than when it is not. 5. If turbulent flow can be maintained, an annular velocity slightly higher than the slip velocity of the largest cuttings to be transported should keep the bore hole clean. This implies velocities of 100 to 125 ft per minute rather than the presently used 175 to 225 ft per minute. INTRODUCTION Power Savings by Reduction of Annular Velocities A large portion of the power expended in drilling operations is consumed in circulating the drilling fluid. An important factor in establishing the rate of mud circulation is the minimum velocity in the annulus necessary to remove bit cuttings. Empirically, it has been found that average annular mud velocities of about 200 ft per minute will remove cuttings. It was not definitely known, however, whether annular velocities of about 200 ft per minute were just above the minimum necessary to remove cuttings, or whether such velocities could be materially reduced without sacrifice of the ability of the mud to remove cuttings. It is apparent that if annular velocities could be reduced without impairment of cutting removal, a considerable saving in power requirements would result. Need for Research on Carrying Capacity The ability of a drilling fluid to transport cuttings is called its carrying capacity. Although it has been recognized that the carrying capacity of a mud is affected by mud properties such as viscosity and density1,2,3,4 there have been various views in the industry as to the effects of these mud properties on carrying capacity. The economic importance of the problem of carrying capacity and the scarcity of information on the subject indicated that research on the problem was needed. THE FACTORS AFFECTING CARRYING CAPACITY Qualitative Determination of Factors The mechanism of cutting transport is closely related to that involved in the separation of material by settling processes. A considerable amount of research has been done on settling problems, and discussions of sedimentation theory can be found in standard texts.5,6 Consideration of the information available from these sources, together with consideration of the mechanism of cutting transport, leads to the conclusion that the factors affecting carrying capacity are the dimensions of the system, the physical properties of the cuttings. and the physical properties of the drilling fluid. system Dimensions and Their Effect The dimensions of the fluid circulating system of importance to carrying capacity are the bore hole size, drill pipe size, pump capacity, and pump speed. These dimensions determine the annular velocity of the drilling fluid. Physical Properties and Their Effects The physical properties involved in the interaction between mud and cuttings are the density and shape of the cuttings and the density, viscosity and gel strength of the drilling fluid. The effect of the density factor on carrying capacity is fairly obvious; high density difference between cuttings and fluid results in a low buoyant force and therefore decreases carrying capacity. The effect of cutting shape is less obvious. Although

Jan 1, 1951

By R. W. Heckel, R. L. DeGregorio

The DeHoff method of determining the size distribution of ellipsoid-shaped, second-phase particles has been applied to the spheroidization of cementite in a eutectoid steel. The surface area of Precipitates determined from the various size fractions in the distribution was correlated with surface-area measurements based on the number of intersected interfaces on a random lest line. The precipitate particles were found to be oblate ellipsoids with an axial ratio of about 0.90. The size distributions were found to be log-normal. A method is proposed whereby the shrinkage of small particles and growth of large ones can be determined from the experimental data. The experimental data are compared to previously proposed mathematical models describing diffusion-controlled kinetics and various types of interface-controlled kinetics. The experimental growth and shrinkage rates are considerably slower than those predicted by diffusion-controlled kinetics. The best fit is obtained for a model describing interface-controlled kinetics limited by the rate of formation of cementite at the growing interfaces where the interfacial reaction rate is proportional to the solute thermodynamic activity gradient across the surface. THE subject of spheroidization of second-phase particles has been considered previously by other investigators. Livingston1 has studied the precipitation of the cobalt-rich phase from copper alloys containing 0.7 to 3.2 wt pet Co. His results indicate that the average particle size increases as the cube root of the heat treatment time in accord with diffusion-controlled kinetics.'-' Komatsu and rant' in their studies of the growth of SiO2 in a dispersion-strengthened copper-silica alloy found that the initial growth of SiO2 proceeded by diffusion-controlled growth and later stages were limited by interface-controlled growth. The values of the activation energy obtained for the interface- controlled process led them to the conclusion that the process was limited by the dissociation of SiO2 at the shrinking interface. The transition from diffusion-controlled growth to interface-controlled growth was characterized by a particle size which varied with the heat-treatment temperature. It is also interesting to note that the particle-size distribution as found by Komatsu and Grant exhibits log-normal behavior when replotted on log-probability coordinates. Dromsky, Lenel, and Ansell9 have observed the growth of Al2O3 particles having a mean free path of about 1.5 to 13 µ. Their photomicrographs indicate that the Al2O3 particle sizes were larger than those observed by Komatsu and Grant. Dromsky, Lenel, and Ansell concluded that the Al2O3 coarsened by an interface-controlled growth mechanism limited by the solution of A12O3 at the shrinking interfaces. Bannyh, Modin, and Modin10 have studied the spheroidization of a eutectoid steel (0.83 wt pet C). Their spheroidization (tempering) treatments were carried out in the range from 210o to 700°C for times between 1.5 sec and 20 hr. Measurements of mean particle size as a function of time indicated a cube root of time dependence of size at 700°C, in agreement with previous analyses of diffusion-controlled kinetics.2°7 At lower temperatures, the time dependence was less than the one-third power. It is important to note that, although mathematical models of growth* considering particle-size distribution have been available, measurements of only mean particle size have been carried out. DeHoff11 has presented a quantitative metallography technique which is applicable to the determination of the size distribution of ellipsoids of constant shape. This method is applicable to both oblate and prolate ellipsoids of all ratios of minor to major axis and is based upon an extension of Saltykov's analysis12 of the distribution of spheres of varying size. DeHoff's analysis is based upon measurements of the minor axis of the particles on a random plane of polish in a unit area. This method provides a measure of the number of ellipsoids in various size ranges per unit area. As pointed out by DeHoff, such measurements may be used to obtain surface area and total precipitate volume data. Thus, the accuracy of the distribution analysis may be checked by comparison of the surface and volume

Jan 1, 1965

By G. T. Davis, C. C. Mattax, M. O. Denekas

The effects of crude oil cornponents on the wellabil-ities of sandstone and limestone were investigated. Fractions containing cornponents differing in molecular weight and molecular structure were obtained from crude oils by distillation, extration and chromatography. Individual fractions were then tested for their effects on rock wettability. Tests indicate that sundstone wetta-bility may he changed by a complex variety of surfactants varying both in molecular structure and molecular weight. Limestone appears to be particularly sensitive to basic, nitrogenous surfactants. INTRODUCTION Investigations in recent years have shown that petroleum reservoir rock wettability can exert a significant influence on the efficiency with which oil can be produced by water flooding. While most reservoirs are presumably water-wet, they niay range in their degree of water-wettability from near-neutral to strongly water-wet.'" Reservoir wettabilities other than strongly water-wet are likely to be induced by adsorption of surface-active components froni the crude oil on the pore walls of reservoir rock.:' Little is known, however, about the nature of the surface-active materials which are likely to be adsorbed by the reservoir rock. Due to the complexity of crude oils. attempts made in the past90 isolate these surface-active components have met with only limited success. It is probable that many different types of surface-active materials arc indigenous to crude oils and that many of these may be adsorbed to varying degrees by reservoir rock. This was cxolored in the studies discussed in this paper. The over-all objective in these studies is to ascertain whether the wettability of a given reservoir can be determined by examining the surfactant content of the reservoir crude. To this end, crude oils were examined to determine the variability of indigeneous surfactants with regard to chemical type and molecular weight. Crude oils were separated by distillation into fractions differing principally in molecular weight, by chroma-tography into fractions containing compounds differing in polarity, and by solvent extraction into nitrogenous and non-nitrogenous fractions. Individual fractions were then tested for their effects on the wettabilities of sandstone or limestone rock samples. EXPERIMENTAL PROCEDURES Fractionation of the Crude Oils Samples of Miocene, Eocene and Jurassic crudes were distilled at temperatures not exceeding 200°C. The final stages of distillation were completed in a molecular still at pressures down to three microns of mercury. Fifteen to 30 fractions were obtained from each crude oil. These cuts were sufficiently broad that separation can be considered to have been effected principally on the basis of the molecular weights of the constituents of the crude oil. A considerable portion (20 to 40 per cent) of the crudes would not distill under these conditions. The residues were recovered and tested with the other fractions. Fractions differing in polarity were separated from a crude of Pennsylvanian age and an extracted sample of Miocene oil by chromatography, using a solid adsorbent. Since surfactants are, for the most part, polar compounds, chromatography should separate many of the surfactants from the crude oil. Such a separation should provide fractions containing compounds differing in molecular structure. Nitrogeneous compounds were extracted from Miocene crude oil with a solution of sulfuric acid in meth-anol. The residual oil was further processed by chonia-tography. Each of the fractions obtained by thesc procedures was dissolved in a non-polar solvent (xylene) and diluted to its original concentration in the crude oil. No attempt was made to maintain an anaerobic atmosphere above the samples while they were being dissolved. These solutions of the fractions were then tested for their effects on the wettability of sandstone and limcstone as discussed in the next section. Measurement of the Effects of Crude Oil Fractions on Rock Wettability No entirely satisfactory method for measuring rock wettability has yet been developed. All methods used are empirical. The imbibition test was used in these studies. This test is based on the tendency of a rock to imbibe the wetting phase spontaneously. For example, if a strongly water-wet rock is first saturated with oil and then placed in water, the water will quickly invade the rock by capillarity and much of the oil will be displaced. If the rock is slightly water-wet, water irnbibition will proceed more slowly and, in many instances, considerably less oil will be displaced. A water-saturated, oil-wet rock will imbibe oil. The initial rate with which water (or oil) imbibition takes place indicates, qualitatively, the degree of water (or oil) wettability of the rock.

By M. T. Simnad, G. Derge, Ling Yang

STUDY of diffusion in molten substances is important in at least two respects. Diffusion data, combined with thermodynamic and kinetic information, throw light on the structure of the liquid state. Moreover, a knowledge of diffusion coefficients and their temperature dependence is useful in ascertaining the controlling step in many metallurgical reactions. Although diffusion measurements have been made on a number of molten salts, slags, metals, and alloys,'-'" the results available are still limited and widely scattered, especially for the high temperature melts. It is the purpose of this investigation to establish reliable procedures for the measurement of self-diffusion coefficients in high temperature melts and to use these procedures to determine the self-diffusion coefficients of iron in molten Fe-C alloys of different carbon contents. Experimental Measurement of self-diffusion coefficients in high temperature melts is usually carried out by using one of two methods. In the first, diffusion takes place between two cylindrical samples of the same material, one of which is made radioactive. The diffusion coefficient is calculated from the radioactivity penetration curve in the solidified sample after the diffusion. In the second method, samples contained in capillaries of an inert substance are immersed in an infinite reservoir of the same material. Either the material in the capillary or that in the reservoir is made radioactive and the diffusion coefficient is calculated from the change of the radioactivity of the sample in the capillary after the diffusion. The second method is simpler because a radioactivity penetration curve is not needed for the calculation of the diffusion coefficient; however,.it is valid only when no convection has occurred in the capillary during the diffusion. A radioactivity penetration curve is therefore always useful in indicating that the required conditions for the diffusion are ful- filled. Towers and Chipman" recently studied the self-diffusion of calcium and silicon in CaO-Al,O,-SiO, melts by using the capillary method. Instead of measuring the change of the radioactivity of the sample in the capillary, they autoradiographed the sample after the diffusion and calculated the diffusion coefficient from the intensity distribution of the autoradiograph. Their method is useful when the radioactive isotopes are weak ß-emitters, but is very difficult, if not impossible, to apply to cases involving strong ß or y-emitters. For such cases, sectioning of the sample according to the method of Morgan and Kitchener' may be used for the construction of the radioactivity penetration curve. The self-diffusion of iron in molten Fe-C alloys has been studied in this manner and the experimental procedures are described as follows: The diffusion apparatus is shown schematically in Fig. 1. The bath consisted of about 200 g of an Fe-C

Jan 1, 1957

By G. Sachs, E. P. Klier, W. Beck

HYDROGEN embrittlement of steels has recently attracted much attention because it is asso- ciated with a variety of failures, especially those of aircraft structural components.' For instance, one of the undesirable properties of the ultra-high strength steels used for landing gears is their pronounced susceptibility to hydrogen embrittlement during plating. The presence of hydrogen in these steels becomes particularly apparent through delayed or sustained load failures of parts which have been subjected to low loads for an extended time. A number of variables are involved in causing a reduction of strength and ductility through hydrogen

Jan 1, 1957

By Donald C. Barton

OF the four papers that comprise this Technical Publication, three are case histories of individual geophysical prospects, subsequently tested by drilling. The bibliography of Dr. Barton's published scientific paperst includes investigations in physiography and surface geological mapping, as well as his geophysical papers, and from this list it is to be observed that he early recognized the place of different types of geophysical prospecting methods in the search for geological structures of economic importance. Moreover, his viewpoint was not merely that the structures should be found, but that the geophysical data should be examined quantitatively to determine the geometry of the structures. In other words, that although these data are insufficient to deduce a unique form for the structure that caused the effects measured in the data, the engineering computations should be carried out to give as much of a definite configuration to the structure as the data permitted, in order that the testing of the structures could be conducted in the most economical manner and with the idea that the experience so gained could be later incorporated in the study of structures subsequently found. Dr. Barton continually emphasized the quantitative use of geophysical observations, whereas at the time that he began his specialization in geophysics it was considered sufficient to use observations only qualitatively. He, more than any one else, was responsible for the first volume on geophysical prospecting issued by the Institute in 1929, and his three articles in that volume stressed the quantitative use of geophysical prospecting. The fourth article in this present Technical Publication is a further contribution to this branch of geophysical interpretation, and is a supplement to the paper in the 1929 volume, "Calculations in the Interpretation of Observations with the Eötvös Torsion Balance." From the successful demonstration by Dr. Barton of the usefulness of quan-

Jan 1, 1946

By Donald C. Barton

OF the four papers that comprise this Technical Publication, three are case histories of individual geophysical prospects, subsequently tested by drilling. The bibliography of Dr. Barton's published scientific paperst includes investigations in physiography and surface geological mapping, as well as his geophysical papers, and from this list it is to be observed that he early recognized the place of different types of geophysical prospecting methods in the search for geological structures of economic importance. Moreover, his viewpoint was not merely that the structures should be found, but that the geophysical data should be examined quantitatively to determine the geometry of the structures. In other words, that although these data are insufficient to deduce a unique form for the structure that caused the effects measured in the data, the engineering computations should be carried out to give as much of a definite configuration to the structure as the data permitted, in order that the testing of the structures could be conducted in the most economical manner and with the idea that the experience so gained could be later incorporated in the study of structures subsequently found. Dr. Barton continually emphasized the quantitative use of geophysical observations, whereas at the time that he began his specialization in geophysics it was considered sufficient to use observations only qualitatively. He, more than any one else, was responsible for the first volume on geophysical prospecting issued by the Institute in 1929, and his three articles in that volume stressed the quantitative use of geophysical prospecting. The fourth article in this present Technical Publication is a further contribution to this branch of geophysical interpretation, and is a supplement to the paper in the 1929 volume, "Calculations in the Interpretation of Observations with the Eötvös Torsion Balance." From the successful demonstration by Dr. Barton of the usefulness of quan-

Jan 1, 1946