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By George C. Fryburg

The oxidation of platinum at high temperatures (above 800°C) is controlled by boundary-layer diffusion, except at the lowest pressures. The rate of oxidation is determined by the rate of diffusion of oxide through the boundary layer away from the platinum. This is in contrast to the situation in tungsten and molybdenum oxidation, where the rate is controlled largely by the diffusion of oxygen through the boundary layer towards the metal. The difference in mechanism is a consequence of the much lower rate of oxidation of platinum. Evidence is presented that supports this mechanism for the oxidation of platinum. SOME years ago we reported1 a study of the oxidation of platinum in ordinary oxygen in the temperature region above 800°C, where the oxide is volatile. All the data available up to that time had been obtained with platinum crucibles or plates heated in tube furnaces. The results were widely variant and highly dependent on the flow rate of gas through the furnace: the faster the gas flow rate, the higher the measured oxidation rate. These results indicated to us2 that reaction equilibrium was being approached in the furnace and that the rate was diffusion limited. To minimize these effects, we employed1 electrically heated ribbons placed in a cooled bulb. We were primarily interested in the low-pressure region, but some experiments were performed at pressures up to 1 atm. We found a peculiar pressure dependency which was explained on the basis that the rate of oxidation was proportional to the pressure at all pressures, but that with increasing pressure an increasing fraction of the volatilizing oxide was back-reflected to the ribbon by the surrounding gas molecules. The oxide molecules are not stable at the temperature of the platinum and are decomposed on impact, the platinum being re-deposited on the specimen. Because of the limitations of space, this explanation was offered summarily without detailed support. Recently, Jaffee and associates3, 4 have suggested that the pressure dependency of our data up to 0.5 torr could be explained on the basis of a Langmuir-type adsorption of molecular oxygen followed by dissociation. Since the correct explanation of the effect of pressure on the oxidation rate is a necessary requirement to the development of the basic mechanism of the oxidation reaction, we felt that the back-reflection theory should be presented in more detail. This is the object of the present paper. RESULTS AND DISCUSSION A typical set of results showing the pressure dependency of the oxidation reaction is presented in Fig. 1, where we have plotted, on logarithmic scales, the rate of oxidation, R, vs the pressure, p. For comparison some results of Krier and Jaffee4 and of Raub and plate5 are also shown. These data were taken at atmospheric pressure using furnaces. The effect of reaction equilibrium within the furnace is apparent from the much smaller values that these observers obtained: Raub and Plate In O2 found a rate of 3.1 µg cm-2 hr-1 compared to our value of

Jan 1, 1965

By J. Suiter, H. F. Ryan

H. F. Ryan and J. Suiter (CSIRO)—In this paper the authors have presented "a physical model which has as its central hypothesis the solution strengthening of regions along grain boundaries in the order of tens of angstroms thick", and their calculations have used 40Å as the zhalf-width of this boundary region. Selection of this value by the authors suggests that they were unaware of a number of recent field-ion microscope observations of grain boundary structures (e.g., Refs. 29 and 30). The accompanying figure, Fig. 9, shows a portion of an ion micrograph of a tungsten specimen containing a grain boundary, and the regular arrangement of atoms in various crystal planes in each grain can be seen, except in the boundary zone which is not more than two atom diameters in width. Since it is expected that solute atoms will segregate only to the region where the lattice is disturbed, it would seem that a value of 4Å for the half-width of the boundary region would be more appropriate than the value of 40Å assumed by the authors. If the former value is used in Eq. [8] of their paper to obtain curves showing solute concentration in the grain boundary as a function of temperature, the resulting curves differ significantly from those obtained by the authors. Although there are only relatively slight changes in the regions corresponding to higher temperatures (i.e., grain boundary concentrations of approximately 1 at. pet), at lower temperatures the curves are no longer realistic. For example, the curve corresponding to u = 7000 cal per mole gives a solute grain boundary concentration in excess of 100 pet at a temperature of approximately 360°K, and "flattens out" at a grain boundary concentration of about 300 pet! Similar results are obtained with each of the other curves. Ion microscopy of dilute solid-solution alloys has shown that solute atoms give rise to image points which in most cases are of higher intensity than those of the solvent atoms.31 If the same behavior occurs when the solute atoms are present in much lower concentrations then ion microscopy should provide a sensitive tool for studying the segregation of impurities to the grain boundary regions. Although many grain boundaries in tungsten have been examined after different thermal and mechanical treatments, there has not been, as yet, any systematic study of such segregation. In general the micrographs show no clear indications of marked grain boundary segregation, but occasionally areas are found where the grain boundary contains an appreciable number of image points of high intensity in a very narrow zone, see Fig. 9. If it is assumed that these correspond to impurity atoms then it is possible to estimate the impurity concentration both in the grain boundary and within the body of the grains. Application of this method (to a larger area

Jan 1, 1965

By L. Obert, D. E. Stephenson

The objectives of this investigation were to develop a laboratory procedure in which core discing could be produced under known (and variable) stress conditions, and to study the discing characteristics of several fypes of rock. Discing of rock cores refers to the formation of discs or wafers of relatively uniform thickness which fracture or rupture on surfaces approximately *Fracture is a type of failure in which there is a complete loss of cohesion and fresh surfaces are created. Rupture is a type of failure in which there Is only a partial loss of cohesion. normal to the axis to the core (see Fig. 1). Usually the surfaces of the discs are concave-convex with the concave side toward the collar of the hole. The surface of the fractured discs are like those created by a tension failure (or possibly a shear failure with virtually no normal compressive stress). This phenomenon has been observed by a number of investigators1-5 in the course of diamond drilling in underground mines, especially in areas suspected of being under high stress. The state of stress in the core required to produce discing is not exactly known. Tranter and craggs6 theoretically investigated the stress distribution in an infinite cylinder, subjected to hydrostatic pressure, minus p, from z = 0 to z = 8 and unloaded from z = 0 to z = 8, Fig. 2. The exact solution to this problem shows that a tensile stress develops in the loaded region near z = 0 with the greatest tensile stress on the axis of the cylinder. A tensile stress also developed on the surface of the cylinder at a point just outside of the loaded zone. Jaeger and Cook3 experimentally investigated the discing mechanism by biaxially loading cores in a pressure jacket sealed at the ends by O-rings. According to the Tranter and Craggs theory it would be expected that failure should occur at the pressure discontinuity at the O-rings. The experimental results showed that if the specimen was unjacketed it broke at random points within the pressurized zone and at a pressure somewhat greater than the tensile strength of the specimen, presumably due to the development of a

Jan 1, 1965

By D J. Murray

This paper outlines the principles of friction hoisting and the components involved, and gives a description of a specific mine hoist. Friction hoisting is compared with conventional drum hoisting, and the depth of shaft at which friction hoists become more economical than drum hoists, with respect to power consumption, is determined. Introduction T HE purpose of this paper is to outline the principles of friction hoisting, to describe the components and to show the advantages of multi-rope friction hoisting. Some calculations are made to show that the power requirements and the initial costs of friction hoists are less than those of conventional drum hoists, once a certain depth of shaft has been reached. The use of multi-rope friction hoists is gradually superseding the employment of the conventional drum hoist in many parts of the world. It results in heavier payloads from deeper levels, an increase in shaft safe-ty and a more compact installation for protection against adverse weather conditions. It was observed that where drums and friction sheaves exceeded 30 feet in diameter, a number of mechanical disadvantages were being experienced;

Jan 1, 1965

By L. H. Adami

The heats of formation of anhydrous cadmium sulfate, cobalt sulfate, copper sulfate, nickel sulfate, and zinc sulfate were determined by hydrochloric acid solution calorimetry. The values at 298.15° K for formation from the metal, rhombic sulfur, and oxygen gas follow (cal/mole): CdS04J -222.0 ± 0.3; CoS04, -212.0 ± 0.4; CuS04) -183.4 ± 0.6; NiS04, -208.1 ± 0.2; and ZnS04, -233.1 ± 0.2. Corresponding heats of decomposition to form the metal oxide, sulfur dioxide, and oxygen were derived from these results; heats of decomposition to form the metal oxide and sulfur trioxide were also derived.

Jan 1, 1965

By W G. Forbes

SOME 20 years ago, upon finishing second year at the University of Manitoba, I was faced with the choice of whether I wanted to be a geologist or a chemist. Accordingly, I sought out Professor Brownell, Head of the Department of Geology, to ask him what a geologist did. His reply contained the statement that following graduation one went out into the field in northern Canada for 5 to 15 years to reduce to practice what had been learned at university. To a young man, very socially conscious, even one year, let alone 5 to 10, in a small mining community sounded like being banished to a monastery in the Himalayas and thus I turned to chemistry. Moving to the present, last month I asked a geologist, and then a mining engineer, what does the fresh graduate in their field do these days? The reply was: usually serve an apprenticeship for an indeterminate period either underground or in the field learning the job.

Jan 1, 1965

By W W. Moorhouse

A survey of recent literature indicates that sulphides occur in the volcanic rocks of the Archean, or in sedimentary rocks intercalated with the volcanic rocks. The thick sedimentary sections are generally poor in sulphides. Thus, the widespread pyrite and pyrrhotite mineralization in the Archean may be largely of volcanic origin. Introduction I N this paper, commercial base-metal deposits will not be considered, as they are dealt with in other papers of the Symposium. Instead, attention will be focused on those sulphides, often associated with graphitic argillites or tuffs, which have appeared in such embarrassing abundance in electromagnetic surveys of Archean areas. The data on which the paper is based are drawn from recent reports of the Ontario Department of Mines, the Quebec Department of Natural Resources and the Geological Survey of Canada. The information available from these sources is unfortunately limited, because sulphides commonly occur in sheared rocks, such as black argillites and tuffs, which rarely form conspicuous outcrops, and may not be exposed at all. Thus, in the absence of geophysical information, even detailed mapping may fail to reveal the presence of sulphide-rich rocks.

Jan 1, 1965

By A. S. Michaels, M. C. Porter, A. Stancell

Previous laboratory studies have demonstrated that the injection of small quantities of reverse wetting agents during water displacement can increase oil recovery from unconsolidated porous media.9 In the present investigation, an attempt has been made to determine more fully the effects of reverse wetting treatments and to clarify the mechanism by which increased oil recovery is effected. Water-oil displacements were performed in beds of 140-200 mesh silica sand. Hexylamine slugs (injected after 0.25 pore volume of water throughput), when adequate in size and concentration, were effective in promoting additional oil recovery. Their effectiveness increased with the quantity of amine injected. However, slugs of sufficient size and concentration to stimulate oil production at water flow rates of 34 ft/day did not do so at 4 ft/day. Visual studies in a glass grid micromodel have shown that the stimulation of oil production, via ayueous hexylamine, is a result of transient changes in the oil wettability of the pore walls. if the amine slug is of sufficient size and concentration to induce significant changes in the adhesion-tension, large continuous oil masses will be formed. if the superficial water velocity is high enough to result in rapid desorption of the amine, a favorable "wettobility gradient" may be established across the masses; under such conditions, high oil mobility is observed, and increased oil recovery results. INTRODUCTION It is generally agreed that the efficiency of oil displacement by water in porous media is limited in part by capillary forces which cause the retention of isolated masses of oil — resulting in the so-called "irreducible minimum oil saturation". Recent estimates10 indicate that there are about 220 billion bbl of petroleum in United States reservoirs which are not economically recoverable with present techniques (such as water flooding). This amounts to almost five times the known recoverable reserves. It has been recognized for some time that a suitable alteration in the water-oil interfacial tension and/or the contact angle, as measured between the water-oil interface and the solid surface, should result in better displacement efficiency. Surface active agents can be used as interfacial tension depressants to accomplish this objective,1,2,7 but unfortunately, the additional oil recovery is seldom commensurate with the treatment cost. In contrast to interfacial tension depressants, the effect of contact angle alterations on water-oil displacements has received relatively little attention in the literature. It is known that the wettability affects the displacement process.3,4,11 Displacements in water-wet systems generally result in lower residual oil saturations than those in oil-wet systems. The effect of "'transient" wettability alterations concurrent with the displacement process have been investigated by Wagner, Leach and coworkers,4,11 wherein it has been demonstrated that the establishment of water-wet conditions during water flooding of oil-wet, oil-saturated porous media is accompanied by significant increase in oil displacement efficiency. Michaels and Timminss studied the effects of transient contact angle alterations resulting from chromatographic transport of reverse wetting agents through unconsolidated sand. It was demonstrated that chromatographic transport of short-chain (C4 through C8) primary aliphatic amines can improve oil recovery and that the recovery increases with the quantity of amine injected (i.e., with either the amine concentration or the volume of the slug injected). Circumstantial evidence indicated that the increased displacement efficiency resulted primarily from transient changes in wettability of the porous medium. In the Present investigation. additional information has been obtained on the effects of reverse wetting treatments and the mechanism by which increased oil recovery is accomplished. Hexylamine slugs of varying size and concentration were chromato-

Jan 1, 1965

By B. A. Joyce, R. W. Bicknell, R. J. Bennett, P. J. Etter

Epitaxial layers of silicon have been grown on single-crystal quartz and alumina by two types of chemical reaction the hydrogen reduction of trichlorosilane and b) the pyrolysis of silane. These reaction systems are described. The cqsfallography of the two systems, as determined by electron and X-ray diffraction, is discussed, and epitaxial mechanisms suggested. The electrical behavior is briefly considered, and the design and properties of field-evert devices fabricated in the epilaxial material are also discussed. RECENT work carried out in these laboratories" has shown that it is possible to obtain epitaxial deposits of silicon on single-crystal quartz and alumina. The purpose of this paper is to describe the method of preparation of these layers using both the hydrogen reduction of trichlorosilane and the pyroly-sis of silane, to compare the crystallographic behavior of films on the two substrates, and to present some initial results of the electrical behavior of silicon layers on alumina. The structural study has been carried out using electron and X-ray diffraction and electron microscopy. The electrical assessment has been made in terms of conductivity and mobility determinations by the van der pauw3 technique, and by measurements on metal-oxide-semiconductor assemblies. 1) FILM PREPARATION Both quartz and alumina substrates, approximately 1 sq cm in area and 0.4 mm thick. were prepared from slices cut parallel to within a few degrees of (11.0), (10.0), and (00.1), and polished mechanically down to about 0.3 p diamond grade. Chemical polishing of alumina slices, using phosphoric acid at elevated temperatures, has also been used; epitaxial silicon layers have been grown on these substrates, but the process is not entirely reliable, possibly because the large strain present in the Verneuil-grown alumina crystal affects the chemically prepared surface. The two reaction systems are fairly conventional and are described briefly below. a) Trichlorosilane-Hydrogen System. The apparatus is shown schematically in Fig. 1. The substrate was heated by induction, with a fused-quartz encapsulated graphite hemicylinder as susceptor. The procedure for carrying out a deposition was to heat the substrate to reaction temperature in a stream of

Jan 1, 1965

By K. E. Brown, A. R. Hagedorn

Continuous, two phase flow tests have been conducted during which four liquids of widely differing viscosities were produced by means of air-lift through 1%-in. tubing in a 1,500-ft. experimental well. The purpose of these tests was to determine the effect of liquid viscosity on two-phase flowing pressure gradients. The experimental test well was equipped with two gas-lift valves and four Maihak electronic pressure transmitters as well as instruments to accurately measure the liquid production, air injection rate, temperatures, and surface pressures. The tests were conducted for liquid flow rates ranging from 30 to 1,680 BID at gas-liquid ratios from 0 to 3,-270 scf/bbl. From these data, accurate pressure-depth traverses have been constructed for a wide range of test conditions. As a result of these tests, it is concluded that viscous effects are negligible for liquid viscosities less than 12 cp, but must be taken into account when the liquid viscosity is greater than this value. A correlation based on the method proposed by Poettmann and Carpenter and extended by Fan-cher and Brown has been developed for 1¼-in. tubing, which accounts for the effects of liquid viscosity where these effects are important. INTRODUCTION Numerous attempts have been made to determine the effect of viscosity in two-phase vertical flow. Previous attempts have all utilized laboratory experimeneal models of relatively short length. One of the initial investigators of viscous effects was Uren1 with later work being done by Moore et al.2,3 and more recently by Ros.4 However, the present investigation represents the fist attempt to study the influence of liquid viscosity on the pressure gradients occurring in two-phase vertical flow through a 1¼-in., 1,500 ft vertical tube. The approach of some authors has been to assume that all vertical two-phase flow occurs in a highly turbulent manner with the result that viscous effects are negligible. This has been a logical approach since most practical oil-well flow problems have liquid flow rates and gas-liquid ratios of such magnitudes that both phases will be in turbulent flow. It has also been noted, however, that in cases where this assumption has been made, serious discrepancies occur when the resulting correlation is applied to low production wells or wells producing very viscous crudes. Both conditions suggest that perhaps viscous effects may be the cause of these discrepancies. In the first case, the increased energy losses may be due to increased slippage between the gas and liquid phases as the liquid viscosity increases. This is contrary to what one might expect from Stokes law of friction,' but the same observations were made by ROS4 who attributed this behavior to the velocity distribution in the liquid as affected by the presence of the pipe wall. In the second case, the increased energy losses may be due to increased friction within the liquid itself as a result of the higher viscosities. The problem of determining the li- quid viscosity at which viscous effects becomes significant is a difficult one. Ros4 has indicated that liquid viscosity has no noticeable effect on the pressure gradient so long as it remains less than 6 cstk. Our tests have shown that viscous effects are practically negligible for liquid viscosities less than approximately 12 cp. Actually there is no single viscosity at which these effects become important. These effects are not only a function of the viscosities of the liquids and of the gas but are also a function of the velocities of the two phases. The velocities in turn are a function of the in situ gas-liquid ratio and liquid flow rate. Furthermore, the role of fluid viscosities in either slippage or friction losses will depend on the mechanism of flow of the gas and liquid, i.e., whether the flow is annular. as a mist, or as bubbles of gas through the liquid. These mechanisms are also a function of the in situ gas-liquid ratios and the flow rates. It would thus seem that the best one could hope for is to determine a transition region wherein the viscous effects may become significant for gas-liquid ratios and liquid production rates normally encountered in the field. The viscous effects might then be neglected for liquid viscosities less than those in the transition region but would have to be taken into account when higher viscosities are encountered. There are numerous instances where crude oils of high viscosity must be produced. The purpose of this study has been to evaluate the effects of liquid viscosities on twephase vertical flow by producing four liquids of widely differing viscosities through a 1 % -in. tube by means of air-lift. The approach used in this study was as follows:

Jan 1, 1965

By A. D. Marlin, A. J. Gentile, E. F. Jordan

Metallurgical changes in SAE 52100 ball-bearing components resulting from overload testing are described. Changes in microstructure, hardness, and resiclctal stresses crre discussed zuitlz re.ference to material cleanliness obtained by various steel-melting practices and are compared with work by otlzer investigators. Evidence is presented to show that the initialion and development of microstruc-tural alterations are characterized by two separate reactions: the appeavance of a "dark etchingJ' constituent, and "gray lines" or a light etclzing constituent. The dependency of these tzvo reactions on material cleunliness, running tirne, and contact stresses is discussed and a failure mode related to material cleanliness and microstructural transformation is proposed. THE study of ball- and roller-bearing contact fatigue has been paced by a strong emphasis on bears ing application performance. Particular attention has been paid to conditions that effect the spalling-type failure that is characteristic of rolling contact fatigue in through-hardened components. Some of the conditions investigated are lubrication and atmosphere,1-3 material characteristics and finish,475 and speed and design fa~tors."~ A typical spalling-type failure is shown in Fig. 1. The arrow shows the motion of the ball relative to the inner-ring race surface. The leading edge of the spall is usually sharper than the trailing edge. The race surface near the trailing edge also shows small dents caused by debris from the spall. In this type of testing very little metallurgical investigation is done on failed bearings. Emphasis is placed on test conditions and statistical analyses of endurance data. More basic work has been done relating micro-structural changes to fatigue performance. Dyer" and Wood, Cousland, and sargant9 have used mostly simple materials, such as single crystals and single-phase polycrystalline specimens, under simple alternating strain to identify a systematic process of fatigue damage. drutowski" was concerned primarily with the relationship between steel structure, contact stress, and energy losses in rolling contact. dones11 and Bush, Grube, and Robinson12 utilized changes in microstructure and residual stress in overload-tested rolling contact elements as a means of investigating the fatigue process. Work is being done on an ASME-sponsored contract,13 using both simple and complex materials, but there is still a long way to go before such theories as pore and void growth in simple structures can be applied to the relatively complex bearing steel microstructure. The purpose of this paper is to report on an investigation into the effect of steel cleanliness on the structural alteration and residual stress changes found in overload-tested ball bearings. Using these results and those of previous investigators, we will propose probable failure mechanisms in both overload- and normal load-tested ball bearings.14,15 PROCEDURE Ball bearings? 3208 size, were fabricated from SAE 52100 steel obtained by five different melting practices. The melting practices, chemistry, and inclusion ratings for the five lots of steel are summarized in Tables I and 11. The nonmetallic inclusion ratings were determined by the Jernkontoret method described in ASTM E45-51 Method A. This technique consists of microscopically examining a series of polished samples taken from specified locations in the ingots, billets, or bars. Each sample is surveyed at XlOO magnification and the inclusion types and sizes are compared to standard fields. Because of the nature of these ratings all values in Table I1 are rounded to the nearest half. The elec-

Jan 1, 1965

Jan 1, 1965

By E. P. Klier, Jane Jellison

The course of the transformations on cooling in a series of Cu-A1 alloys has been followed by means of thermal analysis, X-ray diffraction, and optical metallogrAphy. Specimen size was found to have a pronounced effect on the time of completion of the pearlite transformation due to modification in the unmber of nuclei. The ordeving transformation zvas observed for all cooling rates for all alloys studied, and is considered insuppvessible. At intermediate cooling' rates, a transitional struchire for 011 alloy compositions and based ox the bainite reaction was observed. The alloys of aluminum and copper possess a eu-tectoidal region at from about 9.4 to 16 pct Al. Above the critical temperature, the disordered bcc phase, 0, is stable. At subcritical temperatures, the 0 phase decomposes under equilibrium conditions into the stable phases, a and y,. At the eutectoid composition, these phases develop a lamellar pearlite structure, in appearance much like that found in steels. During rapid quenching from supercritical temperatures, the diffusion processes required for the formation of the equilibrium phases are suppressed, and the 0 transforms to an acicular martensitic phase, designated B or y' depending on the aluminum content, or to a mixture of the two. Early investigators of this system concentrated on determining the equilibrium phase diagram, ''' the structure of the equilibrium phases,3 and later the isothermal decomposition of the 0 phase at subcritical temperatures, or the decomposition of the martensite on tempering. Other work which treated the nonequilibrium transformations concentrated largely on the martensite transformations and the structure of the b and y' phases.15"17 Since the pearlite and martensite transformations in this system resemble those in steels, the one being formed by nucleation and growth of adjacent lamellae of the equilibrium phases, and the other by a diffusionless, shear-type transformation, the present study has been undertaken to investigate the structures formed on continuous cooling, with the objective of constructing cooling transformation diagrams analogous to those derived for alloy steel systems. In particular it was desired to determine whether parallels between the A1-Cu and iron-iron carbide systems on continuous cooling extended to encompass the intermediate phase, namely the bainite structures, which form by a combined martensitic-diffusion mechanism,'' but which are supersaturated with respect to the equilibrium phase upon which their crystal structure is based. To this end the transformations in representative alloys of the Cu-A1 B eutectoid system have been followed, using the methods of thermal analysis, X-ray diffraction, and optical microscopy. EXPERIMENTAL PROCEDURE Materials. The materials tested were those used by Klier and Grmko 5 in their study of the isothermal decomposition of these alloys. The alloys were melted in graphite crucibles and chill-cast into 5 by 2 by 1/4 in. ingots. The ingots were then hot-rolled to sheets 1/8, 1/16, and 1/32 in. thick. The compositions are given in Table I. Specimen Preparation. Specimens for thermal analysis were in the form of small squares approximately 1/4 in. on a side. For the 11.9 and 13.5 Al-Cu alloys, the sheet thickness was 1/16 in. and for the 10.5 A1-Cu alloy the 1/32-in. sheet was used. One lead of a chromel-alumel thermocouple was spot-welded to either face of the square with the specimen itself thus forming the hot junction of the thermocouple. Specimens for X-ray analysis were prepared as filings from martensitic sheet stock and were sealed in glass ampoules under 1/2 atm of argon. Metallographic examination of the powder specimens was carried out on a portion of the heat-treated filings mounted in lucite. All specimens were examined metallographic ally after etching

Jan 1, 1965

By H. Conrad, K. Janowski, E. Stofel

In a previous paper,1 the occurrence of (0001) and (0111) twins was reported for compression tests of 60-deg-oriented sapphire rods in the temperature range from 1100° to 1300° C. Subsequent to this initial work, additional tests have been conducted, and twinning has been found to occur at temperatures as high as 1500° C. Also, the temperature and strain-rate conditions for the two types of twins and for slip have been established in more detail. The present note covers this more recent work. The compression-test data are summarized in Table I. The techniques for identifying the twins are optical examination up to X1000 and X-ray analysis.' It is evident that (0711) twins are pre-

Jan 1, 1965

By R. H. McLean

Jet impingement produces two mechanisms to clean the bottom of a borehole during jet-bit drilling operations. One is an impact-pressure wave in the immediate area of jet impingement. The other is crossflow, which spreads across the bottom away from the pressure wave. Measurements of the vertical distribution of the cross-flow at several positions beneath a 4 3/4-in. tricone jet bit in a laboratory model show that the maximum velocity in the crossflow is directly proportional to the square root of the product of the rate of flow and the velocity of the jets through the nozzles (QV). Other measurements in the laboratory model show that gradients in the impact-pressure wave are directly proportional to the jet QV if the diameters of the nozzles are held constant. Consistency of the basic relationships through changes in the Reynolds numbers of the jets from 31,000 to 93,000 suggests that the laboratory results should be representative of typical flow in field operations having higher Reynolds numbers. Estimates of the impact-pressure waves under conditions other than those in the jet-bit model may be made by comparison with a less complex model—impingement of a jet against an unrestricted flat surface normal to the jet. Equations derived from current jet technology describe the wave in this simple system for a wide range of conditions. INTRODUCTION The efficiency of rotary drilling operations is strongly linked to the efficiency with which cuttings are removed. Cuttings remaining on the bottom of the borehole will impede further penetration by the bit until they are removed. Wasteful regrinding is prevented if the fluid circulated past the bit removes cuttings as rapidly as they are made. Most investigations of bottom-hole cleaning under bits have been concerned with the rate-of-penetration effects of bit type, nozzle configuration, fluid properties, pressure gradients and utilization of hydraulic horsepower. These investigations have shown that drilling muds, weighted to keep the pressure in the borehole greater than in adjacent formations and carrying material which forms a filter cake, apparently plaster cuttings against the bottom, making them difficult to remove. In addition to a demonstration of the factors causing poor cleaning, the most significant result of these previous investigations has been the increased use of jet bits accompanied by better hydraulic programs and better selection of drilling fluids. Undoubtedly, these practices have improved bottom-hole cleaning, but rates of penetration when drilling with muds are still often lower than would be expected with perfect cleaning." Although there is general agreement with the concept that increasing hydraulic energy at a jet bit often increases the rate of penetration by improving cleaning, research workers have differed as to the best criterion for evalyating hydraulics. Some lean toward maximizing the product of the rate of flow and the velocity through the nozzles (QV) others prefer to maximize the hydraulic horsepower at the bit;'"-' "till another says that neither criterion is universally suitable."' This controversy shows that conclusive field evidence has not established the superiority of either of these criteria. Analysis of the fluid flow which cleans the bottom should contribute to resolving the controversy. Impinging jets clean the bottom by creating two mechanisms capable of dislodging cuttings. One is the impact from the momentum of the jet and the other is the flaw parallel to the bottom away from the area of impingement. The impact force appears in the form of a pressure wave on the bottom and, in this paper, is called the impact-pressure wave. The flow parallel to the bottom is called crossflow. Fig. 1 illustrates these two mechanisms. This paper describes crossflow and the impact-pressure wave beneath jet bits and relates them to controllable parameters. Through these relations, criteria for use in designing hydraulics to achieve maximum use of the mechanisms of cleaning are derived. PROPERTIES OF CROSSFLOW CONCEPTS DEVELOPED IN PREVIOUS INVESTIGATIONS Concepts of scavenging the bottom by crossflow have been well discussed by Bobo, et al." They examine the means by which crossflow may create forces on cuttings and conclude that the cleaning action of crossflow can be increased by increasing the velocity of the flow stream close to the bottom. Using boundary layer theory, they indicate that a reduction in the viscosity of the drilling

Jan 1, 1965

By E. D. Hummer

During the planning phase of the fine coal cleaning addition at the Gary Coal Preparation Plant, careful consideration was directed toward the problem of minus 48 mesh refuse disposal. The plant flow sheet included wet screening the raw coal at 1/4 inch, pumping the minus 1/4 inch raw coal to bowl desiltors for desliming, and then cleaning the disliked raw coal on tables. The material to be removed from the circuit as minus 48 mesh refuse consisted of the minus 100 mesh desiltor overflow thickened in two 120 foot diameter thickeners and minus 1 mm screened from the table refuse. Later a flotation plant was added to recover coal from the desiltor overflow, and a classifier replaced the screens to make a sharper size separation of the table refuse at 48 mesh Today the minus 48 mesh refuse at Gary consists of thickened flotation tailings and thickened spiral classifier overflow. The transportation of large quantities of fine wet refuse filter cake mixed with jig and table refuse over existing conveying equipment would have been neither dependable nor economical. Filtration was therefore impractical, and disposal of the fine materials was a problem. The decision was to pump the material to storage ponds

Jan 1, 1965

By Arnold E. Lamm

The degree of economic, progress of a nation is measured by its possession and use of energy, sources. The future of coal in the West hinges on its ability to participate and grow in the energy market. A source of energy is, in the long run, only as good as the ability of the industry to develop its reserves economically. The economic development of the tremendous coal reserves, literally hundreds of billions of tons of coal in the States of Colorado, Utah, Wyoming, Montana, New Mexico, and Arizona, poses a very real question in the light of the known mining technology of our day. Basically in America today, coal is mined from the earth either by the strip mine or underground mine method; in the West, the large long-term, contracts now in force with utilities are mostly from coal mines utilizing the strip mine method. However, the preponderance of the known coal reserves of the West are located deep underground and will have to be mined by the various; underground mining processes. The problems encountered in the West with regard to underground mining vary from state to state but, on the whole, do not present what might be considered a miner's bonanza. I do not mean to' infer that the underground coal of the West is unmineable, but I do want to emphasize that the tremendous reserve figures do not present a true picture in the light of present day technology.

Jan 1, 1965

By R. E. Ogilvie, J. I. Goldstein, R. E. Hanneman

The interdiffusion coefficients for the Fe-Ni system were determined as a function of composition in both the a and y phases at 1 atm pressure. The inter diffusion coefficients were also determined in the y phase at 40 kbar pressure. The concentration gradients were measured with an electron probe, and the diffusion coefficients were calculated by the Matano analysis. At 1 atm, Ey increases with nickel content up to 65 at. pct Ni. The relationship of Dy with temperature and nickel concentration, up to 50 at. pct Ni, is given by the equation DY-l atm = exp(.0519 CN~ +1.15) MANY of the transformations that occur in the solid state are diffusion-controlled, especially those involving precipitate growth in most metallurgical systems. Multicomponent diffusion is usually expressed in terms of a chemical or an inter diffusion The activation energy Q at 1 atm decreases from pure iron to 60 to 70 at. pct Ni and decreases from pztre nickel to 60 to 70 at. pct Ni. The Kirkendall marker movement indicates that DFe is greater than DNi zcp to about 60 at. pct Ni. Above 60 at. pct Ni, however, DNi becomes peater than DFe The inter diffusion coefficients were also compared with those calculated from self-diffusion data. A comparison between calculated and measured coefficients shows only rough agreement. The effect of 40 kbar pressure is to decrease DyPl atm by an order of magnitude. The activation volumes for high-pressure diffusion are in favorable agreement with theoretical models developed for self-diffusion. coefficient which determines the rate at which material is transferred from the matrix phase to the precipitate and hence determines the growth rate of the precipitate. Since the numerical values of the diffusion coefficients differ widely as a function of the metallic system, temperature, and pressure, the diffusion coefficients must be determined for each particular environmental condition. Of long-standing interest is the growth of the classic Widmanstatten pattern in metallic (Fe-Ni) meteorites. The growth rate of the pattern is controlled by the diffusion coefficients in the Fe-Ni system. Since these coefficients are essential to calculating the growth rate of the pattern, we found it necessary to determine the diffusion coefficients

Jan 1, 1965

By J. O. Brittain, E. P. Lautenschlager, D. A. Kiewit

Compression tests were run in the temperature range of 700° to 900°C ox 0' phase NiAl intermetal-lic alloys of several grain sizes. At these temperatures the minimum strengths were observed at the stoichiometric composition. While significant increases in strength occurved in both the low-nickel (vacancy) and high-nickel (substitutional) regions, the highest strengths were found in the high-nickel region. During deformation serrated flow was sometimes observed in the low-nickel alloys. After deformation transgranular cvacking and deformation striations were observed in all compositions tested. AS part of a general investigation of the properties of NiAl inter metallic compounds, a preliminary study of the role of point defects upon plasticity was made by high-temperature compression tests on ß' NiAl specimens of several grain sizes and compositions. ß' NiAl is an intermetallic compound having a CsCl structure and a rather wide range of composition from A1-45 at. pct to 60 at. pct Ni.1 According to Bradley and Taylor2 and to cooper,' it possesses a defect lattice in which departures from stoichiometry in the direction of decreased nickel content lead to the presence of vacant nickel sites (although Cooper's work indicates that a small amount of substitution also occurs) whereas departures on the high-nickel side lead to substitution of nickel on aluminum sites. NiAl forms congru-ently from the melt at approximately 1650°C,1 and thus has a higher melting point than either of its component elements. Up to this time, although this and other high-melting intermetallic compounds have been suggested for elevated-temperature usage,4 only the hardness4 and a few tensile-strength measurements5 have been reported for NiAl at high temperatures. In the present investigation the effects of composition upon the compressive-strength properties in a range of 700° to 900°C have been measured for NiAl of several grain sizes. EXPERIMENTAL PROCEDURES The alloys were made as described elsewhere6 from an A1-46.8 at. pct Ni master alloy furnished by the International Nickel Co. with additions of high-purity nickel and aluminum. The charges were vacuum-induction-melted in A12O3 crucibles with small amounts of helium added to the atmosphere to suppress vaporization. They were cooled slowly from the melting temperature to achieve uniform grain size. In order to refine the as-grown grain size a special rolling technique was developed. Alloys were packed into 0.10-in. wall-type 302 stainless-steel tubes which were partially filled with magnesium oxide to prevent bonding between the alloy and the steel jacket. The ends of the tubes were closed by hot forging, and the packets were then hot-rolled. The alloys with greater than 50 at. pct Ni were rolled at 1100°C, but it was found necessary to increase the temperature to 1350° C before alloys with less than 50 at. pct Ni would roll without cracking. With these temperatures, reductions as high as 48 pct were achieved in a single pass. The rolled alloys will hereafter be referred to as "fine grained" whereas the as-grown material will be designated "coarse-grained''. The compression specimens were made by cutting square cross-sectional pieces, approximately 3/16 by 3/16 by 1/2 in., with a water-cooled diamond cut-off wheel from the as-grown or the rolled alloys. Specimens were ground to their final dimensions by polishing through 3/0 grit silicon carbide papers. The final shape was a rectangular parallelepiped of square cross section having a height-to-width ratio of 3:1. Compression testing was carried out in a compression rig of our own design mounted on an In-stron Floor Model. The specimen chamber could be heated to 1000°C and was controlled within ±2°C. The compression rig was enclosed within a bell jar and was maintained at a 50 µ of mercury vacuum throughout the duration of the test. The test cham -ber was heated from room to test temperature within 15 min. Specimens were then held at the test temperature 30 min prior to testing. Previous experiments indicated that no grain growth would occur within this time. An Instron Variable Crosshead speed unit was used to adjust for small variations in specimen lengths in order to have a constant initial strain rate, €, for all specimens of a group. For the fine-grained specimens the strain rate was changed rapidly at constant temperature by a factor of 10 with the speed lever on the Instron. For a given € the compression data was analyzed in terms of true plastic strain (E) and true compressive stress (0).

Jan 1, 1965

By E. Wainer, K. D. Burnham

A wet beneficiation technique for producing wollas-tonite from its ore in high yield and purity has been evaluated in a pilot plant operation at the rate of 75 tons per month. Finely crushed, unsized wollastonite ore mixed with water is passed through a high in tensity oscillating wet magnetic separator of unique design and in a single pass over 90% of the wolla-stonite exhibiting a crystal purity of 99.8% is obtained irrespective of size of feed fraction. Thereafter, the material is processed by closed cycle standard wet milling and classification techniques to yield a 1µ size product, though any mesh size up to and including 50 mesh may be obtained, if desired. Costs appear to be significantly lower than those available from dry processed techniques. Wollas tonite made by this unusual wet process appears to have potential utility in the following fields: ceramics, paints, plastics, paper, organic finishes, reinforcement of portland cement items, controlled porosity refractory ceramic foams, cinder and concrete block paint, and the like. The 1µ and certain chemically processed varieties of wollastonite may have unusual utility in the paper industry both as a filler and as a coating material and in the organic finish industry. Extensive deposits of wollastonite ore equivalent to an average tenor of 50% to 60% of this latter mineral in easily separable form exists in and around Essex County in northern New York State in reserves of the order of several tens of millions of tons. While important portions of these deposits are susceptible to open pit mining techniques, one operation near Wills-boro, N.Y., involves tunnel mining and dry milling and beneficiation techniques. This mill and tunnel mine is presently being operated by The Cabot Corp. and a variety of particle sizes are now sold into markets in the ceramic, paint, plastic finish, floor tile and in similar fields in substantial tonnages on a repetitive basis. Serious investigation and study over the past several years has indicated that, outside of the obvious economies of open pit techniques for mining purposes, wet beneficiation and milling procedures applied to the ore not only represent a potential for greater economies in the production of a superfine finished product but yields products of improved properties exhibiting increased market potential which may not be available from the dry ground product. The Lewis and Deerhead deposits, controlled by the Adirondack Development Corp., appear to be identical to the Wilisboro deposit. Utilizing ore taken from the Lewis and Deerhead deposits, a pilot plant process for the wet beneficiation, milling and classifying of wollastonite ore has been operated for several months. After scalping a marketable garnet product from a minus 16 mesh dry crushed feed on a high intensity roll magnet the balance of the material is then roll crushed in a closed cycle until it will pass a 50 mesh screen. The product constitutes the feed of the wet magnetic separator. The heart of the new beneficiation process is a cyclically operated wet magnetic separator which exhibits the unique feature that unsized feed is easily handled. Product yields of higher purity are equal to that obtained with dry magnetic separations which use closely sized dry ore and multiple passes, but only produce wollastonite of about 98% mineral purity as determined by sink float techniques. It was anticipated that the wet processing through the grinding, milling and classification stage would yield a low cost 1µ ground product which should make available greatly increased applications for the mineral beyond those presently enjoyed. The improved purity was also expected to provide coarser sizes which might be utilized as a raw material for chemical modification which again would expand the uses of wollastonite. The evidence thus far collected appears to indicate that this premise may be expected to be fulfilled. There are on the surface of wollastonite particle sites at which cheinical reactions may occur1. It is believed that wet ground material provides a better base which will allow wollastonite a deeper entree into the field of chemical raw materials. Wet ground at 20µ and finer permits with certainty a number of chemical reactions, some of which are mentioned later in this article. While well crystallized wollastonite makes up the majority of the ore, the balance consists mainly of very weakly magnetic diopside of the hedenbergite-

Jan 1, 1965