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By James B. Duke, Ernest W. Greene

An idea of what is meant by "Ultrafine Minerals Or Slimes" as used in the title can be had by an examination of Fig. I. Particle size distributions are presented for a crude kaolin clay, a coarse fraction and a fine fraction. The crude kaolin as mined was blunged with water, degritted through a 325-mesh Tyler screen, and dispersed with sodium silicate. The dispersed crude was then centrifuged in the laboratory into the coarse and fine fractions shown in the figure. The distribution curves were obtained by the well known sedimentation technique of Casagrande' using a long arm centrifuge to obtain equivalent spherical diameters down to 0.2 microns on the finer fraction. Fig. 1 shows the coarse fraction kaolin to be 50% finer than 3 microns, while the crude kaolin is 50% finer than 1.4 microns, and the fine fraction 50% finer than 0.6 microns. For comparison 53 microns on the horizontal scale would represent Stokesian diameters which would just pass a 325- mesh Tyler screen, taking into consideration the Andreasen sieve correction factor of 1.22 X the screen opening.' Another helpful comparison is the surface areas, which in square meters per gram, are 0.044 for 53 micron particles, 0.77 for 3 microns, 1.65 for 1.4 microns, and 5.0 for 0.46 micron particles. Fig. 2 is an electron micrograph of a similar fine fraction kaolin showing the hexagonal plate- like particle shapes.

Jan 10, 1962

By C. W. George, Bruce Chalmers

The authors enumerate the factors which appear, from their observations and practical experience of failure of aircraft components in Great Britain, to be responsible for causing a metal or alloy to fail by stress corrosion. The essential conditions for promoting failure by stress corrosion are: (I) tensile stress at the surface of the component, (either residual or applied), and (2) an attacking medium that may be a solution or a liquid metal. Particular attacking agents are effective only on certain metals. In all instances of stress-corrosion failure experienced, cracking of an intercrystalline form has occurred and examples of such failure in aluminum alloy, steel and copper alloys are described and illustrated. The relation between microstructure and stress corrosion is mentioned and methods of investigating the susceptibility to stress-corrosion failure of metallic materials are described. The precautions to be taken in selecting materials for particular aircraft components and the importance of adequate protection against chemical attack are considered. The authors have given a factual survey of stress corrosion and have made no attempt to advance any scientific explanation of the phenomenon.

Jan 1, 1945

By W. V. Green

Creep of tantalum was measured at temperatures from 0.6 to 0.89 of the absolute melting temperature. The creep curves include first, second, and third stages. Steady-state creep rate depends on the fourth power of stress. The activation energy for creep throughout this temperature range is approximately 114 kcal per mole, measured by the aT technique. Subgrain formation occurs as a result of creep strain, and pile-up dislocation arrays are observed in etch-pit patterns. BECAUSE of its high melting point-which is exceeded only by those of rhenium and tungsten—and its high room-temperature ductility compared to most of the other high-melting-point metals, tantalum will undoubtedly be utilized in an increasing number of high-temperature applications. Alloying studies directed toward increased high-temperature strength must use data on tantalum itself as a base line in order to evaluate the effectiveness of the alloying additions. However, to date, no systematic study of creep of tantalum at temperatures above one-half of its melting point has been reported in the literature. Conway, Salyards, McCullough, and Flagella1 have measured linear creep rate of tantalum sheet as a function of stress, but at only one temperature, 2600°C. This paper describes a relatively thorough study of the high-temperature creep of tantalum. METHOD Material Tested. The commercially supplied, l/2-innch-diameter tantalum rod used for this work was electron-beam-melted, cold-forged, rolled, swaged, cleaned chemically, and vacuum-annealed for 1 hr at 1000°C, all by its manufacturer. The vendor's analysis included 60 to 170 ppm C, 3.4 to 4.2 ppm H, 60 to 80 ppm 0, 15 ppm N, and a hardness ranging from 66 to 81 Bhn and averaging 76 Bhn. Creep eimens Used. Two creep-tested specimens are shown in Fig. 1. The 1/4 in.-diameter gage section was 3/4 to 1 in. long, and terminated either at shoulders 5 mils high or at 20-mil-diameter tantalum wires spot-welded to the circumference of the gage section. Both kinds of shoulders served equally well as fiducial marks for optical strain measurements. The spot welding did not alter the creep behavior in any detectable way; the 5-mil- high sharp shoulders did not result in any detectable localized effect on the strain. Before testing, each tensile bar was first mechanically polished -id then electrochemically polished according to the method referred to by Forgeng2 as the "Thompson Ramo Woolridge" method, which was suitable for tantalum after small adjustments of technique were made. Two tensile bars tested at low stresses had 1/8-in.-diameter gage sections and utilized only the weight of the bottom grip for the applied load. Although these diameters were smaller than were desired for other reasons, applied loads were known with high precision in the tests in which they were used. Testing Procedure. Two different constant-load creep-testing machines were employed, one of which has been described by Smith, Olson, and Brown.3 In both, the tensile bar is held vertically on the axis of a cylindrical tungsten tube or screen heater by threaded tungsten grips. The tensile bars and associated grips are heated by radiation from the incandescent heaters, which are heated by their own electrical resistance. Both testing machines use pins to hold the bottom grips in place. The load is applied to a tensile bar through hanging weights, a constant force-multiplication lever, a pull rod sealed to the chamber lid, and a top grip threaded to the pull rod at one end and to the tensile bar at the other. In one machine, the vacuum seal is a bellows with a low spring constant; in the other, the seal involves a rotating "0 ring". With the latter, rotation is converted to translation with a crank shaft, so that elongation of the tensile bar is accommodated with no change of tensile load. The incandescent tensile bar is viewed by an external optical system through slots in the radiation shields and heater, and an enlarged image is projected on a ground-glass screen. Gage-length measurements are made on this image with cathetometers on traveling microscopes. With regard to creep-test results, the two machines were identical. Thorium oxide coatings were applied to the threaded ends of the tensile bars, to prevent diffusion welding of the tensile bars to the grips during testing. Specimen temperatures were measured with an L. & N. optical pyrometer which had been calibrated against a standard carbon arc, and were corrected fir window absorption by calculation from the measured spectral transmittance of the quartz observation windows. Longitudinal temperature gradients in the tensile-bar gage length and temperature drifts during testing were detectable but small, and were estimated to be 10°C or less. Accuracy of temperature measurement was confirmed by comparing the temperature measured on the surface of a special

Jan 1, 1965

By M. E. Fine, A. A. Henderson

Investigation of the tensile properties of silver based aluminum alloy crystals was undertaken because it appeared attractive for studying strengthening effects due to Suzuki locking with minimum complication. Yield drops were observed in all alloy crystals (1, 2. 3. 4, and 6 at. pct Al) after strain aging at room temperature. No yield drops were found in similarly grown and tested silver crystals. The yield effects are attributed to Suzuki locking but the major portion of the solid solution strengthening to other mechanisms. INVESTIGATION of the tensile properties of single crystds of silver alloyed with aluminum was undertaken because it appeared to be a system in which segregation at stacking faults associated with partial dislocations1 would be the dominant factor in anchoring dislocations. First, silver and aluminum have closely similar atomic sizes and thus solute atom locking of a dislocation due to elastic interactions should be unimportant. Second, while both X-ray2 and thermodynamic3 investigations show short-range ordering in silver-based aluminum alloys, the degree of local order is quite small (X-ray measurements give v = EAB - 1/2(EAA + EBB) = - 0.025 ev and thermodynamic measurements give v r -0.007 ev) and should not be important in strengthening dilute alloys. Third, the stacking fault energy of silver is probably low (as indicated by the profusity of annealing twins) and is very likely diminished further and quite rapidly by aluminum additions since the A1-Ag phase diagram shows a stable hexagonal phase at only 25 at. pct Al. Also, a careful investigation in this laboratory4 has shown that the ratio of twin to normal grain boundaries in recrystallized alloys increases with aluminum content. Thus, with minimum complication from other factors, Ag-A1 alloys seem attractive for studying strengthening effects due to segregation at stacking faults of extended dislocations. EXPERIMENTAL METHOD Single crystals measuring 250 by 5 by 1.5 mm of pure Ag (99.99 pct) and Ag-A1 alloys (A1 of 99.999 pct purity) of nominal compositions* 1, 2, 3, 4, and 6 at. pct were grown in high-purity graphite molds from the melt under a dynamic vacuum (1 x l0-5 mm Hg). The technique consisted of moving a furnace having a hot zone (which melted about 0.5 cm of alloy) over a horizontal, evacuated quartz tube con- taining the mold and alloy at a rate of 3/8 in. per hr. Chemical analysis showed roughly the first inch of the crystal to be solute poor, the last inch solute rich; and the center section uniform in composition within the sensitivity of the analytical method (± 0.2 at. pct Al). The center section of the crystal was cut into five specimens. Gage lengths of reduced cross section, measuring from 1.5 to 2 cm in length, were mechanically introduced by means of jeweler&apos;s files and fine abrasive cloth with the crystal firmly held in polished steel guides. One-third of the cross section was then removed by etching and electro-polishing, the crystals were all subsequently annealed for several days at 850°C in a dynamic vacuum (<1 x 10-5 mm Hg) and furnace cooled to 200°C. The crystal orientations were determined using the usual back-reflection Laue technique. The Laue spots were sharp and of the same size as the incident beam. However, microscopic examination showed the crystals to contain substructures with subgrains of the order of a micron in diameter. The details of this substructure are presently under investigation. Tensile testing was done with a table model Instron using a cross-head speed of 0.002 in. per min. For testing at various temperatures the following media were used: 1) 415oK, hot ethylene glycol; 2) 296ºK, air, acetone, water; 3) 273ºK, ice water; 4) 258ºK, ethylene glycol "ice" in ethylene glycol; 5) 200°K, dry ice in acetone; 6) 77ºK, liquid nitrogen. EXPERIMENTAL RESULTS A) Yield Behavior—A portion of an interrupted stress-strain curve for a 6 at. pct A1 crystal of the indicated orientation tested at room temperature is shown in Fig. 1. Initially, at (a), there is a small, gradual yield drop of about 10 mg per sq mm2. However, on stopping the test, and aging for a few minutes at (b), a sharp yield drop is found. Aging for longer times at (c) and (dl results in larger yield drops (and larger AT&apos;S). At, defined in Fig. 1, is usually larger than the yield drop by about 20 pct; however, this increase in the lower yield is transient since extrapolations of the flow stress curves join as may be seen from Fig. 1. (Both Laue and low-angle scattering photographs revealed no evidence of precipitation in a strain-aged 6 at. pct A1 crystal.)

Jan 1, 1962

By F. H. Vitovec, D. W. Hoeppner

Pusk-pull fatigue tests were conducted on copper tricrystals of 99.988 pct purity to ascertain the role of grain boundaries in the initiation and propagation of fatigue cracks. Significant differences in behavior were found for specimens which possessed different transverse-boundary misorientation. In speciwens with low boundary angles cracks initiated within the transverse boundary, while higher angles led to transcrystalline fatigue failure. It is suggested that at low angular misorientation moving dislocations may interact with dislocations of the boundary or dislocations present in adjacent pains on favorably oriented glide planes, thus initiating a fatigue crack. MANY fatigue studies have been concerned with fatigue-crack initiation within grains and the mechanism causing initiation and propagation1-3 Although the initiation of fatigue cracks in or near grain boundaries of pure metals has been observed and reported in the literature, the mechanism of this phenomenon has received little attention.4"11 EXPERIMENTAL PROGRAM Testing Procedure. To investigate the role of grain boundaries regarding initiation and propagation of fatigue cracks, copper tricrystals were tested in push-pull. Axial-stress tests were used to avoid the stress gradients introduced by stressing of some other nature. Copper was selected as the most suitable test material since extensive work has been done on the formation of fatigue-induced slip in copper. Tricrystal specimens were used to provide a grain boundary geometry with one boundary transverse to the principal stress axis and one or more boundaries nearly coincident with the direction of maximum resolved shear stress. The boundary energy and the slip characteristics in the vicinity of the transverse boundary depend on the relative orientations of grains across the boundary. Testing was done at room temperature, at a frequency of 700 cpm, in an atmosphere of either air or argon. It is known that the incidence of grain boundary cracking increases with increasing temperature and decreasing frequency.4 The fatigue machine applied a uniaxial tension-compression load to the specimen by a flat spring which was actuated by an adjustable eccentric. Use was made of an adjustable head and a load cell which had strain gages mounted at 120-deg intervals around its periphery, thus providing a means for eliminating any detectable superimposed bending moment. A clip gage was mounted between the gripping heads to record the cyclic strain amplitude applied to the specimen. Each specimen&apos;s hysteresis characteristics were recorded by supplying the load and strain signals to an oscilloscope. Microstructural changes were observed and recorded with an optical microscope which was mounted on the fatigue machine. Immediately prior to insertion in the machine, each specimen was chemically polished. Extreme care was exercised while inserting the specimen in the test machine to avoid either bending the specimen or introducing a mean load. Each specimen was stressed in the tensile direction first and subsequently the load was reversed. Specimen Preparation. Tricrystal fatigue specimens of 99.988 pct Cu were grown from the melt using a modified Bridgman technique. Ingots about 1 in. high were grown to the configuration shown in Fig. 1. Upon sectioning the resultant ingot, several specimens were provided with an identical shape and grain boundary orientation. Except for plane sectioning and final polishing, this method eliminated machining the specimens. The apparatus used for growing the tricrystals is shown in Fig. 2. A spectrographically pure graphite mold, Fig. 3, was inserted in a vycor tube which was mounted on a vertical zone-refining table. Prior to insertion in the tube the mold was assembled as follows. The insert and graphite rods were fixed in position in the mold. The copper was then placed in the mold and the entire mold assembly was positioned in the vycor tube, Fig. 2. At this point the tube was sealed, evacuated, purged with helium gas, and finally placed under a slightly positive helium pressure. The heating coil was then adjusted to melt the copper charge, after which it was raised at a speed of 4 in. per hr. It is also possible to use

Jan 1, 1964

By L. D. Hall, S. J. Rothman

The diffusion of lead and of trace amounts of bismuth in liquid lead have been investigated by the capillary method, using ROD and ROE as tracers. The results are compared with existing theories of diffusion in liquids, the agreement with theory being fair. The heat of activation for self-diffusion in lead is found experimentally to be close to the corresponding activation energy obtained from viscosity data. The pioneer data of Groh and von Hevesi for the self-diffusion of liquid lead, using ThB as a tracer, fit in with the present results. OMPARED with the volume of effort expended on solid state diffusion, there has been little attention paid to diffusion in liquid metals. A review of experimental work in this field, covering most of the studies up to 1951, was given by Jost.&apos; More recent papers include those by Hoffman2 on self-diffusion in mercury, Morgan and Kitchener" and Stark, Shchilishchev, and Kazachkev4 on the diffusion of various elements in liquid iron, and Grace and Derge on the diffusion of bismuth in bismuth-lead alloys. The need for more experimental data to aid in the evaluation of existing theories prompted the

Jan 1, 1957

By O. C. Baptist

The Umiat oil field is in Naval Petroleum Reserve No. 4 between the Brooks Range and Arctic Ocean in far-northern Alaska. The Umiat anticline has been tested by 11 wells, six of which produced oil ; however, [lie productive capacity and recoverable reserves of the field are subject to considerable speculation because of unusual reservoir conditions and because several wells appear to have been .seriously damaged during drilling and completion. Oil is produced at depths of 275 to 1,100 ft; the depth to the bottom of the permanently frozen zone varies from about 800 to 1,100 ft, .so that most of the oil reserves are in the permafrost Reservoir pressures are estimated to range from 50 to 350 psi, increasing with depth, and the small amount of gas dissolved in the oil is the major source of energy for production. Laboratory tests were made on cores under simulated permafrost conditions to estimate oil recoverable by solution-gas expansion from low saturation pressures. The cores were also tested for clay content and susceptibility to productivity impaiment by swelling clays and increased water. content if exposed to fresh water. The results indicate that oil can be produced fronz reservoir rocks in the permafrost and that substantial amounts of oil can be produced from depletion-drive reservoirs by a pre.s.r~lrr drop of as little as 100 psi below the saturation pressure. Freezing of formation water reduces oil productivity much more than that due to increased oil viscosity: Failure of we1ls drilled with rtuter-base mud to produce is attributed to freezing of water in the urea immediately surrounding the wellbore. Swelling clays apparently contributed very little to the plugging of the wells. INTRODUCTION Naval Petroleum Reserve No. 4 lies between the Brooks Range and the Arctic Ocean in northern Alaska. The Umiat oil field is located in the southeastern part of the Reserve and is about 180 miles southeast of Point Barrow (the only permanent settlement in the Reserve and the primary supply point for drilling of the wells at Umiat). Eleven wells were drilled for the U. S. Department of the Navy, Office of Naval Petroleum and Oil Shale Reserves, between 1944 and 1953 to test the oil and gas possibilities of the Umiat anticline. Six of these wells produced oil in varying quantities and the best one pumped about 400 B/D.&apos; Estimates of recoverable oil range from 30 to 100 million bbl. The main oil-producing zones are two marine sandstone beds in the Grandstand formation of Cretaceous age: these are referred to as the upper and lower sands. Good oil shows were found throughout the sand settions in the first three wells drilled on the structure, but the highest rate of oil production obtained on any 01 the many tests was about 24 BOPD. These first wells were drilled with conventional rotary methods using water-base mud; later wells were drilled either with cablc tools using brine or rotary tools using oil or oil-base mud. These experiments were successful as is shown by comparing the oil production from Well No. 2 with that from No. 5. These two wells are only 200 ft apart and are located at about the same elevation on the structure. Well No. 2. drilled with a rotary rig using water-base mud, was abandoned as a dry hole after all formation tests were negative. Well No. 5. drilled with cable tools and reamed with a rotary using oil, pumped 400 BOPD which was the maximum capacity of the pump and less than the capacity of the well. These field results indicated that the producing sands were extremely "water sensitive" and it was assumed that the cause of this sensitivity was the presence of swelling clays in the sands. Because of the very unusual reservoir conditions and the difficulties encountered in completing oil wells in the permafrost. the Navy asked the U. S. Bureau of Mines to make laboratory studies under simulated permafrost conditions to assist them in estimating the production potential of the field and the recoverable reserves. These tests were designed to determine the cause of the plugging of wells in the permafrost and to test oil recovery from frozen sand by solution-gas expansion with the oil gas-saturated at very low pressures. EXPERIMENTAL METHODS AND PROCEDURES Samples Analyzed Core samples were analyzed that represent the lower sand in Umiat Well No. 7, the upper sand in No. 3. and both the upper and lower sands in No. 9. These sands should be productive in all of the wells because of their location on the structure. Core samples from

By J. D. Miller, R. J. Smith

The hot water process for Utah tar sands differs significantly from that used for Canadian tar sands due to inherent differences in respective bitumen viscosities and the nature of bitumen-sand association. These differences have led to the identification of certain design criteria necessary to achieve satisfactory phase disengagement during digestion (Sepulveda and Miller, 1978; Misra and Miller, 1980). Subsequent flotation of digested tar sand is a subject of current attention and is considered in this publication for the Asphalt Ridge deposit. Although contact angle measurements of solvent extracted Asphalt Ridge bitumen indicated moderate hydrophobicity, air bubble attachment to the bitumen concentrate is not possible. This surprising result suggests that flotation separation is dependent on air bubble entrapment rather than on air bubble attachment due to surface hydrophobicity. The entrapment of air bubbles in the bitumen was apparent from examination of the bitumen concentrate, especially at lower flotation temperatures. A factorial design of the major operating variables in flotation separation indicated that the quality of separation was significantly dependent on the flotation temperature and to a lesser extent on the degree of agitation. For a flotation temperature of 77°C a recovery of 96.7% was realized at a grade of 61.0% bitumen. The improved separation at higher flotation temperatures was found to be due to the decrease in bitumen viscosity resulting in more effective rejection of coarse sand from the concentrate. This research effort, which has been sustained for the past six years at the University of Utah, is being continued to provide necessary design data for the construction of a pilot plant to treat Utah tar sands.

Jan 1, 1982

By R. L. Dalton, L. A. Rapoport, C. W. Carpenter

Procedures have been developed to study the performance characteristics of unconfined pilot water floods using scaled laboratory models. The effects of operating conditions on pilot performance for variozrs well patterns have been investigated. The limitations of the laboratory model studies are outlined. Relationships between the oil recoveries of pilots and large-scale floods have been established. The applications of model studies to the prediction of large-scale waterflood performance and pilot flood design are discussed. INTRODUCTION Pilot water floods are undertaken to evaluate operational procedures and to gain advance information about the performance of an extensive water flood. In general, however, the performance of a pilot flood is not directly indicative of what can be expected from a large-scale pattern water flood. This difference stems from the fact that the over-all flow configurations are not the same for the two systems. A water flood normally consists of an array of identical well patterns. In such an array, the perimeters of the well patterns are axes of symmetry and act as impermeable boundaries. Thus, an extensive, pattern water flood can be visualized as a repetition of "confined" floods. In contrast, a pilot water flood involving only one or a few well patterns is "unconfined". Here the well patterns are not balanced by other flood units; hence, the perimeter of the pilot area does not act as an effective boundary. Accordingly, only a portion of the fluids injected (and also of those originally contained within the pilot area) is captured by the producers of the pilot. The rest escapes into the surrounding reservoir. This usually causes the amounts of oil and water produced in the pilot to be different from those recovered by a producer in an extensive water flood. Moreover, the recovery observed in the pilot can be expected to be greatly influenced by operating conditions, i.e., by the bottom-hole pressures at the injection and producing wells. The above considerations show that full utilization of pilot test results and reliable prediction of large- scale water floods require a knowledge of the relationship between the recovery performance of confined and unconfined well patterns. To date, only limited basic information is available on the behavior of pilot water floods. Craig, et al,&apos; have investigated the effects of initial gas saturation, oil-to-water mobility ratio, and well damage on the oil recovered from a single, "normal" five-spot pilot pattern (Fig. 1). Rosenbaum and Matthews2 studied the effect of initial gas saturation and mobility ratio on the ratio of production rate to injection rate for various groupings of five-spot patterns. Paulse113 investigated the effect of mobility ratio and distance from the pilot to the edge of the reservoir on the areal sweep in a single "inverted" five-spot (Fig. 1). However, none of these studies considered the effect of operating conditions on pilot flood behavior. Moreover, hardly any of the work to date dealt explicitly with the oil-recovery performance of the pilot floods. The purpose of this paper is to introduce the concept of interrelation between pilot flood behavior and operating conditions, to illustrate this interrelation by means of experimental data and to compare the recovery performances of dif-

By J. A. Herbst, K. Rajamani, Y. C. Lo

In spite of potential theoretical and economic advantages of large-diameter ball mills, many manufacturers elect not to build them owing to what is perceived as an excessively large design risk. This is because traditional predictions for mill scaleup to large diameters are not always accurate. Alternative methods of analysis and scale-up are required. Recent studies have shown that detailed population balance models which account for important grinding subprocesses (grinding kinetics, material transport, and classification) are capable of predicting the performance of small- and intermediate-diameter mills (up to 4.3 m, or 14 ft) from small-scale batch tests. These same models are used in the current study to predict the performance of a "borderline "large ball mill (4.7 x 5.5 m, or 15 x 18 ft) at Asarco&apos;s Sacaton operation, a ball mill (5 x 5.8 m, or 16.4 x 19 ft) at Kennecott&apos;s Chino operation, and one of the world&apos;s largest ball mills (5.5 x 6.4 m, or 18 x 21 ft) at Cities Service Pinto Valley operation. Model parameters required for scale-up have been estimated in a 380-mm-diam (15-in.-diam) batch mill. Predictions are compared with the results of detailed plant sampling in the three plants. For the Sacaton and Chino operations, the error of the predictions was found to be less than 2.5%, while the corresponding error for the Pinto Valley operation was less than 2.7%. It is concluded that proper representation of the major subprocesses of grinding in the model equations is the key to achieving accurate scale-up. Of special importance is the need to account for the size distribution of the grinding media and the influence of the size distribution environment in the mill on grinding kinetics.

Jan 1, 1986

By R. Silverman, H. Blumenthal

It was found that despite the similarity of chemical analyses of different titanium carbides used as base materials for cermets, the physical properties, especially transverse-rupture strengths, of test bars were different. Hence this metallographic study attempts to link physical properties to micro-structures. It is shown that microstructure, grain shape, and grain growth are functions of three interrelated factors: 1—powder production procedure, 2—surface conditioning of the particles, and 3—impurities either contained in the original powder or acquired during ball milling. An explanation is offered for the "coring effect," long observed, but heretofore of unknown origin. The explanation is based on assumption of an oxide film and on chemical analyses which substantiate these findings. TITANIUM carbide has become in recent years a material of great interest in the high temperature field. Consequently, many manufacturers in the United States and Europe are producing titanium carbide for cermet applications as well as for additions to the well known tungsten carbide tools. All present commercial processes of titanium carbide production utilize the chemical reaction of titanium dioxide and carbon to form as nearly as possible stoichiometric Tic. This reaction is carried out in three ways: 1—in a menstruum of molten metal,&apos; 2—in the solid state, either in a protective atmosphere2 or in vacuum;" or 3—in an are-melting operation. In spite of the fact that the pure carbides obtained in these operations are almost identical chemically, the physical properties vary considerably when they are combined with a binder (Ni, Co) to form cermets. This fact led the authors to examine metal-lographically nickel-bonded titanium carbide in order to find the possible reasons for this behavior. Materials and Methods Five different titanium carbides were used in this investigation. They are identified in Table I. The first four materials were used in the as-received condition. Material E, received in lumps, was crushed to —100 mesh and carried through a flotation process in order to bring its graphite content in line with the other products. A Galagher flotation cell was used with pine oil as frothing agent. The chemical analyses of the investigated materials are given in Table 11. The binder used was carbonyl nickel of 9 to 14 microns particle size, supplied by A. D. Mackay. The materials were ball milled at a ball to charge ratio of 6:1 using procedures described under "Experiments and Results." All particle sizes mentioned are averages determined with a Fisher Sub-sieve Sizer. Test bars (lx0.40x0.16 in.) were prepared by 1—hot pressing to 85 to 95 pct of theoretical density at pressures between 1 and 1½ tsi and temperatures from 1600" to 1800°C, 2-—-cold presssing after 3 pct camphor had been added, or 3—wet pressing, both 2 and 3 at pressures between 5 and 10 tsi. All pressed bars were sintered in a vacuum of 105 to 10-6 mm Hg for 2 hr at 1350 °C. Transverse-rupture strengths were determined by breaking on a Baldwin Universal Testing Machine over a 9/16 in. span. Densities were measured by water displacement. The preparation of the specimens for micrographs was done according to Silverman and Doshna Luscz." All magnifications are at X1000. A sodium picrate electrolytic etch was used. Experiments and Results The influence of ball-milling procedure, ball-milling medium, pressing procedure, and sintering procedure on the microstructure of 80/20 — TiC/Ni were investigated. Ball Milling of Materials A, B, and C in a Steel Mill: Figs. 1 and 2 show microstructures of hot-pressed and vacuum-sintered test bars of materials A and B after the respective materials had been ball milled to 2.1 microns particle size in a steel mill and mixed with 20 pct Ni binder. Material A (Fig. 1) shows considerable grain growth. Also evident is a tendency of the carbide grains to coalesce. The density is 98 pct and the low transverse-rupture strength of 111,000 psi is probably caused by many large grains and an unfavorable packing factor. Almost all grains show a slight indication of "coring." Material B (Fig. 2), although showing grain growth, still has many small particles and a better distribution of binder and carbide due to the relative absence of the coalescing tendency. "Coring" can be observed in almost all grains. The high transverse-rupture strength of 179,000 psi and the density of 100 pct are believed to be due to the many small grains completely surrounded by the binder phase. There is also a preference to form spherical grains with material A, while most grains of material B preserve their angular shapes. Material C, of which no picture is given, stays between A and B in every respect. Rounding of some grains can be observed as well as coring, but the latter to a lesser degree than with material B. Its densification is good and the transverse-rupture strength obtained is 142,000 psi. Ball Milling of Materials A, B, C, and E in a WC Mill: When the Tic powders were ball milled to 2 microns particle size in a we mill, then ball-mill mixed with 20 pct Ni binder, hot pressed, and vacuum

Jan 1, 1956

By J. J. Forbes

&apos;"THE Federal Coal Mine Safety Act (public Law T. 552. 82nd Congress) was approved oil July 16, 1952. It incorporates, as Title I, the Coal Mine Inspectio1.1 and Investigation Act of May 7. 1941 (Public Law 49, 77th Congress), which gave Federal inspectors only the right to enter. coal mines for inspection and investigation purposes but no power to require compliance with their recommendations. Title 11 contains the enforcement provisions of the act; its purpose is to prevent major disasters in coal mines from explosions, fires. inundations. and man-trip 01. man-hoist accidents. At this point a brief account of events that preceded the enactment of the Federal Coal Mine Safety Act seems appropriate. The hazardous nature of coal mining was recognized by the Federal Govermment as long ago as 1865, when a bill to create a Federal Mining Bureau was introduced in Congress. Little was done, however, until a series of appalling coalmine disasters during the first decade of this century provoked a demand for Federal action. As a result an act of Congress established a Bureau of Mines in the Department of the Interior on July 1, 1910. The act made it clear that one of the foremost activities of the Bureau should be to improve health and safety in the mineral industries. One of the first projects selected by the small folce of engineers and technicians then employed was to determine the causes of coal-mine explosions and the means to prevent them. By investigations aftel mine disasters the fundamental causes and means of prevention were soon discovered, and the coal mining industry was informed accordingly. However, despite this knowledge and the enactment of State laws and the Federal Coal Mine Inspection and Investigation Act of 1941, mine disasters continued to occur with disheartening frequency and staggering loss of life. The devastating explosion at the Orient No. 2 mine on December 21, 1951, resulted in the death of 119 men. The Orient disaster rekindled the memory of the Centralia. Ill., disaster of March 25. 1947, which caused the death of 111 coal miners. These two tragedies ultimately brought about enactment of the Federal Coal Mine Safety Act. The act is a compromise measure. Senator Matthew M. Neely of West Virginia and Congressman Melvin Priec of Illinois introduced almost identical versions in the 82nd Congress, but they were considered too drastic. The final version was introduced by Congressman Samuel K. McConnel, Jr., of Pennsylvania, after considerable discussion and amendment in committee hearings. It was passed by the Congress and became effective when signed by the President on July 16, 1952. The act is somewhat limited in scope because it applies only to approximately 2000 coal mines in the United States and Alaska that employ regularly 15 or more individuals underground. It exempts approximately 5300 mines employing regularly fewer than 15 individuals underground and all strip mines, of which there are about 800. Moreover, it covers only conditions and practices that may lead to major disasters from explosion, fire, inundation, or man-trip or man-hoist accidents. According to Bureau records, such accidents have resulted in less than 10 pct of all the fatalities in coal mines. It is important to mention that the law is not designed to prevent the day-to-day type of accidents that have caused the remaining 90 pct or more of the fatalities, because it was the specific intention of the Congress to reserve the hazards which caused them to the jurisdiction of the coal-producing states. Many who opposed any Federal legislation that would give the Federal inspectors authority to require compliance with mine safety regulations claimed that such legislation would usurp or infringe upon States&apos; rights. To assure that the principle of States&apos; rights would be preserved, the act provides for joint Federal-State inspections when a state desires to cooperate in such activities. The Director of the Bureau of Mines is required by the act to cooperate with the official mine-inspection or safety agencies of the coal-producing states. The act provides further that any state desiring to cooperate in making joint inspections may submit a State plan for carrying out the purposes of this part of the act. Certain requirements are listed: these must be met by a state before the plan can be accepted. The Director of the Bureau of Mines, however, is required to approve any State plan which complies with the specified provisions. The Director may withdraw his approval and declare such a plan inoperative if he finds that the State agency is not complying with the spirit and intent of any provision of the State plan. When this paper was prepared, agreements for joint Federal-State inspections had been entered into with Wyoming and Washington. A few other states have indicated their desire to submit a State plan and negotiations toward that end are now under way. Reluctance to enter into such agreements may be due to the mine operators&apos; knowledge that in the states that adopt a cooperative plan they are prohibited from applying to the Director of the Bureau of Mines for annulment or revision of an order issued by a Federal inspector and must appeal directly to the Federal Coal Mine Safety Board of Review for such action. Experience has proved that review by the Director as provided in the act is a less expensive and time-consuming procedure to all concerned than applying to the Board. Reluctance also may stem from the fact that joint Federal-State inspections somewhat restrict the movements of the State mine inspectors and tend to reduce the number of inspections of mines. Where a State plan is not adopted, the Federal coal mine inspector is responsible under the law to take one of two courses of action if he finds certain hazardous conditions during his inspections. The first action involves imminent danger. If a Federal inspector finds danger that a mine explosion, mine fire, mine inundation, or man-trip or man-hoist accident will occur in a mine immediately or before the imminence of such danger can be elim-

Jan 1, 1955

By R. J. C. Tait

INTRODUCTION Process Control at the Ecstall Concentrator begins in the open pit at the Kidd Creek Mine. While this paper, naturally, emphasizes the instrumental and technical features of the Process Control system within the concentrator itself, it would not be complete without some mention of the selective mining methods and grade control practices at the mine, and of certain features of plant design, which are simple, but highly effective, elements of the Process Control system. The success of the entire Process Control system, from pit to concentrate load-out, owes much to the high degree of cooperation and mutual understanding among all the operating departments at Ecstall Mining Limited and to the willingness of management to accept, from the start, an overall control philosophy based upon the inter-dependence of mining and metallurgical operations. INFLUENCES OF MINERALOGY AND METALLURGY ON MINE PLANNING AND PLANT DESIGN Mineralogically, the Kidd Creek ores are fine grained and mostly very complex. Because of complex mineral associations and extensive inter-locking, very fine grinding and regrinding of middling fractions are necessary and selective flotation requires a very delicate touch. Four separate concentrates are made for shipment to copper, lead and zinc smelters. The Process Control system is tailored to the metallurgical objectives of maximum recoveries of copper, lead, zinc and silver into concentrates of optimum quality, for maximum economic returns. For example, zinc and lead in copper con-

Jan 1, 1970

By V. B. Kurfman

The temperature, strain rate, and orientation deDendence of defbrnzation of single-crystal MgAg has been examined. The crystals exhibit a tendency to single glide and little or no hardening at 25°C for many orientations. A much higher hardening rate is observed when multiple glide occurs, such as can be initiated by surface defects. The tendency for easy glide becomes less dependent on surface preparation and orientation as T — 100°C and bars so tested often fail after one-dimensional necking-. At T > 200°C (transition temperature for single-crystal notch sensitivity and poly crystalline ductility) single glide diminishes and two-dirnensionul necking begins. The crystals do not strictly obey a critical resolved shear stress law, but show the influence of {loo) cracks in determining the slip mode. The results are correlated with the difficulty of sciperdzslocation intersection and semibrittle behavior of this compound in single-crystal and poly crystalline form. Comparisons are made with the slip selection mode observed in tungsten, with the reported observations of easy glide in bee metals. and with the mechanical behavior of poly crystalline MgAg. PREVIOUS work on tensile deformation of polycrys-talline MgAgl and bending deformation of single-crystal MgAg2 has shown that the compound is semi-brittle (i.e., notch and grain boundary brittle). If this semibrittleness is supposed to result from the difficulty of multiple glide (associated with the problems of superdislocation intersection) one might expect single crystals deformed in tension to show pronounced single glide and strong orientation dependence of hardening rate. These experiments were done to examine this supposition and to study the tensile deformation of a highly ordered system which may be considered bcc if the difference between the two kinds of atoms is ignored (actual structure: CsC1). EXPERIMENTAL Single-crystal ingots were grown by directional freezing as previously described.&apos; These ingots were sliced into a by a by 2 in, rectangular bars by electric discharge machining, then round tensile bars were conventionally machined to 1/8-in.-diam by 1-in.-long reduced section. The bars were typically tested without an anneal because of the problem of magnesium vapor loss and they were typically tested as mechanically polished. The analyses are within the same limits as those reported earlier; i.e., the average composition for each specimen is within 0.5 at. pct of stoichiometry, while the total range from end to end in a given specimen varies from 0.7 to 1.4 at, pct. There has been no indication in the results of any variation in slip or fracture mode attributable to the composition fluctuations. The slip systems were determined by two-surface analysis of the bars after testing to failure at room temperature. Single glide was so dominant that there was little difficulty in identification of the dominant slip system even though the tensile elongation to failure often approached 7 to 8 pct in room-tempera- ture tests. Elevated-temperature testing was done in a silicone oil bath and low-temperature testing was done in liquid Np or a dry-ice bath. All stress measurements are reported as engineering stress unless otherwise specified, and crosshead travel is used as the strain measurement. RESULTS The tendency toward single glide is best seen in the pictures, Figs. 1, 2, and 3, which depict deformation at fracture as a function of test temperature. While it is possible to find regions of secondary slip by careful microscopy, such regions are very small. The development of a ribbon-shaped configuration from an initially round section bar pulled at 100°C is typical, occurred by single glide, and illustrates the degree to which such glide continues. At temperatures =100°C the bars typically show elongation of 20 to 50 pct by predominently single glide. Despite the large elongation, fracture even at 150°C occurs in a brittle mode, Fig. 2, in the sense that it is an abrupt failure which shows no discernible necking in the second dimension of the bar&apos;s cross section (i.e., there is no appreciable action of any slip modes which would decrease the broad dimension of the cross section). Near 200°C the fracture mode changes slightly. Although most of the sample extension is by single glide, after the bar develops the characteristic ribbon shape it begins to neck in the second (i.e., broad) cross-sectional dimension. The bar becomes very thin in the "necked down" region, Fig. 3, and the reduction in area approaches 100 pct. Often there oc-

Jan 1, 1967

By W. C. Hagel, H. J. Beattie

Seven austenitic alloys of varions base compositions and minor-alloy additions were solution-treated, aged systematically between 1200oand 1800oF, and examined by X-ray and electron metallography. Intragranular preczpitations of µ, Laves, s, ?&apos;, Ni3Ti, and x phases were observed as a function of composition and aging time and temperatwre. Phase solubility limits were detevtnitzed within 100Fo intervals. These inter metallic compounds fall into two distinct general classes, and whichever class predomznates depends on base composition. It has become increasingly evident that multicom-ponent austenitic alloys are well characterized by their precipitation processes. Since certain groups of elements act as one, the relationships among these processes are reasonably simple; complete identification of such processes is usually attainable by a systematic aging study with a combination of techniques centered on microscopy and diffraction. Several nickel- and cobalt-base alloys illustrating cellular precipitation and its interaction with general precipitation were reported previously.1 The group of alloys covered in the present paper demonstrates precipitation-hardening reactions involving two distinct classes of intermetallic compounds where the predominating class appears to depend on base composition. This dependency ties in with a crystal-chemistry regularity first observed some twenty years ago by Laves and Wallbaum but never amplified to our knowledge. Results of electron-microscope and X-ray diffraction studies on systematically aged hot-rolled alloys known commercially as S-816, S-590, Rene-41, Incoloy-901, M-308, and M-647 are reported here. Some of these alloys have previously undergone minor-phase analyses by other investiators. Alloy S-816 was investigated by Rosenbaum, Lane and Grant,3 and Weeton and Signorelli.4 Rosenbaum found only CbC in hot-rolled bars. Lane and Grant found CbC and a small amount of M6C in the cast structure and stated that both carbides form during aging, most of the precipitation being CbC. Weeton and Signorelli found CbC, M23C6 and a weak indication of a phase after a slow step-down cooling cycle from 2250°F. Rosenbaum also investigated hot-rolled samples of S-590 and identified CbC and M6C. Preliminary information on Rene-41, gained partly from the present work, was reported by Morris.5 Long-time precipitation phenomena in Incoloy-901 at 1350°Fwere investigated by Clark and Iwanski.B heir raw data re- semble those of our present heat with 0.1 pct B, while their interpretation of these data resembles our interpretation of data from another heat with only 0.001 pct B; they made no statement as to boron content. No previous minor-phase studies of alloys M-308 or M-647 have been reported. EXPERIMENTAL METHODS Table I gives alloy compositions in both weight and atomic percent. Specimens were solution-treated from 1700º to 2200ºF, aged at logarithmic-time intervals up to 1000 hours between 1200 and 1800 F, and examined in accordance with procedures previously described in detail. &apos; &apos; Phase extractions were carried out in electrolytic cells containing 800 ml of either 7 pct HC1 in denatured ethanol or 20 pct H3PO4 in water. After electrolysis for 48 hr at 0.1 to 0.2 amp per sq inch, residues were separated by filtration or centrifuging. X-ray powder patterns of residues were recorded on a diffractometer for accuracy and on film for sensitivity. Lattice parameters were calculated by least-squares analyses of indexed sin 8 values, and relative abundances were estimated from intensities of strongest lines of each phase. These phase abundances denote relative amounts with respect to each other rather than to the alloy. Mechanically polished specimens were etched in a freshly mixed solution of 92 pct HC1, 5 pct H2SO4, and 3 pct HNO3. Parlodion replicas for the electron microscope were chromium-shadowed in high vacuum at a glancing angle of 20deg. All electron micrographs are reproduced here with the shadowing source above. The correspondence betweenelectronmicrostructures and phases identified by X-rays was established by a high redundancy of correlation between relative amounts at different stages of aging and examination above and below critical transformation or solubility temperatures. EXPERIMENTAL RESULTS S-816 and S-590—The phases found in S-816 and S-590 after various aging and solutioning treatments are listed in Table 11. These data and the observed

Jan 1, 1962

By Chikaosa Tanimoto

INTRODUCTION The committee on Rock Mechanics, Japanese Society for Civil Engineers, has been discussing &apos;soft rock engineering in Japan&apos; and presented several papers concerning dam, tunnel, bridge and slope constructions to International Symposium on Weak Rock, Tokyo 1981. This is the summarized paper based on References of Okamoto et a1 (1981), Iida et a1 (1981), Working Group on Tunneling-JSCE (1981), Working Group on Bridge Foundations-JSCE (1951) and Kikuchi et a1 (1981), which can convey general view on engineering experiences with weak rocks in Japan. From the point of view to the origin and/or distinctive physical properties, weak rocks in Japan may be classified into (1) sedimentary, (2) weathered, (3) low welded-pyroclastic and (4) fractured ones. Their typical characteristics are summarized in the following section. Concerning dam foundations on soft rock, several hundreds have already been constructed and, at present, nearly one hundred are under construction or at planning stage. These dams, almost without exception, have some problems such as site selection, material selection for fill-type and concrete dams, design of dam and its foundation, and construction procedures, requiring special ingeneous and cautious measures to cope with the local geotechnical difficult situations. In tunneling, for the decade of 1970s, the number of tunnels in soft rock either completed or under construction was at least 160, including Seikan Tunnel of 53.9 km long, Nakayama Tunnel of 14.8 km long and so on. Most of these tunnels are distributed in the northern half of Mainland, consisting of a basement of Paleozoic strata and Plutonic rocks, overlayed by Neogene Tertiary formations which include large

Jan 1, 1982

By R. R. Vandervoort, W. L. Barmore

Tensile creep experiments were conducted on high-purity, poly cvystalline rhenium from 1500" to 2300°C at stresses from 1500 to I0,OOO psi in a vacuum of 10-a torr. The apparent activation energy for creep was 60 kcal per mole, and the steady-state creep rate varied directly with stress to the 3.4 power. Dislocation substructure that developed during creep was studied by transmission electron microscopy. Possible rate-controlling deformation mechanisms are discussed. The creep behavior of most metals at elevated temperature can be represented by the following equation:&apos;&apos;&apos; t = Cf(s)(^)(s/E)nD [1] where i = steady-state creep rate, C = constant, f(s) = a function involving microstructure, s = applied stress, E = the average elastic modulus at test temperature, n = constant, D = diffusion coefficient According to this well-established relationship, metals with higher elastic moduli and lower diffusion coefficients should have greater creep resistance at the same stress and temperature and equivalent mi-crostructures. While no diffusion data are available, the diffusivity of rhenium should be less than that for most other refractory metals because of its high melting point and hcp crystal structure. The Sherby-Simnad relation for calculating atomic mobility in metallic systems3 predicts that the diffusion coefficient for rhenium is less than that experimentally determined for tungsten4 in the temperature region 1500. to 2200°C. At these temperatures the elastic modulus for tungsten5 is only slightly larger than the extrapolated modulus for rhenium.6 Thus, rhenium is a good possibility for a a high-temperature structural material, but few data on the creep of rhenium have been reported. This investigation was undertaken to study the high-tempera-ture deformation behavior of rhenium in detail. EXPERIMENTAL TECHNIQUES The material used in this study was consolidated from high-purity powder. After cold pressing the powder to a plate a in. thick, the billet was sintered in hydrogen at 2250°C for 24 hr. The plate was reduced to 0.100 in. by cold cross rolling with intermediate anneals at 1650°C for 20 min between passes. The plate was further reduced to 0.060 in. by unidirectional cold rolling with similar heat treatments between passes, and then finally stress-relieved in hydrogen at 1650°C for 30 min. Specimens tested at 1900°C and below were pretest-annealed at 1900°C for 2 50 hr. Specimens tested above 1900°C were pretest-annealed at 2400°C for 5 hr. The impurity content in the "as-received" plate was quite low, table I. Essentially no change in impurity levels was detected in specimens after creep testing. All creep tests and annealing treatments were conducted in a vacuum of 10-8 torr in a test furnace heated by a tungsten mesh element. The load was applied to the specimens through a bellows, and stresses were maintained to ±1 pct of the selected value by periodic corrections for changes in specimen cross-sectional area during creep and for changes in the bellows spring force due to load column extension. One-inch-diameter tungsten force rods were used in the hot zone of the furnace. Deformation at temperature was measured by optically tracking gage marks on the specimen. Temperature was measured by a calibrated optical pyrometer and was determined to ±5"C. Grain sizes were determined by the linear intercept method and specimens were examined in the "as-polished" condition, using polarized light. Specimens annealed at 1900°C had a grain size of 52 ± 5µ , and those annealed at 2400°C had a grain size of 148 * 11 µ. Pieces were cut from the gage section of creep-tested specimens and planed to a thickness of about 0.010 in. by spark discharge machining. Thin foils for viewing by transmission electron microscopy were obtained by electropolishing in a solution of 6:3:1 ethyl alcohol, perchloric acid, and butoxy ethanol, respectively, using the window technique. Bath temperature was —4OoC, and the cell potential was 35 v. The foils were examined in Siemens Elmiskop I, operating at 100 kv. RESULTS AND DISCUSSION In order to analyze the results from creep experiments, Eq. [I] is rewritten in the following form: <=Kf(s)ne-/RT [2] where K = constant, ?// = apparent activation energy for creep,

Jan 1, 1970

By B. C. Allen

Grain boundary grooving has been studied in chromium, molybdenum, and tungsten under a variety of conditions using high vacuum techniques and tantalum -gettered argon. The average surface free energy of solid chromium, and the chromium-liquid silver interface free energy were respectively found to be 2200 ± 250 and 500 i 130 ergs per sq cm from groove formation kinetics and estimates of pertinent volume difffusion coefficients. The results for chromium were unffected by variations in interstitial content ranging from 0.003 to 0.09 pct C, or 0.003 to 0.03 pct O. Surface diffusion is the primary mechanism of groove formation in chromium under 1 atm argon at 1200" to 140O°C, and is essentially unaffected by 0.003 to 0.09 pct C, 0.003 to 0.03 pct O , metastable nitrogen contents up to -0.01 pct, and up to 2 torr Ag vapor. At higher temperatures, the major mechanism is volume diffusion in argon or evaporation-condensation in stutic vacuum. Surface diffusion occurs in molybdenum at 0.5 to 0.96 and in tungsten at 0.5 to 0.9 of the absolute melting tempera -ture by a single mechanism, possibly by the migration of single adatoms or vacancies. Results were slightly affected by up to 23 tory Sn vapor, and in molybdenum were essentially unaffected by 0.5 Ti or carbon in the range 0.002 to 0.02 pct. Volume difffusion through the liquid is the mechanism of groove formation in chromium-liquid silver at 1200" to 1400°C and in molybdenum-, Mo-0.5Ti-, and tungsten-liquid tin at 1200" to 2000°C. The solid-liquid interface free energies involved were estimated from grooving kanetics. WHEN a grain boundary intersects a solid surface, a groove tends to form along the line of intersection at temperatures above about half the absolute melting point (0.5 TM). The groove progressively grows by preferential atomic migration either by diffusion or evaporation. Establishment of a groove angle occurs in accordance with the grain boundary and surface free energies involved. The motivation for groove formation is a reduction in the total surface free energy of the system. This study is a continuation of previous work on thermal grooving of chromium, molybdenum, and tungsten.&apos; The temperature ranges were extended, and the effect of metallic and interstitial impurities was evaluated. The results were such that certain interface free energies and surface self-diffusion coefficients were deduced from the grooving kinetics. EXPERIMENTAL WORK Materials and Preparation. As indicated in Table I, the 0.05-0.08-cm-thick chromium, molybdenum, and tungsten sheet used was nominally 99.99 pct after recrystallization. Two lots of molybdenum with about the same analysis, Mo-0.5Ti,* and tungsten were ob- *Alloy compsitions are expressed in weight percent . tained commercially. Extruded chromium rod,&apos; prepared from iodide process crystals, was warm rolled to sheet at 700°C. Sheet of three Cr-0 impurity alloys containing up to 0.03 pct 0 was prepared by warm rolling arc melted, extruded, and swaged rod. Two Cr-C impurity alloys containing up to 0.09 pct C were made by equilibrating unalloyed chromium with a known amount of CH4 for 24 hr at 1150°C in previously evacuated quartz capsules. Chromium containing nominally 0.015 and 0.06 pct N was similarly prepared by equilibration with NH3. The sheet was recrystallized to give a stable grain size about equal to the sheet thickness. Molybdenum and Mo-O.5Ti were recrystallized in a tantalum resistance furnace 1 hr at 1 x lo-5 torr at 2300" and 220O°C, respectively. Tungsten was similarly annealed for 1 hr at 2500°C. Chromium and its impurity alloys were outgassed at 1100°C and recrystallized 1 hr at 1700°C under 1 atm Ar. Except for nitrogen, the impurity content stayed roughly constant. Nitrogen in both alloys was reduced to <0.001 pct. In fact, over 80 pct of the added nitrogen was lost after outgassing at llOO°C and annealing sheet 1 hr at 1300°C in argon in the presence of tantalum. Such a rapid loss can be rationalized since -2 torr N are required for equilibrium with 0.04 pct N in solution,3 while the equilibrium pressure is ~10-5 torr over tantalum at 1300°C.4 The recrystallized sheet was cut into small coupons which were metallographically ground and polished on one side with a minimum of grain boundary relief. The surface roughness was on the order of 0.01 µ. The tin and silver used were nominally 99.999 spec-trographically pure. After being outgassed at 1100°C and equilibrated in a molybdenum crucible for 0.5 hr at 1800°C in argon, the tin contained 3 ppm 0, <0.3 ppm N, and 0.1 ppm H. Following outgassing at 900°C and equilibration in a chromium crucible 1 hr at 1400°C in argon, the gas content of the silver was 1 ppm O, <0.5 ppm N, and 0.3 ppm H. Grooving Under Argon or Vacuum. All specimens were placed in unsealed containers made from rod or sheet of the same alloy, thereby enabling the polished surface to achieve gas-solid equilibrium. The annealing fixtures are shown in Fig. 1. The specimen was placed in a resistance furnace with a tantalum or Ta-10W heating element plus tantalum fixtures or radiation shields. Chromium was outgassed at 1100°C, and molybdenum and tungsten were outgassed at 1900°C to 1 x l0-5 torr or at the grooving temperature, whichever was lower. In vacuum anneals, the specimen was then heated directly to the intended grooving temperature. In argon anneals, 99.996 Ar was admitted

Jan 1, 1970

By J. J. Reed

The mines of southeast Missouri&apos;s Lead Belt have been in operation since 1864, almost 100 years. During this period about 10 pct of the total ore available has been left in place as pillars, and this now represents the best ore reserve left to the older mines. St. Joseph Lead Co. has been investigating various plans of pillar recovery for several years. The example to be described is only one possible approach under a specific set of conditions. Conditions vary greatly in the different areas within the Lead Belt, and the same approach would be entirely inadequate in certain other areas, but there are important sections where this system is clearly applicable. Horizon mining is practiced in the Lead Belt, and stopes may vary from 10 ft to well over 100 ft high. Fig. 1 is a plan view of 6100 stope, the area to be discussed. For these mines this is a small stope, only 10 to 12 ft high. Before any plans were drawn up for pillar recovery, three independent estimates of the pillar grades were made by the mine superintendent, the mine captain, and the mine geologist. After these results were averaged, pillars indicated to be of economic grade were marked for removal as shown. At this stage several alternatives were considered: 1) retreat with caving, 2) concrete replacement pillars, and 3) systematic bolting and retreat. A retreating system with caving was not chosen because the roof was known to be too bad even to permit loading a blasted pillar before caving would begin. Concrete replacement pillars would have been too costly and would have required a large crew, bulky materials, and unwieldy equipment. Systematic bolting was chosen as being most acceptable for the following reasons: 1) Limited area and spans were involved. 2) Only minor modifications to the jumbo would be required for bolting. 3) Only a two-man bolting crew would be needed. 4) Only compact bolting materials would be required. 5) The bolting plan could be modified to allow

Jan 1, 1960

By C. C. Mattax, J. E. Bobek, M. O. Denekas

ABSTRACT investigations in recent years have shown that rock wettability can exert a profound influence on the displacement of oil by water from oil producing reservoirs. Core analyses frequently show oil recoveries from preferentially water-wet rock to be significantly greater than those from preferentially oil-wet rock. Thus, an accurate prediction of water-drive or waterflood oil recovery is dependent on the evaluation of reservoir rock wettability. Laboratory and field studies have been undertaken to examine and develop methods which may be used to measure rock wettahililiy, to investigate factors which may alter the wettability of reservoir rock, and to determine the wettability of specific reservoirs. It has been found that measurement of the rate and volume of spontaneous imbibition of the wet-ting phase by a rock is a reliable and reproducible test for semi-quantitarive determination of preferential rock wettability. Laboratory tests have shown that the wettability of reservoir rock may depend on both the crude oil composition and the rock type. Field and laboratory tests have indicated that coring flulids and core handling techniques can cause significant changes in the wettability of rock surfaces. However, a few fluids, brine in particular, appear not to affect core wettability and may be used when coring to determine reservoir wettability. Core handling and packing procedures have been developed which preserve core wettability during storage and laboratory testing. The wetfability characteristics of six reservoirs have been evaluated by wettabilify tests performed in the field on fresh cores cut with brine or special water-base muds. The tests indicated that all six reservoirs are water wet; however, the de-gree differed from one reservoir to another. INTRODUCTION Although surface properties of reservoir rock and interfacial characteristics of rock, crude oil, and water systems have been discussed for many years, the full significance of these properties to the production of oil is still in the process of evaluation. It is known, however, that one surface characteristic—preferential wettability of the reservoir rock—-is of paramount importance when the reservoir is being produced by water-flood or water-drive mechanisms. The importance of rock wettability has been pointed out by several authors&apos;.&apos;,%* who have found that pref- erentially water-wet cores flood more efficiently than oil-wet cores; that is, more oil is recovered from water-wet cores in the early flooding stages than from oil-wet cores. Other authors&apos;," indicate that waterflood oil recovery from cores of intermediate wettability may be greater than that from either strongly water-wet or strongly oil-wet cores. These recent investigations emphasize that the true wettability of a reservoir must be known before the performance of waterflood or water-drive reservoirs can be accurately evaluated. When reservoir wettability is to be determined by core analysis, precautions must be taken to maintain the original wettability which can be altered readily during coring5 nd testing.&apos; In the coring operation the core may be partially or completely penetrated by the drilling fluid which, if it contains surface active materials, may drastically change the wettability of the core. Also, improper core handling during stcrage and testing may change its wettability because of evaporation of fluids or exposure to oxygen or surface active contaminants. One purpose of this paper is to discuss methods for obtaining, preserving, and testing cores without altering their original wettability. In addition, the results of wettability tests on fresh and preserved cores from six reservoirs are presented where special precautions were taken to obtain samples without altering their wettability during the coring operation.