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By D. A. Wheeler

Invented by Pierre Boutin in the early 1960s the column was a complete break from the conventional flotation cell. 1. When used as a rougher-scavenger, the column is excellent. 2. When used as a cleaner, the results can be spectacular. The very first column tests were carried out using it as a rougher-scavenger in a reverse float where silica was floated from iron. It produced a concentrate underflow as good or better than that produced from roughing and scavenging stages in cells, The froth tailing overflow was better than that produced by several stages of cell cleaning. Column scaleup progressed rapidly from the two inch diameter unit to a semi automated 12 inch diameter column on material from the Iron Ore Company of Canada. A change in operating philosophy within IOCC brought all flotation development, column or conventional, to a halt. At that time, IOCC had an exclusive right to the use of the column in Canada in the field of iron ore. We moved into the field of sulphides. A Canadian copper producer sent ore for testing and the results led to their purchase of the first commercial size of column - a 36 inch diameter machine. It was a mechanical disaster. It took several years to raise sufficient funds to return to that mill with our basic 18 inch square unit. It was to be tested and modified in order to learn how to properly design a large column. Originally used as a rougher- scavenger, it had to produce tails equal to the final tailings from this well run plant. It did, and did so while producing a rougher-scavenger concentrate almost equal to the plant final concentrate. It was finally used as a cleaner and produced concentrate 5% higher in copper than the plant final concentrate with equal cleaner tails. This phase of the column development was carried out under very difficult circumstances. The mill superintendent had realized that if he took the froth removal system from our original mechanical disaster and applied it to a conditioner while injecting air, he would have a flotation cell. He had personally applied for patents on this Maxwell Cell. Our development work was done in his mill and as our results became better and better, our difficulties became worse and worse. We finally had to terminate this work. The 18 inch column installed at Mines Gaspé 14 years later was identical to the one removed from Opemiska. The 18 inch column was tried on various ores over the following years and always produced excellent results. However, it was not really a production size unit. We had always aimed for the 72 inch column (72" x 72" x 44' 9"). Prior to this huge machine, we needed the intermediate 36 inch column. The failure of the original 36 inch diameter unit at Opemiska had raised the possibility of short circuiting inside the column as the cross section increased. The first 36 inch square unit was tested in parallel with the proven 18 inch column. If the underflow of the 36 incher was not as good as that of the 18 incher, short circuiting was a possibility in the larger unit. It had been designed for insertion of drop in partitions, four feed points had been provided and the 36 inch column would have become a modular unit of four 18 inch columns. Testing showed the underflows of both columns to be identical. There was no short circuiting in the 36 inch column. Once we had the 36 incher, we had no fear of the 72 inch column. It is permanently partitioned into four 36 inch columns but uses only one set of instrumentation. All the component parts of the 72 inch column come from the 36 inch unit. In spite of our results, the mining community did not believe the column could work. Finally, in 1980, Mines Gasp6 ordered an 18 and 36 inch column for their byproduct molybdenum

Jan 1, 1988

By D. Nilsson, B. Aaro

To find out if there are any potential savings in "in-the-wall haulage for open pits," the Swedish companies ASEA and Kiruna-Truck in 1984 gave us financial support to study this solution in more detail. In the study, the use of in-the-wall haulage was studied for three hypothetical open pits with different sizes and shapes. Annual ore production rates also varied. A part of this thor¬ough study was published by the Swedish Mining Research Foundation (see Report F 8444, "The Use of Electric Trucks and In-the-Wall Haulage in Open-Pit Mining," in Swedish with an English Summary). Although in-the-wall haulage is of interest in some open pits, the local terrain is important for profitability. The authors do not think in-the-wall haulage is of any major interest for the mining industry. The following is a summary of some of the author's findings. To place the haul road in the wall is not of interest in open pits with declining metal contents in the bedrock. In such mines, the volumes from the haul roads will not yield reve¬nues. The cost per m3 for an underground haul road is much higher than for a haul road in the pit. This means that it is only of interest to place the haul road in the wall when mining gets deeper than about 50 m (165 ft). In-the-wall haul roads will reduce flexibility in the pit, and it will make necessary the use of smaller equipment with lower productivity and higher costs per ton. As Hustrulid, et al. show (Table 4), excavation savings of material hauled are very low, $0.10 to $0.25/t (0.09 to 0.27 per st). The extra operating cost, due to lower productive equip¬ment, will normally be much higher and thus destroy the whole idea with in-the-wall haulage. If electric trucks are profitable for in-the-wall haulage, it is normally also profitable to use electric trolley assist for trucks on the haul road in the pit. But the profitability of using electric power is different in different countries, and depends on the relation between the cost for electric power and diesel fuel. In the US, diesel fuel is inexpensive compared with electricity, but in a country like Sweden, diesel fuel is much more expensive. In most open pits, the trucks have to move a considerable distange from the loader until they reach a final haul road in the wall. A trolley line along such temporary haul roads will be exposed to flyrock. It is normally less expensive to perform rock support from the open pit than from underground ramps in the wall. In Fig. 8, Hustrulid et al. gives the impression that the underground haul roads will be very close to each other. This is seldom the case. Figure 1 shows a haul road in the wall. The haul road passes through each cross-section only once. Ar¬ranging a reliable dewatering and rock support system from only one underground ramp is probably impossible. Many more drifts are therefore necessary. In our report, we also studied what would happen if the final pit slope is increased by 5°, using underground drifts in the wall. Our conclusion was that the extra cost for drifts, rock support, pumps, etc. destroys the whole idea, and that it was better to accept a higher stripping ratio with the haul road in the pit and to use conventional low-cost open pit equipment. Finally, we think it is would be difficult to try to reduce the safety factor when determining the slope angle by moving the haul road in the wall. Minimizing the risk for pit wall collapse is also important with in-the-wall haulage, primarily because men and equipment will be working in the pit, but also to guarantee many accesses between the pit and the haul road in the wall.

Jan 1, 1989

By Ernest E. Thurlow

Introduction Today, more than 50% of rail-carried commodities are mineral industry related, with coal being the most important single commodity moved by rail. In 1980, coal accounted for more than 5.7 million of the total 22.6 million carloads moved by rail. Metallic ores were third behind grain, with more than 1.4 million carloads. Crushed stone, gravel, sand, and other non-metallic minerals totaled almost 2.3 million carloads. Chemicals and allied products, including fertilizer and coke, added another 1.7 million cars, with petroleum and petroleum products totaling 300,000 carloads. Coal Several things happened in the 1970s that gave rise to increased consumption of coal-particularly western coal-and to its dominant position among rail-carried commodities. First, the Clean Air Act of 1970 required generating plants to make significant reductions in sulfur dioxide emissions. To comply, utilities could either invest in scrubbers or switch to low-sulfur western coal. Many opted for the latter. By 1972, increasing demands by the utility companies halted what had been a 25-year decline in national coal consumption. Second, the Arab Oil Embargo of 1973 put an end to cheap oil and gas, limiting their future as fuels for electric generating purposes and increasing the potential for coal. Third, in 1977, President Carter announced an energy program with coal as its cornerstone, calling for an annual two-thirds increase in national coal production by 1985. He also called for conversion to coal by utilities and large industrial users. Finally, he proposed a 10-year, $10 billion program to encourage domestic coal production and stimulate development of export markets. Coal bounded into world prominence. Foreign demand for steam and metallurgical coal increased tremendously, while US demand for western coal also shot up. This meant greater demands on the transportation sectors that traditionally carried coal to market. Many railroads began programs to serve the coal industry. One example is Burlington Northern's commitment to handle increased western coal tonnages. The company spent more than $1 billion in recent years to develop a system capable of moving more than 91 Mt (100 million st) of coal each year. Other leaders in this renewal were Norfolk and Western, Union Pacific, Santa Fe, and Southern Pacific railways. The importance of the rapid growth of coal traffic to the railroads is shown in the accompanying table, which gives percentages of total tonnages hauled and revenues attributed to coal. With coal providing the railroad industry with a substantial share of its revenues, there is keen competition among the rail companies themselves and among railroads and other transportation sectors for coal haulage. But there is also cooperation when more than one railroad is involved in delivering the coal from mine to market or when a combination of transportation modes is more economical. The latter is represented by Conrail's interest in working with the port authorities of New York and New Jersey to establish a new coal port that would serve not only export markets, but also utilities and industries in the northeast. Iron Ore Next to coal, iron ore (taconite) is the most important single mineral commodity handled by railroads. In Minnesota, where most iron ore is produced, rail transportation is primarily by Burlington Northern and the Duluth, Missabe, & Iron Range Railway Co. (DM&IR). The DM&IR, owned by US Steel, serves several producers on the Mesabi Iron Range. Two of the larger producers, Erie Mining Co. and Reserve Mining Co., also own railroads that operate between the mines and the ports of Silver Bay and Taconite Harbor on Lake Superior. Several iron mines and taconite plants in Michigan are served by the Chicago and Northwestern, and the Soo Line. Total 1981 shipments of taconite and iron ore are estimated at 55.9 Mt (55 million It), compared with about 61 Mt (60 million It) in 1979 the most ever shipped in one year. Still, with annual production capacity of the eight Mesabi Range

Jan 10, 1982

By H. C. Chang, N. J. Grant

Creep of very coarse grained high purity aluminum was studied at 400°, 700°, and 1100°F at initial stresses of 50 to 1200 psi. Local strain measurements were made across the grain boundaries and in different regions of various grains during creep, thereby permitting the drawing of component creep curves. The relative amounts of elongation as measured across a grain boundary and in the grains adjacent to the boundary depend on the temperature of testing. The significance of creep curve equations and activation energies is discussed. THIS paper presents some of the results of a research program devoted to the study of the mechanism of creep in high purity aluminum. Previous publications have dealt with the cyclic processes of alternating grain boundary sliding and migration, and the deformation in the grains caused by these processes;' the direction and the driving force of grain boundary sliding and migration;' the deformation in the grains and the restricting effects of the grain boundaries on this deformation." These previous papers were based mainly on either microscopic observations or X-ray data, or both. Sometimes creep curves across two closely spaced reference marks (about 0.6 to 0.7 mm apart) were also presented with a view to correlating the elongation values with the optical observations in general, and with certain deformation processes in particular. These curves shall henceforth be referred to as component creep curves. No attempts were made, however, to compare either the component creep curves which were obtained in different regions of a specimen, or those obtained from different specimens subjected to different creep test conditions. It is the purpose of this paper to present these component creep curves. Among the factors influencing the behaviors of these curves, those studied were stress, temperature, and grain arrangements in the specimens. It is proposed to show how greatly the deformation can vary from grain to grain and within an individual grain in a coarse grained specimen. The experimental technique and procedure have been presented.' It remains necessary to emphasize that the reference marks were produced by pressing a thin sewing needle into the surface of the specimen before the final annealing at 900°F for 24 hr and at 1150°F for 12 hr. The cold work around the needle indentations was therefore removed. The depth of these holes after electropolishing the annealed specimens was about 0.01 mm. This depth and area were negligible in comparison with the thickness of the specimens, 2.3 mm, and hence would not affect the creep behavior. Results Fig. 1 shows a development diagram of specimen P-8. The dots on the surface locate the needle point reference marks used to obtain the component creep curves. A curve obtained between two dots across a grain boundary measures not only the boundary deformation but also the deformation associated with boundary sliding occurring in the grains in the region between these indents. The original distance between two reference marks was about 0.6 to 0.7 mm. The maximum error of measurement was 0.01 mm, or in terms of percentage elongation, of the order of & 1.5 pct. Whereas the component creep curves shown in the figures to follow were drawn as a gross average of the points, in view of the fineness of some of the steps of grain boundary sliding and migration, as shown in the previous publications,¹,2 it appears logical to expect that some of the finer cycles of movement have not been delineated for the strain sensitivity of the measuring system. It seems justifiable to say that the curves are not as smooth as shown. 700°F Tests: Fig. 2 shows component creep curves across four of the grain boundaries in specimen P-8, tested at 700°F and 85 psi. These curves clearly show alternate cycles of increasing and decreasing

Jan 1, 1954

By L. D. Jaffe

From data found in the literature, a method has been derived for calculating hardenability of titanium alloys from their composition. A single graph gives the contributions of each alloying element. These are simply added to a base hardenability for unalloyed titanium. Results agree satisfactorily with measured harden-abilities. RECENTLY the importance of hardenability of titanium alloys in permitting attainment of high strength and hardness has become apparent. If a titanium-base alloy has adequate hardenability for the section size and quenching practice used, it can generally be heat treated to high strength and hardness either by simple quenching or cooling from temperatures near the ß transus, by quenching and tempering (aging), or perhaps by direct isothermal transformation of ß1,2 If the hardenability is inadequate, high strength cannot be attained. Preliminary charts translating hardenability requirements for shapes quenched in various media into terms of Jominy end quenched hardenability specimens or ideal round sizes are now available for titanium alloys." The method proposed in 1942 by M. A. Grossmann for calculating hardenability of steels from composition has proved to be of great practical value.' It appeared worthwhile to see whether, using information available in the literature, a corresponding method for calculating hardenability of titanium-base alloys could be derived. Data No systematic experimental study of the hardenability of titanium-base alloys has yet been made. There is available, however, a considerable quantity of scattered data bearing on hardenability. Some investigators determined Jominy curves on one or several alloys. Others reported as-quenched hardness for specimens of a few alloys cooled at various rates or in various media. Still others gave the as-quenched hardness for systematically varied composition, using one or several cooling mediums. The measurements utilized in this work were limited to hardness. Strength measurements were not used because a low strength may reflect high hardness combined with brittleness. Since, in general, the hardness of titanium alloys goes through a peak as the cooling rate is varied from extremely fast to extremely slow, the cooling conditions at which peak hardness was found were taken as the measure of hardenability.1,2 When as-quenched hardness was found to drop as the content of an alloying element (believed to increase hardenability) was raised, this was taken as an indication that the cooling rate was faster than that giving peak hardness; otherwise, the hardness should go up because of solid solution hardening. Also, if the hardness increased on tempering at low temperatures, this was again taken to indicate that the cooling rate had been faster than that giving peak hardness. Many of the data did not indicate precisely the cooling conditions for peak hardness but merely set a maximum or a minimum bound, or a bracket. Since the sizes of specimens quenched and the location of the hardness readings were not always given, it was occasionally necessary to estimate reasonable limits for them. Only the nominal compositions were available in some cases. As quenching from below the ß transus is equivalent to starting with a mixture of a and ß phases, whose individual composition would differ from the overall composition of the alloy, only measurements after quenches from above the ß transus were used. Hardness measurements on samples heated during metal-lographic mounting were also discarded. Because of their bulk, the data used will not be reproduced. They have been or will be published elsewhere.5-22 Approach All data were first translated into terms of ideal round size. For conversion from Jominy or quenched round or sheet, the author's graphs were used." For a few furnace cools or helium quenches where cooling rates were given, conversion was made on the basis of equal cooling coefficient.23 Plots of ideal round size for peak hardness against percentage of alloying element were next made for

Jan 1, 1956

By D. Harker, W. E. Seymour

CERTAIN alloys of iron and nickel, when rolled and annealed, possess a preferred crystal orientation: (001) in the rolling plane and [loo] in the rolling direction, when recrystallized at 850" to 1050°C after approximately 98 pct cold reduction. Since the preferred orientation makes a direction of easiest magnetization coincide with the rolling direction, these alloys, especially a 50 pct iron in nickel alloy, have found wide application in the electrical industry' for choke coils and special types of transformers. The rate of the recrystallization reaction was studied at temperatures ranging from 500° to 600°C. The heat of activation for the reaction was calculated from the observed rates, and crystal orientation determinations were made before and after re-crystallization. A vacuum melted iron-nickel alloy* analyzing 49.6 pct nickel, 0.018 pct carbon, and 0.30 pct manganese was used for the experiments. The alloy was cold-rolled 98 pct into strips 1/2 in. wide by 0.002 in. thick. Specimens 1 in. long were sealed under a vacuum (approximately 10-8 mm Hg) in 1/2 in. ID pyrex glass tubes. For heat treatment these tubes were fastened to Nicrohm wires and submerged in a molten salt bath controlled to ±2°C. (The maximum measurement error was within 3°C.) The time at temperature was varied logarithmically from one sample to another, and runs were made at 500°, 525", 550" and 575°C. A molten lead bath was used for a run at 600°C which was controlled to the same accuracy. To determine the extent of recrystallization after a particular time at a given temperature, a method was used suggested by the work of Decker, Asp, and Harker.3,4 This method employs an X-ray spectrometer whereby X rays are diffracted from crystallites whose diffracting atom planes are parallel to the rolling plane of the specimen. The intensities of the diffracted rays are measured by a Geiger counter. The counter can be rotated through a range of angle, and can be motor driven through this range at a speed of 2" per min. The measured intensities are plotted vs. angle by a potentiometer recorder. In a 50 pct iron-nickel alloy it was found that only (200) reflections were obtained from the rolling plane with recrystallized material, and that only (220) reflections were obtained from the rolling plane with unrecrystallized material. No other reflections were obtained under these conditions over a range of Bragg angle of 0 to 45" using either type of specimen. As a consequence, the intensity of the (200) reflections from the rolling plane was taken to indicate the amount of recrystallized ma-terial present in a specimen, and the corresponding intensity of the (220) reflections was taken to indicate the amount of unrecrystallized material present. To insure flatness and proper alignment of the reflecting specimen in the spectrometer, the sample was laid in a slot 1/2 in. wide x 0.001 in. deep which was machined in a 3/4x2x1/2 in. steel carrier. The specimen then was taped down with cellophane tape. This steel cradle was mounted vertically in the specimen holder of the spectrometer so that the bottom edge of the carrier rested against a horizontal shoulder. Intensity data used in plotting the percent of recrystallized material vs. time at temperature were obtained by directly counting the diffracted beam of nickel filtered copper Ka radiation used throughout the work. The X-ray spectrometer was employed also in obtaining pole figure data to be used for orientation determinations. At the beginning of this investigation a transmission pole figure holder was used." As a thickness of 0.002 in. of this alloy was found to be opaque to the copper Ka radiation, it was necessary to reduce the thickness of the pole figure specimen. A cold-worked sample was etched in a 50 pct HCl solution for 5 min and was found to transmit a

Jan 1, 1951

By Euclid P. Worden

In 1977, an article in World Mining1 reported a total of 2726 rotary blasthole drills in service. This figure included only those machines produced by three of the manufacturers building drills of this type. The total, therefore, is much higher. Rotary drilling in the mining industry is big business to the manufacturers and suppliers involved, and a significant cost item to mine operators. The time has come to take a hard look at rotary drilling technology with an eye to reducing costs by increasing drilling efficiency. The efficiency of any rotary drilling operation is best measured in terms of the rate of penetration achieved by the bit. In blast hole drilling, there are five factors which affect the rate of penetration. They are: (1) bit selection, (2) weight on the bit, (3) rotary speed, (4) hole cleaning, and (5) formation properties. Of these factors, all but one may be controlled by the operator. Looking at any one in detail may reveal possible improvements in the system. One of these factors -- proper hole cleaning - will be discussed in this paper. In order for a bit to perform at its maximum capability, each tooth or insert should strike fresh clean rock as it falls into its drilling position. If the tooth or insert lands on previously drilled cuttings, a major portion of the energy delivered to the bit is absorbed in redrilling this broken material. A major portion of the interest, therefore, should be directed to the proper cleaning of the bottom of the hole. In an in-depth study of the cleaning of large diameter holes, Allen2 reports that horizontal air velocities of 38.10 m/s are necessary to prevent the saltation of drilled cuttings on the bottom of the hole. The exact flow pattern on the bottom of the hole, however, is not generally known. The air leaves the bit through the jet nozzles and the mouths of the cones, but where it goes from there is uncertain. This problem should be investigated by the bit manufacturers because they can best utilize the results of such an investigation to provide a more effective product. Some work has been initiated in this area and competition will probably increase its intensity. Bailing velocity is the best criteria to measure the cleaning of the hole, including the bottom, and is the factor on which efforts toward improvement must be concentrated. The first consideration is "What should the bailing velocity really be?" In drilling deep holes for oil and gas, 15.24 m/s is the generally accepted figure. In blasthole drilling, the figures of 25.40 m/s for average rock to 35.56 m/s for iron ore were first mentioned by Capp3 in 1962. The recommendations are the same to this day. A number of questions could be asked in regard to the apparent disparity between these two sets of figures. Various investigators have derived formulas which support one or another of these criteria. A thesis on the subject was written by Alexander4 who derived a formula based on research which resulted in velocities in the lower end of the ranges quoted previously. He set out to compare this figure to laboratory tests and his tests indicated that the velocities given by the derived formula appeared to be high.1 Perhaps the best reason that the 25.40 to 35.56 m/s range has been used, is that these velocities seem to work. Below the accepted figures, low bit life and slow penetration rates occur. Above these figures, increasing amounts of abrasive wear on the drill pipe and stabilizers seem to appear. There is a fallacy to this entire approach, however. The entire velocity calculation is made using nominal bit and pipe sizes and compressor deliveries with no compensation made for losses in the system. Perhaps an examination of some of the things that are not presently considered could lead to some practical improvements in the operation.

Jan 1, 1980

By J. L. Huitt, D. K. Lowe

This laboratory flow study covers propping agent transporl in horizontal fractures as influenced by the characteristics of the propping particles, fluid and fracture. Correlations are presented for the transport of particles, deposition and fingering through dunes. For particles moving individually, the article velocity in some cases may be low compared to the hulk average fluid velocity; in other cases, the particle velocity may exceed the bulk average fluid velocity. At high propping agent concentration or low fluid velocity, the likelihood of particle deposition and dune formation increases. Fingering and channeling accompany dune formation. Dune formation can be limited to the outer region of tile fracture by adjustment of pump rate, fluid viscosity and particle concentration. A method is presented by which pump rate and fluid vircosity may he selected to control dune formation for given propping agent concentrations. INTRODUCTION The area and flow capacity of a fracture predominantly control the stimulation derived from hydraulic fracturing. Generation of fracture area exposes the rock matrix to a flow channel; the flow capacity of the fracture controls the flow through the channel to the wellbore under a given pressure gradient. This paper pertains to an important factor that affects the flow capacity of a fracture: the transport of the propping particles in the fracturing during the hydraulic fracturing treatment. With a better understanding of particle transport, fracturing treatments may be designed to obtain more effective distribution of the propping agent. RELATED STUDIES In recent years, the approach to obtaining high fracture flow capacity has been partial monolayer propping. Three papers1-3 have dealt with various facets of this concept. However, in some papers dealing specifically with particle transport, the results generally indicate that packing the propping particles within a fracture is inevitable. In early work&apos; with a sand slurry flowing in a pie-shaped flow cell, qualitative results showed that particle deposition in a fracture during transport should be expected. In other studies"" correlations based on slurry flow in vertical linear flow cells showed particle deposition was primarily a function of fluid velocity. In a recent paper the rate of sand advance (movement of dunes) in a horizontal linear flow cell was discussed. Subsequently, a method was given for designing fracturing treatments, based on the extent of sand advance during a treatment. In this work, particles whose diameter was small relative to the fracture width (i.e., dl W< 0.2) were primarily considered. The particle transport approaches that of sand transport in a stream bed. The industry trend, however, has been to use larger size propping agents. That is, particles with diameters approaching fracture widths predicted by Perkins and Kern.&apos;&apos; This trend has led to generally better fracturing treatments with particle relative sizes in the range 0.2 <d/W < 1.0. In all of the particle transport studies previously cited, the fluid characteristics were discussed. However, little or no attention was given to the parzicle characteristics. In this study the particles. as well as the fluid and fracture, are considered. VARIABLES AFFECTING PARTICLE TRANSPORT In the exploratory work to set LIP a program for this study, it was noted that particles within a batch moved at different velocities in a horizontal linear flow cell. In some cases the particles moved independently. In others there was particle interference. Also, particle deposition and fluid fingering occurred in some cases (Fig. 1). As a result of observing the easily distinguishab&apos;le types of particle movement, the particle variables as well as the fluid variables were included. In addition, the fracture width was included because the fluid velocity profile surely must affect the movement of the larger particles differently than that of smaller particles. Particle variables were density, diameter (based on a sphere of equal volumetric displacement), long and short dimensions, drag coefficient and velocity. Fluid variables were density, viscosity, yield shear strength and velocity. Fracture variables were the width and the angle between the plane of flow and a horizontal plane. Two factors which may prove to be important were omitted because of the complexity resulting from the parameters cited above. These are the fracture-surface roughness and gross irregularities that cause changes in the direction of flow. EXPERIMENTAL EQUIPMENT AND PROCEDURE A linear parallel-plate flow cell (Fig. 2) was used in the study. Lucite plates 1 in. thick formed the test section and permitted a viewing section 11 ft long and 10 in. wide. Spacing between the plates was adjusted with shims to give fracture widths 1/36 to 1/2 in. The model could be tilted to an angle of 45" with the horizonltal plane. Fluid flow was maintained with a Moyno positive displacement pump. Single particles were placed in the flow stream with a particle injector. A .4 - in. diameter plunger moving at a constant rate in a

Jan 1, 1967

By D. W. Frommer

Processing nonmagnetic taconites by selective flocculation-desliming and flotation requires large volumes of water. If impounded without treatment, these off-process waters require excessively large areas for containment. To discharge the waste water into natural waterways would contribute to stream pollution and likely would not be permitted. In U.S. Bureau of Mines experiments conducted in the Twin Cities Metallurgy Research Center&apos;s 900-lb per hr pilot plant, approximately 85% of water requirements for the flotation-based treatment of a Michigan nonmagnetic taconite were met by reclaimed water. Water reclamation of the off-process streams from flotation was accomplished by controlled additions of lime, sodium carbonate, and a synthetic flocculant to reduce turbidities to 51000 ppm equivalent SiO*, while maintaining a Ca(II) content of =16 ppm in the finished effluent. Flotation concentrates of good quality were obtained using the reclaimed water. The cost of chemicals used in water reclamation was approximately equal to the savings in flotation reagents attributed to recycling of the water. Water quality is perhaps as important to flotation as are the reagents used. The character of water is extremely variable, depending on whether the source is a well, lake, or stream, upon the season and temperature, upon prior use, and upon the character of the watershed. All of these factors influence the water hardness and the quantity of other dissolved inorganic salts, turbidity, dissolved and suspended organic matter, dissolved gases, and pH. Frequently, the differences in water quality can measurably influence flotation selectivity, often to the point of spelling success or failure. Water hardness is particularly troublesome in flotation systems employing fatty acids, but other unrecognized constituents may also contribute to peculiarities in flotation behavior. Furthermore, a given water source may be entirely satisfactory in one flotation system, but entirely inappropriate in another. In recent years, society has given more attention than formerly to water use, even in areas where water is plentiful. However, both the demands of a growing population, with increased per capita needs, and also those of industry must be met. As a result, riparian rights must be negotiated with the appropriate government agency or agencies so that consumption of water is often allocated or otherwise controlled. Furthermore, the disposal of off-process industrial and domestic water is coming under the increasing scrutiny of these same governmental units. In these respects, the mineral industry is no exception, so that conservation, water reclamation, and reuse may be expected to assume increasing importance. In 1932, it was stated that, "water reclamation is generally more expensive than the economy in water and reagents resulting from its use. It is employed only if it is urgent to save water."&apos; The economic aspects of this statement may still be true, but the unrestricted use of water is becoming less and less an option of the user. The purpose of this paper is to discuss an investigation conducted by the U.S. Bureau of Mines (USBM), in which water reclamation and treatment were undertaken to develop procedures for, and to assess the effects of, water reuse on the flotation treatment of nonmagnetic taconites. This investigation is a logical extension of previous work described by the author and associates at the Twin Cities Metallurgy Research Center employing selective flocculation-desliming and anionic flotation of silica from low-grade, nonmagnetic iron ores2,8 The requirements for the selective flocculation-de-sliming and the anionic flotation of silica processes determined the direction of the investigation. Previous studies had indicated that pH levels of about 11.0 and 11.8 were required for selective flocculation and flota-tlon, respectively. The calcium content of the water was believed to be of importance in both of these operations, and since Minneapolis tap water with a Ca(I1) content of about 16 ppm had been successfully used, an attempt was made to reclaim the process water at an equal level of dissolved calcium. Additionally, the objective was to nullify or effectively limit the effects of dispersants and fatty acid residuals from prior stages of processing. Last but not least, the system of water treatment had to have the capability of reducing turbidities to workable levels. With about half of the effluent being derived from the selective flocculation-desliming step and carrying about 25,000 ppm of highly dispersed, suspended fines, this last objective appeared formidable at the outset. Procedures for water reclamation were derived, in part, from well-known mineral dressing practices, from past observations and investigations, and from concepts contained in various pertinent publications on water treatment."c These procedures involved: 1) flocculation with lime and poly electrolyte-type flocculants, 2) lime-soda-ash softening, 3) chemical precipitation, and 4) mineral surface adsorption. Control was exercised at various stages of water reclamation by frequent measurements of Ca(11), pH, and turbidity.

Jan 1, 1971

By A. S. Odeh

The mechanism of two-phase flow in porous media has been a subject of wide controversy. One of the properties essential for understanding the dynamic behavior of two-phase flow is relalive permeability. Relative permeability to a certain phase is defined as the ratio of the effective permeability of that phase to its permeability when it is the only fluid present and powing. In this research, a theoretical analysis was made to determine the effect of viscosity ratio between the non-wetting and the wetting phase on relative permeability. Experimental work was conducted to test the validity of the derived equations. The experiment was conducted on four natural cores. Four oils were used as the non-wetting phases with a viscosity range of 0.42 to 71.30 cp and two wetting phases with a viscosity range of 0.86 to 0.96 cp. Oil and bring were made to flow simultaneously at various ratios, and relative permeability curves were constructed. A total of eight relative pertileability cycles representing eight viscosity ratios were run oil each sample. It was found that relative permeability to the non-~cletting phase varies with viscosity ratio. The relative effect of this variation on relative permeability values was a function of the sample&apos;s single-phase permeability, decreasing with its increase. It was concluded that, for .samples of single-phase permeability over I darcy. the effect of viscosity ratio could be disregarded, and relative permeability would be, in effect, a function of satrtration only. INTRODUCTION Two-phase as well as multiphase flow occurs in many fields of science. This type of flow is of particular interest in petroleum production. The knowledge of relative permeability, which describes the dynamic behavior of two-phasc as well as multiphase flow, is essential for solution of problems arising in that field. Thc relative permeability ot a porous medium to a given phase in multiphase flow. is generally considered to be only a function of the saturation of that phase, independent of the properties of fluids involved and ranging in value from zero to unity. Work by Leverett&apos; and Leverett and Lewis&apos; apparently supports this concept. In his experiments Leverett used a clean, packed unconsolidated sand of high permeability (3.2 to 6.2 darcies) with two phases (water and oil) flowing and a viscosity ratio range of 0.057 to 90.0. His results showed that the wide range of viscosity had practically no effect on relative permeability-saturation relationship. Recently accumulated evidence from work performed by several laboratories and a paper by Nowak and Krueger,2 in which relative permeability to oil of a few core samples in the presence of interstitial water was considerably greater than single-phase permeability to water, cast some doubt on the conclusions reached by Leverett&apos; and subscribed to by a large number of individuals in the oil industry. One explanation advanced to explain this behavior states that it is caused by the variable extent of hydra-tion of clay minerals present in the sand. The greater the water saturation, the greater will be the area of contact between water and clay minerals; therefore, the greater will be the extent of swelling with corresponding reduction in permeability. Yuster4 presents another explanation for the recently accumulated evidence. Utilizing Poiseuille&apos;s law, he analyzed concentric flow in a single capillary where the non-wetting phase flows in a cylindrical portion of the capillary and concentric with it. The wetting phase flows in the annulus between the non-wetting phase and the capillary wall. The equations obtained indicate that relative permeability to the non-wetting phase is a function of saturation and viscosity ratio. Although Yuster&apos;s equations show that fractional rel-ative permeability to oil could be greater than unity, as was indicated by the data of Nowak and Krueger,1 they failed to present an explanation to the experimental data of early investigators such as Leverett.1 Due to the importance of relative permeability in understanding the flow behavior of petroleum reservoir fluids, this work—theoretical as well as experimental —was undertaken to determine whether relative permeability is a function of saturation only as was concluded by Leverett1 or a function of saturation and viscosity ratio as was theorized by Yuster.4 THEORETICAL ANALYSIS An equation will be derived for the rate of oil flow through a porous medium that is initially filled with water. Based on this equation, an analytic expression for relative permeability will be developed. The porous medium will be assumed to consist of .straight circular capillaries of different radii. It will also be assumed that there are no interconnections among the capillaries and no mass transfer across the oil-water interface. Consider a porous sample initially saturated with a wetting phase (water). As a non-wetting phase (oil) is

By Arnulf Muan, Klaus Schwerdtfeger

Equilibrium ratios C02/C0 of a gas phase coexisting with selected phase assemblages of the system Fe-Mn-0 have been determined in the temperature range 1000" to 1300°C. The oxygen pressure for the "hfnO" +hfn30, equilibrium and for the "(Fe,hTn)O" + (Fe,Mnh 0* equilibrium at high manganese contents has been determined by electromotive force measurements using stabilized zirconia as a solid electrolyte. The notstoichometry 01&apos; "hTnO" and of "(Fe, iM1z)O" solid solutions has been determined by ther-mog-/avi?netry and by wet-chemical analysis. The data obtained are used to derive activity-composition relations in "(Fe,hfn)O" and (Fe,Mn),O4 solid solutions. WUSTITE "FeO" and manganosite "MnO" form a continuous series of solid solution at high temperatures,&apos; and so do magnetite Fe304 and the high-temperature, cubic modification of Mn304 (Ref. 2) (high hausmannite, -1170). The oxides "FeO" and "MnO" are cation-deficient phases.495 The nonstoi-chiometry of "(Fe,Mn)O" solid solutions has been studied by Engell and ~ohl&apos; at two selected C02/C0 ratios at 1250°C. The two oxide end members of the spinel solid solution, FesO4 and Mn,04, however, are known to be close to stoichiometric under the experimental conditions used in the present investigation.&apos;&apos;&apos; The oxygen pressures of "(Fe,Mn)07&apos; solid solutions in equilibrium with iron have been determined by Schenck and coworkers,8 by Foster and welch," and by ~n~e1l.l&apos; The two former groups equilibrated the condensed phases in C02-CO atmospheres of lmown compositions, whereas Engell" used a galvanic cell with stabilized zirconia as a solid electrolyte. The results of these investigators are not in good agreement. Activities of FeO in manganowiistite as calculated from the results of Foster and Welch show ideal behavior, those of Engell yield a pronounced positive deviation, and those of Schenck et 01. show a moderate positive deviation from ideality. In the present work oxygen pressures for the iron + manganowiistite and manganowustite + spinel equilibria and the nonstoichiometry of manganowiistites have been measured. The data were used to calculate activities in the manganowiistite and spinel solid solutions. EXPERIMENTAL METHODS The COz/CO ratios at which manganowustite and iron are in equilibrium were determined by thermo-gravimetric and quenching methods. Experimental details are described in a previous publication.&apos;2 In the thermogravimetric technique, incipient reduction of manganowiistite pellets to metallic iron was observed as a break in the weight vs log COZ/CO curve. In the quenching technique, manganowiistite samples were partially reduced to metallic iron, or the metallic iron of manganowustite + metallic iron mixtures was partially oxidized to manganowustite, in atmospheres of constant C02/CO ratios. After quenching the composition of the oxide phase was determined by X-ray lattice parameter measurements and comparison with a standard curve obtained from oxide solid solutions of known compositions. The nonstoichiometry of "MnO" and "(Fe,Mn)07&apos; solid solutions was determined by chemical analysis of samples equilibrated in C02-CO atmospheres and quenched to room temperature, as well as thermo-gravimetrically by reducing (Fe,Mn),04 or Mn304 to manganowiistite or manganosite. The equilibrium between manganowiistite and (Fe,Mn),04 was measured thermogravimetrically by reducing (Fe,Mn),04 solid solutions having composition in the range of %„ l(NFe +NM) from 0 to 0.63. No experiments could be performed with this technique at higher manganese contents, because the equilibrium C02/C0 ratios are too large for accurate control. An additional difficulty arises at the higher manganese contents due to the strong increase in oxygen content of the manganowustite phase with increasing log Py near the manganowiistite-spinel boundary. Consequently a sharp break in the weight loss vs log C02/CO curve cannot be observed at the phase boundary. At high manganese contents of the manganowiistite, e.g., (NMn/(NF~ + NMn) > 0.9, electromotive force measurements with stabilized zirconia as a solid electrolyte were made to determine the equilibrium oxygen partial pressure. Experimental details are described in a previous paper.* Mixtures of "(Fe,Mn)O" and (Fe,Mn),04 were pressed to pellets, and the oxygen pressure of the equilibrated samples was compared to that of Ni + NiO mixtures in the cell The composition of the manganowiistite in the equilibrated two-phase mixture was determined by lattice parameter measurements and comparison with known standards. The oxygen pressure for the Ni + NiO equilibrium was taken from available data.l3~l4 No reliable results were obtained with the electromotive force technique on iron-rich oxides. The electromotive force drifted strongly with time in this composition range. An additional difficulty arises from the partial de-

Jan 1, 1968

By P. G. Shewmon, H. E. Collins

We have studied the effect of adsorbed sulfur on the surface self-diffusion of copper using eight diflerent surface orientations and the grain boundary grooving method. The eight orientations studied were the four lying near the low-index surfaces—(loo), (Ill), and two directions in the (110)-plus four higher-index surfaces. Surface-diffusion measurements were made over a range of HZS concentrations (in Hz) from 3 to 1500 ppm between 830°and 1050°C. The results can be divided into two groups—Group 1 contains the two (110) surfaces while Group 2 contains the remaining six surfaces. In Group 1, increasing the temperature increases the effect of Hz S on DS for the Hz S range 5700 ppvn. Qs and Do increase with increasing H2S concentration in this Hz S range. Beyond this range, increasing the temperature decreases this effect on D,; also Q, and Do decrease. In Group 2, increasing the telnperature decreases the effect of H2 S on D, for the H2S range studied, and Qs and Do decrease with increasing Hz S concentration. In any study of surface phenomena, there invariably arises the question of the possible presence of and effect of adsorbed impurities. Such questions are well-founded since the presence of adsorbed atoms can sometimes produce marked changes in the kinetics of surface-energy-driven processes. In the last few years, values of the surface self-diffusion coefficient, D,, have been determined on a variety of metals by studying the decay of scratches or the growth of grain boundary grooves.L~3-L0~L3 Yet there has been relatively little work done in which the concentration of an adsorbed impurity was systematically varied and the effects observed. Work of this sort would provide some basis in fact for the assertions often made about the ro1.e of adsorbed impurities in the differences between the results of different workers in different atmospheres and on different metals. It also is relevant to those cases in which surface monolayers produce profound effects in commercially important processes. The most marked example of such effects is the ability of nickel or palladium to increase the sintering rate of tungsten by many orders of magnitude.&apos; The aim of this work was to study the effect of sulfur partial pressures on the surface self-diffusion of copper. It was felt that this in conjunction with a study of the degree of adsorption and type of active sites involvedL8 would provide a wide range of data for one system and hopefully lead to some insight into the mechanism by which sulfur adsorption influences copper diffusion. The main reasons for choosing the Cu-S system were, first, faceting was reported not to accompany the adsorption of sulfur. This is required if our experimental technique is to work. Second, Oudar has determined a high temperature adsorption isotherm for this system, an event which puts the Cu-S system almost in a class by itself.I4 EXPERIMENTAL PROCEDURE Initially, we considered studying the effect of an adsorbed impurity on surface self-diffusion of copper using isolated (or single) scratch smoothing as the technique and oxygen as the impurity. Copper was chosen as the material because the effects of orientation and anisotropy of the surface self-diffusion coefficient, D,, of copper in a dry hydrogen atmosphere had been studied extensively by Gjostein&apos; and by Shewmon and ~hoi.~,~ The isolated scratch technique was chosen because both the effects of surface orientation and anisotropy of D, in a given surface could be easily studied with this method.~ Oxygen was tried as the impurity because Robertson and Shewmon""~ had studied its adsorption on copper at 1000°C over the range of oxygen partial pressures of 10"22 to 10-l3 atm. After several preliminary runs, it became evident that neither the scratch technique nor the impurity oxygen would be satisfactory for this work. Scratching deforms an annealed surface so that the region near the scratches recrystallizes, thereby disrupting the scratch profiles. One can avoid this by deforming the specimen sufficiently before scratching to give complete recrystallization on subsequent heating.4 However, as a result of Gjostein&apos;s success in scratching and annealing undeformed gold single crystals without local recrystallization,13 we attempted something similar with copper single crystals using a 0.7-mil diamond phonograph needle mounted in a Tukon hardness tester. All specimens recrystallized upon being annealed. Also, some copper specimens were sent to Gjostein to be scratched using his technique. The results were the same. As a result, the scratch technique was dropped in favor of the grooving of symmetric grain boundaries. Preliminary work using oxygen showed that faceting began to occur before oxygen adsorption had any measurable effect on D, at 938°C (at Pbo/P, = 0.12). Since heavy faceting would interfere with the measurement, we decided to use a sulfur-containing atmosphere (H2S/H2). Work by Oudar and Benard&apos; and Robertson" showed that sulfur absorbed on copper and that faceting was not observed.

Jan 1, 1967

By O. A. E. Jackson

Pebble milling has been practiced in the reduction works of South Africa gold mines for well over 50 years. Originally flint pebbles were imported from Denmark to grind stamp-mill amalgamation-process tailing, which contained a good deal of extractable gold, but local operators soon found that large pieces of ore could be used for the same purpose. The ore is a hard, tough conglomerate in which quartz pebbles are cemented together by a matrix of redeposited silica interspersed with pyrite crystals. The gold, rarely visible, occurs as fine particles mostly segregated at the interface of the pebble and matrix, although a small fraction occurs within the pyrite crystals. There is seldom any gold in the pebbles themselves. Following the usual South African practice in pebble milling, Union Corp. grinds the ore wet in two or three milling stages incorporating classification. The sized broken ore used as grinding media is separated from the main ore stream in the crushing section that prepares the ore for milling. Where the ore channel, or reef, is narrow there is a shortage of large pebbles. In this case primary grinding may be done in ball mills or, more recently, in rod mills, which cost less per ton to operate. The trend, however, is to prepare finer feed for the milling section. This makes it possible to use smaller primary pebbles and eliminates the need for steel. REDUCTION WORKS OF UNION CORP. LTD. Union Corp. Ltd. exercises financial and technical control over a group of seven gold mines in the Transvaal and Orange Free State. In the Transvaal, with one exception. the mines lie 20 to 40 miles east of Johannesburg, in flat or gently rolling countryside. Winkelhaak, the first of several new mines that will be developed by Union Corp., is located in similar terrain in an entirely new gold mining district about 80 miles east of Johannesburg. Table I gives details of milling units for six of the Union Corp. mines, together with the tonnage milled in 1957. Winkelhaak Mines Ltd. is not included, as it did not begin milling until 1958. This reduction plant has no crushing section; ore is ground directly from the mine (autogenously) in 12x16-ft mills. Because these operations are still in development, they are not described in this article. It will be noted that certain reduction works have mills of more than one size in the same milling stage. This came about when plant extensions in- corporated larger units. In the case of Geduld Propty. Mines Ltd., which began milling operations 50 years ago, the primary stage is stamp milling. The reduction works follow a uniform pattern and are usually joined to the main ore shaft. Ore from other shafts is brought by standard-gage railway and dumped into a common transfer bin. The trend is to increase surface storage capacity to enable the crushing and milling sections to operate at a steady rate, independent of fluctuating ore deliveries from mine. Milling and cyanide extraction divisions of new mines are always designed to allow for extensions as mine production increases. The conveying, washing, and screening system of the crushing section is usually laid out in final form, with additional space for more crushing equipment. The crushing sections operate on one shift during early years of mine production; a second shift is introduced when the mining rate warrants it. Ample surge capacity is provided. Crushing and milling is done only on weekdays, as the law does not allow these operations to take place on Sunday in any plants constructed since 1911. The cyanide extraction sections, however, operate continuously seven days a week, drawing on mill pulp gradually built up in the thickeners during the week. Construction and equipment of milling plants follow standard practice. Dilution water is drawn from a large, high-level tank to obtain constant pressure, but gland service water for the pulp pumps is reticulated from high-pressure, two-stage pumps. The mills are equipped with the most up-to-date machinery and are designed to save labor. They compare favorably with milling plants in countries where native labor does not exist, and automatic controls are being installed wherever feasible. Hydrocyclone classifiers have replaced mechanical classifiers in modern milling plants, chiefly because of the saving in capital outlay, maintenance, and building space. The hydroclones are fed from steady head boxes rather than directly from pumps, and dilution water is introduced into these boxes. Tests have shown that in steadiness of operation and separating efficiency cyclones are comparable to mechanical classifiers. but protective stationarv screens are needed to keep the spigots clear. Rubber-lined pumps are used for pulp of about 3 mesh or finer and metal-lined pumps for coarser material. None of the Union Corp. milling plants practices gravity concentration of coarse gold by amalgamation or the use of corduroy blankets. Studies have proved that no economic case can be made for these methods, which complicate the milling process and demand extra precautions against theft.

Jan 1, 1960

By R. L. Moment

The anisotropic elastic behavior of rolled beryllium sheet has been measured, using a pulse echo technique, and compared with X-ray diffraction data. Calculated elastic stiffness constants compared favorably with published values for beryllium single crystals which were attributed to the strong (0002) rolling plane texture. Variations of Young&apos;s modulus in the yolling plane could be associated with the velative distribution of (0002) planes out of their ideal position in the rollitzg pkule. WHEN a metal is subjected to cold working such as drawing, forming, or rolling, a crystallographic texture develops which can significantly alter its physical properties. One method for detecting this texture is X-ray diffraction, but Alers and Liu&apos; have recently pointed out how the prediction of anisotropic physical properties from pole figures alone is not always accurate due to differences in interpretation. Variations in Young&apos;s modulus with orientation or, more completely, the values of the effective elastic constants of the worked metal, also serve to indicate the presence of a texture. In fact, as Alers and Liu&apos; pointed out, calculated variations in Young&apos;s modulus for assumed orientations, when compared with experimental data, can be used to eliminate some of the uncertainty in interpretation of X-ray pole figures. Thus, elasticity measurements can serve not only to clarify any unusual elastic behavior of worked metal, but also to detect and in part determine the nature of its texture. X-ray determination of the texture of rolled beryllium has been reported by Smigelskas and Barrett,2 who found a strong texture of (0002) in the rolling plane with (1070) planes normal to the rolling direction. In the case of metal rolled at room temperature, they reported that [1010] directions also appeared at positions 60 and 120 deg from the rolling direction in the rolling plane, while in more recent work Keeler3 found these directions were also tilted towards the rolling plane. The texture for beryllium rolled at 80O0C, however, only showed (1010) planes normal to the rolling direction and the spread of (0002) planes out of the rolling plane was less. In looking for elastic anisotropy one might consider unidirectional rolling of a metal as introducing an or-thorhombic symmetry through reorientation of the grains, since the three deformations, compression, extension in the rolling direction, and extension in the cross direction, are orthogonal to each other and unequal in magnitude. Thus the rolled sheet could be treated like an orthorhombic single crystal and the nine stiffness constants of the elasticity tensor used to calculate the anisotropy of Young&apos;s modulus, the shear modulus and Poisson&apos;s ratio. In this case we could write: which is symmetric about its diagonal. Borik and Alers4 have recently used this approach on rolled die steel with very good results. They found, however, that instead of displaying orthorhombic elastic symmetry their specimens could be considered tetragonal in which case Cr1 = c22, c13 = Ca, and c44 =cjj. This conclusion was made solely on the basis of the measured tensor elements, and serves to point out the advantage of this method for studying the anisotropy of rolled metals. Their calculated values for Young&apos;s modulus as a function of angle in the rolling plane also checked very well with direct measurements made on different specimens using the resonance technique. In the present study, cross-rolled beryllium was used which had been unidirectionally rolled about 11 pct for the final reduction. This imparted a slight anisotropy in the rolling plane which was detected both by X-ray techniques and elasticity measurements. For purposes of discussion in this paper, the rolling direction is that direction in which the most reduction passes were made and cross direction is the normal to the rolling direction in the rolling plane. It was also decided to consider the rolled sheet as displaying orthorhombic symmetry for the purpose of obtaining elasticity samples with the direction defined as in Table I. Any change in the final symmetry attributed to the sheet would then be made on the basis of the measured elastic stiffnesses. The final data would then be compared with that expected from the X-ray study and that reported for beryllium single crystals. EXPERIMENTAL PROCEDURE Rolling Schedule. The samples used in this study were taken from a large sheet which, because of its size, had to be unidirectionally rolled for the final reduction. The resulting texture was that of cross-rolled metal with a slight unidirectional texture superimposed. A cast beryllium ingot, 9.500 in. sq by 3.325 in. thick, was cross-rolled to 81 pct reduction followed by unidirectional rolling for an additional 11 pct to give a total reduction of 92 pct. The thickness of the final sheet ranged from 0.265 to 0.280 in. Reduction up to 67 pct was done at 980°C and the final 25 pct at 870°C. Analysis for metallic impurities showed aluminum 0.06 pct, iron 0.19 pct, and silicon 0.11 pct, giving a beryllium purity of 99.64 pct.

Jan 1, 1968

By James C. M. Li

The Petch relation between the flow stress and the gain size is derived from a consideration of gain boundary sources of dislocations without the need of dislocation Pile-ups. Three mechanisms for inierpreting the yield stress: the gain boundary strength, the unpinning of Frank-Read source near a grain boundary, and the generation of dislocations from the grain boundary are compared and the condition of their equivalence is shown. The effect of the average angle of misfit of pain boundaries is found to be sma11 and so is that of the average angle of misfit of subboundaries having impurities. The effect of impurities on the ledge density in the grain boundary is treated thermodynamically and a relatwn is proposed for the variation of Petch slope with impurity activity. The effect of temperature on the Petch slope is interpreted as due to the change of ledge structure in the grain boundary. It is indicated that the effect of annealing temperature may be more important than that of the test temperature and therefore should be studied. The effect of plastic strain on the Petch analysis is deduced from a work-hardening equation in which the generation of dislocations has first-order kinetics and the annihilation of dislocations has second-order kinetics. It is concluded that the Petch slope will decrease with plustic strain if the rate of annihilation of dislocations is sufficiently large. Critical experiments which may shed light on the mechanism for the Petch relation are suggested. THE relation between the yield or flow stress, 0, and the grain size, l, was first proposed by all&apos; and later studied more extensively by Petch and co-workers, who also proposed a similar relation for the fracture stress and deduced from these a grain-size effect of the ductile-brittle transition temperature. The microscopic mechanism used by all&apos; and petch2 involves a pile-up of dislocations of like sign generated from a Frank-Read source. The yielding or flow takes place when the pile-up exerts sufficient stress at the grain boundary so that the plastic deformation can propagate from one grain to another. If the average strength of the grain boundary is ai and the average length of the pileup is lp, the Petch slope, k, is given by" where p is the shear modulus, b the Burgers vector, and v the Poisson ratio. This slope will be independent of the grain size if l/lp is a constant. This is possible, since, if the Frank-Reed source is situated near the grain boundary, lp = 1, and if it is situated in the middle of the grain, Ip = 1/2. cottrell,12 also using the pile-up mechanism, proposed that the stress concentration at the grain boundary will initiate Frank-Read sources near the grain boundary and in this manner a Lüders band can propagate from one grain to another. Assuming that the average distance between the Frank-Read sources and the grain boundary is 1, and the unpinning stress of the Frank-Read sources is op, Cottrell obtained the following Petch slope: This slope will be independent of the grain size if ls is independent of the same, which is not as obvious as the condition, Ip = I for Eq. [2]. In addition to this assumption, the direct relation between the Petch slope k and the unpinning stress, up, was recently questioned by Johnsonon grounds that it is inconsistent with the following observations: the independence of k with temperature and strain rate, and the small k in columbium, which, like iron, has a sharp yield point. As pointed out by ohnson," the most important objection both to the Hall-Petch mechanism, in which the strength of the grain boundary plays the role in yielding, and to the Cottrell mechanism, in which the unpinning of Frank-Read sources plays the role in yielding, is the lack of direct observation of the pile-ups. The dislocation structure in deformed iron has been examined recently in the electron microsope.&apos;-&apos; Dislocations appear to be generated from grain boundaries or other interfaces; they form clusters and tangles within the grain at very early stages of deformation, even in the Lüders band, if the deformation is slow or at normal and elevated temperatures. Although it is still too early to interpret bulk properties from thin-film observations, it does seem worthwhile to look for a mechanism for the Petch relation which does not require dislocation pileup. SUBBOUNDARY SOURCES In order to show that a consideration of grain boundary sources can lead to the same Petch relation as does the consideration of the strength of the grain boundary, we shall first discuss the case of a simple tilt boundary whose elastic properties have been studied in detail.17 The strength of a partially

Jan 1, 1963

By H. H. Podgurski, H. E. Knechtel

Annealed Fe-Al alloys do not react readily to form AlN when held at 500ºC in NH3-H2 gas mixtures, but do so upon the introduction of dislocatims. Nuclea-tion of the nitride phase occurs on dislocation sites. In turn, the growth of the aluminum nitride particles causes the ferrite phase to yield plastically, generating more dislocations for the nucleation process. The nitride phase extracted from an Fe-2 pct A1 alloy nitrogenated at 500°C was identified as stoichio-metric aluminum nitride with a hexagonal crystal lattice. THIS investigation reveals the role that dislocations play in initiating and sustaining the nitriding reaction in Fe-A1 alloys. As early as 1931 the work of Meyer and Hobrock1 suggested that the initiation of the nitriding reaction could involve a nucleation controlled process. Recently Bohnenka2 depicted the gas-phase nitriding process below 600°C as one of mixed control limited by nitrogen penetration through the surface, by nitrogen diffusion, by aluminum diffusion, and by nucleation of the nitride phase, Fig. l(a). In our research in a comparable alloy (0.57 pct Al) at 575ºC, we have observed a nitrogenation which we feel is better described by Fig. l(b). In the case of a 2 pct-A1 alloy partially nitrided at 500°C we propose the profiles shown in Fig. l(c). For a complete and accurate description of the process, a concentration profile of the dislocation density in the test specimen would be needed. EXPERIMENTAL Nitrogenization was conducted between 500" and 575°C in a variety of NH3-H2 gas mixtures on three Fe-A1 alloys: 1) zone-refined iron + 0.16 i 0.2 pct Al—levita-tion melt, 2) zone-refined iron + 0.57 0.02 pct Al— levitation melt, 3) plastiron + 2 pct Al—melted by induction heating. To demonstrate the effect of dislocations on reactivity, both cold-worked and annealed samples were investigated. All nitrogenation rate studies were conducted gravimetrically with a gold-plated invar balance4 contained in a gas-flow system. To avoid contamination of the specimens in the reaction zone of the system, the reaction chamber was constructed of high-purity dense alumina. The activity of nitrogen was fixed by specific NH3-H2 gas mixtures whose compositions were continually monitored by calibrated thermal conductivity gages and checked by chemical analysis. Variations of ± 0.1 pct NH3 could easily be detected by both methods. Throughout this paper the activity of nitrogen is defined as PN3 /PH23/2 , where PNH3, and Ph2 are partial pressures in atmospheres. Electron transmission, density measurements, and chemical analyses were made on specimens before and after nitrogenating in order to reveal structural and chemical changes. Similar studies as well as X-ray diffraction studies were conducted on nitride extractions from the nitrogenated 2 pct-A1 alloy. These extractions were obtained by the use of an anhydrous bromine-methyl acetate solution which dissolves the iron and leaves the insoluble nitrides as a residue. Hardness profiles were obtained on cross-sections of partially nitrided specimens to demonstrate the extent of nitriding through the thickness of the specimens. RESULTS AND DISCUSSION The nitrogen activity in the NH3-H2, atmospheres was never allowed to reach a level capable of producing iron nitride (Fe4N). Hence, the term nitriding as used in this paper refers only to the formation of aluminum nitride whereas nitrogenation refers to the total uptake of nitrogen regardless of how it is distributed throughout the alloy. The weight increases observed during the initial stage of a nitrogenating treatment are due primarily to the solution of nitrogen in the ferrite phase, particularly when starting with annealed specimens. Because this initial nitrogenation rate in the case of the 0.57 pct A1 alloy, see Figs. 2 and 3(a), was most rapid the weight change that occurred thereafter might be attributed to the nitriding reaction with the exception of a small weight increment due to the irreversible pickup of oxygen by aluminum. The oxygen (<70 ppm) came from traces of H2O and 0, in the hydrogen and ammonia gases. On the basis of discrepancies between total weight increase and the increase in the nitrogen content of the sample as determined by chemical analysis, it was estimated and later established by activation analysis, that as much as 200 ppm of oxygen were taken up by a fully nitrided Fe-0.57 pct A1 specimen at 575°C. Most of the oxygen could have been picked up from the nitriding atmosphere on the surface of the samples during cooling to room temperature. Even 50 ppm of water in the gas phase will become oxidizing to iron before the sample has cooled to room temperature. The lack of reactivity* of these alloys in the annealed

Jan 1, 1970

By C. L. Prokop

A laboratory investigation has been made of the effects of mud hydraulics upon the formation and erosion of mud filter cakes. The tests were conducted to simulate drilling conditions as nearly as possible. The formation of mud filter cake in a drilling well does not proceed at a uniform and unbroken rate. Instead, the rate of cake accumulation depends upon whether or not the mud is being circulated. If the mud column is quiescent, filter cake formation is a smooth function of the filtration characteristics of the system. If the mud is being circulated filter cake formation depends not only upon the filtration characteristics of the mud but also upon the erosive action of the flowing mud column Filter cakes formed during continuous mud circulation were observed to reach an equilibrium thickness after several hours&apos; circulation. Mud circulation was maintained at a constant volumetric rate throughout each experiment. The fluid velocity at equilibrium cake thickness was dependent upon the thickness of the filter cake. Muds having exceptionally high water loss deposited thick filter cakes in spite of very high eroding velocities. The muds having good filtration characteristics deposited thin filter cakes at equilibrium circulating velocities well within tile range of those in a drilling well. It was observed that filter cakes deposited during stagnant filtration were quite difficult to erode by mud circulation. The - rate of crosion computed from the rate of filtrate accumulation after equilibrium cake thickness had been reached was in reasonable agreement with the rate of erosion obtained by direct observation. Continuous mud circulation usually caused the permeability of the filter cake to decrease with time. INTRODUCTION Many of the difficulties encountered during tile drilling of a well have been attributed to the loss of water from the mud and the attendant deposition of solids upon the walls of the hole. Past experience has shown that a reduction of the filtration rate of the drilling fluid eliminates or greatly reduces these difficulties. Definite filtration requirements, however, are hard to establish for a given set of conditions. This is due. in part, to the fact that the usual filtration test performed upon mud doe? not simulate well conditions as closely as desirable. The filtration characteristics of a mud are customarily determined by means of the standard low-pressure API wall-building tester.&apos; In this instrument a filter cake is deposited upon a horizontal bed under a pressure differential of 100 psi. The rnud is quiescent during the filtration period. In actual practice. mud filtration occurs within a well under quite different conditions. One of the major differences is that mud flows upward across the filter bed as the filter cake forms. This undoubtedly produces a change in the filter cake which cannot be reflected in the results of the API test. The laboratory work described in this paper had as its primary objective a better understanding of the influence of mud circulation upon the thickness and ,characteristics of the filter cakes deposited under conditions similar to those existing in a drilling well. ANALYSIS OF PROBLEM Once a permeable formation is penetrated by the bit, filtrate from the mud flows into the formation. &apos;he mud solids plaster against the walls of the hole, forming a filter cake. If the mud column is stagnant, that is, if it is not being circulated. the filter cake will increase in thickness until the hole is filled. Prior to the time that the hole is filled, the thickness of filter cake existing at any given time will be a function of the filtration characteristics of the mud, the temperature, and the pressure differential. The effects of these variables have been investigated in the past for both flat bed filtration2&apos;3 and for radial filtration.&apos; When the mud is circulated in a hole in which a filter cake i. being deposited. some of the solids that would ordinarily deposit in the filter cake will be carried away by the eroding action of the mud. This will limit. filter cake thickness. Some work has been done to determine the effect of flow upon the filtration rate in a circulating mud system&apos; but little work has been done upon the factors which determine the filter cake thickness existing in a circulating system. On first sight it would appear that the major factors controlling filter cake formation in a circulating system should be: 1. The rate of deposition of solids from the mud. 2. The erosive force that the flowing mud exerts upon the filter cake. &apos;A. The erodabilitv of the filter cake. 4. Any change in filter cake characteristics attributable to the scouring action of the mud. The rate at which solids are deposited from the mud will be controlled to a large degree by the filtration characteristics of the mud, the pressure differential. the temperature under

Jan 1, 1952

By D. E. Coates, G. R. Purdy, S. V. Subramanian

The morphological stability of the planar solid-liquid interface in dilute ternary alloys, undergoing steady-state unidirectional solidification, is analyzed in terms of both the constitutional supercooling principle and the perturbation methods recently developed by Mullins and Sekerka. First, various steady-state solutions for the two solute distributions ahead of a planar interface are examined. The nature of the solutions depends on the size and concentration dependence of the off-diagonal diffusion coefficients. W~thin the framework of the constitutional supercooling principle, a cumulative contribution to instability frorn the two solutes is found to exist in the absence of diffusional interaction. It is shown that the latter can produce a further enhancement of instability or can have a stabilizing influence, depending on the form of the liquidus surface and on the sign of the solute-solute interaction. A perturbation analysis, which ignores diffusional interaction, verifies the cumulative influence of lhe solute fields and demonstrates that the Mullins-Sekerka stability criterion for binary systems (with capillarity accounted for) can be readily extended for application to ternary systems. SOME time ago, Tiller et al.&apos; calculated the solute concentration distribution ahead of the planar solid-liquid interface of binary alloys undergoing steady-state unidirectional solidification. An earlier qualitative proposal that the transition from planar to nonplanar growth morphologies is associated solely with the onset of constitutional supercooling in the liquid layer ahead of the moving interface2 was used in conjunction with this calculation to put the now well-known constitutional supercooling (C-S) stability criterion into quantitative terms. Mullins and Sekerka,3 in a recent and very elegant analysis, established a more complete criterion (hereafter referred to as the M-S criterion). Interfacial stability was investigated by determining the time derivative of the amplitude of a sinusoidal perturbation of infinitesimal amplitude which had been introduced into the originally planar shape of the moving interface. Of particular importance is the fact that capillarity was included in the boundary conditions of their calculation. The purpose of the present paper is to extend all of this earlier work on dilute binary systems for application to dilute ternary alloy solidification. The analysis is divided into three sections. In the first the two solute distributions ahead of a moving planar interface are considered. Mathematical solutions are de- termined for situations in which: a) diffusional interaction is negligible, 6) diffusional interaction must be considered but circumstances permit use of constant diffusion coefficients, and c) the concentration dependence of off-diagonal diffusion coefficients can be described by first-order dilute solution approximations. In the next section, a stability criterion analogous to the C-S criterion is developed and the influence of diffusional interaction on interface stability is analyzed. Finally, the perturbation formalism of Mullins and Sekerka, with capillarity included in the boundary conditions, is extended for analysis of ternary systems in which diffusional interaction is negligible. The study of interface stability in binary systems usually commences with the assumption that the equilibrium distribution coefficient and the slope of the liquidus line are constant at values corresponding to infinite dilution. Similar assumptions have not been introduced into the present treatment; that is, we do not assume planar solidus and liquidus surfaces joined by tie lines which yield constant distribution coefficients. The latter involves the assumption of no ther-modynamic interaction between solute species in both the solid and liquid. We consider a ternary phase diagram for which the solidus and liquidus surfaces are, in general, nonplanar and of course pass through the corresponding binary solidus and liquidus lines. These lines are not assumed to have constant slope. In the dilute regions we are concerned with, the following assumptions are made: i) The solidus and liquidus surfaces are of a form such that both the solidus and liquidus temperatures are monotonically varying functions of each solute concentration. ii) The tie lines are such that the equilibrium distribution coefficient of a given solute is greater than unity for every point on the solidus (or liquidus) surface or it is less than unity for every point. STEADY-STATE SOLUTE DISTRIBUTIONS IN THE LIQUID As will be demonstrated in the next section, a knowledge of the steady-state solute profiles is not a necessary prerequisite for the formulation of a ternary C-S stability criterion. However, in that details, such as the complete description of the equilibrium liquidus temperature profile, require an evaluation of the solute distributions, the overall treatment is enhanced if these distributions are determined. Consider a ternary system (solvent plus solutes 1 and 2) for which a planar solid-liquid interface is in unidirectional motion at constant velocity V. At this stage it is unnecessary to limit ourselves to dilute solutions. For a stationary frame of reference the generalized forms of Fick&apos;s equations are:

Jan 1, 1969

By M. R. Annis, P. H. Monaghan

The control of mud properties affords two practical means of tnitigating pipe sticking caused by differential pressure: (I) teducing weight and, therefore, differential pressure; and (2) reducing the friction berween the pipe and mud cake. This paper describes investigation of the second of these—the friction between the pipe and the mud cake. Friction between a steel plate and a mud cake, held in contact by a differential pressure, was measured in the laboratory while maintaining a constant area of contact. Experiments were performed to determine how this friction varied with changes in mud composition and with changes in experimental conditions such as the differential pressure, time of contact of plate and mud cake, and filter-cake thickness. It was found that the apparent coefficient of friction, or the "sticking" coeficient, was not a constant; instead, it increased with increased time of contact between plate and mud cake, and with increased barite content of the Mud. The sticking coeficient varied from about 0.05 to 0.2 afer 20 , and eventually reached values of 0.1 to 0.3 after two Hours. Quehracho or ferrochrome lignosulfonate reduced the sticking coefficient at short .set times but did not reduce the maximum value. Carboxy-~t~etlz~lcellulose had no effect on the sticking coeficient. Emulsification of oil in the mud reduced the sticking coefficient. Some oils reduced the sticking coefficient to about one-third of its Value in the oil- free base mud, while other oils reduced it only slightly. Addition of certain surfactants with the oils further reduced the sticking coefficient. Spotting a clean fluid over the stuck plate caused a reduction in sticking coefficient only if the differential presslrrr was reduced, either temporarily or- permanently. INTRODUCTION Often during drilling operations the drill string becomes stuck and cannot be raised, lowered, or rotated. This condition can be brought about by a number of causes, such as sloughing of the hole wall, settling of large particles carried by the mud, accumulation of mud filter cake during long stoppage of circulation and, finally, sticking by pressure of the mud column holding the pipe against the filter cake on the hole wall. This paper is concerned with the last-mentioned phenomenon. Helmick 2nd Longley&apos; in 1957 suggested that a pressure differential from the wellbore to a permeable formation covered with mud cake could hold the drill pipe against the borehole wall with great force. This situation occurs when a portion of the drill string rests against the wall of the borehole, imbedding itself in the filter cake. The area of the drill pipe in contact with filter cake is then sealed from the full hydrostatic pressure of the mud column. The pressure difference between the mud-column pressure and the formation pressure acts on the area of drill pipe in contact with the filter cake to hold the drill pipe against the wall of the borehole. Helmick and Longley also presented laboratory cxperiments which showed that the force required to move steel across a mud cake increased with increasing differential pressure and with the time the stcel and mud cake had been In cuntact. Their data indicated that replacing the bulk mud with oil reduced the force required for movement. Field evidence was rcported that spotting oil over the stuck interval sometimes freed the pipe. Outmans- in 1958 presented a theoretical paper which described the sticking mechanism and explained the increase of sticking force with time with equations derived from consolidation theory. Since publication of these papers, there has been interest in the differential pressure sticking of drill strings, and several mud additives to reduce sticking or special equipment to free stuck pipe have been proposed."" Haden and Welch" have recently reported laboratory evidence showing that the composition of the filter cake influences the force necessary to move steel on the filter cake. There seems no doubt that differential pressure sticking is a real phenomenon and that its severity depends on the magnitude of the pressure differential across the mud cake, the area of contact and the friction between pipe and mud cake. The mud weight required to control a well is determined by the highest formation pressure in the well: hence, the magnitude of the differential pressure opposite normal or subnormal pressure formations cannot bc reduced. The area of contact may be minimized in several ways (control of filter-cake thickness, use of stabilizers and spirally grooved drill collars), but there arc practical limitations which prevent reduction of contact area from becoming a complete solution of the problem. However. the mud composition might bc altered to reduce the friction between pipe and mud cake. This paper presents quantitative measurements of the friction between steel and mud filter cake and shows how the friction varies with mud composition for given experimental conditions.

By Lloyd Pollish, Robert N. Breckenridge

SUCCESS in any underground mining operation is determined by accessibility of the orebody, which in turn is dependent upon maintenance of passageways to the mining zones and temporary support of the voids caused by extraction of ore. This is accomplished by one or a combination of the following methods: timbering, back-filling, pillaring, or, more recently, rock bolting. Timbering has usually been the principal means of maintaining these underground openings necessary for mining operations. Timber, however, does not prevent ground movement beyond the scope of localized sloughing, which is indicated by the gradual failing of the timber itself. Besides this, timbering has always been a costly process, and with the decline of available supplies of timber close to the mining areas, mining men have constantly sought other methods of controlling ground. Rock bolting is now replacing timbering at an ever increasing rate. Experience has proved that this form of ground support is just as applicable to blocky igneous rock as to stratified rock. Besides preventing sloughing of the walls and back of underground openings, Fig. 1, rock bolting has a stabilizing effect on the surrounding ground in much the same manner that steel reinforcing rods add to the strength of concrete structures. Further, rock bolting is flexible and may be applied to any shaped excavation, whereas timber sets are in a fixed pattern and the ground must often be changed to conform with this pattern. Rock-bolting installations were made in metal mines of the Northwest as early as 1939. An exhaust air crosscut was driven that year in one of the Butte mines of the Anaconda Copper Mining Co. The crosscut was rock-bolted and gunited at the time it was driven and is still being used to exhaust hot humid air from the 3400 level of the Belmont mine. It is interesting to note that no sloughing or caving has taken place in the 14 years it has been open. Even though these early installations of rock bolts were successful, few men recognized their potentiality until recent years, when the coal mines started their programs of mechanization and the great trend toward roof bolting began. In some areas of the Northwest stopes that previously required heavy timbering and close backfilling are now being mined by the more economical cut-and-fill and shrinkage methods. When used in conjunction with timbering, rock bolting increases the efficiency of the operation by decreasing hanging wall dilution and by making it possible to blast larger rounds. Most of the rock bolts installed to date in mines of the Northwest have been the 1-in. diam slot and wedge type, but there has been a recent trend to- ward using the 3/4-in. diam expansion shell bolt shown in Fig. 2. In addition to these commercially manufactured steel bolts, wooden bolts have been used with considerable success by the Day Mines of Wall&apos;ace, Idaho. Installation of the slot and wedge type requires three distinct operations, with tools for each operation: 1—drilling the hole to proper diameter and depth, 2—setting the bolt, and 3—tightening the nut. Holes are drilled and bolts set with pneumatic rock drills. A number of setting or driving tools have been used successfully, but most follow the same general pattern. Usually the driving tool is designed to accommodate a short length of drill steel on one end and the rock bolt on the other end. In this manner the hammering effect of the rock drill is transmitted through the steel and driving tool to the bolt. When machines not having stop rotation are used, slippage is allowed between the driving tool and bolt or between the drill steel and driving tool. The rock bolt nuts are tightened either with pneumatic impact wrenches or with hand wrenches. Impact wrenches are desirable because they are faster and assure adequate tightness. Expansion shell bolts have the following advantages over slot and wedge rock bolts: 1—No special equipment other than a wrench is needed for their installation. 2—Installation is faster. 3—They are removable. 4—Holes need not be drilled to a specific depth as the expansion shell will anchor anywhere along the length of the hole. These advantages are offset somewhat by the lesser strength of the bolt, since expansion shell bolts are generally made from 3/4-in. diam steel as compared to 1-in. diam steel for the slot and wedge type. One manufacturer, however, is now fabricating expansion shell rock bolts from steel of high tensile strength, which gives this ¾-in. bolt a much greater strength than that of the mild steel bolt. Table I illustrates tests made by the Anaconda Copper Mining Co. to determine the proper hole size to use with various types of bolts and to determine

Jan 1, 1955