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By P. Dosmond

In ore mining technology, the loading and hauling operations are undoubtedly the area where the most spectacular progress has been made during the last twenty years. In the iron ore mines of Eastern France production of 62 million tons for 1962 and 19863 constitute a worthwhile experience worldwide. These deposits which are located in Lorraine are of sedimentary origin and they contain many mineralized horizons with workable seams varying in depth from 330 to 830 ft.

Jan 1, 1970

By L. B. Pankratz

Enthalpies above 298° K were determined for AgCl to 1,400° K and for AgBr to 1,200° K by copper-block calorimetry. Before melting, both compounds showed an anomalous increase in enthalpy, an effect associated with lattice defect formation. Melting points and heats of fusion were determined to be AgCl, 730° K and 2,945 cal/mole; AgBr, 700° K and 2,030 cal/mole. The heat capacity of both melted substances decreased with increasing temperature over the entire liquid ranges investigated. Enthalpies above 298° K were tabulated at even temperatures along with derived entropy increments and heat capacity values. The results were combined with the known heats of formation and entropies at 29.8.15° K to obtain values of the heats and free energies of formation over the range 298.15° to 1,400° K for AgC1 and 298.15° to 1,200° K for AgBr.

Jan 1, 1970

By M. Metzger, J. C. Bilello

Microyielding in 99.999 pct Cu occuwed in two distinct parabolic microstages and was substantially indeoendent of grain size at the relatiz~ely large grain sizes stzcdied. The strain recouered on unloading was a significant fraction of the forward strain and was initially higher in a copper-coated single crystal than in poly crystals. Results were interpreted in terms of cooperative yielding and short-range dislocation motion activated otter a range of stresses, and a formalism was given for the first microstage. It was suggested that models involving long-range dislocation motion are more appropriate for impure or alloyed fcc metals. THERE are still many unanswered questions concerning the degree and origin of the grain size dependence of plastic properties. In the microstrain region, a theory of the stress-strain curve proposed by Brown and Lukens,' based on an exhaustion hardening model in which the grain boundaries limit the amount of slip per source, accounted for the variation with grain size of microyielding in iron, zinc, and copper.' This theory assumes N dislocation sources per unit volume whose activation stress varies only with grain orientation. Dislocations pile-up against grain boundaries until the back stress deactivates the source, which leads to a relationship between the axial stress and the strain in the microstrain region given by: where G is the shear modulus, D the grain diameter, a the flow stress, and a, is the stress required to activate a source in the most favorably oriented grain.3 If this or other grain-boundary pile-up models are correct, then the reverse strain on unloading would be much larger for a polycrystalline specimen than for a single crystal. Also, the microplasticity would become insensitive to grain size if this could be made larger than the mean dislocation glide path for a single crystal in the microregion. These questions are examined in the present work on polycrys-talline copper and a single crystal coated to provide a synthetic polycrystal. EXPERIMENTAL PROCEDURE Tensile specimens 3 mm sq were prepared from 99.999 pct Cu after a sequence of rolling and vacuum annealing treatments similar to those recommended by Cook and Richards4-6 to minimize preferred orientation. Grain size variation from 0.05 to 0.38 mm was obtained by a final anneal at temperatures from 310" to 700°C. Dislocation etching7 revealed pits on those few grains within 3 deg of (111). For all grain sizes dislocation densities could be estimated as -107 cm per cu cm with no prominent subboundaries. The single crystals, of the same cross section, were grown by the Bridgman technique with axes 8 deg from [Oll] and one face 2 deg from (111). An anneal at 1050°C produced dislocation densities of 2 x 106 cm per cu cm and subboundaries -1 mm apart in these single crystals. A Pb-Sn-Ag creep resistant solder was used to mount the specimens, with a 19 mm effective gage length, into aligned sleeve grips fitted to receive the strain gages. All specimens were chemically polished and rinsed8 to remove surface films just prior to testing. The synthetic polycrystal was made by electroplating a single crystal with 1 µ of polycrystalline copper from a cyanide bath. Mechanical testing was carried out on an Instron machine using two matched LVDT tranducers to measure specimen displacement, the temperature and the measuring circuit being sufficiently stable to yield a strain sensitivity of 5 x 107. At the crosshead speeds employed, plastic strain rates were, above strains of 10¯4, about 10¯5 per sec for polycrystalline specimens and 10-4 per sec for the single crystals. Plastic strain rates were an order of magnitude lower at strains near l0- '. A few checks at strain rates tenfold higher were made for reassurance that the initial yielding of polycrystalline copper was not strongly strain-rate dependent. Test procedures followed the general framework outlined by Roberts and Brown.9,10 An alignment preload of 8 g per sq mm for polycrystals, and 2 to 4 g per sq mm for single crystals, was used for all tests. These gave no detectable permanent strain within the sensitivity of the present experiments; although at these stress levels, small permanent strains are detectable in copper with methods of higher sensitivity.11 12 stress and strain data are reported in terms of axial components. RESULTS General. The initial yielding is shown in the stress vs strain data of Fig. 1. For polycrystals, cycle lc, the loading line bent over gradually without a well-defined proportional limit, and almost all of the plastic prestrain appeared as permanent strain at the end of the cycle. The unloading curve was accurately linear over most of its length with a distinct break indicating the onset of a significant nonelastic reverse strain at the stress o u, indicated by the arrows. The yielding in subsequent cycles, Id and le, had the same general character. The single crystal behavior, shown to a different scale at the right of Fig. 1, was different in that initially the nonlinear reverse strain was unexpectedly much greater than for polycrystals. It should be noted that these soft crystals had a small elastic

Jan 1, 1970

By H. V. Fairbanks

This report covers a study of three different methods for drying ultrafine coals by sound waves. Ultrafine material is classified as coal which passes through a 100-mesh sieve. During the investigations, it was found that the addition of acoustic radiation to the drying of ultrafine coal is effective in increasing the rate of drying; the effect of acoustic radiation to improve drying decreases with an increase in the temperature of the system; the drying rate increased 10-40% when acoustic radiation was introduced into a rotary kiln but was dependent upon the environmental conditions; the application of vertical vibrations to multi-tiered drying screens increased the rate of moisture removal ten times over that obtained in the rotary kiln; the formation of coal balls in any of the drier systems retards the rate of drying; the higher the initial moisture content of the coal the greater the amount of coal balls formed.

Jan 1, 1970

Jan 1, 1970

By John V. Beall

If there is one thing that makes a fellow feel like the years are catching up with him, it is to go through a second cycle in which the adequacy of mineral resources is being "viewed with alarm." The first time we experienced such a flap was in 1951. At that time, the United Nations convened a meeting at Lake Success to study ways and means of averting a crisis in minerals. Presently there is some sentiment being expressed about the mineral scarcities that will occur in the decades ahead, in view of world population trends and increasing per capita consumption of metals. To be greatly concerned about the adequacy of metal supplies is to be highly pessimistic about the capabilities of technology. As in the past, shortages will be of temporary duration for as far ahead as the most ambitious prognosticators are projecting. The study of mineral economics is a fascinating and surprising subject. The law of supply and demand is but a starting point. The iron ore market for the steel industry is an example which comes to mind because of our receipt this week of the United Nations report "Survey of World Iron Ore Resources."

Jan 1, 1970

By C. J. Lewis

Considerable amounts of the world's known reserves of elemental sulfur are found near the surface in areas of volcanic activity both active and inactive. Because such deposits cannot in general-be mined by the well-known Frasch process, and because other methods of recovery have not proven to be economically competitive except in isolated instances, at present these reserves remain relatively undeveloped. However, projections of world sulfur demand indicate that new sources of marketable sulfur will be needed in future years 2/, 19/. For this reason, recovery of elemental sulfur from these near-surface deposits is of continuing interest. Solvent extraction as an approach to recovery of elemental sulfur from open pit-mined ores of these non-Frasch deposits has received considerable attention particularly at the research and development level 3 /, 7/, l l /, 16/, 21/,23/, 29/ This method has been and continues to be attractive because it presents the potential of high sulfur recovery and purity of product coupled with a relatively simple process flowsheet in which low energy requirements and reasonable operating costs are thought to be possible. However, the physical and chemical characteristics of the native-sulfur ores, of elemental sulfur, and of the known solvents, have presented difficulties in the development of solvent extraction processes. Up to the present time, viable processes have not been realized within the framework of sulfur marketing conditions.

Jan 1, 1970

By L. C. Noakes

Despite a long history of mining. Australia had no Commonwealth organization dealing specifically with the mineral industry until 1946, when the Australian Bureau of Mineral Resources, Geology and Geophysics was established. Once formed, this new organization quickly expanded to include a Mineral Economics Section, which was established in 1947. Australia's slowness to develop a Federal bureau for the mineral industry can best be explained in the light of her political history. From a group of British crown colonies, Australia evolved into six sovereign states which had no unified federal government until they formed the present Commonwealth in 1901.

Jan 1, 1970

By Robert W. Gordon

The art of excavating tunnels with continuous, full-face boring machines began almost 90 years ago, in the early 1880's. At this time, Colonel Beaumont designed and manufactured a seven-foot diameter tunneler for boring under the English Channel, Despite the absence of modern materials and manufacturing techniques, Beaumont's tunneler, powered by compressed air piped in from the surface, was quite successful. During its short, but impressive existence, this machine set a record of advancing in chalk 50 feet per day for 53 days - which is impressive even by today's standards. Despite the apparent success of this early tunneler, almost 80 years passed before any further significant development was accomplished in this field. Demands from the construction and mining industry and society itself have motivated the development of the modern tunneling machine. Our rapidly growing civilization needs faster, less expensive and safer means of excavating tunnels. Space age technology and materials have played a major role in making hardrock tunneling machines possible.

Jan 1, 1970

By Richard A. Queeney, Lance G. Peterson

ESTIMATES of the stacking fault free energy of copper reported in the literature show an extensive divergence of results. Based on measurements of dislocation node radii, Thornton et al.7 find the lower limit of stacking fault energy to be 60 ergs per sq cm: Jossang and coworkers4 estimate the same value should be less than 40 ergs per sq cm. Assuming stacking fault free energy to be twice the coherent twin boundary free energy, Valenzuela8 reports 72 ergs per cm, while Inman and Khan2 cite a value of 24 ergs per sq cm. which can no doubt be accounted for by almost complete absence of interstitials in solution. However, the minute concentration was sufficient to permit observable recovery of dislocation damping. Assuming a dislocation density of 1010 CM -2 and an average loop length of 0.5 , a concentration of interstitials as low as 0.01 at. ppm is sufficient to reduce dislocation damping by more than a factor of ten. The concentration of interstitial solute atoms in Ferrovac E-0.15 pct Ti was thus estimated at 0.01 at. ppm < (C + N) < 2 at. ppm. The absence at elevated temperature of strengthening due to interstitials, Fig. 1, was therefore anticipated in the titanium alloy. The temperature dependence of the flow stress below 300°K was unaffected by addition of either titanium&apos; or zirconium.&apos; Observed, however, was an initial difference in the absolute value of the flow stress below 320oK, Fig. 1. Grain size may account for the difference; the grain diameter of Ferrovac E was 30 to 45 µ and that of Ferrovac E-0.15 pct Ti 65 to 90 µ. Although second phase particles in the form of titanium carbides and nitrides precipitated in the Ferrovac E-0.15 pct Ti alloy, the spacing was too large to produce any strengthening effect. The mechanical properties measured, therefore, were inherent to the bcc lattice. 1W. C. Leslie and R. J. Sober: Trans. ASm, 1967, vol. 60, pp. 99-111. 2 H. Conrad: Journal of Metals, 1964, vol. 16, pp. 582-88. 3 A. S. Keh and W. C. Leslie: Materials Science Research. H. H. Stadelmaier and W.W.Austin, eds., vol. 1.pp. 208.50, Plenum Press, New York, 1963. 4A. S. Keh, Y. Nakada, and W. C. Leslie: Dislocation Dymmics, Rosenfield, Hahn, Bement, Jr., and Jaffe, eds., pp. 381-406, McCraw-Hill Book Co., New York, 1968. &apos;W. J. Bratina, J. T. McCrath, and H. E. Rosinger: Can. Met. Quart., in press. 6 W. J. Bratina, J. T. McGrath, and D. Mills: Suppl. Trans. Japan Inst. Metals. 1968, vol. 9, pp. 436-43. &apos;H. E. Rosinger and C. B. Craig: Can. Met. Quart., In press. %. Mills. J. T. McGrath. and W. J. Bratina: ScriptaMet,, 1968, vol. 2, pp. 311-13. The purpose of this note is to present the results of a direct measurement of the stacking fault free energy in copper. The present method avoids both the question of interaction forces of nodal dislocations and the assumption that the coherent twin boundary free energy is one-half that of a stacking fault. Fig. 1 shows a transmission electron micrograph of a stacking fault intersecting a high angle grain boundary in copper: Fig. 2 is a schematic representation of the intersecting interfaces. To produce the specimen, pure copper was rolled to 0.002 in. thickness and annealed for several hours at 875°C. These foils were strained in tension to l04 µ in. per in., and rean-nealed to 8 min. Recrystallization and/or grain growth were not observed during the second anneal, indicating that intersections such as Fig. 1 are equilibrium configurations. Many such stacking faults were observed, but few were noted as intersecting grain boundaries in well-illuminated areas. The intersection of Fig. 1 was well away from the specimen edge. Since similar defects have not been observed in fully recrystal-lized and annealed copper, it is felt that this defect is due to the tensile straining. Electron transmission

Jan 1, 1970

By R. W. Carpenter, J. C. Ogle

It is possible, by using pack-rolling instead of conventional rolling, to reduce a number of metals to thicknesses of 2µm or less. Such thinfoils are generally made at room temperature without intermediate annealing. In addition, pack-rolled foils fail by developing pinholes at thicknesses near 2µm instead of developing the shear cracks usually observed in cold-rolled ductile metals. This paper presents the results of a general investigation of the deformation substructure and texture developed in copper and iron pack -rolled from 130 to about 2µm thickness. Electron microscopy showed that in both metals a fine (0.2 to 0.5?µ m) deformation subgrain structure formed during pack-rolling; in neither case was this substructure grossly different from substructures formed during conventional rolling. The deformation texture formed in pack-rolled iron was quite similar to usual bcc textures; however, in the case of copper, the cube texture was stable during pack-rolling and the normal copper deformation texture was unstable. It is shown analytically that the constraining pack induced a large hydrostatic pressure in the foils during pack-rolling. The pinhole failure mechanism is attributed to the presence of the large hydrostatic pressure during pack-rolling; this strongly suppressed the growth of shear cracks. The stability of the cube texture in copper is also probably due to the unusuul stress distribution developed during pack-rolling. EXPERIMENTS at several laboratories have shown that very thin foils of the common structural metals and many of the rare earths can be made by "pack-rolling". 1-3 The technique was originally developed to make specimens for nuclear scattering experiments and foils for X-ray filters. It is also useful for making experimental laminar metallic composite bodies and foils thin enough for direct examination by ultra-high voltage electron microscopy without the need for special thinning techniques. Pack-rolling in the present context means a three-layer pack, with the material to be rolled into foil comprising the center layer. The outer two layers, which constrain the foil during reduction, are ordinarily austenitic stainless steel. Typically, a 130 µm (0.005 in.) metal strip can be reduced to a final thickness of 2 µm or less by this process. This is accomplished at room temperature, without intermediate annealing. It has been observed that foils produced by this process do not exhibit at any stage of their reduction the severe work-hardening found in strip rolled by conventional cold-rolling methods. Neither is the failure characteristic the same."&apos; Conventionally cold-rolled ductile metal strip fails by developing shear cracks on planes whose normals nearly bisect the angle between the rolling direction and normal to the rolling plane; these are planes of maximum shear stress. In pack-rolling this mechanism has not been observed; failure occurs by the formation of pinholes on the foil surface (penetrating the foil). If pack-rolling is continued the hole density increases. These differences in behavior imply the existence of appreciably different substructure in pack-rolled foils compared to substructure in conventionally rolled material, or perhaps that the geometry of pack-rolling has an effect on the foil behavior. This paper describes an investigation of deformation substructure and texture in some specimens of pack-rolled copper and iron, and some considerations of the stress distribution in the foils during rolling that result from the geometry of pack-rolling. EXPERIMENTAL DETAILS Three different materials were used for pack-rolling in the present work: soft copper sheet (99.8 pct Cu, 0.03 pct 0, electrolytic tough pitch) and two types of iron, Ferrovac E* and Armco iron. Each was "Crucible Stccl Co. initially in the form of 130 µm annealed strip with grain size ranges of approximately 10 to 40 µm. The initial texture of the copper (determined as noted below) was the normally observed cube type (001)[100]; there was evidence of a small amount of material in the cube-twin orientation reported by Beck and Hu.4 The initial texture of the Ferrovac E was similar to that reported for recrystallized iron by Kurdjumov and sachs,5 who list the principal orientations as {111}<112>, {001}<110> 15degfrom RD and a weak component {112}(110) 15 deg from RD. The starting texture of the Armco iron was not determined. Pack-Rolling Procedure. A four-high mill was used for all specimens. The work roll and backing roll diameters were 1.625 and 5.25 in., respectively. The peripheral roll speed of the work rolls was about 2.5 in. per sec. All foils were initially reduced from 130 to 100 µm by conventional straight rolling and then inserted into a pack, without any intermediate annealing, for further reduction. The pack consisted of an 0.033 in. (838 µm) thick 3 by 6 in. polished sheet of austenitic stainless steel, folded to make a 3 by 3 in. jacket. After folding, the jacket was given a small reduction to close the fold tightly before insertion of the foil. During pack-rolling a constant change in roll spacing was made every third pass. The roll-spacing change corresponded to a 5 pct reduction in thickness for a new pack. This approached a 10 pct reduction when the pack had decreased to about half its original thickness. At this point the deformed pack was discarded and a new one

Jan 1, 1970

By E. S. Tankins

The main purpose of this work was to study the effect of gold on the activity coefficient of oxygen in the liquid Fe-Au alloy and to determine how copper and silver change the activity coefficient of oxygen. A preliminary investigation has been made of equilibrium in the reaction of hydrogen with oxygen in some of the liquid gold alloys. The experimental method, which has been described in detail elsewhere,&apos; consisted of bubbling accurately known H-A-water vapor mixtures through the Fe-Au alloys contained in alumina crucibles within a vertical closed furnace. When equilibrium was reached, the samples were quenched by rapidly lowering the crucible under an atmosphere of argon to a water cooled brass fixture at the bottom of the furnace tube. The melts were found to freeze from the top in less than 4 sec. The heats were carefully prepared for oxygen analysis. The oxygen content was determined by vacuum fusion analysis.&apos; Only high purity electrolytic materials were used in this investigation. The activity and free energy of oxygen in the liquid iron alloys were studied by means of the reaction; The data for the 80 Fe-Au alloys, obtained as a function of temperature, are summarized in Table I and presented in Fig. 1, where log is plotted against . The results can be expressed by: The data were obtained using water vapor-hydrogen ratios between 0.04 and 0.30, and a 25 pct H2-75 pct A mixture. An oxygen content between 0.030 and 0.060

Jan 1, 1970

By Gordon M. Bell

Water has received little attention as a variable in flotation, even though it is a known fact that water hardness often has an adverse effect on purity and recovery, particularly on the flotation of non-metallic minerals. Because of this fact, process water used in some flotation plants is treated to reduce hardness to an acceptable level. In the laboratory, distilled water is usually used as the flotation medium in order to standardize conditions, whereas in flotation plants locally available water is used. At Rosiclare Works of Aluminum Company of America, Rosiclare, Illinois, where a vein-type of fluorspar deposit was being processed by flotation to make an acid-grade fluorspar concentrate until February of 1968 when the plant was closed, qualitative correlations had been observed between metallurgy and reagent consumption and the seasons of the year. The observed effects were thought to be due to seasonal variations in the quality of Ohio River water used as the flotation medium. Figure 1 shows the variations in total hardness and chloride contents of Ohio River water at Rosiclare for the period September 1964 through September 1967. During this period, the sulfate content varied from 85 to 245 ppm (as Na2SO4), the calcium from 90 to 160 ppm (as CaCO3) and the magnesium from 50 to 70 ppm (as CaCO3). The data in Figure 1 show that the total hardness and chloride contents are highest in the late summer and fall which are usually periods of low water and lowest in late winter and spring which are usually periods of high water.

Jan 1, 1970

By C. D. Michaelson

Bridging the gap between have and have-not nations is one of the necessities of the present era. The responsibility for accomplishing this must be assumed by the affluent industrial societies of the world, both through their governments and through private enterprise. Despite a discouraging number of instances where companies established in underdeveloped countries have been expropriated, U.S. industry must not abandon such ventures. Instead, it should tailor them to the needs and aspirations of the host nations. One way in which industry can minimize the danger of expropnation is to enter into partnership with the government of the host nation. Kennecott Copper has recently done this in Chile, becoming 49% owner of a company formed to expand and operate the El Teniente mine. So far, the partnership has produced marked benefits not only for Chile, but also for Kennecott. The memory of D.C. Jackling serves chiefly to remind us how much we owe to the pioneers of our industry. Jackling was one of the giants. Orphaned at the age of two, he made his way through sheer persistence and plain hard work. His brilliance gave rise to a vision, and his tenacity made his vision a reality. Foreseeing that economies of scale would make the handling of low-grade ore profitable, he introduced the revolutionary concept of open-pit copper mining. During World War I, the defense effort of the United States was irnrneasurably strengthened by the tremendous supplies of copper from the western mines that Jackling had made possible. Again in World War 11, the demands for copper were supplied, and the nation once more had profound reason to be grateful to this rugged, stubborn man who had long ago ventured into the mountains and unlocked their wealth. We are now embarked upon another great era of change, and we must devise new concepts to meet it. The task is not only to create new techniques of mining, but to forge better ties between men and institutions which will let us work in harmony with the techniques we have. We might recall that while Jackling was a man of towering pride and formidable will, he was also adept at getting others to share his vision and join his purpose. Today our reach for cooperative endeavor must go far beyond our own shores as we seek to develop the buried riches of distant lands. And we would do well to remember that Jackling&apos;s remarkable insight would have come to nothing had not British investors been willing to provide much of the initial capital. As was true of so many early enterprises in America, European capital was absolutely essential. CORPORATIONS ABROAD - AN EXPANDING ROLE Today the situation is quite different. The United States is now a capital-surpIus nation and looks abroad for opportunities to employ its capital profitably. On the other hand, we have become dependent on foreign sources for supplies of vital raw materials, while we seek

Jan 1, 1970

By John E. Feddcck

New York City&apos;s $360 million North River Water Pollution Control Project is part of New York State&apos;s plan to clean up the Hudson River. The project is to provide a sewage treatment facility capable of accomodating a peak waste water flow of 330 MGD which will in great measure eliminate the 192 MGD of raw sewage that N. Y. C. discharges into its surrounding waters. Eleven miles of intercepting sewer lines must be constructed along the west side of Manhattan Island to service approximately one-half of the island. The first contract award was for a 4134 ft. sewer tunnel with a finished inside dimension of 16&apos; x 16&apos;. This main intercepting sewer will feed a sewage treatment plant located on and adjacent to the Hudson River. The tunnel is parallel to the river and is located under 12th Avenue between 125th Street and 143rd Street. The Penn- Central Railroad tracks are above and just to one side of the tunnel location. The working tunnel diameter is 21 ft. and numerous problems of support, mining method, and ground control have been encountered. (see Dwg. 1)

Jan 1, 1970

By S. P. Hansen

Gravity sedimentation is one of the most widely used processes for separating solids from liquids whether it be for ore and mineral processing or for treating municipal sewage or industrial wastes. Investment in sedimentation equipment can represent a significant portion of the total capital costs associated with a processing or treatment facility. In spite of the importance of sedimentation, little attention has been devoted in recent years to improving this equipment by applying the basic principles involved in sedimentation. In the water and waste treatment field, design criteria established one half-century ago is still the accepted standard and in reflection of this lack of progress, sedimentation and thickening equipment has remained virtually unchanged. The primary purpose of this paper is to present and describe a new innovation in gravity sedimentation which has been applied to water and wastewater treatment and could definitely have application in the field of ore and mineral classification. A secondary object is to introduce the mixed media filter which has been widely used to treat municipal drinking supplies, industrial process water and to provide tertiary treatment of sewage and industrial wastes. The tube-type clarifier was developed primarily to be applied in the field of water and waste treatment where it was found that it could be used to considerably reduce the size and cost of clarification facilities. A logical extension of the tube clarifier would be to the area of minerals classification, ore separation, and for treating waste water associated with these activities. In water treatment practice, most clarification processes are followed by a filtration step to provide further polishing of the water prior to use. This paper will also discuss the mixed media filter which is graded from coarse to fine in the direction of filtration and is capable of operating at high filtration rates and with greater applied suspended solids loading than other filter designs while providing a high qualify filtrate.

Jan 1, 1970

By John M. Gomes

Two methods for electrowinning tungsten from wolframite [(Fe,Mn)W04] were investigated. The first method, direct electrowinning from wolframite concentrate dissolved in molten salt mixtures composed essentially of various combinations of sodium phosphates, sodium borates, and sodium halides, yielded impure products. The second method was electrowinning from a halide-tungstate melt that was obtained from a high-temperature, two-phase extraction of tungstic oxide (W03) from wolframite. Electrolysis in electrolytes prepared from addition of sodium metaphosphate (NaPO3) and boric oxide (B2O3) to the halide-tungstate melt produced tungsten metal of 99.9 percent purity. Tungsten carbide (WC) was electrodeposited from the halide-tungstate melt when the melt was adjusted to contain 82 mole-percent NaCI and 6.0 mole-percent each of W03, sodium metaborate (Na2B204), and caustic soda (NaOH).

Jan 1, 1970

By John W. Burd

A system is described for the simultaneous deposition of epitaxial layers on as many as eight substrates. A high degree of uniformity of both physical and electrical characteristics is achieved in the films. Variation of film thicknesses is consistently less than ±10pct within a wafer and from wafer to wafer within a run with the variation typically on the order of 55 pct. Composition variation of GaAs1-x PX layers within a wafer and from wafer to wafer within a run is consistently less than 51 pct. Electrical evaluation of the films by several techniques indicates excellent doping uniformity within a wafer and from wafer to wafer within a run. Mobilities for lightly doped GaAs films at 300°K are consistently >6000 cm2 v-1 sec-1 and mobilities > 7000 cm2 v- 1 sec-1 are regularly attainable. Techniques for the preparation of material with carrier concentrations from 1 x 1015cm-3 to 1 x 1019 cm-3 n-type and 5 x 1016 to 5 x 1018 cm-3 p-type are discussed. METHODS for the preparation of 111-V compounds by vapor phase reactions have been extensively reported in the literature.1-6 Almost all of the apparatus described for these various methods are suitable for processing one or at the most a very limited number of wafers simultaneously. With the recent rapid advances in the use of vapor grown GaAs for microwave oscillators and GaAs1-xPx as visible light emitters the requirements for these materials are steadily increasing. In order to satisfy these requirements it is necessary to move from a laboratory scale apparatus to one which is capable of processing a large number of wafers simultaneously. Desirable features would be a high degree of uniformity among the wafers and good reproducibility from run to run. The apparatus to be described fulfills these requirements very well. DISCUSSION The various methods reported in the literature can be classified under three headings: 1) closed tube, 2) open tube, and 3) the close-spaced method. Of these three the open-tube method is the most amenable for scale-up to a manufacturing process. It is the most versatile and the various operating conditions can be more precisely controlled than with the other two methods. A number of chemical reactions may be used to achieve vapor-phase growth of 111-V compounds. Sev-era1 of the more generally used reactions are shown in Fig. 1. All of these reactions have the following points in common: 1) generation of a volatile group III(Ga) species by the reaction of the transport agent (halide or HC1) with either Ga or GaAs, 2) introduction of the Group V(As and/or PI component, 3) a method of adding dopant, if desired, and 4) a region in which deposition from the vapor will occur and form as a single crystal epitaxial film on the substrates. The laboratory scale reactors permit the hot re-actant gases to flow into the relatively cooler deposition zone and pass successively over the several substrates which are arrayed along the long axis of the tube parallel to the gas flow. With this arrangement the composition of the reactant stream is continually changing as solid material is deposited on each successive substrate. As a result of this changing gas composition the reaction driving force also changes from substrate to substrate and the degree of uniformity of layer thickness, doping level, and so forth, is poor. This effect can be partially overcome by imposing a controlled temperature gradient along the deposition region to compensate for change in gas composition. However, even when this is done variations in layer thickness on the order of 30 to 40 pct are common and as high as 50 pct are frequently experienced between adjacent wafers in the tube. To expand this arrangement to a large number of wafers would only increase the nonuniformity from the first to last wafer in the line. From the above discussion the two undesirable features of changing gas composition and temperature gradient become evident. A reactor system which eliminates or minimizes these undesirable features is one in which the apparatus is mounted vertically as shown schematically in Fig. 2. The vertical mounting permits the disposition of a number of substrates on a suitable support so that all wafers are at the same vertical height in the furnace and hence at essentially the same temperature. By using only a single row of wafers the reactant gas mixture passes over only one substrate in its path through the reactor. Thus the two undesirable features of changing gas composition and temperature gradient are minimized. An additional design feature which further minimizes temperature variations is rotation of the substrate holder. Rotation serves to integrate any radial temperature gradient existing around the resistance heated furnace. A photograph of a reactor assembly at the completion of a run is shown in Fig. 3. MATERIAL PREPARATION Apparatus. Although any of the several chemical systems shown in Fig. 1 are adaptable for use in this apparatus the one generally used is System 2, the hydride synthesis system. This system has been de-

Jan 1, 1970

By Edward A. Mihok

This paper presents plant design and cost estimates for limestone treatment of acid mine water covering a wide range of quality and quantity conditions. The treatment process consists of limestone neutralization, aeration, solids settling, and concentration. The design criteria for the various operation functions are based on pilot plant performance, laboratory data, and established mine water treatment standards. Unit costs have been assumed and are related to general market prices and conditions. These estimates serve as preliminary indicators of what it would cost to construct and operate a mine water treatment plant.

Jan 1, 1970

By C. T. Young, J. L. Lytton

In recent investigations,1,2 the strength and thermal stability of dislocation substructures prepared by 5 to 25 pct room temperature tensile straining and recovery annealing at 120°, 160°, and 200°C have been studied in randomly oriented polycrystalline high purity aluminum. The techniques of transmission electron microscopy revealed that a major source of the strength and stability of dislocation substructures was the formation, during room temperature straining, of well-defined cells bounded by dislocation tangles which rearranged into nearly perfect dislocation networks during recovery, forming the boundaries of subgrains. The strength of such substructures increases with decreasing cell or subgrain size,2"6 and the formation of fine subgrain structures can provide thermally metastable strength at low temperatures and can favorably alter the course of primary creep at elevated temperatures.7&apos;8 For maximum benefit, however, sub-grain growth should be reduced or eliminated. It was, therefore, decided to investigate the use of heterogeneous precipitation on dislocation networks as a means of imparting increased strength and thermal stability to subgrain structures through effective pinning. C.T. YOUNG, STUDENT MEMBER AIME, and J. L. LYTTON, Member

Jan 1, 1970