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By R. H. Frazier, F. W. Boulger

THE performance of welded structures is closely associated with the ductile-to-brittle transition temperature of the steel from which they are made. A low transition temperature is desirable because it indicates that the steel is less likely to fail suddenly at low ambient temperatures. Structures such as bridges, ships, storage tanks, and pipelines are usually made from hot rolled semikilled steel. Changes in rolling practice or chemical composition appear to be the most practical methods for improving the toughness of such materials. This results from the fact that production is likely to be seriously curtailed if improvements were obtained by recourse to heat treatment or complete deoxidation. This paper discusses the effect of variations in carbon and manganese contents on the properties of semikilled steels. The transition temperature, a property to which considerable importance is attached, varies with specimen configuration, testing method, and criterion of performance. Both the Navy tear test' and the keyhole Charpy test were used in the investigation. According to the terms used by Vanderbeck and Gensamer,V he tear test was used to measure a fracture transition and the Charpy test to measure a ductility transition. In either case the specimens absorb considerably less breaking energy in tests below the transition temperature than in tests above the transition temperature. Decreasing the testing temperature of notched-bar specimens seems to be equivalent in its effect to increasing the severity of loading on fabricated structures. Therefore, structures built from steels exhibiting lower transition temperatures in laboratory tests are expected to be less susceptible to sudden brittle fractures in service. Consequently, changes in composition which lowered the transition temperature of the experimental steels were judged desirable. Materials and Methods The steels for this study were made in a laboratory induction furnace and rolled to 3/4 in. plate, using a finishing temperature of 1850°F. Precautions taken to insure reproducible melting and testing practices are discussed in detail elsewhere.' All tests were made on hot rolled steels. The analyses of the experimental steels are given in Table I. The list includes steels with manganese contents ranging from 0.21 to 1.46 pct, at each of five carbon levels. The phosphorus, silicon, sulphur, and nitrogen contents of the steels are reasonably constant. The tensile and notched-bar properties of the experimental steels are presented in Table 11. Both upper and lower yield points are listed, and all values are averages for duplicate specimens. Transition temperatures based on three criteria are given. The keyhole Charpy transition temperatures are the temperatures at which the energy-temperature curves based on averages of four specimens cross the 20 and 12 ft-lb levels. Both definitions of Charpy transition temperatures have been used by other investigators. Charpy tests were made at intervals of 10°F, using a pendulum with an available striking energy of 220 ft-lb and a velocity of 18.1 ft per sec. The specimens were oriented parallel to the rolling direction and notched normal to the surface of the plates. The tear test transition temperatures are based on the usual' criterion of the highest temperature at which at least one of four specimens exhibits brittle behavior. The dimensions of the tear test specimens are shown in Fig. 1. The specimen is loaded eccentrically in tension, with pin and shackle fixtures, through the large holes while submerged in a liquid bath at the proper temperature. A specimen developing a fracture area with less than 50 pct shear or ductile texture is classed as brittle. Tear tests were made at intervals of 10°F.

Jan 1, 1955

By C. R. Johnson, R. A. Greenkorn, L. K. Shallenbarger

This paper describes a study, based on core data, of the directional permeability of a sandstone reservoir. Directional air permeabilities are explained and correlated with lithology by the tensor theory of permeability, which is extended to the more general case of heterogeneous anisotzopic porous media. In this case, the permeability tensor is made up of two components: (I) anisotropy (variation around a point) which correlates with bedding, and (21 heterogeneity (variation from point-to-point) which correlates with grain size. INTRODUCTION Previous studies of directional permeabilityl.5-8 have concerned themselves only with anisotropy at a point, rather than with both point-to-point differences and local anisotropies. In this paper, we present the existing tensor theory of permeability for anisotropic porous media and then extend it to the more general case of heterogeneous anisotropic porous media. The laboratory measurements of directional permeability are explained in view of this extended theory and the data are discussed in terms of the lithologic factors that correlate with it. The results show what the heterogeneity and anisotropy of the reservoir element are, and that the directional permeability correlates with lithology. Data used in this paper are measurements of air permeability in eight directions, spaced at 45° intervals, on 142 2-in. vertical plugs from 30 cores. The core data are meaningful in terms of directional permeability because the cores were oriented to within 45O during drilling and coring.3 Although we initially thought that only 60 per cent of the core material was reliable, subsequent study showed that almost all of it was reliably oriented. After determining the air permeabilities, the data were reduced to three independent variables for each plug: the major and minor permeability axes, and the direction of the major axis. These were obtained by converting the permeability data to the reciprocal square root of permeability and fitting the transformed data with ellipses according to the tensor theory of permeability.8 The point-to-point areal variation of the minimum permeability axis is related to grain size. The direction of the permeability axes, where the major axis exceeds the minor axis by at least 5 per cent (measured variation is about 4 per cent), correlates with the bedding. The permeability tensor used in this study must be considered as the sum of a scalar and a tensor, with the scalar being the minor axis permeability as a function of position, and the tensor the directional effect, which is additive permeability over the minor axis. In this case, the point-to-point variation or heterogeneity (minor axis) is substantially larger than the variation at a point or anisotropy. It may be important that this separation of "directional permeabilities" be recognized when considering migration of fluids due to permeability variation. Local migration may be due to anisotropy and point-to-point migration may be due to heterogeneity, but the direction and magnitude of these may not be the same. Furthermore, in truly heterogeneous systems, one would expect that anisotropy would be the smaller of the two effects. THEORY TENSOR THEORY OF PERMEABILITY FOR ANISOTROPIC POROUS MEDIA8 Darcy's law for flow in porous media in its usual form is where qis the flow rate vector, k is the permeability, is the viscosity, is the vector differential operator, and P is the Pressure. Consider flow, q, through a unit area in the direction of the unit vector n from elementary flow tubes parallel

Jan 1, 1965

By N. K. Chen, C. H. Mathewson

Single crystals of high purity aluminum of various orientations were carefully documented after plastic extension. Special attention was given to the formation of slip lines, deformation bands, and asterism. An explanation for the geometry and mechanism of formation of deformation bands is considered. WHILE the general process of plastic extension of face-centered cubic metals is well understood,' the accompanying structural changes due to slip and rotation are far more complex than ordinarily assumed. In the case of stretched single crystals of aluminum, the complicated behavior is especially marked by the formation of deformation bands, as first indicated by Collins and Mathewson." Such bands were believed by them and also by others,".'7 who have discussed banded structure in general, to represent one of the important modes of lattice reorientation and to be intimately connected with the recrystallization process. Yet, despite their fundamental importance to the understanding of the mechanism df both plastic deformation and recrystallization, practically no study of the crystallographic features of these bands in their relationship to the conventional slip process has been attempted. This paper describes part of an extensive investigation on the structural behavior during plastic deformation of aluminum single crystals and is especially concerned with the characteristics of deformation bands. The investigation of the subsequent re-crystallization of deformed aluminum single crystals will be discussed in a later publication. Experimental Procedure Single crystal specimens of 99.996+ pct pure aluminum, Yz in. in diam and 5 to 6 in. in length were made both by the Bridgman method5 nd by a modified temperature gradient method.'* Crystals were selected in which the lineage deviation did not exceed 2"; i.e., as determined from the back-reflection Laue X-ray photograms. These crystals were radiographed to insure that no internal porosity was present. The orientations showed good coverage of the whole area of the Taylor and Elam triangle.' Orientations of the crystals were obtained by the back-reflection Laue technique described by Greninger." Crystals so selected were tapered very carefully in a lathe to obtain a linear decrease in diameter from 0.500 to 0.350 in. along a gage length of 3 in. This is considered desirable because it permits a strain gradient to be introduced in a single specimen at one initial orientation. The advantages of tapered crystals for studying the development of slip lines and recrystallized grains have been pointed out by previous investigators." The cold-worked layer resulting from the machining operation was removed by alternate etching in aqua regia and careful polishing with 2/0 emery paper until undistorted Laue back-reflection spots were obtained. A homogenization treatment at 600 °C for 24 hr was then introduced to insure the removal of residual stress. Two of the crystals so prepared were also checked by use of a glancing angle technique. Using a copper target, at 30 kv and 10 microamperes, a monochromatic beam was positioned at right angles to the axis of the crystal about which it rotated. The time of exposure was 24 hr. From these X-ray photograms, it was concluded that the present method of preparation of single crystals is satisfactory. Following this procedure, the crystals were elec-trolytically polished in a 2:l solution of methyl alcohol and concentrated nitric acid. Intermittent

Jan 1, 1952

By Narendrakumar A. Chevli

Exploratory work was conducted in the fabrication of integrated circuitry, specifically linear amplifier circuits, by three general methods: 1) monolithic diffused silicon; 2) a combination of metal thin-film and monolithic diffused silicon; and 3) a hybrid of metal films and diffused silicon on an alunina substrate. In these linear amplifier integrated circuits the followzng conditions were desired: very high-frequency response, high voltage gain, and good thermal tracking stability of electrical characteristics. The resulting circuit designs imposed problems of isolation between elements, layout and smallness of size of active elements, and close tolerances on electrzcal characteristics of the passive elements. Interconnection problems for specific designs resulted from the small dimensions involved and the topography of the hybrid fabrication techniques. The desired integrated-circuit characteristics were achieved with the technologies of categories 2 and 3 above. Solutions to the problems imposed by these characteristics lay in the ability to isolate czrcuit elements of small size while providing a layout designed to minimize element-to-element variations. Sufficient freedom in the formation of passive elements was achieved by uniting the metal film and the monolithic silicon technologies. The most satisfactory designs were based on the beam-lead interconnection and isolation technique. SINCE the advent of integrated circuits, major emphasis has been on fabricating digital integrated circuits. Linear circuits require high performance, high voltage, and tighter tolerance components which are not always compatible with the capability of process technology available for fabrication of these circuits into integrated form. Fortunately the growth of newer and improved processes and materials for fabricating integrated circuits has been an accelerated one. This has now made possible the translation of stringent performance requirements of the linear circuits into microminiature integrated circuits of the same performance. In the exploratory work of fabricating high-performance Linear Integrated Circuits—LIC, the following objectives were formulated: i) fabrication of high-frequency transistors such as the type 2N918 isolated on a single silicon substrate; ii) fabrication of medium-frequency transistors having a very high gain at low collector currents such as the types 2N930/2N2484 isolated on a single substrate ; iii) fabrication of tight-tolerance, high-valued resistors having low temperature coefficients of resistance and stable thermal tracking characteristics, these resistors to be fabricated on an active or passive substrate; iv) simultaneous fabrication of complementary transistors—pn and pnp-on the same silicon substrate; v) fabrication of newer active elements such as MOS, FET transistors along with the conventional active and passive elements on the same silicon substrate. State-of-the-art assessment f all the available processes, materials, and technology to meet above objectives indicated that economic fabrication of LIC cannot be achieved by a single technology for all types of linear circuits. Where design and performance of a given linear circuit can be modified and tolerated to the extent of a particular technology, then alone is it possible to fabricate a LIC using a single process technology such as all diffused, planar technology. In order to evaluate this economic breakpoint with design and performance compromise in fabricating LIC, it is essential that a thorough understanding be obtained of techniques, potentials, and limitations of all the various process technology and materials

Jan 1, 1967

By Hsun Hu

Direct observations were made on the recrystalli-zntion of a cold-rolled (110) [001] crystal of 3 pct Si-Fe by annealing thin sections of the specimen inside the electron microscope during examination. Subgrain formation, presumably by polygonization, occurs rapidly, followed by a slow increase in the subgrain size before recrystallization can be detected. No migration of the subgrain boundaries was observed, and the formation of recrystallization nuclei by coalescence of subgrains is suggested. Re-c~ystallization characteristics of various texture components were individually examined. AS reported in a previous paper: orientations of the various deformation texture components in a 70 pct cold-rolled (110) [0011 crystal of 3 pct Si-Fe were completely confirmed by transmission electron diffraction patterns taken at various areas of the specimen. These orientations can be summarized as follows: Over most areas of the deformed crystal (111) planes are parallel to the surface. These areas correspond to either $- the two main defor: mation textures, the (111) [112] or the (111) [112].2-5 Within a few areas, (100) planes parallel to the surface are frequently found. These areas represent the minor deformation texture component, the (100) [Oll] type, which is derived from rotated Neumann bands.2'4'5 Only in very rare instances are (110) planes found parallel to the surface. This orientation corresponds to the very weak texture component of the (110) [001] type. In a pole figure, this (110) [0011 orientation is located within the orientation spread between the two main (111) [1121 type textures. Usually the electron diffraction patterns taken at various areas of the specimen are very simple ones, i.e., for any one area the pattern consists only of sharply defined spots of a single orientation. In some areas, however, more or less continuous rings of weaker intensities are superimposed on a simple pattern, indicating the presence of a wide range of additional orientations. In order to understand in detail the recrystallization of this cold-worked crystal, the recrywtallization characteristics of each of the various deformation texture components must be examined. This can best be done by using a high-temperature stage and transmission electron microscopy techniques, whereby small areas corresponding to the various texture components can be selected individually for examination. The present paper presents results obtained by this method. MATERIAL AND METHOD Specimens were prepared from a previously studied1 single crystal of a commercial grade 3 pct Si-Fe alloy with an initial orientation (110) [00l], cold-rolled 70 pct from 0.014 in. to 0.004 in. in thickness. Thin foils were prepared by electrolytic polishing as described in the earlier paper.' Specimens of this thin foil were then mounted in a high temperature stage similar to the one designed by Whelan.6 A direct current was used as the heating source. The temperature of the heating grid was calibrated by means of a Pt vs Pt-10 pct Rh thermocouple in a vacuum chamber (0.01 to 0.02µHg). Maximum variation within the temperature range of 250o to 000°C was about ± 25°C. After the desired areas were selected for examination, the specimen was heated to a low temperature for some time while the selected area was constantly watched. When no further change in structure and orientation could be observed, a higher temperature was applied. Photomicrographs and diffraction patterns were taken from time to time during examination, with the heater temporarily turned off* while the photographs were

Jan 1, 1962

By J. S. Kasper, R. M. Waterstrat, B. F. Decker

THE existence of v phase in the Mn-Mo system was discovered in this laboratory several years ago,' but neither the conditions of its formation nor its composition were known, and preliminary attempts to reproduce the phase were unsuccessful. We wish now to specify the information appropriate to phase formation on the basis of experiments performed since that time. The starting materials were in every case electrolytic manganese and high purity molybdenum. Two methods of preparation were employed: l—arc-melting varying combinations of the elements in an inert atmosphere and subsequent heat treating, and 2—sintering compressed mixtures of finely divided powders of the elements. In the latter method, the powders were first passed through 200 mesh screen and then compressed into cylinders of % in. diameter and % in. length, which were sintered at elevated temperatures in an atmosphere of dry hydrogen. For some samples, the sintering temperature was 1200°C (for 1 hr), and these were then heat- treated at lower temperatures for times up to 24 hr. Eventually it was found, for the proper composition, that essentially pure a phase could be produced by sintering at 1125°C for 3 hr. Quenching to room temperature was effected by means of a stream of cold, dry hydrogen in a water-cooled chamber. The arc-melting procedure was found to be unsatisfactory after an investigation of many samples at different compositions and temperatures. Large quantities of manganese were vaporized during melting and none of the products were homogeneous or contained extended regions of pure phase. Nonetheless, these experiments established that no formation occurs in the Mn-Mo system below 1115oC, and indicated, at least roughly, the composition range of interest for further exploration. The more definite results obtained from samples produced by the second method are given in Table I. A portion of sample 2 heated for 16 hr at 1000°C in a Vycor tube transformed to molybdenum plus unidentified phases of complex X-ray pattern. From these few results it appears that the region of phase is quite narrow in composition. It is of interest that the composition is such as to make for difficulties in correlating this structure on an electron atom basis with other a structures of iron, cobalt, and nickel. In that respect Mn-Mo shows the same anomaly as Mn-Cr and Mn-V systems.' A second feature is that in common with the two other known molybdenum (Fe-Mo and Co-Mo), Mn-Mo v exists only at elevated temperatures. The X-ray powder pattern of the pure a phase of Mn-Mo is given in Table 11. It agrees well with the patterns established for other structures, especially with that for Fe-Mo as given by Goldschmidt.An attempt is being made to establish whether an ordering of the respective atoms occurs and such information will be reported in a future publication. Acknowledgment The authors acknowledge gratefully the assistance of Mrs. J. R. Belanger in some portions of this work. References 'J. S. Kasper, B. F. Decker, and J. R. Belanger: Journal of Applied Physics (1951) 22, p. 361. 2 A. H. Sully: Journal Inst. Metals (1951) 80, p. 173. H. J. Goldschmidt: Research (1949) 2, p. 343.

Jan 1, 1954

By C. H. Samans, G. F. Tisinai

HARDENING and embrittlement of the ferritic chromium stainless steels at temperatures near 885 °F have been known for a long time.' However, no satisfactory explanation has been given. Both ordering and precipitation hardening have been suggested. Fisher, Dulis, and Carroll2 discovered a chromium-rich body-centered-cubic precipitate in embrittled alloys. Subsequently, Williams' and Wright4 also have found evidence of this body-centered-cubic constituent. William's hardness, electrical resistance, and magnetic studies led to his proposal of a new constitutional diagram for the Fe-Cr alloys. The new feature of this diagram is the eutec-toidal decomposition, below about 970°F, of the s phase into two stable body-centered-cubic solid solutions, one rich in iron and the other rich in chromium. An observation of Heger5 that the amount of s phase has increased and the amount of chromium-rich body-centered-cubic phase decreased in the interval 5000 to 32,600 hr at 900°F, even though the alloy increased in hardness, casts some doubt on this diagram. If precipitation hardening causes the embrittlement, the precipitate probably is always coherent with the matrix, since no evidence of overaging has been reported. It cannot be stated positively, however, that Fisher's body-centered-cubic constituent is the embrittling phase. According to Preston's data,6 such a chromium-rich phase should have a parameter less than about 0.5 pct larger than that of the iron-rich matrix lattice. Moreover, the constitutional relationships whereby Fisher's constituent forms, and whether it is stable, metastable, or a transition phase, are not yet completely clear. The recent studies of Wright4 and of Lommel,7 as well as the earlier studies of Becket8 and of Hochmann,9 have shown that 885°F hardening occurs in relatively pure Fe-Cr alloys. No evidence of its occurrence or absence in chromium itself has been reported. The rate of hardening in high purity alloys seems appreciably slower than that in alloys containing larger amounts of impurities (chiefly carbon and nitrogen). This may be due merely to the absence of hardening and straining effects from precipitated carbides and/or nitrides. These observations on high purity alloys make it seem unlikely that 885 °F hardening is caused by a constituent containing other than iron and chromium atoms, e.g., carbides and/or nitrides. Wright,4 Lommel,7 and Lena and Hawkes10 emonstrated the accelerating effects of a finely dispersed precipitate of (probably) chromium nitride on the hardening reaction. This appears to be evidence that lattice straining increases the rate of nucleation of the hardening constituent. Some new observations on 885°F hardening are reported here. They show an effect of preheat treatment that should contribute to a better understanding of the 885°F hardening phenomenon. They also clarify a discrepancy which exists in the literature. Some investigators have reported most rapid hardening at 885", whereas others have reported it at 930°F. The present work also shows that 885°F hardening does not occur in electrolytic chromium, and that any long range ordering type of reaction affecting any sizeable part of the volume is unlikely. Materials Studied Table I shows the currlposition of the alloys used in this investigation. In these alloys carbon and nitrogen are present in roughly similar amounts. Presumably both elements precipitate, as carbides and/or nitrides, during the heat treatments given.

Jan 1, 1958

By Lane Mitchell

A ceramic product or processed material is a solid composed of materials which have been subjected to heat above 468.3°C (875°F). The raw materials, which are blended together (or in some cases used singly), are selected and utilized for various reasons such as ease of fabrication, aid to processing, to yield desired properties after processing, lack or controllable degree of toxicity or hazard, availability, cost, and perhaps other considerations. Almost all solid inorganic, some organic, and some liquid and gaseous materials have the potential to be used individually in some ceramic product. There are several fundamental functions to be fulfilled in every ceramic product and a number of secondary functions are desirable in specified products. These functions are generally met by the most widely occurring minerals and rocks of the earth and their debris. This fact characterizes ceramics as a field utilizing the raw materials most available to man. Of course, specified products utilize synthetics, organics, and rare inorganics to produce desired results. Any solid nonmetallic product processed by subjection to temperature above a red heat may be called a ceramic product. Widely used construction materials and units, domestic utensils and units, industrial parts to facilitate manufacture, technical components, and aesthetic creations are very often of a ceramic nature because of their durability, inertness, hardness, ease of fabrication, cost, and availability of the ingredients. Often, organics or metals cannot meet desired specifications for some of these products. The rocks and minerals and mineral debris of the earth are largely siliceous. Oxygen and silicon comprise roughly 75% of the earth's crust with aluminum, iron, calcium, and the alkalies following in abundance. Silica (SiO2) and silicates can be melted to form glasses. Alumina (A1203), present in a mineral compound, gives greater durability, hardness, and strength, but lessens the glass-forming property. Iron, calcium, and the other alkalies flux silica and reduce melting points. Thus sand, which is generally almost pure SiO2, and clay, which is generally hydrated alumina silicate, are the most widely used of all ceramic raw materials-principally because of the glass-forming propensities of silicates. In ceramic formulations, clay is generally a refractory filler or skeletal material, having in the raw state a plasticity derived from its colloidal grain size and its water-loving nature. On the other hand, silica sand is a glass former or nonplastic filler. Clay and silica sand in pure forms are quite refractory, i.e., not easily melted. Clay, although siliceous, is less of a glass former than pure silica and is more refractory. Natural contaminants, such as iron oxide or limestone, adulterate many clays and some sands. These contaminants act as fluxes and reduce the fusion points of the mineral or blends. Glass is made from silica sand by fluxing the sand with strong bases, usually soda ash and limestone. Red building bricks are hard and durable because the sand and clay have been partially fused with help of natural iron oxide serving as a flux. The iron oxide performs a dual function, serving as a pigment as well as a flux. In a blend of clay and sand and iron oxide, the sand is more susceptible to fusion than is the clay. Although silica sand and clay are the most widely used raw materials in most ceramic products, many other minerals, and some nonminerals are utilized in products where these materials can produce or aid in achieving desired results. Limestone and dolomite, feldspars, pigmentary minerals, refractory oxides or carbides, and special property producers can

Jan 1, 1983

By M. D. Hassialis

[Surface Areas of Concentrates and Collector Coatings (T.P. 2002, by A. M. GAUDIN and G. S. PRELLER, Min. Tech., May. Discussion by M. D. HASSIALIS and the authors) . I Activation of Minerals and Adsorption of Collectors (T.P. 2082 by J. ROGERS and K. 1'. SUTHERLAND, Min. Tech., Nov. Discussion by A. F. TAGGART and the authors). . . . 3 Correlation between Mineral Behavior in Cataphoresis and in Flotation (T.P. 2005 by A. If. GAUDIN and S. C. SUN, Min. Tech., May. Discussion by M. D. HASSIALIS). . . . . . 8] Surface Areas of Concentrates and Collector Coatings M. D. HASSIALIS.*-In the current flotation theories there exists a common gap spanned by a common assumption pertaining to the arrangement and orientation of the collector ions at the solid surface. Also common is the belief that contact angle and flotation performance are dependent upon the arrangement and orientation of collector ions. This stimulating and informative paper sheds some light upon this general problem. One of the indices of arrangement is the area available per collector ion; in this connection, Gaudin and Preller have applied the B.E.T. method for surface determinations. In a surprising number of cases, their results show a greater specific surface for tailing than for concentrate. This cannot be accounted for by the differences in specific gravity and is attributed to the presence of clay minerals of "primary" sluices in the tailing. This is not a satisfactory explanation, for experience shows that when free slimed clay minerals are present in a flotation cell they will be carried mechanically into the concentrate. A part of the answer to the decreased specific surface of the concentrate would appear to be its usual flocculated condition, yet this should not entirely account for the large spreads reported. The possibility occurs that the nitrogen adsorption isotherms for clean mineral and collector-coated mineral are different. If that were true, and if the coated mineral surface exhibited decreased adsorptive powers, the discrepancy might vanish. In discussing the disposition of collector ions at mineral surfaces, the authors adopt the more consistent viewpoint that there exists some agreement between the ions of the substrate and those of the superstrate. In the case of xanthate ions on galena, a possible arrangement is shown in Fig. 2. This arrangement shows every xanthate ion being shared by two lead ions, whereas the chemical composition calls for two xanthate ions for each lead ion (p. g). This whole discussion is misleading. In the first place, it is known that xanthate ions are not abstracted by unoxidized galena, hence Fig. 2 should show as the substrate not Pbs but PbS„ Om. It would be equally erroneous to use the lattice arrangement of PGSO4, since the surface properties of xanthate-conditioned anglesite differ from those of xanthated galena. It is highly probable that the state of the galena surface exploited in its flotation is ephemeral, since weathered galena is only poorly, if at all, collected by xanthate. Just how a substrate of oxidized galena is to be pictured depends upon one's conception of the transformation from galena to anglesite. This writer is inclined to the following sequence of events. Surface sulphide ions undergo progressive oxidation. As more oxygen is taken up by the sulphide ions they become displaced from their equilibrium positions in the galena lattice, thus accommodating for the larger volume of the S„ Om ions. Concomittant with this change the forces acting on the lead ions

Jan 1, 1946

By K. K. Kershner, W. A. Calhoun, C. W. Funk

Future resources of aluminum may require the utilization of low grade ores to provide a more permanent protection for the nation. Aluminum minerals such as cloy, shale, and high iron laterites may become important sources. An evaluation of reserves is given. New laboratory results are reported on the Vereinigte desilication process. THIS report on future resources of aluminum metal emphasizes the necessity for investigating utilization of low grade potential ores to provide more permanent protection for the nation. Partial or complete interruption of the importation of high grade aluminum ores must be given consideration. Ultimately, aluminum minerals such as clay, shale, and high iron laterites may become the principal sources of aluminum. The development of extractive processes for treating these low grade materials is a step in long-range national preparedness that should receive more attention. In formulating such processes, the application of beneficiation methods for the purpose of classifying the several types of minerals before subjecting each type to the more expensive extractive procedures should be considered, and a careful survey of the basic factors of power sources, transportation facilities, and sources of raw material should be made. Domestic Bauxite Resources Of the domestic supply of current, treatable-grade bauxite, 95 pct comes from Arkansas. The present reserve of Arkansas bauxite suitable for metal production, including abrasive-grade, Bayer-grade, and modified Bayer-grade ores, is 34,000,000 tons. The total reserve of bauxite of all grades is approximately 75,000,000 tons. Reserves are estimated on a mined and dried basis. Data available to the Bureau of Mines in 1948 to 1949 were used in preparing Table I, which shows a breakdown by grades of bauxite for about a half of the reserves of the state. The modified Bayer ore, 10,555,500 long dry tons, is based on a cutoff of 8 to 15 pct silica. The sub- marginal 10,074,700 long dry tons is assumed to contain more than 40 pct gibbsite, more than 15 pct silica, and less than 32 pct available alumina. A considerable amount of this low grade material was consumed in 1949 and 1950. Additional tonnages of bauxitic and kaolinitic clays are indicated by the Bureau of Mines drilling project.' Applying a 50 pct factor to arrive at long tons mined and dried, the results of this project are approximately 31,500,000 tons kaolinitic clay at +35 pct Al²O3 and 11,800,000 tons kaolinitic clay at 20 to 35 pct A1,0,. Total reserves of kaolinitic clays are probably quite extensive—several times the reserves shown in the Bureau's work. Total reserves of bauxitic and high iron clays from the drilling program and previously established figures are 63,980,000 tons. The mineral dressing methods,' the lime-sinter process, he lime-sinter modification of the Pederson process," the lime-soda sinter process,"-' and the Alcoa combination processa. have been described in the literature and will not be elaborated upon here. The less familiar Vereinigte Aluminium-Werke process used by the Germans during World War 11 may require some amplification. It was used to bene-ficiate boehmite ores containing 12 to 18 pct silica for a feed to the European Bayer process. Ore was

Jan 1, 1952

By Gerald C. Mathis

FERGUS County, Mont., shown in Fig. 1, is known for its once famous gold mines near the old towns of Gilt Edge, Maiden, and Kendall. But at Heath, a small farming community near the foothills of the Snowy Mountains, thousands of tons of gypsum have been mined since 1916. The value of the gold taken from the mines of Fergus County runs into millions of dollars; the value of the products made from the gypsum of the Heath mine is also in the millions. The gypsum mine will continue to produce for many years, while the gold mines are closed today. The Heath gypsum mine was developed by the Northwest Gypsum Co. in 1916. The products of the small mill built by this company were plaster, agricultural gypsum, and raw gypsum for cement manufacturing. The United States Gypsum Co. prospected the adjacent property in 1916 and 1917 by means of two adits and some exploration drill holes. During World War I, the company abandoned operations at Heath, but again became active in this area in 1928 hen it purchased all the property of the Northwest Gypsum Co. A long range program of expansion was begun with the building of a block plant and the purchase of additional land and mineral rights. A modern wall board plant was built in 1936. When the old wooden mill purchased from the Northwest Gypsum Co. burned in 1937, an all-metal calcining plant located at Blue Rapids, Kansas, was dismantled, moved to Heath, and erected on the site of the mill. In August 1951 a new mine was opened 3000 ft north of the mill. Rock is conveyed from the mine to the mill by an 18-in. belt conveyor. The Heath gypsum deposit lies at the base of the Ellis formation of Jurassic Age. The Ellis at Heath lies unconformably on the black fissle shale of the Heath formation of the Big Snowy Group, which is Mississippian in age. The strike of the gypsum bed is N45°E and the dip approximately 3" NW; the regional strike and dip of the area. The gypsum lies in a series of six layers separated from each other by thin seams of shale. The lower layer is composed of' gypsum and shale intermingled and is not of commercial grade. The upper five layers are high in purity, but only the middle four layers are mined on the advance, as the top layer is left for roof support. This top layer is mined on retreating operations at the same time the pillars are robbed. Total thickness of the gypsum layers varies from 12 to 14 ft. Fig. 2 shows the average thickness and arrangement of the layers. Mining Methods The mine was originally developed by driving an adit into the gypsum horizon. The Northwest Gypsum Co. mined in the top four layers, the top layer being split, leaving about 12 in. for roof support. A modified room and pillar method was used: entries were 15 ft wide and rooms varied between 20 and 30 ft and were turned on 90" from the entries. Crosscuts between the rooms left pillars from 10 to 20 ft square. The rock was loaded by hand into 1-ton mine cars and pulled to a central gathering point by mules; from the gathering point, mules or horses were used to pull the string of cars to the mill tipple. This method was continued by the United States Gypsum Co. from 1928 to 1937.

Jan 1, 1954

By Adam L. Wesner, A. C. Richardson

DURING World War II the demand for electrode carbon was greater than could be met by the supply of petroleum coke available for this use. It was believed that coke made from an extremely low-ash coal might be a suitable substitute for petroleum coke. Requirements for electrode carbon to be used for the production of aluminum are that the silicon plus iron content shall be not more than 0.14 pct of the coke. However, during the period when petroleum coke was in short supply, it appeared that relaxations of the specifications might be allowed to permit 0.4 pet iron plus silicon in the coke. For this work, the specifications were that the coal should contain less than 1 pet of ash, and the combined iron and silicon content of the coal should not exceed 0.28 pct. Heavy-liquid separations made on a number of coals showed that if certain size fractions of some coals were separated at low specific gravities the resulting float products would meet the required specifications. The objective of this work was to develop a continuous, commercially feasible process for producing low-ash coal. After consideration of various processes, the method chosen was a float-and-sink separation using a solution of calcium chloride as the separating medium. Eagle Seam coal was used for the experiments. The -10 +35 mesh fraction was found to be the most promising feed for producing the low-ash [ ] content coal. A batch of 30 tons of -3/8-in. coal was screened at 10 and 35 mesh; the yield of -10 +35 mesh was 20 pct of the feed. This fraction comprised the feed for the separation tests. In spite of the fact that this portion was screened a second time at 35 mesh, the coal still contained 16 pct that was finer than 35 mesh. Three-fourths of the undersize was in the -35 +48 mesh range. A representative portion of the -10 +35 mesh fraction was subjected to batch float-and-sink separations to determine the best gravity to be used in the continuous tests to obtain a high recovery of low-ash content coal. The heavy liquid used was a mixture of carbon tetrachloride and benzene which assured complete wetting of all of the particles. As usual in batch separations, adequate time was allowed for each separation so that even the near gravity particles had ample time to separate. The separations were made at increments of 0.01 sp gr from 1.25 to 1.28 and also at 1.32 and 1.59. Each specific-gravity increment was assayed for ash content. From these data it was concluded that 1.27 sp gr was best for the continuous separation of the coal. The products from the batch separation were composited into float 1.27 and sink 1.27 sp-gr fractions; these were assayed for ash, iron, and silicon. Table I shows the results of the batch separations. The composite float 1.27 fraction contained 66.04 pct of the total weight, and had an analysis of 0.79 pet ash, 0.073 pct iron, and 0.112 pct silicon, or 0.185 pct iron and silicon combined. These data are indicative of the results possible if a perfect separation is made at 1.27 sp gr under static conditions. Inasmuch as the method under investigation is a dynamic system these results could not be obtained. It remained to be determined, however, just how close to the theoretical results the actual continuous separation would be.

Jan 1, 1952

By A. F. Henderson, C. F. Cornell, A. F. Dunyon, D. A. Dahlstrom

IN processing magnetic taconites several steps of crushing, grinding, classification, and magnetic separation are required to produce a 60' pct Fe concentrate. Usually the final concentrate is in a slurry form of 55 to 70 pct solids by weight and is further characterized by a particle size of 60+ pct —325 mesh. In taconite plants already completed or under construction the conventional method used to obtain pellets suitable for blast furnaces is to filter the concentrate slurry, ball the filter cake, and then harden the green pellets in a traveling grate or in a vertical shaft furnace. Large tonnages must be handled in minimum floor space, with reduced maintenance and lowest possible operating cost. Filtration must therefore achieve two objectives: I) high filtration rate—in terms of pounds of dry solids per hour per square foot of filtration area—at a low filtrate solids concentration, and 2) a filter cake moisture that will always permit efficient balling within the normal fluctuations of ' plant operating conditions. If moisture contents are too high, balling may be impossible or result in a mushy ball .without enough green strength for the firing operation. Development work has met these objectives. At low investment and operating costs, filtration rates of 250 to 600 dry lb per hr per ft2 have been attained for concentrates of 60' pct —325 mesh. By combining the disk-type continuous filter with proper agitation, the Agidisc filter produces a homogeneous filter cake, easily discharged from the disk sectors. This application provides the lowest initial cost per square foot of filtration area, minimizes floor space, reduces down time for changing filter media to a negligible factor, and simplifies process control and maintenance for the operator. It is now possible to predict very closely the taconite concentrate filtration rates for a wide variety of conditions—either by experience or with a few simple leaf tests. When balling and pelletizing operations began on a continuous basis, it became apparent that moisture content of the filter cake was a critical factor and must always be controlled by the filter operator below some maximum allowable value. Accordingly the Reserve Mining Co. and the Eimco Corp. joined in a study of the many variables affecting filter cake moisture content. The study was conducted at the Reserve Mining Co. taconite plant at Babbitt, Minn. To process plant tonnage the Babbitt plant utilizes a 6-ft diam Agidisc filter with six disks and an 8-ft diam drum filter with 10-ft face. However, most of the plant filter investigations were made on the Agidisc because of its superior performance. A considerable amount of small-scale test work was first carried out to study more closely the individual variables and ascertain their effect on filter cake moisture content. A general correlation method was then developed which allowed reasonable prediction of moisture content at any operating conditions. This step was made necessary by the fact that in full-scale filtering, operating variables usually interact to produce a combined rather than a singular effect. Studies were then made on the full-scale filters to prove the validity of the correlations developed, and past operating records were examined to ascertain whether or not significant variations could be traced to any single factor or to a combination of factors.

Jan 1, 1958

By A. G. Weber, H. J. Welge

A published calculation method for predicting incompressible, multidimensional fluid displacement has been adapted to the problems of water and gas coning in oil wells. Since depth and radial distance from the wellbore are the two key dimensions affecting the shape of a gas or water cone, coning calculations are well suited to the use of two-dimensional methods. The alternating direction implicit procedure (ADIP) was used for relaxation calculations of two-phase potentials in a two-dimensional grid. From the potentials and the capillary pressure relationship, saturation and pressure distributions were calculated which trace cone growth with time. Predictions have been made for well producing histories both before and after core breakthrough. To check validity of the method, two-dimensional calculations have matched the coning behavior and produced water-oil ratio history of a laboratory sand-packed model. They have also matched the coning behavior of several producing wells, for which the calculations were compared with produced water or gas cuts and logs showing water or gas cone movements. INTRODUCTION The application of two-phase, two-dimensional calculations using ADIP to various reservoir flow problems has been described in the literature.1-3 When adapted for computer solution, this method has proved to be a powerful tool for simulating well and reservoir behavior. This paper discusses the method as applied to well coning calculations. Single-well and coning calculations comprise an especially difficult class of two-dimensional problems which require special techniques for computer calculation and determination of reservoir characteristics. Refs. 4 through 8 describe previous approaches to the coning problem. Several examples of water and gas coning calculations, including studies on both laboratory models and producing wells, are presented here. The two-dimensional method accounts realistically for the most critical parameters affecting coning behavior, including production rate, formation stratification, horizontal and vertical permeabilities, depth of well penetration, gravity and capillary forces. The method considers the different densities and viscosities of the two phases and the relative permeability and capillary pressure characteristics of the rock and fluids. In addition to tracing cone growth in the vicinity of the wellbore, the method calculates the overall movement of the fluid interface throughout the well's drainage volume. Incompressible fluid flow is assumed to occur between the producing interval and the well's limit of drainage. Calculations can be made for the producing history both before and after cone breakthrough. A typical two-dimensional grid or array of blocks used to solve a coning problem contains about 400 blocks. The well's cylindrical drainage volume can be represented by about 20 radial subdivisions and the formation thickness by 20 vertical subdivisions. The grid spacing is normally smaller near the withdrawal interval to define the cone shape accurately. For this work we used an IBM 7074 digital computer having a core memory of 10,000 ten-digit words. A typical study, covering 5 to 10 years of well producing history, required from three to six hours of computing time. MATHEMATICAL SIMULATION OF CONING BEHAVIOR BASIC METHOD In coning calculations, the reservoir volume drained by the producing well is represented by a two-dimensional system of blocks as shown in Fig. 1 for water coning studies. The horizontal dimensions of the blocks increase with radial distance from the well axis in geometric progression, i.e., the block size is small near the wellbore and large near the well's drainage radius (re). Vertically, the blocks are bounded by horizontal planes located at different depths through the

Jan 1, 1965

By A. D. Schwope, L. R. Jackson, A. M. Hall

IN the course of an extensive investigation of the comparative properties of several types of copper, data were obtained on the cold working and subsequent recovery and recrystallization of the copper. In this paper, relations between the degree of cold work and the course of recrystallization are developed. In particular, it is shown that the course of recrystallization over long periods of time and at low temperatures can be predicted with reasonable accuracy from short-time high-temperature recrystallization data. MATERIALS USED IN THE INVESTIGATION Three types of copper were used in this investigation; these were tough pitch, OFHC, and OFHC copper with 15 oz per ton of silver added identified herein as Lots C, D, and F, respectively. The material was supplied by the American Metal Co. Ltd., and processed by the Rome Cable Co. The analyses of the three types of copper are given in Table 1. Originally, it started as wire bars 4 X 4 X 54 in. These bars were heated to 871°C in air and hot rolled to 3/8 in. rod. This rod was cold drawn to 0.204 in. rod (70 pct reduction) in three passes and annealed at 427°C for 4 hrs. A portion of the 3/8 in. rod was saved for more detailed cold-drawing experiments. Starting with the annealed 0.204 in. rod, hard-drawn wires were produced by cold drawing to 0.081 in. wire in 7 passes (84.4 pct reduction in area). Half-hard wires were made by cold drawing the 0.204 in. rod to 0.102 in. wire, (75 pct reduction) in 6 passes and annealing at 427°C for 4 hrs. This annealed wire was then drawn to 0.081 in. wire, (37.1 pct reduction) in 2 passes. Square rod was made by hot rolling wire bars to 9/16 in, rod in 8 passes. This rod was then cold drawn to 0.445 in.-diam rod and annealed for 3 1/2 hrs at 538°C. It was then cold drawn to 0.325 in. rod and again annealed at 538°C for 3 1/2 hrs. Hard square rods were then made by cold rolling this material to 0.257 X 0.257 in. rod, a reduction in area of 20.5 pct. Half-hard square rods were made by cold rolling to 0.268 X 0.268 in. square, annealing for 332 hrs at 538°C and cold rolling to 0.257 X 0.257 in., a reduction of 8.5 pct. Soft wire or rod was made from all types of copper by annealing the hard-drawn material at 343°C for 3 hrs in steam. The grain size of the annealed 0.081 in. wire varied slightly among the three lots: from 0.015-0.025 mm in the silver-bearing OFHC to 0.035-0.045 mm in the OFHC copper. The annealed 0.257 in. wires were more uniform in grain size, averaging about 0.035-0.045 mm. Representative structures are shown in Fig I. EFFECT OF COLD DRAWING AND TENSILE STRAIN ON STRENGTH OF COPPER Conventional tensile tests were performed on the three types of copper in the various degrees of hardness described above. Results of these tests are tabulated in Table 2. The results in Table 2 are

Jan 1, 1947

By W. T. Turrall, M. J. Cook

A discussion of modern developments in beneficiation of fine sizes of anthracite, this paper includes a description of the plant flowsheet, an analysis of operating results, and a summary of fundamentals of mineral separation relative to plant operation. DURING the past several years Lehigh Naviga-tion Coal Co. has installed equipment at Tamaqua and Lansford collieries for cleaning and sizing No. 4 buckwheat —3/32 + 3/64 in. and for recovering and cleaning flotation coal —20 + 200 mesh at Tamaqua colliery. Papers describing some of these installations have been presented to AIME. At Coaldale colliery, however, methods used to clean fine coal were inadequate and inefficient. Management decided upon a thorough investigation of all existing processes before building a plant to treat the combined three sizes mentioned. Investigation, carried out on company property and at other plants, entailed a study of hydrotators, hydroclassifiers, tables, spirals, flotation machines, methods of screening, and methods of dewatering. On the basis of this investigation a flowsheet was designed which necessarily excluded many processes in use, and the writers wish to emphasize that no criticism is implied by omission of processes or machines. A determining factor in selection of many machines was the policy of standardizing equipment wherever possible. Flowsheet and Operational Data The first principle to be considered in designing of any plant is efficiency of cleaning as related to laws of classification. Beneficiation of coal may be described as separation of two materials having different specific gravities. Although there is an inherent ash content even in the purest coal which slightly affects its specific gravity, it is recognized that many particles are true middlings. The percentage of these particles allowable in the final product depends upon the ultimate ash, or specifications of the consumer. Richards in his study of free settling and hindered settling classification' determined that particles of equal size and different specific gravities had unequal settling velocities. He also determined a definite size relationship for equal settling velocities with free settling and hindered settling conditions. Considering the design of machines used to clean No. 4 and No. 5 buckwheat, it may be assumed that both free settling and hindered settling conditions exist and that ratio of size for practical operations is between the established values. The essential factor is that the more efficiently and closely sized the feed is maintained, the more nearly perfect the resulting separation. Flowsheet design was governed primarily by factors related to the 1200 to 1500 tons per hr feed to the main plant. It should be stressed that because of the many sources of supply from mine and stripping, the physical characteristics of this feed varied considerably. The most significant influence was varying percentage of fines, necessitating that all machines be capable of operating under maximum peak load during periods of surge. Since cleaning practice is a wet process, about 9000 gal per min containing 14 to 15 pct solids, or 350 tons per hr, must be treated. This slurry contained all the fines, or —3/32 in., but also percentages of oversize, up to 1 % in., dependent on spills or breaks in screen jackets, a not uncommon occurrence in preparation plant practice. The flowsheet developed is shown in Fig. 1. Circled numbers represent points of sampling. Table I gives operational data including size, ash by size, composite ash, rate of flow in gallons per minute, percent solids dry weight, and average tons of solids per hour. It should be noted that these results are subject to human error in sampling practice. Detailed information reported is a representative evaluation of plant operation.

Jan 1, 1954

By R. B. Rosene, G. L. Foster, A. R. Hendrickson

he properties of some of the common fracturing oils, such as sand-falling rate, fluid loss and viscasity, are a function of the three major constituents of the oil. These are: asphaltic material, parafin waxes and a base oil. The base oil can be either high or low viscosity. Asphaltic material increases viscosity by thickening the oil, decreasing the rate of fall of sand through the oil. at temperatures up to 200" F. When large arnorrnts of parafin wax are present, much of the wax i.s not dissolved, but is present in the form of rnicroscopic crystals. 7'his, of course is limited to temperatures below the melting points of waxe.s. As a result, parafin waxes clo not function primarily as thickener.7, but rother as bullting materials. The functiori of wax, without asphaltic material, in a low viscosity base oil is uniquely unlike that of wax with asphalt coexistent in the oil. The resulting difierence in wax crystal size governs the sand-falling rate to a large extent. An ideal type of fracturing oil is one containing neither asphalt nor waxes. In such cases, the viscosity and resulting low sand-falling rate are apparently due to soluble resin- ous hydrocarbons, which are compatible with formation oils. INTRODUCTION Since the introduction of hydraulic fracturing as a method of stimulating production from oil and gas wells, a variety of fluids have been employed to open the fractures and carry the propping agent. Such fluids include gels, emulsions, and oils. In the latter category, the use of refined oils has increased tremendously, and it is probably safe to assume that such oils represent more than one-half of the total fluid used in fracturing. The general acceptance of refined oils for fracturing can be accounted for on the basis of their relatively low cost and general applicability. To minimize transportation costs, such refined oils are generally obtained within the local areas of operation. As a result there are several kinds of oil used in different areas, with a wide variation in the basic composition. These types may vary from a fair grade of lubricating stock to a highly viscous cut-back asphalt. or road oil. Originally, little attention was paid to the composition of the oils used for fracturing, and any oil which would carry sand was considered satisfactory. Recently, however, service companies and well operators have become more concerned with the type of oils used for fracturing. With this in mind, the present work was undertaken to evaluate and compare many widely used fracturing oils to determine which constituents were most desirable for fracturing purposes. Some of the important properties of fracturing fluids are sand-falling rate, viscosity, and fluid loss. Other properties, that are actually of no less importance, include flash point, pour point, emulsifying tendencies with formation brines, and compatability with the formation oils. This discussion has been limited, however, to the first mentioned properties in order to give some idea of the general composition of the refined oils, how they function, and why. PROPERTIES OF FRACTURING OILS The properties of fracturing oils are a function of the three major constituents of the oil. These may be designated as: (1) asphaltic material, (2) paraffin waxes and (3) a base oil, which may be of either high or low viscosity. The asphaltic material clas-

Jan 1, 1956

By J. R. Hornaday, A. E. Morris, N. A. Parlee, D. C. Carmichael

Rates of absorption and effusion of hydrogen in solid iron were measurede by a Sieverts type of apparatus. With clean a iron these rates are diffusion controlled down to 420°C and are represented by the equation D = 6.70 x e-'100' crn2 sec-I Certain surface impurities can affect these rates at all temper-atuves. Thin oxide films lower, the apparent diffusivity of annealed iron markedly. Cold-worked iron (75 pct) annealed at 430°C has practically the same solubility and diffusivity as anealed iron. THE mechanism of absorption and evolution of hydrogen in solid iron alloys is not fully understood despite the large number of investigations on the subject. While there appear to be many instances of simple solid-state diffusion control of rate, there are many cases where investigators have either concluded that surface reactions are rate controlling or that some "nondiffusible" hydrogen resides in discontinuities. The purposes of this research were 1) to develop a sound method for studying this absorption and evolution behavior, 2) to examine it in pure annealed iron, and 3) to determine the effects of important variables, such as cold work, surface condition, and composition. This paper relates the progress toward these objectives. Much of the present knowledge of the movement of hydrogen through iron alloys comes from permeability studies which involve the measurement of the rate of passage (under steady state conditions) through membranes of the order of 1 mm in thickness. This method is open to question on various grounds. If surface reactions are involved, two different surfaces operating under two different conditions must be considered. The presence of defects in the membrane even of microscopic dimensions may lead to erroneous results. A few people have studied evolution of hydrogen into vacuum, under carefully controlled (unsteady state) conditions, and some of the best diffusivity data come from these sources. Most of these methods measure rates of evolution only and thus do not make a rigorous test for reversibility of behavior. It appeared that an "unsteady state" method that would permit the measurement of both rates of evolution and absorption under controlled temperature, pressure, and other conditions would offer several advantages. Accordingly the modified Sieverts apparatus described below was designed and built. APPARATUS This apparatus is shown in Fig. 1. The sample bulb is detailed in Fig. 2. Hydrogen of 99.5 pct purity and argon of 99.99 pct purity were used. The hydrogen was deoxidized and dried by means of a Deoxo unit followed by a "Dri-erite" tower. The argon was only dried. The gas burette was graduated in tenths of a cubic centimeter, and, with the aid of a travelling magnifier, readings could be estimated to the nearest 0.01 cc. The level of mercury in the burette was adjusted by means of a leveling bulb operated by a fine screw adjustment. An electrical system, consisting of two slightly separated platinum electrodes inserted in one leg of the manometer and a small light bulb was used to obtain rapid accurate adjustment of the pressure. The capillary tubing of the Vycor sample bulb was 3 mm bore as was all tubing back to the gas burette. The samples were discs made from vacuum-melted Ferrovac-E iron of greater than

Jan 1, 1961

By D. W. Loughridge

INTRODUCTION Raising capital in the 1990s is a timely subject. However, many of us thought why should raising capital in the 1990s prove to be unlike it was in the 19805, the 1970s, the 1%0s, or earlier? There are a lot of creative people in banking and in corporate treasury departments. New tools and techniques are continuing to emerge, many of which are discussed in other papers in this book. While we have new financing tools at our disposal, the underlying issue has not changed. Projects and investments must be judged on their own merits. If they cannot be justified by conventional financial analysis, they should not be built. If they can be justified, it is likely that the financing will be available. The challenges faced in raising capital in this decade will persist to the next. The issues of the 1980s -- currency fluctuation, disruptive merger and acquisition activity, commodity price volatility, political risk, and debt crisis -- will all persist in an increasingly international business environment. I will focus on the financing we have just completed for the Escondida Copper Project in Chile. The Escondida financing is structured along the classic project financing model developed in the late 1970s, but it deals with issues of the 1980s and the 1990s. The financing was intriguing, not just because of the technical issues involved, but also the challenge of reaching an agreement in a large and diverse group. Escondida had the one essential feature that made its financing possible. It was commercially very attractive. It would produce at low cost a commodity (copper concentrates) that direct consumers felt would be in tight supply. The project had the direct support not only of its sponsors, but also its customers, and, very importantly, its host government. The non- recourse financing of Escondida would not have been possible without the support of these parties, and without the robust economics that made this effort worthwhile. The issue was more complicated. Operations in all parts of the world entail some political exposure. This project is in Chile, where there was a constitutional requirement that a plebescite be held when the project would be in its early stages. This plebescite would determine the fate of a 15 year old military dictatorship. The project is copper, a commodity generally deemed to be in surplus. Copper has a history of price volatility (whose price has varied from $.58 to $1.53 per pound over the past two years). It is politically sensitive, not only in Chile, but in the United States, Canada and other developed countries. The project is international, with all the problems of dealing with a variety of currencies, a variety of cultures, and a variety of laws and commercial practices. The project is also large and capital intensive, with a total cost of U.S. $1.1 billion. ESCONDIDA PROJECT Escondida, the largest known copper ore body in the world, was discovered in March of 1981, by Utah International in a joint venture with Getty Oil Company. In 1984, both Utah and Getty were involved in ownership changes, Utah being acquired by BHP. A later restructuring of the ownership of Escondida resulted in BHP, as manager, carrying a 60% interest, Rio Tinto-Zinc Corporation (RTZ) 30%, and a consortium of Japanese companies led by Mitsubishi Corporation with 10%. The Japanese consortium is incorporated as JECO (Japan Escondida Corporation). This ownership structure, which spread ownership around the world, was the first tangible step toward managing both the commercial and political risk associated with the project.

Jan 1, 1990

By W. A. Tiller, D. H. Lane

A simple zone melting technique for investigating the effect of ultrasonic irradiation upon ingot solidification is described. The effect of i) ultrasonic power level, ii) freezing velocity, iii) constant or variable frequency, iv) direction of irradiation, and v) transducer-cozlpling bar joint upon the grain size of type 316 stainless steel have been investigated. The results of this study support the postulate that the ultrasonic vibrations increase the nucleation probability in the layer of liquid adjacent to the freezing interface. In the first paper of this series,l the possible mechanisms whereby ingot structure may be altered by irradiating a solidifying melt with ultrasonic vibrations have been discussed. A new technique for efficiently introducing the ultrasonic energy into the solid-liquid interface region was presented and applied to ingot preparation by the consumable-electrode arc-melting technique. The experimental results support the postulate that the ultrasonic vibrations may refine the ingot structure by increasing the nucleation probability in the zone of liquid adjacent to the solid-liquid interface. The present paper describes the application of the same technique to a relatively simple laboratory-scale zone-melting apparatus. This apparatus is found to be well suited to the detailed study of ultrasonic technology in this area and allows one to determine, in particular, the minimum ultrasonic power level needed to produce a certain grain size in a particular material. The results of this study support the nucleation mechanism for grain refinement, but do not provide any deeper insight into the specific nucleation mechanism responsible for the effect. EXPERIMENT The apparatus used in these experiments is shown in Fig. 1 and illustrated schematically in Fig. 2. The material to be studied, type 316 stainless steel, was in the form of a 3/4-in. sq bar 30 in. long. This bar was placed in a square open-topped mold with open ends made from high-purity graphite coated with a flame-sprayed Al2O3, skin. Surrounding the crucible was a molybdenum susceptor with 3/8-in. diam holes spaced at 1-in. intervals along its length to serve as sight ports. A tapered transducer horn was brazed to one end of the specimen. The entire assemblage was enclosed in a quartz tube, the transducer itself projecting out one end and resting in a cooling tank. A vacuum seal between the coupling bar and the end plate enclosed one end. A similar plate and seal enclosed the other end. The system is gas tight and can be operated under vacuum or an inert atmosphere. For these experiments, flowing argon at 15 in. of Hg pressure was used. The heat source for melting the stainless steel specimen was a 2-in. long 3-kc induction coil placed around the quartz tube; this source heated the susceptor, inductively melting about a 3-in. zone of the sample by radiation. To move the molten zone at a specified rate, the induction coil was moved down the tube at this rate with the aid of a simple pulling device. Thus, the sample could be irradiated at varying ultrasonic frequencies and power levels and could be solidified at varying rates. The power input to the transducer was measured using a "John Fluke Model 120 VAW-Meter." 1 The power delivered to the interface region is probably only about 50 pct of that measured on the VAW-meter. In a typical run, when the ultrasonic power was turned on, the interface of the molten zone closest

Jan 1, 1961