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By Eckhard Nembach

The phase diagram of the system Pb-In has been investigated between -27° and + 40°C, using nzainly X-ray dijfraction. In accordance with t her mo dynamic measurements by Heumann and Predel, a segregation occurs at low temperatures, though not in the form of a nziscibility gap. THE phase diagram of the system Pb-In has been the subject of extensive investigations,1&apos;1 but recently Heumann and prede13 concluded from their thermodynamic data that a new feature should occur below room temperature. These authors observed that the maximum values for the enthalpy and entropy of mixing, which occurred at a composition of 50 at. pct Pb, were +400 and —1.7 cal per g-atom deg, respectively. From this the authors estimated that a miscibility gap should occur below 30°C, centered at 50 at. pct Pb. Resistivity measurements seemed to support this view. These authors proposed the phase diagram outlined in Fig. 1. Three phases exist at 30°C: the tetragonal indium phase with c/a > 1, the tetragonal intermediate phase a, with c/a < 1, and the fcc lead phase. During an investigation of the superconducting properties of Pb-In alloys. it has been observed4 that aging a specimen with 50 at. pct Pb for 14 days at -18°C decreased the superconducting transition temperature about 0.13"K and tripled the transition width. In this paper, the results of an investigation of the Pb-In phase diagram in the temperature range from — 2T to +40°C are reported. Superconductivity and X-ray methods have been used. 1) SPECIMEN PREPARATION The materials were provided by the American Smelting and Refining Co. According to the manufacturer their purity was 99.999 pct. The weighed amounts of the constituents were sealed in quartz tubes under an atmosphere of 10 torr helium, mixed for 24 hr in a rocking furnace at 380°C, quenched in ice water, and homogenized at 20" to 30°C below the solidus line, established by Heumann and Predel. The annealing times were 144 hr for specimens containing Less than 30 at. pct Pb and 36 hr for the remainder. 2) SUPERCONDUCTIVITY EXPERIMENTS The specimens were quenched from the homogeniza-tion treatment into ice water and their superconducting transition temperatures T, measured. The procedure used has been described in Ref. 4. The transition was detected by the change of the mutual induc- tance of two coaxial coils containing the sample. T, was defined as the temperature at which 50 pct of the total change in inductance had occurred. The repro-ducibility with which T, could be measured was i0.002"K. Then the specimens with lead contents between 38 and 75 at. pct were aged for 7 days at temperatures between -30" and 40°C. If this treatment caused T, to change by more than 0.005"K or the width of the transition to increase by more than 0.002"K, it was concluded that the specimen had undergone a phase change and no longer consisted only of the fcc lead phase: as it did immediately after homogenizing. The result is shown in Fig. 2. From this one can estimate at what temperatures and concentrations phase changes occur. The X-ray measurements were based on these preliminary results. 3) X-RAY EXPERIMENTS Because of the softness of the material, relatively coarse powders. 75 p, had to be used, which were filed in a helium atmosphere from homogenized specimens. The powders were annealed at least 30 min at temperatures between 120" and 16OJC, depending on their concentration, and quenched in ice water. Then their X-ray patterns were taken at -178°C with a Picker diffractometer, model 3488K, and a cold stage. on which the specimen was in thermal contact with a liquid-nitrogen reservoir. In this way the following relation was established for the fcc lead phase: a = 4.697 + 0.00247C for 40 5 C 5 75 11 where n is the lattice constant (A) and C is the at. pct of lead. The coarseness of the powder made it impossible to use lines with 0 > 75 deg; therefore n was averaged from lines with 45 deg 5 0 5 75 deg. The results were reproducible to within i0.05 pct. Relation [I] is very similar to the one found by Heumann and Predel at room temperature. Following this, homogenized specimens with compositions between 15 and 56 at. pct Pb were aged for at least 10 days at temperatures between -27" and

Jan 1, 1970

By Robert S. Shoemaker

Recently we read a short article which stated that Marcona Corp. was studying the use of 25,000-hp autogenous grinding mills for an iron ore project in Alaska. As if that weren&apos;t enough, they were going to dispense with the primary crusher and feed run-of-mine ore to the grinding mills which were to be driven by wrap-around seven-cycle motors. We see also that Bougainville Copper Co. will be grinding 90,000 tpd of ore in only eight 4250- hp ball mills. At Bougainville too, their float section will be the first large one to be completely equipped with the new 350-cu ft flotation cells. After a half century of relatively peaceful growth in the minerals industry, we are now seeing almost exponential advances in both equipment and plant size. At the same time, we are seeing a constant blending of hydro and pyrometallurgical techniques and processes into minerals beneficiation until the sample grind-&apos;em-up-and-concentrate-&apos;em plant is becoming a rarity.

Jan 1, 1970

By C. S. Giggins, F. S. Pettit

The oxidation properties of Ni-Cr alloys with fine grains, coarse grains, and deformed surface layers have been studied at temperatures of 900" and 1100°C in 0.1 atm of oxygen. The oxidation rates of alloys containing between 10 and 30 wt pct Cr have been found to be dependent upon the grain size of the alloy. Finegrained alloys had smaller oxidation rates than coarsegvained alloys because of the selective oxidation of chromium at alloy grain boundaries. In this compositional range alloys with deformed surface layers behaved similar to fine-grained alloys due to recrys-tallization of the deformed surface layer. In the preceding paper1 it was found that during the oxidation of Ni-Cr alloys, the volume fraction of precipitated Cr2O3 could be greater at alloy grain boundaries than at other areas of the alloy surface. In the case of alloys with chromium concentrations equal to or greater than 30 pct,* the volume fraction of Cr2O3 *AIL compositions are given as weight percent unless specified otherwise. precipitated at grain boundaries and within grains on the alloy surface both exceeded the critical amount required for lateral growth of the Cr2O3 particles and the surfaces of these alloys were completely covered with a continuous, external layer of Cr203 during oxidation. However, in the case of alloys with chromium concentrations between approximately 5 to 30 pct, the volume fraction of precipitated Cr2O3 exceeded the critical value required for external scale formation only at grain boundaries.but not within the interior of the grains. Consequently, the surfaces of these alloys had external scales of Cr3O3 over the grain boundaries but internal Cr2O3 subscales with external scales of NiO away from the grain boundaries. Under these latter conditions, it was found that chromium could diffuse laterally in the alloy from those areas covered with an external layer of Cr2O3, i.e., grain boundaries, to areas where the Cr2O3 was present as a subscale. This diffusion of chromium resulted in an increase in the volume fraction of Cr2O3 precipitated in the sub-scale zone and continuous layers of Cr2O3 could be formed at the subscale front in these regions. For the alloys used in the previous studies,&apos; continuous layers of Cr2O3 were formed on Ni-20Cr alloys in the subscale regions after approximately 30 hr of oxidation at 900°C. For shorter periods of oxidation, the Cr2O3 layer was semicontinuous with the continuous portion at the subscale front emanating from points where the Cr2O3 had been formed as an external scale over alloy grain boundaries. Some lateral growth of a Cr2O3 layer in the subscale region was observed on Ni-15Cr and even Ni-10Cr alloys but this layer was never continuous after 30 hr of oxidation. These results indicate that the selective oxidation of chromium in Ni-Cr alloys with chromium contents between 5 to 30 pct may be dependent upon the grain size of the alloy. Fine-grained specimens in this compositional range should have a larger fraction of the surface covered with external Cr2O3 than coarsegrained specimens and the subscale areas required to be sealed via lateral diffusion of chromium should be smaller. It is therefore to be expected that a continuous layer of Cr2O3 can be formed on alloys in this compositional range after short periods of oxidation providing the alloy grain-size is sufficiently small. bo studieS2,3 have established that the oxidation behavior of alloys can be significantly influenced by pretreatments which produce mechanically deformed surfaces. It has been found that deformed surfaces usually promote the selective oxidation of elements in alloys and it is believed that these effects are due to rapid diffusion of elements in the deformed layer. In view of the previous results,&apos; which showed that alloy grain boundaries may play an important role in the selective oxidation of chromium in Ni-Cr alloys, deformed surfaces may promote the selective oxidation of elements in alloys as a result of the numerous grain boundaries formed on the alloy surfaces via recrys-tallization during heating to the oxidation temperature. The purpose of the present studies was to determine the effect of alloy grain size and surface deformation on the selective oxidation of chromium in Ni-Cr alloys at temperatures of 900" and 1100°C in 0.1 atm of oxygen. EXPERIMENTAL The average grain diameter of the alloys used in the previous studies1 was not less than 0.04 mm and alloys with compositions between 5 and 30 pct chromium had average grain diameters between 0.04 and 0.14 mm. Since the oxidation kinetics were already available for these relatively coarse-grained alloys, it was desirable to use these same alloys in the present studies. The surfaces of the alloys listed in Table I of the previous paper were deformed by using a Model F S.S. White Industrial Airbrasive Unit, which delivered a controlled mixture of 25 µ Al2O3 particles in a stream of dry air at high velocity against the surface of a specimen. The amount of surface deformation produced by this treatment was not determined but a re-crystallized layer about 15 µ thick was formed upon annealing deformed specimens. The grain size at the surface of the specimens was reduced to an average grain diameter of 0.01 mm by annealing the deformed specimens, i.e., grit-blasted,

Jan 1, 1970

By J. A. Roberson, A. M. Adair

A plate of an 18 pct Ni (250 grade) maraging steel was homogenized, cold rolled, and re crystallized to produce a fine grained, homogeneous structure. The strength properties were then measured as a function of cold rollinq prior to aging. Material in the solution heat treated condition exhibited substantial strengthening from cold rolling. The strength increase and the rate of strengthening were proportional to the amount of cold work. This benefit, of up to 50 ksi, was retained during aging for 3 hr at 900°F. The structures produced by cold rolling and aging have been systematically investigated by transmission electron microscopy. The dislocation debris produced by cold work influences the morphology and distribution of precipitate particles as well as the rate of precipitation. An essential feature of the high nickel maraging steels is a martensitic transformation from y to a with the resultant production of a supersaturated bcc solid solution. This solution decomposes to form precipitates during a subsequent aging treatment.&apos; The martensitic transformation in low carbon Fe-Ni alloys and the mechanical properties of these alloys have been studied extensively.2"4 The carbon content of maraging steel is kept very low to avoid the embrittling Fe3C phase and to minimize the acicular, or twinned martensite common to high carbon steels. Maraging steels are usually strengthened only by heat treatment, but cold working is also quite effective in this respect as was shown by Decker, Eash, and Goldman,&apos; Kula and Hickey,5 and the present work. There is, however, some disagreement between the present results and those of Kula and Hickey. Because of their unusual combination of strength and toughness, the maraging steels are suitable for applications where reliability at high stress levels is required. The strength level is achieved through a combination of solid solution hardening,&apos; substructure hardening,3 and precipitation hardening,6 of which the last is the most important. The toughness of these steels has been reported to be a result of the absence of brittle grain boundary precipitates,7 and the fact that the matrix is a massive martensite rather than a twinned martensite.&apos; One of the problems in the manufacture and use of maraging steel has been its tendency to develop laminations in sheets parallel to the rolling plane.9,10 The present investigation was intended to determine whether or not an improvement in the microstructure of this steel by thermomechani-cal processing would improve mechanical properties. I) EXPERIMENTAL PROCEDURES A plate ($ in. thick) of an 18 pct Ni-250 grade maraging steel* was obtained and examined metallo- "Analysis, wt pct: 18.1 Ni, 8.6 Co, 5.3 Mo, 0.4 Ti, 0.07 Mn, 0.05 Cr, 0.05 Si, 0.002B. 0.1 Cu. 0.05 Al. 0.002 Zr, 0.016 C, balance Fe. graphically. It was found to contain laminations as described by previous investigators. This plate was then annealed at 2100°F for 24 hr to promote homogeneity. Pilot studies on small coupons had shown that this was the minimum temperature required to accomplish homogenization in 24 hr. Since this treatment caused excessive grain growth, the steel was subsequently cold rolled and recrystallized. Cold rolling was accomplished at about 5 pct per pass to a total reduction of 66 pct. The standard solution annealing treatment (1 hr at 1500°F) was adequate to cause recrystallization of the cold worked steel. The recrystallized steel was then cold rolled and ground by various amounts to produce specimens with uniform thickness and selected amounts of cold rolling. All tensile specimens with less than 90 pct cold reduction were ground to a thickness of 0.050 in. Specimens with 90 pct cold reduction were 0.025 in. thick. All

Jan 1, 1970

By F. H. Froes, D. H. Warrington

Electron microscope evidence which indicates that TaC may precipitate at random sites in the matrix is presented. Initially the particles are almost spherical and coherent with the matrix. However, as they grow in conditions in which there are insufficient vacancies to relieve lattice strain, the particles rapidly lose coherency in two directions and continue to grow as plates with approximately the full lattice mismatch strain present perpendicular to the plane of the plate. The necessary relief of strain comes from dislocations loops which do not become visible until the later stages of aging. The rapid decrease of apparent strain to low values of appoximately 1 pct at small particle sizes arises not from a complete incoherency but from applying a model wrong for the particle shape and strain distribution. PREVIOUS work has shown that MC-type carbides may precipitate intragranularly in austenitic stainless steel on dislocations,1&apos;2 in association with stacking faults,3&apos;4 and randomly through the matrix,5-7 In investigations of the matrix precipitate by thin-foil electron microscopy, considerable lattice strain has been found to occur around the precipitating phase.7&apos;8 Attempts have been made to evaluate the amount of lattice strain by using the methods developed by Ashby and brown.9,10 Values of the linear strain, much less than the 17 pct theoretical mismatch (for TaC), have been reported; it has been suggested that this is due to either a loss of coherency1&apos; or vacancy absorption which occurs during either the initial nucleation or growth of the precipitate." This report is an extension of earlier work7 that dealt with the precipitation of TaC from an 18Cr/12Ni/ 2Ta/O.lC alloy after it had been quenched from 1300°C and aged between 600" and 840°C. In particular, the shape of the precipitate particles and the amount of strain in the matrix, due to the precipitate, have been studied. The work described here is part of a wider investigation of factors that affect carbide precipitation in austenitic stainless steel," details of which are to appear elsewhere. RESULTS The present investigation can be conveniently split into two aspects of the strain-fields surrounding the matrix particles: 1) information derived from the strain-field which indicates the shape and habit plane of the precipitate particles and 2) the magnitude and sign of the strain-field. The Shape and Habit Plane of the TaC Precipitate. In the early stages of aging twin lobes (normally black F. H. FROES, formerly at the University of Sheffield, Sheffield, England, is Staff Scientist, Colt Industries, Crucible Materials Research Center, Pittsburgh, Pa. D. H. WARRINGTON is Lecturer, Department of Metallurgy, University of Sheffield. Manuscript submitted November 1, 1968. IMD on white background, i.e., for the deviation parameter, S > 0) that indicate the strained region of the matrix define the position of the particles by bright field transmission electron microscopy. The actual particles were not detected until they were approximately 120Å diam; below this size they were too small to be imaged in the electron microscope. This meant that particle growth that had occurred before this stage had to be inferred from the matrix strain-field contrast. In all cases when diffraction effects were observed from the precipitate particles, a cube-cube orientation relationship (i.e., (llO)ppt Il<llO>matrix and {1ll }ppt {III} matrix) existed between the precipitate and the matrix. From the matrix precipitate particles lying along edge-on {111} planes (e.g., at A, Fig. I), the precipitates are seen to be plate-like with their diameter being roughly 18 times their thickness after 5000 hr at 650°C. However, the exact shape of the particles cannot be determined because of the masking effect of the strain-field contrast. If a dark-field micrograph, using a precipitate reflection, is studied, Fig. 2, a number of the projected images of the TaC particles [on the (110) foil surface] apear to have straight edges parallel to projected f111) planes. Thus, it appears that in the later stages of aging the TaC particles are plate-like with some tendency for the edges of the plate to be bounded by the matrix close-packed {ill} planes (though the general shape of the particles in the plane of the plate is circular and thus the "diameter" of the particles has a real physical significance). It should be noted that the bands of fine discrete particles observed in Figs. 1 and 2 are not the matrix precipitate discussed in this paper but are precipitates associated with extrinsic stacking faults3j4 occurring on (111) matrix planes. **£** ****** \ *x 23 Fig. 1—18/12/2~a/0.1~ alloy. Solution treated at 1300°C for 1 hr, water quenched, and aged 5000 hr at 650°C. The (112) directions shown are the traces of the e&e-on (111) planes. Foil normal [110]; operating reflection (331); bright field micrograph.

Jan 1, 1970

By J. E. Dooley

Reference mass spectra and analytical correlations for 20 alkylcycloalkyl sulfides and two dicycloalkyl sulfides are presented &apos;to provide information that will facilitate the identification of sulfur compounds occurring in natural or synthetic mixtures. Reference spectra indicate relative intensities in addition to parent and base peak sensitivities. Analytical correlations establish the ionic species that reflect major fragmentation paths for the com-pounds studied. Specifically, the correlations show that base peaks are formed by several different processes: (1) Cleavage of the bond a to the ring, (2) fragmentation of the alkyl chain, and (3) fragmentation of the ring plus fragment contribution from the alkyl chain. Useful correlations for deter-mining alkyl chain length involve the CnH2+3S+ and CnH2n+1 + ions. CnH2n-2+ and CnH2n-1 S+ ions reveal the number of carbon atoms in the cyclic ring. Other important ionic species are also discussed.

Jan 1, 1970

By Thomas O. Breitling

The Mill Design Session at the Annual Meeting in New York next February will have a total of four papers. All of these papers will be concerned with the subject of in-plant dust in the hard-rock mining industry. The emphasis on efficient dust collection is timely, because dust is a problem not yet adequately covered in AIME papers. In general, dust collection should be the step following dust suppression. Dust collection and its return to the ore recovery circuit, or its waste to tailing are sources of added operating cost. If possible, dust should be kept in the main stream of ore flow by suppression.

Jan 1, 1970

By A. K. Mukherjee, J. E. Dorn

A modified Peierls model is Presented for the rationalization of the asymmetric plastic behavior of single crystals of bcc metals. The model assumes that the asymmetry of slip arises from a tendency toward asymnetric splitting of the a/2[111] screw dislocation. The approach differs from former theories however insofar as it assumes that the splitting is so minor ttut only the core energy is modified and that no real partial dislocations exist. As a consequence, the concepts of a line energy of a partial dislocation, interaction between partial dislocations, constriction energies, and stacking fault energies are not invoked. Instead the present analysis is based on a specialization of the Peierls mechanism which assumes an asymmetric dislocation core which is modified by the effective stress and permits cross slip. The theoretical predictions on the stress-temperature -strain rate and orientation relationship agree qualitatively with the limited experimental data that are currently available. Additional experimental work over wider ranges of conditions is suggested to provide more complete evaluation of the possible validity of this theory. RECENT experimental investigations on the low-temperature thermally activated deformation of bcc metals have confirmed the existence of several unique orientation effects. These will be described with the aid of the standard stereographic projection shown in Fig. 1. If slip were determined exclusively by crystal symmetry, the deformation characteristics would be symmetrical about X; = 0 and independent of whether the specimen were subjected to a tension or a compression stress, regardless of what combinations of slip planes might be operative. Experiments, however, reveal that neither of these symmetry based predictions are valid. A schematic representation of the commonly observed asymmetry of both the yield stress and the plane of slip is shown in Fig. 2. A reversal of the direction of stressing results in an inversion of the asvmmetric behavior. 1) Asymmetry bf Yielding. A detailed investigation on the asymmetric yielding in an Fe-2.7 pct Si alloy was repoEted by Tabka, Tikeuchi, and Furubayashi,1 Similar trends have been observed by Keh and Nakada on iron,&apos; Stein on molybdenum,3 Bowen, Christian, and Taylor4 on columbium, Sherwood, Guiu, Kim, and pratt5 on Ta, Cb, and Mo. The degree of asymmetry not only depends on the atomic number and alloying but, in all cases that have been examined, it also increases with a decrease in the test temperature. 2) Asymmetry of the Slip Plane. Asymmetric $I-~: curves of the type shown in Fig. 2 have been found for several Fe-Si alloys6-8,1 and columbium.4 There is general agre_ement that near X: = 30 deg slip occurs by the [111](211) mode so that ?1 = 30 deg. As X; decreases it appears that [111](211) to [111](101) cross slip takes place leading to slip band traces on intermediate planes. And as xi approaches 0 deg, sharp

Jan 1, 1970

By H. W. Kerr, B. Soutiere

THE possibility of using unidirectionally solidified eutectic alloys as high-strength composite materials has been investigated by several workers. Unidirectionally solidified lamellar and fibrous eutectics have been shown to have good short-time structural stability at temperatures close to the eutectic melting temperature.&apos;-4 Several investigations of both short-time high temperature tensile properties and creep properties of eutectic alloys have been carried out,3-" with promising results. Little work has been reported, however, on the thermal stability of eutectic alloys which have been unidirectionally solidified and subsequently deformed in compression. Since processes such as rolling and grinding introduce compressive stresses, and since the properties depend on the spacing and perfection of the composite structure10,11 this aspect is of definite importance if unidirectionally solidified eutectic alloys are to be considered for commercial use. A Cd-Zn alloy made from 99.999 pct starting materials was cast into a graphite boat and zone levelled12 to obtain a completely lamellar structure at one end of the bar. Sections from this region of the bar were removed, recast into 6.5 mm I.D. Pyrex tubing, and solidified unidirectionally upwards at a rate of 2.8 cm per hr. Specimens were cut from the solidified rods, heated in air at 200°C (0.88 of the eutectic melting temperature) for various lengths of time, and examined metal-lographically. Compression specimens were also cut from the solidified rod carefully machined to a length of & in., and deformed with the compressive axis parallel to the original growth axis to produce a total longitudinal strain of 12 pct. Some of these specimens were examined metallographically; others were heated in air at 200°C for various lengths of time and then examined. Metallographic examination of the deformed specimens showed the two types of deformation previously described; slip lines13 (smoothly bent lamellae) and kinks13,14 (sharply bent lamellae). Very close to the specimen ends there were a large number of deformation bands, but at a distance of about -re- in. the deformation was very localized, as shown in Fig. 1.

Jan 1, 1970

By R. A. Vandermeer, J. C. Ogle

Two distinct types of depth-dependent variations in texture have been observed in niobium cold-rolled various amounts up to 99.5 pct reduction in thickness. These nonuniformities are thought to be the results of nonhomogeneous plastic dewmation during rolling. The first type is characterized by a zone at intermediate depths that tends to lack certain strong orientations which are present in the surface and center layers of the rolled stock. This type of texture modification seemed to be associuted with "high" body rolling and may be related to the shape of the zone of deformation in rolling. The second type of texture inhomogeneity found involved the formation of a unique texture in the surface layers of heavily rolled strip. High fiiction forces between work piece and rolls appear to be needed to generate and maintain this texture. We believe that this unique surface texture results from a shear mode of deformation in the surface layers. THE evolution of texture in both the surface and center regions of cold-rolled niobium as a function of increasing deformation from 43 to 99.5 pct reduction in thickness was reported in a previous paper.&apos; It was noted that for strips rolled between 95 and 98 pct reduction a distinctly different texture appeared in the surface layers which was unlike the center texture. Certain other layer to layer textural variations were also detected during the experimental phase of that work but were not described in the paper. Surface textures have been reported previously for the bcc materials iron and Steel2-4 and are well known in the fcc metals.5 It is usually stated that these are shear textures which arise under conditions of high friction between specimen and rolls. Work by Mayer-Rosa and Haessner5 n niobium rolled under conditions presumed to be high roll friction gave no indication, however, of a surface texture in that material. This is indeed puzzling in view of our results.&apos; Thus we undertook additional experiments designed to study the stability of the surface texture for certain rolling variables. The variables investigated were the presence or absence of lubrication, amount of reduction per pass, and reverse vs unidirectional rolling. It is the purpose of the present paper to describe the kinds of depth-dependent textural inhomogeneities that we have observed in rolled niobium as well as to present the results of our recent experiments on the stability of the surface texture. Possible explanations for the depth-dependent texture variations will be discussed in terms of nonhomogeneous plastic deformation during rolling. EXPERIMENTAL Specimens cut from the niobium rolled to different reductions in the previous study1 were examined at various layer levels throughout the strip thickness for textural inhomogeneity. The specimen surfaces were either etched or machine ground and etched to remove material to a specific depth. Textures were determined by means of the Schulz X-ray reflection pole figure method with a Siemens texture goniometer and Cum X radiation. Since the important intensity peaks of the textures in niobium are usually located on the normal direction (N.D.) to rolling direction (R.D.) radius of the (110) pole figures, it was sufficient in many cases to scan only along this radius. At selected depths or where additional information was required the entire (110) pole figure was also obtained. In studying the stability and formation of the surface texture, experiments were conducted on 0.400-in.-thick, fine-grained, randomly oriented niobium specimens extracted from the same starting stock as that used in the earlier study.&apos; Two of these specimens were rolled at room temperature to a total reduction of 96.4 pct. One was rolled between cleaned and degreased rolls with no lubrication. The other was lubricated between passes with Welch Duo Seal vacuum pump oil. The rolling schedules of each were kept as nearly identical as possible. Drafts were of the order of 0.006 to 0.012 in. per pass. Other experiments consisted of rolling specimens at constant fractional reduction per pass, i.e., (ta- tb)/ta equals a constant where ta and tb are the entrance and exit thickness of the rolled stock, rather than at a constant draft, i.e., ta- tb equals a constant. Ten specimens were rolled at room temperature on a two-high, motor-driven rolling mill with 8-in.-diam rolls. These specimens were rolled to thicknesses of between 0.041 and 0.073 in. (82 to 90 pct total reduction) at approximately constant reductions per pass ranging from 9 to 45 pct. Kerosene was used as a lubricant. Half of the specimens were always rolled in the same direction while the other half were reversed end to end at each pass. The texture in the surface regions was determined with the X-ray technique described above. RESULTS The textural inhomogeneities noted in niobium rolled from fine-grained, randomly oriented stock 1.5 in. long by 0.75 in. wide by 0.40 in. thick can be classified into two types. The first may be discussed with the aid of Figs. 1 to 3. Fig. 1 is a three-dimensional plot of the X-ray intensity in units of times random vs f , the angle from the N.D. to any point along the N.D. to R.D. radius of the (110) pole figure, and depth, given as percent of the thickness (?t/to X 100, where at is the thickness of material removed and to is the as-rolled

Jan 1, 1970

By L. F. Elkins

In 1946 Littlefield, Gray and Godbold published a thorough geologic description of the West Edmond Hunton Lime reservoir, located in Central Oklahoma, and discussion of its early performance.l They stressed implications of the nature of the reservoir rock on performance to be expected with production both by natural means and by pressure maintenance with gas injection. The essence of their analysis was that presence of an extensive interconnected system of fractures and solution channels constituting about 10 percent of the total reservoir void space in otherwise very low permeability reservoir rock would result in severe channeling of naturally encroaching water or injected gas through the fractures with little or no benefit to ultimate recovery of oil. Considerations were in progress to unitize the reservoir for pressure maintenance by gas injection. Some other engineers involved in the project had considerably different opinions at the time regarding continuity of fractures and regarding effects of such fractures on performance. The field was unitized Oct. 1, 1947. Subsequently, pilot gas injection tests were conducted in four areas of the field; large scale waterflooding was conducted in two parts of the field in the Bois d&apos;Arc or Upper Hunton; and pilot waterflooding was conducted in the Chimney Hill or Lower Hunton. Full scale water-flooding is now in progress in the Chimney Hill section where it is oil productive. The primary purpose of this paper is to divine some of the secrets of this reservoir through analysis of all aspects of its performance, with the hope that it will be of help to engineers and operators in developing and operating other low permeability fractured reservoirs. In part, this considers variance of actual performance from some widely used conventional reservoir engineering assumptions. For brevity, other aspects of unit operation and its benefits to the owners are not discussed. Oil and Gas in Place For unit participation, net pay in the Bois #Arc defined by the gross SP anomaly on electric logs totalled 2,100,000 acre-ft in the 30,000-acre reservoir. Development of West Edmond predated modem logging techniques that now would be used to determine "net" or "productive" pay. In Fig. 1 this log pick is compared with detailed core analysis and core descripfion by Littlefield et a1.l for one well identified as A on the index map in Fig. 2. Not all of the gross Bois #Arc section had oil staining, but all cores with measureable intergranular permeability were stained. (The committee selection of the Bois d&apos;Arc SP interval also includes the Frisco section as identified from cores by Littlefield.) The Bois d&apos;Arc is oil productive throughout the entire 600-ft monoclinal accumulation from the eastern upstructure erosional pinchout to the west-side oil-water contact. (See Littlefield et al.l and McGee and Jenkins for geologic detail.)

Jan 1, 1970

By John F. Abel

Personal gain seems to be the most powerful incentive to economic progress. One of my first exposures to this phenomenon was the comparison between company stopes and leaser&apos;s stopes in a vein gold mine. The company stopes were 4 to 6 ft wide, whereas the leaser&apos;s stopes were so narrow that in some places one could not turn around. The company leased only that ground it felt was marginal to mine with day&apos;s- pay miners, but by skillful, careful and energetic mining, the leasers managed in most cases to make money for themselves and the company. The Hurting Truth This capitalist system, which puts a premium on successful risk taking, is under attack. Not that it hasn&apos;t been under attack all along. What hurts and angers us at this time is that the attack comes from the children of the system-its youth. Such blasphemy should, of course, be eradicated, root and branch. Or should it? Are we hurt in part because some of the things they say are true?

Jan 1, 1970

By Edmond S. Miksch

The morphology and growth rate of ice grown in supercooled water are markedly affected by convection of the water. A dendritic ice sheet with water flowing past the dendrite tip exhibits deflection of the dendrite spine toward the upstream direction, accelerated growth of secondary spines on the upstream side, and suppression 01" secondaries on the downstream side. Flow causes a thin disk to become corrugated, the corrugations being parallel to the flow. Flow causes an increase in the growth rate of the ice. IF a small seed of ice is placed in slightly supercooled water, it grows initially as a disk with the axis of the disk parallel to the c axis of the ice crystal.&apos; It appears that growth in the c direction is inhibited, while growth occurs with equal facility in all directions in the basal plane. It appears that growth rate as a function of interface temperature is very nearly equal for all directions similarly oriented relative to the c axis. Subsequent to the discoid growth, branching occurs and dendrites develop. The primary dendrite spines grow parallel to the six equivalent a axes of the crystal. Secondary, and in some cases, tertiary spines also grow in these directions. The highly anisotropic: dendritic growth indicates that there must be some finite difference of growth rate for different directions in the basal plane. These differences must be quite small, however, since if they were large, the discoid mode would not occur. Hence, it was expected that the dendrite growth direction could be deflected from the crystallographic direction by perturbation of the thermal field at the dendrite tip. Experiments were done in which perturbation of the thermal field was accomplished by causing the supercooled water to flow past the dendrite tip. The flow direction was perpendicular to the c axis of the crystal, and was perpendicular to the primary spine of the unperturbed crystal. Supercooled water was supplied by a 15 cm cubical copper box, which was refrigerated and insulated so it could cool water to temperatures down to —2oC, and maintain the temperature constant to O.l°C for the duration of a run. A lucite channel of rectangular cross-section, 12 by 24 mm, was mounted horizontally in the box, with one end open so water could flow into it, and the other end leading out through the wall of the box to a length of tubing leading: to an orifice plate 123 cm below. cnunMn s MIKSCH, MemberAiMe, formerly Research Associate, Research Associate, Fig. l(b)—Vertical section of apparatus A horizontal cross-section is shown in Fig. l(a), and a vertical section is shown in Fig. l(b). Means for observing the ice are shown in Fig. l(a). Collimated light passes through the ice sheet and forms an image on the ground glass screen. A lucite box containing dry air was employed to prevent condensation. Ice of the desired orientation was provided by the seed holder shown in Fig. l(b). This device was made of lucite, and had a reservoir in which ice could be frozen by placing it in a freezer. This reservoir com-unicated with the outside only through a narrow gap between two sheets of lucite. The seed holder (after ice had been washed off its exterior) was immersed in the tank of supercooled water, the narrow gap terminating in a slot in the top of the flow channel. Ice growing through a thin water layer in the gap between the two sheets of lucite was oriented so its c axis was perpendicular to the sheets. This orientation is an application of a growth phenomenon2 which causes ice growing along a smooth solid surface in supercooled water to orient itself so its c axis is normal to the surface. After the ice grew into the channel, further orientation was necessary, since the direction of the a axis

Jan 1, 1970

By Manuel Gomez

This report presents prediction equations for 12 variables that are indicative of metallurgical coal quality. The variables include six for coke strength and six for carbonization product yields. All variables were predicted for coking coals having volatile matter contents from 16.3 to 42.1 percent, dry basis. The prediction equations, developed by mathematical-statistical techniques, were based on information from the proximate and ultimate analyses, the size consist, and the petrographic composition of bituminous coals carbonized in BM-AGA retorts at 800°, 900°, and 1,000° C. The equations were evaluated for validity with independent data derived from the 900° C carbonization of 33 binary blends of various coals and 22 binary blends of Pocahontas No. 3 low-volatile bituminous coal with 11 high-volatile bituminous coals. Results show that metallurgical coal quality can be predicted ahead of mining because data used to derive the prediction equations can be obtained at the time of exploration. Capability to forecast coal quality is useful in mine planning and should provide basic information for optimization of blending and crushing techniques and thus lead to the production of uniform coke.

Jan 1, 1970

By Thomas F. Tomb

The penetration characteristics of a horizontal plate elutriator and of a 10-mm nylon cyclone were evaluated. The test aerosols were polydisperse coal-dust particles ranging from less than 0.3 to 15 micrometers in diameter. Particle densities ranged from 1.3 to 1.4 grams per cubic centimeter. Equivalent Stokes diameters were measured using Coulter counter analytical techniques. Experimental results indicate that the penetration characteristics of the horizontal plate elutriator closely approximate the sampling efficiency curve defining the respirable fraction of the dust cloud recommended and adopted by the Johannesburg Pneumoconiosis Conference in 1959. Penetration characteris-tics of the 10-mm cyclone were evaluated at flow rates of 1.4, 1.5, 2.0, 2.5, and 2.8 liters of air per minute. The data indicate that the penetration curve obtained at 2.0 liters per minute most closely approximates the sampling efficiency curve for respirable dust recommended at a meeting sponsored by the U.S. Atomic Energy Commission in 1961.

Jan 1, 1970

By Freeman Bishop

Mercury is the latest ecological disaster. It was believed to be no pollution problem because it is heavier than water and expected to fall to the bottom of streams. But the Food and Drug Administration (FDA) found that mercury in a dozen states and several Canadian provinces was being ingested by fish. A Deadly Dose First to sound the alarm was Canada when a graduate student&apos;s research revealed that mercury contamination in Lake St. Clair had reached 1.4 pmm. which is almost three times the 0.5 ppm the FDA&apos;s allowable maximum.

Jan 1, 1970

By B. H. Eccleston

The Bureau of Mines, in cooperation with the American Petroleum Institute, studied the effect of fuel volatility and front-end fuel composition on the amount and photochemical reactivity of automobile exhaust and fuel-system evaporative emissions. The study involved six gasolines--the base fuel, three fuels of varied volatility, and two fuels differing from the base and from each other in front-end olefin content. Data were obtained from 16 vehicles operated on a chassis dynamometer using a speed-load-time cycle that approximated a typical urban trip. Tests were made at ambient temperatures of 20°; 45°, 70°, and 95° F, using a climate-controlled dynamometer room. The amount of hydrocarbon emission and its probable photochemical effect, a potential contribution to pollution, is expressed as weight (reactivity equivalent) of a moderately reactive material, ethylene. Emissions of oxides of nitrogen, car-bon monoxide, and aldehydes were also observed. Results showed that reduction of volatility from currently typical levels serves to reduce both the amount and the reactivity equivalent of evaporative losses with a slight penalty by way of higher exhaust emissions. Alternatively, reducing the amount of light (low boiling) olefin in the fuel had no effect on the amount of hydrocarbon pollutant but did significantly reduce the reactivity equivalent of the emissions. Neither volatility change nor chemical changes to the fuel significantly affected the nonhydrocarbon emissions.

Jan 1, 1970

By R. L. Jones, H. Conrad

The effects of gain size on the room-temperature tensile properties of commercial(A- 70)-purity and iodide-purity titanium were investigated by concurrent tensile testing and thin-foil electron transmission studies. The mechanical tests showed that the effect of grain size on the yield, flow, and fracture stresses could be expressed by relations of the Hall-Petch type. The magnitude of the grain size effect on the yield stress was larger for commercial-purity than for high-purity titanium, but in both materials it was intermediate between that typically observed for fcc and for bcc metals. The effect of strain on the gain size sensitivity of the flow stress was found to reflect the grain size dependence of strain hardening. The electron transmission study indicated that the tensile behavior could be accounted for in terms of the dislocation densities and distributions formed during deformation. It was concluded that the effect of grain size on strength could be attributed to a relationship between grain size and the dislocation densities generated in initiating and sustaining plastic flow, the difference in stress levels being due to strain hardening. The relationships between recrystallized grain size, uniaxial tensile properties, and dislocation substructure have not been explored in any detail for a titanium. With titanium and its alloys finding increasing applications in aerospace systems, such information has become essential. The research described in this paper had two objectives: first, to document the effect of grain size on the yield, flow, and fracture stresses of unalloyed a titanium by the tensile testing of recrystalliied specimens at room temperature; second, to attempt an interpretation of the mechanical test behavior in terms of the dislocation structures formed on deformation, as observed by transmission electron microscopy of thin foils prepared from deformed tensile specimens. The observations reported here are restricted to room-temperature deformation; the effect of temperature on the yield and flow stresses of a titanium and the athermal nature of the contribution of grain size to the flow stress have been discussed elsewhere.1"3 EXPERIMENTAL DETAILS Two purity grades of unalloyed titanium have been investigated: Crucible Steel A-70, a typical commer- cial-purity product, and a high-purity iodide grade supplied by the Foote Mineral Co. Chemical analyses for interstitial impurity contents are given in Table I, together with values for the total interstitial atom fractions in terms of oxygen equivalents, which were calculated by the method outlined previously.4 ,5 According to the manufacturer&apos;s nominal analysis, the A-70 grade also contains about 3700 ppm of Fe. The A-70 grade was supplied as 1/4-in.-diam centerless-ground rod. The iodide grade was supplied as crystal bar which was consolidated to approximately 1/4-in.-diam rod by a single, rapid, molten zone pass, using electron beam heating. The 1/4-in. rods were cold-swaged to 0.078-in.-diam wires and 2-in. lengths were recrystallized in a vacuum of -5 x 10-5 torr, giving grain sizes in the range 0.8 to 30 . The thermal treatments and resulting grain sizes are summarized in Table 11. Since there was in no case any obvious sign of a bimodal dis tribution of grain sizes, the grain size values quoted in Table I1 are those obtained from mean linear intercept measurements involving >I00 grains. For the two coarse grain sizes the measurements were made using conventional optical techniques. It was noted during these determinations that the etchants used (10 pct HF; 30 pct HN03; 60 pct H20 and 2 pct HF; 2 pct H202; 96 pct H20 were both tried) etched grain boundaries very nonuniformly and optical polarization effects had to be employed to reveal boundaries which might otherwise have been missed. It was found that this problem became more acute with the finer grain sizes as the usefulness of polarization diminished.

Jan 1, 1970

By Rodney R. Krause

In attempting to tell the general public about the coal industry&apos;s land reclamation efforts, we have often said, "We&apos;re not doing things by the book, because we&apos;re still writing it." Like any good catchphrase, the statement is not only striking but true. It is particularly true in the mountains of Appalachia, where the problems of mining; and of reclamation are made more intense by the nature of the terrain. Mining and reclaiming the land "by the book&apos; --which is to say by the methods of contour mining traditionally used in hill country--hasn&apos;t worked too well. So a lot of conscientious coal operators and associations are trying new methods--new ways of mining, new machines for seeding and planting, and new species to seed. Not all their experience can be transplanted to other areas, and of course I don&apos;t believe that Appalachia is the only place where new methods are being developed. Nevertheless, there&apos;s enough action in Appalachia to make a detailed examination rewarding, so let&apos;s focus on the hills to see what&apos;s new.

Jan 1, 1970

The Tuesday morning session opened at 9:00 a.m. and was presided over by John Peperakis, Manager Sunnyside Mines, Kaiser Steel Corporation, Sunnyside, Utah. It consisted of a Round Table. The first speaker was Mr. G. A. Bennewitz, Market Director - Fuels - Denver & Rio Grande Western Railroad, Denver, Colorado. Subject - "Transportation." Mr. Gary Bennewitz has been a Market Director of the Rio Grande R.R. since February 1968. He joined the D&RGW in 1966. Mr. Bennewitz has a degree in Civil Engineering from The Cooper Union in New York City. Following graduation, he spent two years working with a consulting soil engineer. He then went to work for the New York Central R.R. as a Structural Engineer and Transportation Economist. He also had a year&apos;s stint at the Port of New York Authority before moving to Denver. His paper today deals with some of tile economic factors inherent in the development of an efficient, economic unit train system. His experience in this vein includes trains operating from the Sunnyside Mines, of Kaiser Steel, the coal delivery system to Geneva Works of U. S. Steel, and from the facility of Mid-Continent Coal & Coke Co. at Carbondale, Colo.

Jan 1, 1970