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By H. C. Miller

The gas-lift method of flowing oil from wells is the outstanding feature of petroleum technology today. Its forerunner, the air-lift, was used successfully first, in the Baku fields of Russia, in 1899, and later in the Gulf Coast fields of Texas and Louisiana and the Kern River field of California. It is still used to a limited extent in certain oil fields. The use of compressed natural gas for lifting oil from wells has supplanted the air-lift method in a measure in those fields where a sufficient quantity of gas accompanies the oil to make the gas-lift possible, or where natural gas is plentiful and inexpensive. We find, therefore, in California, that natural gas is used at practically every well where a gaseous medium is employed to flow the oil. The use of natural gas has many advantages over that of air. It is possible to recover and save the gasoline from the gas that accompanies the oil to the surface. This gasoline would be wasted if air were used as the lifting medium. Also, certain proportions of air and gas form an explosive mixture that cannot be handled safely by compressors. Another advantage that gas has over air is that gas under pressure is more soluble in oil. Gas in solution in oil reduces the viscosity of the oil that is being produced and causes it to flow more readily through the tubing and flow lines. The gas-lift has made it possible to recover many thousands of barrels of oil from deep wells in California that could not have been produced otherwise. It would not have been economical, had it been mechanically possible, to produce such wells as the world's deepest producing oil well (Miley Athen's No. 6, Rosecrans field, California) by any other method of pumping known today. At this well, production is obtained from between 7305 and 7591 ft. and 11 months after completion of the well, production was being maintained on the gas-lift at approximately 2000 bbl. a month. The crookedness of the hole, or its diameter and depth will not prevent the successful application of gas-lift pumping when other conditions are favorable.

Jan 1, 1928

By C. Goldberg, R. H. Wynne

WHEN using an optical goniometer to determine crystal orientation' it is advantageous to use a preferential etchant so that the etch pits have plane faces which are parallel to crystallographic planes, all of which are of the same "form." "Westinghouse Silver Etch" (WAg), a preferential etch for germanium, is made up as follows: 40 ml of 49.7 pct hydrofluoric acid, 20 ml of 70.7 pct nitric acid, and 40 ml of distilled water containing 2.0 g of silver nitrate. Examination of metallographs of WAg etched surfaces (Fig. 1, for example) indicates that, regardless of crystal orientation, the faces of the etch pits are (111) surfaces. Optical goniometer examination of these WAg etched surfaces also indicates that the faces of the etch pits are (111) surfaces, i.e., all bright reflections are from (111) planes. When using an optical goniometer of the type described by Barrett,' not only (111) reflections from a WAg etched germanium surface but also other reflections of lower intensity will be observed. These latter reflections can cause confusion. We have used an optical goniometer made from a war surplus astrocompass and a galvanometer lamp. The reflections are observed by using the goniometer in a darkened room and letting the reflected light be in- cident upon a piece of white paper. The resulting decrease of goniometer sensitivity enables (111) reflections only to be observed. This in turn permits the crystal orientation to be determined in a matter of minutes, since only two measurements are necessary. The authors wish to acknowledge the help received from R. E. Davis who assisted in making the metallographs and aided the authors in the interpretation of the metallographs.

Jan 1, 1954

By R. E. Grace, H. W. Schadler

DARKEN1 has established the theoretical relation between the self-diffusion coefficients and the Boltzmann-MatanO Or interdiffusion coefficient: D is the Boltzmann-Matano or interdiffusion coef-

Jan 1, 1960

By J. G. Benford, E. B. Stanley

THERE have been numerous papers in the literature1 on the subjects of secondary and tertiary recrystalli-zation in silicon steels. Secondary re crystallization is believed to occur in silicon steel by either a surface-energy phenomenon such as in the usual development of cube texture or by a second-phase phenomenon such as in the usual production of cube-on-edge texture, (110)[001]. Tertiary recrystallization in silicon steel is thought to be a surface-energy phenomenon in which, for example, grains having a (110) plane parallel to the sheet grow at the expense of other grains in the matrix including those having a (100) plane parallel to the plane of the sheet. In all these instances, the orientations involve either a preferred (100) or (110) plane in the plane of the sheet. Until very recently, there had been no experimental evidence reported of the occurrence of a texture by secondary or tertiary recrystallization that involves a (111) plane in the plane of the sheet, although Kohler reported that grains having the (111) plane parallel to the sheet surface can also grow by a surface energy mechanism. Stickels observed a secondary texture in iron described as "near {554}(225)" about 5 deg from {lll}(211).3 Mee reported that in a vacuum-remelted commercial 3 pct Si steel {lll}(hkl) secondary recrystallization took place in a high vacuum and in pure hydrogen.4 Recently in our Laboratory, large-grained structures such as shown in Fig. 1 having an orientation near (111)[211] or (111)[2ii] have been observed. The arrows point to areas of relatively small matrix grains of the kind that the much larger (111) grains consumed while growing. It is of interest that the matrix grains of samples annealed at 2000°F were essentially the same size as those in samples annealed at 2200°F, a matrix-grain-size stability that is characteristic of secondary recrystallization processes. A torque disc taken from Grain 4 of the sample shown in Fig. 1 revealed a very flat magnetic-torque curve, as expected, with a maximum torque of 7000 dyne-cm per cu cm compared to the typical 180,000 dyne-cm per cu cm observed for conventional (110)[001] textured material. A back-reflection Laue pattern for Grain 4 is shown in Fig. 2 and indicates a near-perfect (111)[211] orientation. The other six numbered grains in the sample of Fig. 1 had a similar orientation. The small circles next to each number were the target areas for the X-ray beam. The starting material was an 0.011-in.-thick oriented silicon steel, (110)[001] texture, containing 3 pct Si. It was lightly pickled, cold-rolled to 0.005 in., and annealed 4 hr at 2200°F within a nickel box (not gas-tight) inside a tube furnace through which dry hydrogen was flowing. The samples were heated to 1500°F in 1 hr and then at 60°F per hr to 2200°F. There were other

Jan 1, 1969

By C. G. Dunn, F. W. Daniels, M. J. Bolton

IN recent papers on interface energies in metals¹,² the concept of an equilibrium of forces has been used in the measurement of interfacial tensions. Mathematically the equilibrium of three forces is given by the relations: where the 2's are the interfacial tensions (interface energies per unit area of interface) of three phases or grains meeting at angles 21 22 and 23 (212 relates to the 1-2 boundary formed by grains 1 and 2;223 to the 2-3 boundary, etc.). If these relationships are valid, one can calculate relative values of the interface energies from measured boundary angles on specimens which have been brought to equilibrium. Since Eq 1 may be derived through a mathematical process of minimizing the grain boundary energy under the restriction that the ?'s be independent of boundary orientation: the concepts of surface tensions and equilibrium of forces are not particularly essential. To deal with the general case involving dependence of boundary energy on boundary orientation, it becomes desirable to drop certain concepts formerly held (namely that energy per unit area is identical with force per unit length or surface tension) and to use the energy concept alone. It is appropriate, therefore, to use E in place of ? in deriving and using the more general equations that express the anisotropic nature of the grain boundary energy. Herring3# ' recently has derived the required general equations using the principle of minimization of energy. Specifying the boundary orientations in terms of angles (4) measured with reference to crystal axes within the grains, Herring's equations take the form E23 + E21 cos?8 + E12 cos?2 — sin ?12 + sin?2-?E12/?12 =O [2] where the partial derivatives are measured in the direction of counterclockwise rotation of the boundaries. Eq 2 implies that an infinitesimal displacement of the triple point along the 2-3 boundary produces no change in the boundary energy. Similar equations apply for infinitesimal displacements along each of the other two boundaries. From such equations Herring obtains the following general relationship (1 + E1 E2) sin?8 + (E2 — E1) cos?3 ________ E38______________ = (1+ E2 E8) sin ?1+ (E3— E2) cos ?1 __________^5____________[3] (1 + E sin ?2, + (E1 — E8,) COS ?2 1 E28 where E1 = 1/E23- E25 and PC and c8 have similar expressions. It is apparent that Eq 3 reduces to Eq 1 when the c's vanish. Eq 3 also reduces to Eq 1 when the E'S are all equal. Shockley and Read' have pointed out one limitation to these equations. When E plotted versus 4 appears as an energy cusp, as their theory requires, for example, for the energy near a twin boundary position, then Eq 3 (and therefore Eq 1 also) no longer applies if one boundary is in the minimum energy position. One of the equations of form Eq 2, however, applies if the infinitesimal displacement is along the boundary associated with the energy cusp. From the foregoing treatment it will be apparent that equilibrium angles alone are not sufficient in general for calculating relative interface energies.

Jan 1, 1951

By B. M. Larsen, T. E. Brower, J. W. Bain

A mass of circumstantial evidence is presented to indicate that the main source of alloy losses in open-hearth tapping is oxidation by air, with the steel apparently reacting with an amount of oxygen equivalent to about 30 times its own volume of air. The effect is erratic from heat to heat, depending largely on turbulence and distance of free fall of the stream of liquid metal. THIS paper reports another phase in a general study of oxidation in the open-hearth, various aspects of which have already been discussed in previous papers.1,2,3 It is based on experiments conducted on commercial, basic open-hearth furnaces at various times when opportunity offered, beginning about 1938, in an attempt to determine the mechanism and measure the amount of air oxidation during the flow of the tapping stream through the air into a ladle. This effect is closely connected, not only with alloy losses and control of chemical analysis, but possibly with various questions regarding inclusion content and steel quality and with a true picture of the deoxidation of steel in general. Thus it is believed that discussion of a large part of the results to date may be of assistance to others who are studying problems related to deoxidation or to steel cleanliness and quality. The literature reveals that strangely little attention has been devoted specifically to the effect of pouring steel through open air. Bardenheuer and Henke4 in 1939, in a paper devoted largely to overall losses of manganese in the basic open-hearth, reported that for a number of heats tapped into a tilted ladle held just beneath the runner so that the maximum distance of drop of the stream through the air was held to less than about 30 in., there was in most cases almost no loss of manganese from furnace to ladle. Hultgren,5 in 1945, showed that in high-carbon basic electric steel deoxidized in the furnace and containing no large inclusions as it left the furnace, large silicate inclusions, often rich in manganese oxide, were present in samples dipped from the pool in the ladle; also that the rise in content of large inclusions (above 0.01 mm dim) was greater when the metal stream was made to spray or flow in a turbulent manner. Our interest in this phase of oxidation in the open-hearth was first aroused by a study of alloy efficiencies on ladle additions. The frequency curves of manganese efficiency (net recovery of metal added in ladle) given in fig. 1 are of interest in this connection. Lowest, and also most variable (47 to 95 pct), recovery was in low-carbon heats having no coal additions to the ladle, progressing upward to a maximum average and least variable (82 to 97 pct) recovery in high-carbon heats killed with aluminum and silicon. Both coal additions and higher carbon contents in the tap stream, as well as additions of silicon and aluminum, help to lower the amount of manganese loss. But the most interesting point is the amount of manganese oxidized in many heats tapped at 0.50 to 1.06 pct carbon. It has been shown in a previous paper3 that the amount of oxygen in the tap stream in such heats is very small, usually below 0.01 pct, too small to oxidize any appreciable amount of manganese. Also, the fact that manganese should be oxidized at all in a metal solution containing such more stable oxide-forming elements as aluminum and silicon is an indication of some rather intense oxidizing effect such as could be caused by reaction with the air during ladle filling. Oxygen Balances from Tap Stream to Teeming Stream: Data in the form of alloy efficiencies, such as those shown in fig. 1, are not a proper measure of such a general oxidation effect. Having available

Jan 1, 1951

By E. V. Foran

Among the many newer disclosures that have accompanied the petroleum industry's progressively deeper exploratory drilling is the increased frequency with which the operators are encountering reservoirs of which the products at the time of discovery exist wholly or predominantly in the gas phase. The popular term "distillate pool" is most often used within the industry when referring to this type of reservoir, and in this paper the term is used in that sense. These pools have been observed in many different surroundings. In some places the entire reservoir is filled with the wet gas containing its water-white condensible products in the gas phase but apparently with no dark oil or other hydrocarbon liquids in the reservoir. The 8200-ft. horizon in the Big Lake field in West Texas is a good example of this type. At other places the wet, or distillate-bearing, gas may form a large gas cap directly overlying and in contact with an extensive reserve of dark oil. Oklahoma City, Kettleman Hills, the 8500-ft. horizon in the Big Lake field, and many others are examples of this type. There are also many places in which the wet distillate-bearing gas fills nearly the entire reservoir space, while the dark oil occupies only a narrow, bandlike zone, which marks the boundary of the reservoir along its lowest productive contour. The heavier components of these deep pool gases are generally water white in color, a large portion of which are condensible in a conventional oil and gas separator, when operated under pressures of the order of 400 to 800 Ib. per sq. in. Although the water-white products recovered in the separator sometimes have end points of 650" F. and higher on standard Engler distillation, they occur only in the gas phase in the reservoir. It is entirely possible that even some small amounts of dark colored reservoir components may occur in the gas phase when the temperature is 300" F. and pressures exceed 6000 Ib. per sq. in. Close approaches to these conditions have been encountered in the deepest producing wells. The condensible content of the deep reservoir gases of the many pools that have been tested or produced to date shows a wide variation in both condensible content, per 1000 cu. ft. of gas, and physical character.

Jan 1, 1939

By E. V. Foran

Among the many newer disclosures that have accompanied the petroleum industry's progressively deeper exploratory drilling is the increased frequency with which the operators are encountering reservoirs of which the products at the time of discovery exist wholly or predominantly in the gas phase. The popular term "distillate pool" is most often used within the industry when referring to this type of reservoir, and in this paper the term is used in that sense. These pools have been observed in many different surroundings. In some places the entire reservoir is filled with the wet gas containing its water-white condensible products in the gas phase but apparently with no dark oil or other hydrocarbon liquids in the reservoir. The 8200-ft. horizon in the Big Lake field in West Texas is a good example of this type. At other places the wet, or distillate-bearing, gas may form a large gas cap directly overlying and in contact with an extensive reserve of dark oil. Oklahoma City, Kettleman Hills, the 8500-ft. horizon in the Big Lake field, and many others are examples of this type. There are also many places in which the wet distillate-bearing gas fills nearly the entire reservoir space, while the dark oil occupies only a narrow, bandlike zone, which marks the boundary of the reservoir along its lowest productive contour. The heavier components of these deep pool gases are generally water white in color, a large portion of which are condensible in a conventional oil and gas separator, when operated under pressures of the order of 400 to 800 Ib. per sq. in. Although the water-white products recovered in the separator sometimes have end points of 650" F. and higher on standard Engler distillation, they occur only in the gas phase in the reservoir. It is entirely possible that even some small amounts of dark colored reservoir components may occur in the gas phase when the temperature is 300" F. and pressures exceed 6000 Ib. per sq. in. Close approaches to these conditions have been encountered in the deepest producing wells. The condensible content of the deep reservoir gases of the many pools that have been tested or produced to date shows a wide variation in both condensible content, per 1000 cu. ft. of gas, and physical character.

Jan 1, 1939

By William R. Taylor

This paper reviews the mining and related legislation history of in situ uranium mining in southwest Texas with emphasis on the last five years. It also reviews the current regulatory process and some of the more critical concerns and concepts relative to containment and restoration of in situ mines.

Jan 1, 1979

By Francisco Cadena

THE construction of Norris Dam, built by the Tennessee Valley Authority on the Clinch River, a tributary of the Tennessee River, involved the production of coarse and fine aggregate for approximately 1,000,000 cu. yd. of concrete. A hammer-mill plant for the manufacture of sand from quarried rock was indicated as the most economical method of providing this material. The abrasive character of the feed as compared to the average hammer-mill feed made it necessary to control operations rather closely, and this resulted in the accumulation of many data bearing on production and maintenance. This paper will deal only with three specific sets of data, accompanied by such general information as may be necessary to explain the conditions under which they were obtained and followed by discussions on the relation of silica content to hammer wear, comparative costs of slugger and stirrup hammers, and comparative costs of tool-steel and manganese-steel grate bars. Coarse Aggregate Aggregate for the concrete poured at Norris Dam came from a dolomite quarry within 2000 ft. of the west abutment of the dam. Geologically this rock is known as a Knox dolomite. A typical chemical analysis is given in Table 1. TABLE 1 .-Typica.1 Chemica1 Analysis [PER CENT H20,1100F ............................................ 0.0'2 Ignitionloss ............................................. 43.56 MgO .................................................. 19.19 CaO .................................................... 29.07 FezO .................................................... 0.39 A1203 .................................................... 1.94 FezO .................................................... 0.39 A1203 .................................................... 1.94 ..................................................... 5.75 SO2.. .................................................. Tr.] Rock was carried by 12-yd. dump trucks to a 42-in. gyratory crusher set at 6 1/2 in. The product of the primary crusher was taken by a belt conveyor to a double-deck vibrating screen followed by a 5 1/2-ft. cone

Jan 1, 1937

By S. P. Kinney, C. E. Wood, T. L. Joseph

In connection with its investigations of the blast-furnace process, the Bureau of Mines, in cooperation with the Minnesota School of Mines Experiment Station, developed a 6-ton experimental furnace. Such a furnace was needed to determine the feasibility of producing ferroman-ganese from Minnesota manganiferous iron ores, a problem of national importance because of the present need for manganese in the steel industry and our small reserves of ferro-grade ores. Furnace operators are reluctant to use new or untried raw materials or to make decided innovations in practice on account of the financial hazard of experimenting with full-scale equipment. A small furnace which can be operated at a relatively low cost is particularly adapted for testing new raw materials and for determining the feasibility of decided innovations in practice. Laboratory experiments, plus whatever information may be available, are valuable but often do not indicate the net result of changes in an operation involving a large number of interrelated variables. From time to time the cooperation of the Bureau of Mines is solicited in connection with problems involving departures from normal procedure. Under these circumstances some sort of a practical demonstration is a desirable forerunner to full-scale operations which appear feasible after small-scale tests. The Aluminum Co. of America was interested in knowing the practicability of smelting a charge of bauxite, iron ore, and limestone, of proportions that would produce slag of the following composition: A1203, 47 to 48 per cent.; CaO, 41 to 42 per cent.; SiO2,4 to 5 per cent.; TiO2, 2 to 3 per cent.; FeO, 1 percent., and MgO, 1.8 percent. In addition to determining whether it was feasible to operate a blast furnace on slag approaching the composition given above, a quantity of slag was needed for a series of experiments that would show the relative ease and cost of extracting alumina from slag which could be made in the blast furnace, as compared to extracting it from raw bauxite. The value of the slag as a raw material

By E. R. Atkins, G. H. Smith

Results of laboratory tests are presented to show that lire value of "m", in the Archie expression dernlined by the shapes of the particles in the system. Tile value of m "the shape factor", is constant for a system of particles of a given shape for a range of F - + values. Applying this concept, one can predict F - + relationships for mixtures of particles with different shapes, and these predicted relationships are useful in electric log interpretation. It is suggested that an equation of the form 1/F -10mcan be used to describe the properties of natural formations containing varying amounts of sand and clay. From this work and values of "a" and "m" reported in the literature, it appears that in many cases rocks in the same geological horizon have a common primary porosity but contain varying amounts of a particular clay. It is concluded that the equation can be applied to a rock-water system only when values of "a" and "m" have been established for the particular system. INTRODUCTION The petroleum literature contains many reports of the results obtained by determining formation resistivity factor F and porosity + of rock samples from oil fields all over the world. The usual practice is to use data from a large number of samples from a number of fields to find an average relationship between F and +. Several such average relationships have been advanced. In the absence of data on a particular formation or field, it has been the practice to use the average relationships to give a rough approximation of the F - + relationship. The purpose of this paper is to report on basic relationships that exist between F and + for naturally occurring particles in water solutions. Other workers' have found the same relationships apply to the diffusion of hydrogen through packed beds of dry particles. In the work discussed here, relationships for application to unconsolidated sands or shales containing mix- tures of particle shapes are derived. These relationships, developed for unconsolidated formations, may apply to consolidated formations. EXPERIMENTAL To evaluate F- relationships for unconsolidated rocks, the results of laboratory measurements on simple slurries of clay or sand will be used. Such laboratory studies are concerned with the electrical behavior of water-containing rocks. The wet rock constituents are electrically similar in slurries and in rocks. Archie2 defined formation resistivity factor as All resistance measurements were made using a 1,000-cycle impedance bridge with an oscilloscope as the null detector." The accuracy of this bridge was better than * 0.15 per cent. For the particular apparatus employed, no additional reactance was required to achieve balance for samples with resistances between

By D. V. Carter, Dan C. Williams, Franklin M. Hackbusch

During 1939 little of consequence happened in East and East Central Texas in the way of oil discoveries. At the end of the year, there were 47 oil and gas fields in the district. Twelve other fields, 11 oil and one gas, have been abandoned. The ranking fields in order of the number of completions for the year were East Texas, Talco, and Rodessa (Texas portion). There were 511 oil wells (distillate wells included), 32 gas wells, and 257 dry holes completed in the district. Exploration, Discoveries and Extensions During the year, 113 exploratory wells were drilled, the same number as in 1938; four oil fields and one gas-distillate field were discovered. Perhaps the most important discovery, which has been named Barron field, was that of M. Samuel et al., No. 1 Barron in Limestone County. The wells in this field are of the gas-distillate type. Other than the Talco and Sulphur Bluff fields, which produce oil from the Paluxy sand (Upper Trinity), this is the first field on the Corsicana-Mexia fault zone to obtain commercial production from deeper Trinity strata. This "pay" is the Petit lime of the Lower Glen Rose of the Trinity group. The four oil discoveries were: Redland, Angelina County; Bazette, Henderson County; Rowe and Baker, Henderson County; and Marion County Shallow in Marion County. It is believed that the Bazette field, Navarro County, represents an extension of the Flag Lake field. For details concerning discoveries, extensions and important wildcat wells drilled during 1939 see Table 2. Production and Proration The district produced 175,053,729 bbl. of oil (distillate production included) which is a decrease of 4.0 per cent from the 182,369,484 bbl. (distillate production included) produced during 1938. The district's production for the year 1937 was 208,594,453 bbl. The East Texas

Jan 1, 1940

By D. V. Carter, Dan C. Williams, Franklin M. Hackbusch

During 1939 little of consequence happened in East and East Central Texas in the way of oil discoveries. At the end of the year, there were 47 oil and gas fields in the district. Twelve other fields, 11 oil and one gas, have been abandoned. The ranking fields in order of the number of completions for the year were East Texas, Talco, and Rodessa (Texas portion). There were 511 oil wells (distillate wells included), 32 gas wells, and 257 dry holes completed in the district. Exploration, Discoveries and Extensions During the year, 113 exploratory wells were drilled, the same number as in 1938; four oil fields and one gas-distillate field were discovered. Perhaps the most important discovery, which has been named Barron field, was that of M. Samuel et al., No. 1 Barron in Limestone County. The wells in this field are of the gas-distillate type. Other than the Talco and Sulphur Bluff fields, which produce oil from the Paluxy sand (Upper Trinity), this is the first field on the Corsicana-Mexia fault zone to obtain commercial production from deeper Trinity strata. This "pay" is the Petit lime of the Lower Glen Rose of the Trinity group. The four oil discoveries were: Redland, Angelina County; Bazette, Henderson County; Rowe and Baker, Henderson County; and Marion County Shallow in Marion County. It is believed that the Bazette field, Navarro County, represents an extension of the Flag Lake field. For details concerning discoveries, extensions and important wildcat wells drilled during 1939 see Table 2. Production and Proration The district produced 175,053,729 bbl. of oil (distillate production included) which is a decrease of 4.0 per cent from the 182,369,484 bbl. (distillate production included) produced during 1938. The district's production for the year 1937 was 208,594,453 bbl. The East Texas

Jan 1, 1940

By A. L. Mincher, W. F. Sheely

Mechanical properties of columbium have been studied over the temperature range of -196 to 1093oC. The decreased strengthening influence of cold-work at temperatures below ambient has been interpreted in terms of the Peierls-Nabarro effect. Maxima in the rate of strain hardening observed during tensile testing in the range 250-600°C. have been correlated with interstitial impurities to indicate the temperature ranges at which carbon, oxygen, and nitrogen, respectively, are responsible for strain aging. THE growing need for structural materials for use above the useful service temperatures of the iron-, nickel-, or cobalt-base alloys has caused the refractory metals to be considered as potential engineering materials. These metals, which include columbium, tantalum, molybdenum, and tungsten, are called refractory because the lowest melting point among them,that of columbium, is about 1000°C higher than the average melting temperatures of conventional high-temperature alloys. They are all body-centered cubic transition metals and, as such, their mechanical properties have basic characteristics which distinguish them from the face-centered cubic metals. For example, all show a much steeper rise in strength with decreasing temperature below room temperature than do the face-centered cubic metals, and their mechanical properties are strongly influenced by interstitially dissolved impurities. In order that these new metals may be used efficiently, it is necessary that their characteristics of behavior be fully known. In this paper, the mechanical properties of columbium will be examined over a wide range of temperatures. In particular, the influences of cold-work and individual species of interstitial impurity atoms on mechanical properties will be described, and basic mechanisms which may control the observed characteristics will be explored. EXPERIMENTAL The material used in this investigation was Union Carbide Metals Co. columbium roundels consolidated to four 4-in. diam ingots, three by consumable-electrode arc melting and one ingot by electron beam melting. Impurity contents of the ingots and methods of ingot conversion and treatment are summarized in Table I. The only metallic impurity occurring in any significant quantity was tantalum at about 0.1 pct. Iron, silicon, titanium, and zirconium were each less than 0.015 pct; boron was 1 ppm or less. This should have no appreciable influence on properties. The electron beam melted material, being the purest, will be used as the basis for comparison in the discussions to follow. Tensile tests were conducted from-196 to 1093oC, on both cold-worked and fully recrystallized arc-melted and electron-beam melted columbium using standard 1/4-in. diam, 1-in. long gage length test specimens. A strain-rate of 0.005 in. per in. per min was employed until the 0.2 pct yield strength was achieved and then the strain-rate was increased to 0.05 in. per in. per min for the balance of the test. Samples were protected in an inert atmosphere at tests above 300°C. The tensile properties obtained on the electron-beam melted columbium, E, in both the cold-swaged and recrystallized conditions are given in Fig. 1. The yield strength data of Dyson, et al.,' obtained on recrystallized electron beam melted columbium and the tensile strength data reported by Tottle2 on powder metallurgy columbium are included in Fig. 1. The material used by Tottle had been purified by vacuum sintering. There is excellent agreement between Dyson's data and those obtained in the present investigation. The tensile strengths obtained by Tottle were slightly greater than those obtained in this investigation on electron-beam melted columbium but varied with temperature in a similar manner. Tottle's data showed a maximum in tensile strength near 500°C, as did our data on electron-beam melted material, and also showed a small maximum at 300°C. The significance of these maxima will become evident later in the discussion. The tensile properties of cold-swaged and recrys-tallized arc melted columbium are plotted in Fig. 2. It was found that the properties of the recrystallized arc-melted columbium from all three heats showed very close agreement except at temperatures between about 500" and 800°C. A reason for this range of disagreement will be suggested in the discussion. The generally good agreement, however, attests to the ability of cold-working and subsequent recrystal-lization to erase the effects of the three different primary breakdown procedures and to produce nearly equivalent structures in the samples derived from the three different heats. wesse13 reported tensile data on columbium having interstitial impurity contents between those of the

Jan 1, 1962

By G. A. Beske, P. Hilsch, J. Wulff

The effects of the growth precipitates on the su-perconduching properties of an Al- 15 al. pel Zu alloy have been studied using magneization, transition lem-perature, and residual resistivity measurements. Aging at 230C for 1/2 to 11 he produces an increase in Hfp, Ike field of first penetration, and tut increase in trapped flux. The upper critical field, Hc2 remains constant for such aging tunes. Aging at 200°C produces a decrease in Hfp and an increase in trapped flux. The transition temperature remains constant at Tc - 1.227° ± 0.02°K for aging at 220°C for tims of from 1/2 to 10 hr, and for aging at 200°C it remains constant at Tc. = 1.18° i 0.02°K for times from 1/2 hv to 26 hr. The observed behavior indicates that the superconducting matrix when aged at 220°C behaves tike a type U su-perconducior, but when aged at 200°C behares like a type I superconductor. The magnetization changes after aging can be attributed to the growth and clutnge in distribution of the precipitate in a matrix of fixed composition. IT has been realized for some time that the superconducting properties of alloys are highly structure-sensitive. This is evident in the work of Mould and Mapother1 who examined the properties of an aluminum alloy. Precipitation effects have also been briefly mentioned in other studies.2-4 Bonnin and coworkers5 have observed a sharp inc rease in trapped flux in an A1-Mg alloy when the residual resistivity reaches a value that indicates it is a type II superconductor. Recently Blanc, Goodman, and Nemoz5p have reported on precipitation effects in A1-Ag alloys. Detailed studies of precipitation in Pb-Sn and Pb-Cd alloys made by Livingston6 serve to show that the upper critical fields are enhanced by quenched-in solute. Furthermore. at various stages in the precipitation process? the upper critical field is determined largely by the remanent solute. The observed magnetic hysteresis and trapped flux in such alloys result from the interaction between precipitate and the flux filaments in the mixed state. The flux trapping appears to depend largely on the precipitate distribution and is greater if the superconductor is type II than if it is type I. To examine the effect of precipitation in another alloy system, particularly one in which the composition of the superconducting phase does not change significantly during the course of precipitation, the Al-Zn system seems interesting, especially in view of the transition temperature and resistivity studies of Chiou and seraphim.' Furthermore, the recent detailed electron-microscope studies of an Al-Zn alloy by Richards and Garwood8 provide a guide for relating superconducting properties to changes in structure. For these reasons, magnetization, transition temperature, and residual resistivity measurements for varying times of heat treatment at two temperatures were made with a -15 at. pct Al-Zn alloy. The results are reported in this paper. I) EXPERIMENTAL The alloy used was prepared by Cominco Products Inc. from 99.9999 A1 and 99.999 Zn. It was chill-cast, swaged, and drawn to 0.125-in.-diam rod. The analyzed composition was 15.6 at. pct Zn (31.1 wt pct). A jeweler's saw was used to cut the 0.125-in.-diam rod into the 0.875-in. lengths needed for magnetization measurements. The ends of the cylinders were slightly beveled to remove the sharp edges. A portion of the original 0.125-in.-diam rod was drawn into 0.010-in.-diam wire and used for transition temperature measurements. Specimens were suspended from wires within a vertical furnace during heat treatment. All were homogenized at 500°C for a minimum of 3 days and subsequently solutionized for times in excess of 6 hr. The solutionizing temperature was held constant to +3°C. Individual specimens were homogenized, quenched, and aged several times and no effects indicating loss of zinc were noted. The suspended specimens were quenched by cutting the wires and allowing the specimens to fall into a silicone oil bath held at the aging temperature. They were then isothermally transforked by aging in the same bath used for quenching. After aging for the required time (approximately 10 min aging was necessary before the upper critical field reached a fixed value), they were briefly (1 to 2 sec) dipped into an acetone bath at room temperature to remove adherent oil and then immediately transferred to liquid nitrogen where they remained until inserted into the helium bath (usually within an hour). The temperature of the aging bath was held constant to +3°C for longer aging times. The cryostat used for the measurement of superconducting properties consisted of outer and inner dewars for liquid nitrogen and liquid helium, Stokes 6-in. booster diffusion pump and Stokes Model 212 mechanical pump, temperature controller to measure and control the temperature of the helium bath, and a superconducting solenoid with inserted search coils to provide the magnetic field and measure the magnetic moment of the specimens. A schematic diagram of the cryostat is shown in Fig. 1. An ultimate temperature of 0.85°K was reached with this apparatus. The temperature controller used is similar to the one described by Blake and chase.' A 0.5 pct Allen-Bradley carbon resistor and a nichronle heater (200

Jan 1, 1968

By F. Weinberg

The relative concentration of 1" at grain boundaries in controlled orientation bicrystals has been examined by autoradiographic techniques, and by activity measurements of grain boundary surfaces exposed by preferential ,melting. The autoradio-graphs indicate that thallium is concentrated at grain boundaries in as-grown bicrystals, but not in zcell-annealed bicrystals. They also indicate that the solute concentration and the distribution on as-grown bicrystal surfaces are markedly different than that of the bulk material. The boundary surface measurements are in agreement with the autovadiographic evidence. On the basis of these measurements, as-grown bicrystals containing approximately 100 ppm of Tl, solidified at rates between 5 and 30 cm per hr and with tilt boundaries greater than 10 deg, exhibited grain boundary segregation equivalent to roughly 10 atomic planes of pure solute. Higher solute concentrations (equivalent to 140 atomic planes of pure solute) were obtained in bicrystals solidified slowly (0.6 cm per hr); slightly higher values were obtained in specimens containing a large angle nantilt boundary. Annealing for various times over a range of temperatures eliminated grain boundary segregation within the experimental uncertainty of the results (equivalent to 1 atomic Plane of pure thallium at the boundary). The results for the as-grown bicrystals can be qualitatively accounted for by assuming the presence of a groove on the solid-1iq;id interface, at the grain boundary. SOLUTE segregation at grain boundaries may be considered in two parts, namely, nonequilibrium segregation associated with the solidification process, and equilibrium segregation in fully annealed materials.' There is much indirect evidence for nonequilibrium segregation, based on preferential etching at grain boundaries and the mechanical properties of as-cast alloys. In addition, some direct observations have been reported in which radioactive tracers were used as solute additions and segregation detected at the grain boundaries by autoradiographic techniques. However, there is little detailed quantitative data on solute concentrations related to grain boundaries, particularly for different freezing conditions and grain boundary configurations. Equilibrium segregation at grain boundaries has been considered both theoretically and experimentally. cean' has made an estimate of the maximum equilibrium solute concentration that might be expected at a grain boundary, based on the lattice distortions in the boundary region. He arrived at a concentration which was equivalent t a monatomic layer of pure solute. A similar value, based on thermodynamic arguments, was calculated by Cahn and Hilliard for the segregation of phosphorus in iron. Experimentally, much higher values of solute concentration at grain boundaries have been reported recently by both Inman and iler' for phosphorus in iron, and Ainslie et 1.' for sulfur in iron. They observed concentrations equivalent to as much as 20 to 100 atomic layers of pure solute at the grain boundaries. However, in both cases it was shown that the observed segregation was not due solely to equilibrium segregation at the grain boundary. In the former case, precipitation effectss due to trace impurities in the material were believed to account for the large amount of solute present at the grain boundary. In the latter case it was shown that a high density of dislocations in the boundary region could provide a large number of additional sites for solute atoms, other than at the grain boundary. Thomas and chalmera have reported on the equilibrium segregation of po210 in grain boundaries of Pb-5 pct Bi alloys. Using autoradiographic techniques, they observed a concentration of polonium along the boundary trace on the surface of annealed bicrystal specimens grown from the melt. The concentration only appeared after annealing, and varied with boundary angle, increasing as the boundary angle increased. Their conclusions have been questioned by Ward," who pointed out that the segregation they observed along the boundary trace was much too wide to be compatible with the usual concepts of the thickness of a grain boundary of several lattice spacings. Also, Maroun et al.,l1 with specimens similar to those of Thomas and Chalmers, found that segregation could only be detected on the specimen surface, suggesting that Thomas and Chalmers' results were associated with an oxidation effect of polonium, and not equilibrium segregation. Thomas and Chalmers replied12 that they did observed segregation at the grain boundary in the bulk material and suggested further experiments were necessary to resolve the difference. The purpose of the present investigation was to examine both nonequilibrium and equilibrium grain boundary segregation in melt grown bicrystal specimens as a function of boundary angle, growth rate, and solute concentration, and to de-

Jan 1, 1963

By K. L. Fetters, F. M. Walters

ALL previous records were broken by the Iron and Steel Division, in the number of sessions, the number of papers, and the attendance. In addition to ten papers (all preprinted) on properties, structure, aid hardenability of, carbon and alloy steels, eight formal papers were presented on one or more phases of steelmaklng, and a symposium on the determination of hydrogen and nitrogen in steel. This last started at 2 p.m. and was going strong with more than a third of the audience still present at 6 p.m.

Jan 1, 1944

By B. J. Scheiner, A. G. Smelley

The Bureau of Mines, US Department of the Interior, is conducting research on a dewatering technique for fine particles generated during the mineral beneficiation process that will recover a portion of the water now being lost using conventional waste disposal methods and significantly reduce the time required for land reclamation. The technique utilizes a flocculant, polyethylene oxide (PEO), that forms strong stable flocs that can be dewatered rapidly on static and/or rotary screens. Infield tests, phosphate clay waste has been dewatered from a nominal 2.5% solids to greater than 20% solids. In other field tests, coal-clay waste has been dewatered from a nominal 3% solids to greater than 55% solids. In addition, small-scale continuous tests have shown that bentonitic clays can be dewatered from 12% solids to 40% solids.

Jan 1, 1985

W. 0. HOTCHKISS,* Madison, Wis.-When we began to do geological field work in the Lake Superior region, we found a correlation in existence, and, as youngsters, accepted all that as settled. Both Mr. Allen and I, since that time, have seen a great many things that were not apparent nor visible to Van Hise, and those who worked with him; we realize now that the correlation was not final and that much remains to be determined concerning geology of the Lake Superior region. My attitude on this matter is that we should not publish an amended correlation as a final thing. We should avoid, in every way possible, foreclosing the minds of those who follow us in working in the geology of this region. As a matter of fact, no correlation can be final at present, because facts and data are accumulating so rapidly that every classification must be immediately modified to fit further observation. Consequently, my attitude in this matter would be, instead of saying that the iron formations of the Lake Superior region are all Middle Huronian, to say that there may be three Huronians-or four or five- we do not know. I believe it is better policy to hold to our present correlation. I do not believe there is any economic benefit to the mining man or the geologist working on problems relating to explorations for iron ore, that cannot be just as well solved by maintaining our present correlation, with a. wholesome idea of our lack of knowledge and the necessity for further detailed work. Then, if any new horizons are discovered in any particular range, the minds of the investigators will not be foreclosed because some one has said that all the iron formation is in the Middle so that there is no use looking elsewhere for it. There is use looking elsewhere, in many cases, as the ore deposits become exhausted.

Jan 1, 1920