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By P. Pollard

A method has been developed for evaluating acid treatments in fractured limestone fields by breaking down pressure drawdown into three component parts: (I) pressure differcntial across "skin" near the borehole face, (2) pressure differential due to flow resistance in the coarse communicating fissures and (3) pressure differential between the fine voids and the coarse fissures. It is apparent that in most successful acid treatments the first term, skin resistance, has been reduced or eliminated. Further, it is often possible to estimate the volume of coarse fissures associated with the second term, coarse fissure flow resistance. In cases where this volume is comparable with practical acid volumes it seems likely that this resistance also may be attacked with a suitably retarded acid. INTROD UCTION Acid treatment has been successfully applied as a general practice in the limestone wells in the Mara/ Maracaibo districts of Venezuela for some 10 years. At the same time the need has been felt for a more precise method of: (1) evaluating the effect of an acid job and (2) selecting wells which should benefit from an acid treatment. The following method, based on an analysis of build-up curves for wells producing from fractured limestone, provides a means of forecasting the effect acid will have on a well and in many cases the probable order of production rate increase which may be expected. In certain cases it is also possible to calculate the fissure volume through which the acid has to be displaced for best results. Various approximations are introduced in the method, but within the limitations of these the analysis gives an indication of how a well, whether previously acidized or not, may be expected to respond to acid treatment. Suitable build-up curves cannot be obtained on "tight" wells which do not give sustained production and the method is not applicable to such wells. Figs. 1 through 7 illustrate various types of build-up curves obtained from limestone wells in Western Venezuela. Curves are included showing (1) both skin and coarse fissure resistance, (2) skin resistance only, (3 and 4) reduction of skin resistance by acidization, (5) fissure resistance only, (6) reduction of coarse fissure resistance by acidization, and (7) acidization failure. This theory has been successfully applied for over three years during which 22 acid treatments have been carried out specifically to reduce skin resistance and three treatments to reduce coarse fissure resistance. The method has been found to be a useful aid in the selection of wells for acidization.

By Amitava Gangulee, Michael B. Bever

The effects of changes in short-range order on some thermodynamic, electrical, and mechanical properties of the silver-rich Ag-Mg solid solutions have been investigated. The heats of formation at 273°K of several alloys after two different thermal treatments were measured by liquid metal solution calorimetry. Their electrical resistivities were measured at temperatures ranging from 4° to 773°k. Tensile tests and microhard-ness measurements were carried out at room temperature. An effective short-range order parameter and an effective interaction energy are defined. The measured changes in the properties are interpreted in terms of these quantities. The short-range order parameter is evaluated separately from calorimetric and X-ray data; the results are in fair agreement. Increasing short-range order lowers the resistivity of- the silver-rich Ag-Mg alloys but does not measurably affect the temperature dependence of the resistivity. Short-range order increases the yield stress of these alloys but does not affect the ultimate tensile stress. Changes in the effective short-range order parameter independently obtained from measured changes in the heat of formation, resistivity, and yield stress are in fair agreement. THE thermodynamic, electrical, and mechanical properties of solid solutions have been investigated as functions of composition in many alloy systems, but the effects of configurational variables, such as short-range or long-range order, on these properties have received much less attention. The silver-rich terminal solid solutions in the system Ag-Mg are well-suited for the investigation of the effects of order. The composition of these solid solutions may be varied over a range extending to about 27 at. pct Mg.1 Appreciable short-range ordering is likely to take place in these solid solutions; the degree of short-range order can be varied by suitable thermal treatments. In the alloy Ag3Mg long-range ordering is possible.2 This paper is primarily concerned with the effects of short-range order on some thermodynamic, electrical, and mechanical properties of the silver-rich Ag-Mg solid solutions.-The long-range ordering transition is the subject of a concurrent paper.3 1) EXPERIMENTAL PROCEDURES 1.1) Preparation of Specimens. Ag-Mg alloys containing up to 26.4 at. pct Mg were prepared by melting 99.99 pct pure Ag (obtained from Baker Chemical Co.) and 99.99 pct pure Mg (obtained from Eastman Chemi- cal Co. or Johnson Mathey & Co.) in graphite crucibles under molten potassium chloride. The solidified ingots were homogenized at 823°K for 10 days in evacuated Vycor capsules. A surface layer 6 in. thick was then removed by machining. The ingots were swaged into rods (2.5 mm diam) which were drawn into wires (1.0 mm diam). The wire specimens were annealed at 773°K for 24 hr in vacuum and either quenched into iced brine or cooled to room temperature over a period of 15 days. The average grain diameter (obtained from the linear intercepts) was about 0.1 mm. 1.2) Calorimetry. The heats of formation of the alloys were measured in a tin solution calorimeter as the difference in the heat effects of alternate additions of samples of an alloy and the mechanical mixture of its component elements. The additions were made from 273°K to the bath at about 623°K. The heat effect on addition of the alloys was approximately 5.5 kcal per g-atom. The procedure and the method of calculation have been described.4 1.3) X-Ray Diffraction. Short-range order parameters of two alloys were calculated from diffuse scattering intensities,' obtained with briquettes made from powdered specimens. A GE-XRD 5 diffractometer with filtered copper radiation was used. The absolute intensities were based on calibrations with paraffin. 1.4) Resistivity Measurements. The electrical resistivities were measured by a potentiometric method in which the potential drop across the specimen was compared with that across a standard resistance. For measurements below room temperature, the specimens were immersed in liquid helium (4°K), liquid nitrogen (78°K), dry ice and trichloroethylene (195°K), or ice and water (273°K). Measurements above room temperature were made on specimens held in a furnace under helium or in vacuum. The resistivity measurements were reproducible to ±0.5 pct or less. 1.5) Mechanical Tests. Tensile tests were carried out at room temperature with a Tinius-Olsen XY elec-tromatic Universal testing machine. Wire specimens (nominal gage length 1 in.) were used. The strain was measured with an extensometer, which had a sensitivity of 4 x 10-5; the strain rate was 10-3 min-1. Microhard-ness measurements were made with a square-pyramid indenter and a 100-g load.11 2) RESULTS AND DISCUSSION All measurements were made on two parallel sets of specimens, one quenched and the other slowly cooled from 773°K. The reported values are the averages of at least three measurements. In the range of magnesium concentration substantially below that of the composition Ag3Mg, quenched alloys have less short-range order than slowly cooled alloys. As the magnesium concentration approaches that of Ag3Mg, slow cooling develops long-range order. Quenching sup-

Jan 1, 1969

US 4,134,618-Method for restoring an underground reservoir subsequent to the solution mining of an ore body of uranium, copper, nickel, vanadium, molybdenum, silver, rhenium, or selenium. Clean water a cycled through the mined area, via the injection and production wells used during mining, at a flow rate sufficient to entrain residual dissolved solids. The solids are separated at the surface and disposed of, e g., in a deep disposal well, while clarified water is recycled C A. Kossack, assigned to Atlantic Richfield Co. Jan 16, 1979 4 pp. (299-5) Filed. 12-29-77 (865,646) US 4,155,982-In situ leaching of a subterranean uranium ore deposit The ore is leached with a dilute aqueous solution of ammonium bicarbonate containing a small amount of hydrogen peroxide in order first to convert tetravalent uranium in the ore to the hexavalent state and second to dissolve the hexavalent uranium preferentially to the other metals or elements commonly occurring In such ore The uranium- enriched leach liquor IS brought to the surface, and the uranium recovered by means of adsorption on a particulate ion exchange resin, elution with an acid, and treatment with ammonia to precipitate relatively pure ammonium diuranate. G G. Hunkin, T P. Fife, and J R Stano, assigned to Wyoming Mineral Corp. May 22, 1979. 13 pp (423-7). Filed: 10- 9-74 (51 3,445). Same: Canadian 1,027,849, dated Mar. 14, 1978. US 4,157,847-In the mining of sulfur by the Frasch process hot water accumulating above subterranean sulfur from previous mining operations is recycled downward to contact and heat additional solid subterranean sulfur. Advantageously, pressurized and superheated drive water from above ground is commingled with the underground water to raise its temperature before it is recycled downward R. L Williams, R L Latiolais, J. L Gabriel, and R. L Bouis, assigned to Freeport Minerals Co June 12, 1979. 13 pp (299- 6) Filed 7-28-77 (81 9,879). US 4,158,76%1n this method for determining the uranium content of a solution obtained in the solution mining of an underground uranium ore deposit, the intensity of gamma radiation from the Th-234 daughter of U-238 emitted by the solution is determined as it impinges on a scintillator after being passed successively through filter foils of a ytterbium- tin alloy, a lutecium-tin alloy, and a hafnium-zirconium alloy This scintillation is evaluated as a measure of the uranium content To assure that the uranium-thorium conversion has reached a stable state, the measurement should be made about three months after the uranium solution has been produced R C Smith, assigned to Westinghouse Electric Corp. June 19, 1979 11 pp. (250-255). Filed. 10-20-77 (843,770).

Jan 1, 1980

On the following pages are abstracts of papers published by the Institute during the year 1931 as Technical Publications, Preprints, and in bound volumes. For abstracts of papers that appear in bound volumes in 1931 but that were published as Technical Publications in 1930, see the Transactions, 1930. Papers that appear in the volume in which this list is printed are not abstracted here. Many of the Technical Publications have been reprinted in bound volumes. Information regarding this disposition, and number of pages in each paper, may be found in the list beginning on page 616. The abstracts are grouped as follows: Page Page Metal Mining....................... 578 ing and Metallography of Non-Milling and Concentration........... 578 ferrous Alloys)................586 IronandSteel...................... 580 Coal Division.. ................ 592 Petroleum and Gas.............. 598 Mctallurgy......................... 585 .............. 613 Institute of Metals Division (Found- Geophysical Prospecting......... 613 Metal Mining Use of Models for the Study of Mining Problems. By Philip B. Bucky. (Tech. Pub. No. 425, 12,000 words.)—This paper describes a research project undertaken to provide a means of studying the behavior of weighty structures such as mines, dams, foundations, etc., with models of the same material in the laboratory. The paper shows that in general it can be done. The underlying theory is explained, the apparatus which was developed and built to do this is described, and the results of laboratory experiments with sandstone mine structures are given. There is discussion of the accuracy of results with the present equipment, the model size necessary, and of the size and type of equipment necessary for the obtaining of results of practical value in the field. Milling and Concentration Ball Mill Studies, I. By A. W. Fahrenwald and Harold E. Lee. (Tech. Pub. No. 375. 25,000 words.)—This paper presents the results of an extensive experimental study of some of the numerous elements entering into ball mill grinding. All apparatus used was equipped with ball bearings. Every experiment was accompanied by a power measurement accurate to 0.005 hp. Quartz was used. Each element studied, such as ball load, was varied systematically. Power curves were obtained for the mill for three general sets of conditions; namely, (1) balls only (2) balls and quartz and (3) balls, quartz and water. For each general condition, power curves were obtained for various mill speeds, ball loads and ball sizes. For conditions 2 and 3, feed sizc and weight and pulp dilution also were studied as variables. The mill output, in grams of finished product per unit of time, was obtained for each test. In a general way, output (mill capacity) paralleled the power data and this attached

Jan 1, 1931

By A. N. Mitinsky

Discussion of the paper of A. N. MITINSKY, presented at the San Francisco meeting, September, 1915, and printed in Bulletin No. 104, August, 1915, pp. 1697 to 1705. LAWFORD H. FRY, Burnham, Pa. (communication to the Secretary*). -The author assumes that the proportional limit and the elastic limit are coincident or very nearly so, and then further assumes that the stress corresponding to these two points is the least stress which if repeated will cause failure. The point is extremely interesting and it is to be regretted that the author did not quote experimental data to show the relation between the limit of repeated stress and the other properties of the material. The author's suggestion that a steel of poor quality may have a normal value for the yield point and tensile strength (see Fig. 2) and an abnormally low elastic limit, and that this will correspond to a low resistance to repeated stress, may account for a number of failures of axles in which the tensile tests show normal physical properties. If so and if a determination of the proportional limit would have eliminated the material before it was put into service, this determination will merit most earnest attention. It appears, however, that considerable further research is necessary before any definite conclusion as to the quality of a steel can be drawn from its proportional limit. Mr. Mitinsky's paper is extremely interesting and if it stimulates thought and work along the lines indicated, it may prove of considerable practical benefit. H. V. WILLE, Philadelphia, Pa.-The paper discusses the difference between the proportional limit, or elastic limit, and the yield point, and refers to the fact that much harm results from confusion of the terms yield point and elastic limit. Similar confusion has arisen in this country; the American-Society for Testing Materials does not even consider the elastic limit and proportional limit to be identical and recently adopted the following definitions:

Jan 12, 1915

By J. P. Pritchard, J. T. Pierce, O. G. Slay

This paper discusses the results of a technology-evaluation program to ascertain the feasibility of a piotornask-photoresist technology developed for fabrication of multiple-layer thin-film superconductive circuitry. The uehicle selected for this evaluation was a 120-bil associative data processor requiring a set of nine photomasks to define a similar number of patterned material layers of lead, tin, and polymer insulation. A total circuit area of 4 sq in. involved 2500 actitle and 12,000 passive crossings. Several short-free, electrically continuous specimens were satisfactorily completed under this program. Problems encountered in the preparation and use of the requi-ed set of Photomasks are discussed, as also are the problets of providing suitable external connections. A major retarding factor in the development of the superconducting thin-film cryotron technology for many years was the absence of batch fabrication means yielding necessary device density and count per substrate for practical applications. Early workers in the field desired only limited numbers of devices to permit careful study of discrete devices and representative circuitry integrating logic and memory capabilities. For these purposes mask stencils could be formed to selectively control the placement of materials, sequentially vapor-deposited in vacuum, to form the multilayer structure. In general a distinct pattern was required for each material layer; therefore, mechanical provisions were required to change not only the material source, but the patterning mask as well, before each deposition. All deposition steps were preferably performed in a single evacuation of the deposition chamber. Thus the means for storing, transporting, and registering masks and sources with respect to the substrate existed and were operated within the vacuum environment. In the authors' experience, the approach was and remains serviceable for preliminary device study, but was not extensible to an economical manufacturing method by virtue of the difficulties inherent in mask stencil preparation and use, and the capital investment implicit in the mechanization requirements. Since the commercial attraction of the cryotron technology stems principally from its potential for economical batch fabrication, the authors' program has placed major emphasis on fabrication methods. A highly useful method has evolved through adaptation

Jan 1, 1967

By Louis J. Demer, Paul A. Beck

As reported in a previous publication,1 isothermal grain growth in high purity aluminum and in an aluminum alloy with 2 pct magnesium can be adequately described by means of the empirical relation: [ ] or in some cases, by the simpler relation, [ ] Here, D is the average grain size after an annealing period t. The annealing period includes the time for complete recrystallization R, and the time for grain growth [to]. DA is the grain size as recrystallized, n is a parameter depending on the temperature and on the material. The effect of 2 pct magnesium in solid solution was to decrease D, and to increase R, A and n at a given temperature. The present work was undertaken in order to investigate the above listed effects of magnesium in solid solution, as functions of the magnesium content. The work also includes the study of certain anomalous effects observed in the recrystallization and grain growth of the 2 pct magnesium alloy at 350°C. EXPERIMENTAL PROCEDURE The method of producing the ingots used in this work was described in detail1 and need not be reproduced here. The materials used were high purity aluminum, furnished by the Aluminum Co. of America, of lot analysis shown in Table I and magnesium from a high purity distilled stock of magnesium crystals. [ ] Ingots were prepared for a series of binary aluminum-magnesium alloys of increasing alloy content. The numbers used to designate these ingots and their magnesium contents by chemical analysis are given in Table 2. [ ] The analyses showed no difference in composition between the top and the bottom of the ingots. Spectrographic analysis of the ingots for elements other than magnesium showed, within the limits of accuracy of the method, no increase in impurities over the amounts given in the lot analysis for the high purity aluminum in Table I. Careful microscopic study of ingot 21 in the as-cast condition, at magnifications up t0 1500X, revealed a cer-

Jan 1, 1948

By D. L. Harris

Chemical upgrading testwork on Stillwater chomite concentrate shows that reduction roasting and leaching (sulfuric acid and/or ferric sulfate) can provide upgraded feed to ferrochromium furnaces for making upgraded ferrochromium. Two-stage reduction smelting in electric arc furnaces can make upgraded ferrochromium also. Sulfating roasts and leaching (acid and/or water) results using gaseous SO2—SO3 or solid ammonium sulfate were not satisfactory for upgrading chromite. Chemical upgrading of domestic Stillwater (Montana) chromite has been considered at various times1'2' to provide a material with higher chromium to iron ratio, more like foreign high grade ore, for the production of standard grade ferrochromium. Physical bene-ficiation of Stillwater chromite ore can provide a ratio, Cr/Fe, no higher than the ratio in the chromite mineral, which is approximately 1.7. For comparison the analyses of a foreign metallurgical grade chromite ore, a high grade electrostatic process Stillwater concentrate and a stockpile concentrate from the Stillwater ore are noted in Table I. Single stage smelting of the high grade foreign ore with a ratio, Cr/Fe, of 3.37 can provide a ferrochromium of over 65 pct chromium content. Similar smelting of the Stillwater concentrate with a ratio of 1.7 can provide a ferrochromium of 50 to 55 pct chromium content.' It has been demonstrated on a pilot plant scale that chemically upgraded Stillwater chromite having a ratio, Cr/Fe, of 3.0 also can be smelted to provide a ferrochromium containing over 65 pct chromium.5 Two major considerations for an upgrading process are the ratio, Cr/Fe, in the product and the chromium recovery. A minimum ratio, Cr/Fe, of 3.0 is required in the product but for economic reasons a higher ratio is desirable for blending purposes as long as the recovery is satisfactory. Data from different kinds of chemical upgrading testwork are presented in this report. Some of the testwork was conducted to make a product which was not intended to be feed for ferrochrome smelting, but the data are considered pertinent to chemical upgrading. Results reported by others are noted also for comparison. WORK REPORTED BY OTHERS The U. S. Bureau of Mines has contributed much to the literature on chemical upgrading of chromite and a summary is given in Table 11. Reduction roasting and acid leaching were reported by Boericke and Bangert,1 by Lloyd and Gorst, et a1,2 and by Boericke3 to demonstrate very good success on a laboratory scale and only fair success in pilot plant tests for Stillwater (Benbow) concentrates. This work included basic studies on thermodynamic properties to explain the reduction and leaching results. Canadian workers, Downes and Morgan,9 have reported experimental success in upgrading a low grade Bird River chromite, similar to Stillwater material by the same process. Russian workers1' have noted results on reduction tests of high grade chromite which may apply to low grade ores and which help in understanding the reduction process. The use of flux additives in the reduction process was an innovation of their work. The Canadian workers9 also reported other kinds of experiments, including autoclave leaching of the chromite in a limited amount of sulfuric acid. An insoluble basic chromium sulfate was formed and separated from soluble iron, magnesium, and aluminum sulfates to provide an upgraded material. U.S. Bureau of Mines workers, Lloyd, Rosenbzum, Home and Davis,' reported on autoclave leaching of Benbow concentrates as a means of obtaining chromium alum for electrolysis. This last work required selective crystallization of alum to separate iron from chromium. Chloridizing roasting of Benbow and Mouat concentrates has been reported by Hunter and Banning6 and others8 to show that the iron chloride could be volatilized from the chromite to provide upgraded residues.

Jan 1, 1964

By George D. Graffin.

The first use of graphite is lost in the mists of time. It was used by primitive man to make drawings on the walls of caves and by the Egyptians to decorate pottery. As early as 1400 A.D. graphite crucibles were being made in the Haffnerzell district of Bavaria. Through the Middle Ages graphite was confused with other minerals, especially galena and molybdenite. Two common names that are still used for the mineral are "Plumbago," meaning leadlike, and "Black Lead." The latter name implied that graphite is either composed of lead or at least contains a large percentage of it. Gessner is credited with having recognized it as a separate mineral in 1565, but its composition was not determined until 1779, when Scheele demonstrated that graphite oxidized to carbon dioxide, thus proving its carbon constitution. In 1789, Werner named it "graphite" from the Greek word "graphein," meaning to write. The United States has long relied on foreign countries for its graphite supplies. This reliance has been due more to the lack of suitable domestic graphites than to any particular preference for buying minerals overseas. Ceylon (now Sri Lanka) graphites were imported as early as 1820, and Madagascar graphites have been imported since the properties on that island were opened up about a hundred years later. Mexico has long supplied the United States with most of its requirements for amorphous graphite. Physical Properties and Classification Graphite is found in laminated, flaky aggregates disseminated in schistose rocks. It also occurs in veins and exhibits a foliated or fibrous structure. Graphite is a black lustrous mineral that crystallizes in the hexagonal system, with rhombohedral symmetry. The crystals have tabular form and are six-sided; the faces are commonly striated. The flakes have perfect basal cleavage and are opaque. When well crystallized, the flakes have a black metallic luster while the amorphous material is black and earthy, with a microcrystalline compactness. The flakes feel greasy. Graphite is an excellent conductor of heat and electricity. It melts at approximately 3550°C at a triple point under 1250 psi. It sublimes between 3300-3500°C at 14.7 psi. At 3726°C a second triple point occurs at approximately 100,000 atmospheres. Thermal oxidation in the presence of oxygen begins at 300°C and the rate increases with temperature. The three forms of carbon (charcoal, graphite, and diamond) are distinguished by chemical and physical tests. The specific gravity of charcoal is 1.3 to 1.9, of graphite 2.266 g/ cm3 (crystal density), and of diamond 3.5. Graphite has a hardness of 1 to 2 (Mohs' scale). Natural graphite can be divided into three classes: disseminated flake, crystalline vein (fibrous or columnar), and amorphous. Flake graphite is a lamellar form found in metamorphic rocks, such as marble, gneiss, and schist. Each flake is separate, having crystallized as such in the rock. Crystalline vein graphite is found in the form of well defined veins or as pocket accumulations along the intrusive contacts of pegmatites with limestones. The graphite of such deposits is of two types, foliated and columnar. The important Sri Lanka (Ceylon) deposits are vein type. Amorphous graphite is commonly found as minute microcrystalline particles more or less uniformly distributed in feebly metamorphic rocks, such as slates and shales, or in beds consisting practically entirely of graphite. The latter usually are metamorphosed coal seams and carry as much as 80-85% graphitic carbon, while the former, being altered carbonaceous sediments, commonly range from 25 to 60%

Jan 1, 1983

By S. E. Bronisz, Dana L. Douglass

a Uranium was deformed by cold rolling, and the effects of this plustic deformation on the microstruc-ture of the metal were observed by the technique of transmission elecbon microscopy. The recrystalli-zation of selected cold-wmked samples was also studied by this method. The samples were prepared for examination by electrolytic thinning in a standard metallographic electrolyte which has not been previously reported as being used in producing thin foils of uranium. The microstructural changes observed in the a uranium were generally similar to those seen by optical microscopy. The changes in the microstructure of a uranium following cold work and recrystallization treatments have been the subjects of several studies employing optical and X-ray techniques.12-19 These studies indicated that twinning was the redominant mode of deformation at room temperature20 and that the regions of high energy associated with the deformation twins were preferred sites for the initiation of recrystallization.15,18, Recently several workers have prepared thin foils of uranium suitable for examination by transmission electron microscopy.'-lo The foils thus prepared have been used to study fission fragment damage; a particular dislocation reaction,' and gas precipitation." At this laboratory the microstructural changes occurring during the cold working and recrystallizing of a uranium samples have been studied by using transmission electron-microscopy techniques. The foils used in this work were electrolytically thinned in a polishing bath not reported previously in the literature as being used for this purpose. EXPERIMENTAL PROCEDURE The uranium used in this investigation was depleted a uranium sheet 4 mils thick. The results of a spectrochemical analysis of this material are shown in Table I. The as-received uranium was cut into strips, 1 in. wide by 5 in. long, and annealed in vacuo at 600°C for 2-1/2 hr. The resulting microstructure consisted of relatively uniform, equiaxed grains having diameters of 10 to 50 p. Cold Working. The cold-worked samples were prepared by rolling several of the annealed uranium strips to various thicknesses. The strips were reduced 3.5 ± 0.5, 6.0 ± 0.6, 10.0 ± 0.5, 19.5 ± 1.0, and 28.5 ± 2.0 pct in thickness. It was not possible to achieve these reductions with a single pass through the rolling mill, so the strips were turned end for end during the rolling procedure. The cold-rolled strips were stored in dry ice until samples from them could be thinned and examined (within 24 hr after rolling). Annealing. The samples used in studying the re-crystallization behavior of a uranium were obtained by annealing sections of the strips which had been reduced 10.0 and 28.5 pct. These samples were sealed in evacuated Pyrex capsules and were annealed in a tube furnace at temperatures from 200" to 600°C and for times from 1/2 to 2 hr, see Table l. Thinning: The samples from the rolling and heat treatments were prepared for examination in the electron microscope by electropolishing in a bath composed of 25 g chromic acid, 133 ml glacial acetic acid, and 25 ml water. This electrolyte has been used and recommended for preparing specimens for optical metallography It was necessary to mask the edges of the sample with a stop-off paint in order to prevent preferential attack in these areas. The paint used was made by dissolving polystyrene in benzene. The electrolytic cell consisted of a cylindrical stainless-steel cathode placed in a beaker containing the electrolyte, with the sample as the anode positioned at the cell axis. The temperature of the electrolyte was held below 15°C by cooling with liquid

Jan 1, 1963

By R. M. Caves

High-purity dense tungsten coating is obtained by means of a modified de Boer-van Arkel iodide process using tungsten bromides. The all-glass reaction system is pumped, baked, and sealed (pinched-off) at about 10-7 mm Hg pressure. The bromides then formed in situ are decomposed, depositing tungsten on heated tungsten surfaces. Heating of the specimen is done inductively in a novel arrangement that avoids electrodes of glass-to-metal seals. The tungsten, deposited at specimen temperatures from 2000° to 2800°F and bulb (halide) temperatures of 225" to 725°F, was adherent and uniform, and ranged in thickness to 1/8-in. REFRACTORY metals are of interest at NASA for use in hypersonic aircraft, in rocket engines, and in other thrust devices where very high temperatures are encountered. Tungsten, with a melting point about 6100° F, is potentially very useful for some of these applications. Considerable research on tungsten and its alloys is currently being conducted at the NASA Lewis Research Center. In this tungsten research program, there is need for a method of depositing high-purity, nonporous tungsten coatirlgs. Metallurgical bonding of the coating both to itself and to the substrate is required. In addition, it is necessary to be able to deposit thin, uniform coatings on substrates of a variety of shapes and sizes for laboratory test purposes. A survey of the methods previously used for depositing tungsten coatings indicated that none would likely meet these requirements for high purity, good uniformity, and high density except thermal decomposition of the halides. The method for coating that was selected for investigation was the thermal decomposition of tungsten bromide. This is a variation of the van Arkel and de Boer iodide process established years ago and recently reviewed.1,2 This process is applicable to the transition metals in general. More recently, the application and techniques were extended with chlorine3 and fluorine,4 and included the coating of tungsten. This is believed to be the first report on the use of the bromide for tungsten coating. Bromine was chosen over the other halogens because it promised a lower temperature for tungsten

Jan 1, 1962

By P. D. Frost, H. A. Robinson, J. R. Doig, M. W. Mote

The mechanism of hardening in heat-treatable zirconium alloys was foUNd to be analogous to that for titanium alloys. Zirconium containing a relatively large addition of a ß -stabilizing element such as molybdenum or columbium can be hardened by the following transformation: Lean alloys, having insufficient alloy content to retain ß at room temperature are hardened by the following transformation: Application of these findings in Zr-Mo-Sn and Zr-Nb-Sn alloys produced strengths as high as 190,000 psi with reasonable ductility. PRIOR research on zirconium alloys has been concerned with development of greater strengths and creep resistance by solid-solution hardening or by dispersion hardening. Although solution and aging heat treatments had been applied earlier to zirconium alloys, quenching frequently produced low ductility. The possibility that the ß-to-w transformation, discovered earlier in titanium alloys,' might also occur in zirconium alloys and cause low ductility was considered, and, indeed, was found as predicted2 to be the case. In the earliest experiments, the heat-treatment response of titanium, too, was disappointing. However, by avoiding the formation of the embrittling w phase, it became practical to obtain room-temperature strengths higher than 180,000 psi, with elongation values of 10 pct.3 Based on the present concept of titanium heat treatment, the principal requirement for a heat-treatable zirconium alloy is that it contains a certain minimum amount of one or more ß -stabilizing elements. Only molybdenum, columbium, and tantalum, when present in sufficient amounts, are known to stabilize ß zirconium to room temperature during rapid cooling from the ß field. Tantalum was undesirable because of its high thermal-neutron cross section. Aluminum and tin are effective a stabilizers, but aluminum has been shown to seriously decrease the corrosion resistance of simple zirconium alloys in hot water. Therefore, for the present study, tin was used as the stabilizer addition. The alloys selected for this evaluation are presented in Table 1 along with their analyses and ß-transus temperatures. The analyses indicated that intended compositions were usually realized. EXPERIMENTAL PROCEDURES All of the alloys were melted from sponge zirconium and fabricated to sheet for heat treatment

Jan 1, 1960

By W. C. Hagel, H. J. Beattle

DURING an earlier examination of high-temperature alloy, A-286, the presence of an unknown intermetallic compound was verified by X-ray diffraction. Owing to its prominent appearance at grain boundaries, the arbitrary name of G phase was assigned.' Low-silicon, vacuum-melted heats were found to contain no G phase, and this investigation was initiated to determine the influence of silicon on G-phase formation; additional work was undertaken to extend existing data on other intermetallic compounds and the aging reactions in this group of alloys. Taylor and Floyd2-4 observed that the Ni3Al phase (y') and the Ni8Ti phase (7)) are the only equilibrium intermetailic compounds in nickel ternary alloys containing up to 25 pct Cr and 10 pct Ti or Al. They found that y' can dissolve considerable nickel, chromium, and titanium, although the stoichio-metric composition of 7 remains fixed. Nordheim and Grant5 confirmed that age hardening of 80 pct Ni-20 pct Cr alloys of the Nimonic-80 type is due to precipitation of y', where aluminum is partially replaced by titanium. They suggest that optimum hardness and ductility result from increasing the titanium to aluminum ratio toward the end of the y' solubility range and from increasing total titanium and aluminum content to the maximum limit permitted by processing. Such information is necessary for those seeking to improve the service-temperature range and long-time structural stability of high-temperature components. Experimental Methods Compositions of materiais studied. are listed in Table I. Alloys D, E, and F possess representative A-286 analyses; silicon increases from less than 0.02 to 1.75 pct in alloys A to H; in alloys I to K, titanium decreases from 2.24 to 0.39 pct, and aluminum increases from 0.1 6 to 240 pct. Alloys A and D were solution heat treated for 4 hr at 1700°F, oil quenched and aged for 0.5, 2, 6, 12, 30, 70, 200, and 1000 hr at 1200°, 1300°, 1400°, and 1500°F. Therefore, a total of 33 specimens was required for each

Jan 1, 1958

By C. N. J. Wagner, E. N. Aqua

The bee alloys of the terminal solid solution of rhenium in niobium were investigated by X-ray diffraclion methods. The analysis of the broadening of the powder pattern peaks from the niobium-rich alloys, cold-worked by filing, showed evidence for faulting on (211) planes. The alloys with larger rhenium concentrations were brittle, and fractured when filed. The analysis of the shapes of the diffraction profiles from powders produced by hammering with steel plates) of these brittle alloys indicated that the broadening was due predominantly to platelets bounded by clibe planes. This result was consistent with the Laue patterns from single-cleazlage facets which showed evidence for clearage fracture on {100} planes. The influence of faulting on the mechanical properties of face-centered cubic (fcc) metals and alloys, i.e., how faulting affects the various dislocation configurations in fcc metals, is well-known.' The important question is whether or not faulting occurs in body-centered cubic (bcc) metals and alloys, and, furthermore, if faulting does occur, to what extent it affects the mechanical properties. Theoretical calculations indicate that the stacking-fault energy is rather high in most bcc metals.2 The results of sev-eral studies using transmission electron microscopy have indicated that faults are present in well-annealed and lightly deformed bcc metals and alloys, such as tungsten,3 vanadium,4 and Mo-Re alloys.5,6 These faults, as have been observed, may be stabilized by the presence of interstitial (C,N,O) atom segregation to the extended dislocations. In addition, there is considerable X-ray diffraction evidence for faulting in bee metals,7-8 using the same techniques that were successful for the study of faulting in fee metals and alloys.7 This X-ray diffraction method is currently the only technique applicable for the investigation of faulting in metals with high stacking fault energies, i.e., when severe amounts of deformation are required to produce sufficient amounts of faulting to be detectable by X-rays. The thinned films of heavily deformed metals will become opaque in the electron microscope due to the high dislocation densities present. In a previous investigation of faulting8 in bee metals of group Vb and VIb, the authors observed that niobium was ductile when filed at room temperature, and showed the highest density of faults on the (112) family of planes. A niobium-base alloy system was therefore chosen to study the effect of alloying on the occurrence of faults in a bcc alloy. There is a large range of terminal solid solubility of rhenium in the alloys of the bee refractory metals. All of the Group VIb-rhenium alloys, i.e., Cr-Re, Mo-Re, and W-Re, exhibit solid solution hardening without loss of ductility.9 In fact, the ductility reaches a maximum for alloys with compositions near to the limits of solubility. This enhanced ductility has been attributed to the lowering of the stacking-fault energy in the alloy; i.e., the increased amounts of twinning provide an additional mode of deformation, resulting in the observed high ductility.' Because of this demonstrated effect of rhenium in bee alloys, it was decided to study a series of alloys of Nb-Re. Using the same X-ray diffraction methods as described in the previous investigation,' one is able to identify the possible causes of broadening of the powder pattern peaks, e.q., particle size, microstrains, stacking faults, and/or twin faults. The separation of these various contributions to the measured peak shape is accomplished by the Warren-Averbach analysis.7 I) EXPERIMENTAL PROCEDURE A series of seven bee solid solution alloys containing from 2.5 to 21.5 at. pct Re (remainder niobium) were prepared at the General Electric Research Laboratory. Buttons, weighing 25 g, were alloyed from electron-beam-melted niobium chips and random rhenium sheet by arc melting in a water-cooled copper crucible, under an argon atmosphere. The buttons were inverted and completely remelted to promote homogenization. The nominal alloy compositions are listed in Table I. Samples of the cold-worked alloys were obtained by filing to produce a powder for the X-ray study. Alloys too brittle to be filed were hammered with steel plates. The resultant filings or brittle impactings were screened through 150-mesh classifiers and compacted to the required shape for the diffractometer holder. The X-ray diffraction peaks were automatically recorded by fixed time counting at uniform 28 intervals, or by continuous registration with a ratemeter. In all cases, the (110)-(220) and (200)-(400) pairs of peaks and the (211), (310), (222), and (321) reflections were measured on a GE-XRD5 diffractometer using CuKa radiation with nickel filter or MoKct radiation and a LiF monochromator in the diffracted beam. The first part of the data reduction, completed with the aid of a series of programmed computations,10 was the analytical resolution of the Kol component of the diffraction profile. Subsequent computations were then made with reference only to the resolved Kol peak shape. These included the measurement of the

Jan 1, 1967

By W. M. Gray

The determination of the state of stress existing at a point in any solid body requires the determination of the six components of the stress tensor relative to a convenient set of axes. One general method of doing this in rock is to make strain or deformation measurements associated with local relief of stress in a number of boreholes penetrating a limited volume in the vicinity of the point at which the stress is to be determined. The stress is assumed to be constant throughout this volume. Leeman1 has described a number of the instruments that have been developed for making deformation or strain measurements in boreholes. Panek2 has described the application of statistical methods to the determination of the average components of ground stress from sets of measurements made in boreholes by means of deformation meters of the type developed by the U.S. Bureau of Mines. In this paper attention is given initially to the strain cell developed for use on the flattened ends of boreholes by the Council for Scientific and Industrial Research (CSIR) , South Africa. The equations required for evaluating the average components of ground stress from measurements made by means of the CSIR strain cell are derived. These equations are similar in form to those applying to measurements made by the borehole deformation meter developed by the U.S. Bureau of Mines. The results of an investigation of the properties of the equations are described. These results are important in the practical use of both the instruments mentioned above and any instrument based on similar principles.

Jan 1, 1968

By A. G. Weber, K. H. Coats, M. H. Terhune, R. L. Nielsen

Two computer-oriented techniques for simulating the three-dimensional flow behavior of two fluid phases in petroleum reservoirs were developed. Under the first technique the flow equations are solved to model three-dimensional flow in a reservoir. The second technique was developed for modeling flow in three-dimensional media that have sufficiently high permeability in the vertical direction so that vertical flow is not seriously restricted. Since this latter technique is a modified two-dimensional meal analysis, suitably structured three-dimensional reservoirs can be simulated at considerably lower computational expenses than is required using the three-dimensional analysis. A quantitative criterion is provided for determining when vertical communication is good enough to permit use of the modified two-dimensional areal analysis. The equations solved by both techniques treat both fluids as compressible, and, for gas-oil applications, provide for the evolution of dissolved gas. Accounted for are the effects of relative permeability, capillary pressure and gravity in addition to reservoir geomety and rock heterogeneity. Calculations are compared with laboratory waterflood data to indicate the validity of the analyses. Other results were calculated with both techniques which show the equivalence of the two solutions for reservoirs satisfying the vertical communication criterion. INTRODUCTION Obtaining the maximum profits from oil and gas reservoirs during all stages of depletion is the fundamental charge to the reservoir engineering profession. In recent years much quantitative assistance in evaluating field development programs has been provided by computerized techniques for predicting reservoir flow behavior. Because of the spatially distributed and dynamic nature of producing operations, automatic optimization procedures, such as those now in use for planning refining operations, are not now available for planning reservoir development. However, present mathematical simulation techniques do furnish powerful means for making case studies to help in planning primary recovery operations and in selecting and timing supplemental recovery operations. A number of methods have been reported which simulate the flow of one, two or three fluid phases within porous media of one or two effective spatial dimensions>-4 However, applying computer analyses to actual reservoirs have been limited mostly to two-dimensional areal or cross-sectional flow studies for two immiscible reservoir fluids. To obtain a three-dimensional picture of reservoir performance using such two-dimensional techniques, it has been necessary to interpret the calculations by combining somehow the results from essentially independent areal and cross-sectional studies. To the authors' knowledge, the only other three-dimensional computational procedure, in addition to those presented here, was developed by Peaceman and Rachford8 to simulate the behavior of a laboratory waterflood. Two computational techniques which may be used to simulate three-dimensional flow of two fluid phases are described in this paper. The first method, called the "three-dimensional analysis", employs a fully three-dimensional mathematical model that treats simultaneously both the areal and cross-sectional aspects of reservoir flow. The second method, called the vertical equilibrium (VE) analysis", is applicable

By C. M. Loeb, T. E. Norman

The use of ball, rod and tube mills for grinding ore, cement and other materials has grown so rapidly during the past forty years that the world's annual consumption of ferrous grinding media for these mills is now estimated to be between one half million and one million tons per year. Ferrous grinding balls constitute the major portion of this tonnage. Obviously they represent suficient value to justify thorough studies of the factors governing their performance. The selection of grinding balls is governed principally by: I. Quality (wear resistance, impact resistance, soundness, and the like). 2. Sources of supply and delivered cost. 3. Grinding characteristics or efficiency in the ball mill. This paper deals principally with the quality of ferrous grinding balls. In the study of these factors certain data relative to the fundamental nature of ball wear in ball mills have been obtained. These data are also presented and discussed briefly. The Development of a Suitable Wear Test A study of the fundamental factors governing the quality of grinding balls has been hampered seriously by the fact that a competent test has, in the past, involvetd the purchase of several hundred tons of halls of a specific type which were then run in one or more ball mills for a period ranging from several months' to several years' duration. Often, during the period of test, it became necessary to change operating conditions or the character of the ore fed to the test mill with the result that the rate of ball consumption changed and the test figures became of little value. Under such circumstances, progress in the development of better grinding balls, has been necessarily slow. Economic factors and variations in the quality of balls produced by different sources of supply generally make it necessary for each mill operator to determine for himself the most suitable type of balls for his mills. In our own ball mill grinding operations at Climax, Colo., we were faced with this problem. After we had run a few large scale wear tests at considerable expense we decided to investigate the possibilities of a small scale wear test which would be capable of testing numerous types of balls within a relatively short time. The most important requirement of any test is, of course, that it give results which can be used to predict accurately the wear in full scale operations. It was known that Ellis and his associates1'2 had developed a method of testing grinding balls by small scale tests run at the Ontario Research Foundation. Ellis' method of testing was used as a starting point in our investigations. In the course of our tests a number of modifications of the original method were found to be desirable so that, by an evolutionary procedure, a method of small scale

Jan 1, 1949

By C. M. Loeb, T. E. Norman

The use of ball, rod and tube mills for grinding ore, cement and other materials has grown so rapidly during the past forty years that the world's annual consumption of ferrous grinding media for these mills is now estimated to be between one half million and one million tons per year. Ferrous grinding balls constitute the major portion of this tonnage. Obviously they represent suficient value to justify thorough studies of the factors governing their performance. The selection of grinding balls is governed principally by: I. Quality (wear resistance, impact resistance, soundness, and the like). 2. Sources of supply and delivered cost. 3. Grinding characteristics or efficiency in the ball mill. This paper deals principally with the quality of ferrous grinding balls. In the study of these factors certain data relative to the fundamental nature of ball wear in ball mills have been obtained. These data are also presented and discussed briefly. The Development of a Suitable Wear Test A study of the fundamental factors governing the quality of grinding balls has been hampered seriously by the fact that a competent test has, in the past, involvetd the purchase of several hundred tons of halls of a specific type which were then run in one or more ball mills for a period ranging from several months' to several years' duration. Often, during the period of test, it became necessary to change operating conditions or the character of the ore fed to the test mill with the result that the rate of ball consumption changed and the test figures became of little value. Under such circumstances, progress in the development of better grinding balls, has been necessarily slow. Economic factors and variations in the quality of balls produced by different sources of supply generally make it necessary for each mill operator to determine for himself the most suitable type of balls for his mills. In our own ball mill grinding operations at Climax, Colo., we were faced with this problem. After we had run a few large scale wear tests at considerable expense we decided to investigate the possibilities of a small scale wear test which would be capable of testing numerous types of balls within a relatively short time. The most important requirement of any test is, of course, that it give results which can be used to predict accurately the wear in full scale operations. It was known that Ellis and his associates1'2 had developed a method of testing grinding balls by small scale tests run at the Ontario Research Foundation. Ellis' method of testing was used as a starting point in our investigations. In the course of our tests a number of modifications of the original method were found to be desirable so that, by an evolutionary procedure, a method of small scale

Jan 1, 1949

By Walter H. Bucher

This symposium is designed to lay the basis for a general discussion of the place of geophysics in the training of geologists. As there is danger that in the ensuing debate individual interests may be given emphasis out of proportion to their place, we shall do well to view the whole field of geological inquiry in order to see the problem in true perspective. The Nature of Geological Inquiry "Basic" and "Complex" Sciences It is convenient to divide all science into two major divisions, the basic and the complex sciences. The basic sciences separate out from reality such entities as "substances" and "movements," describe their behavior in terms of arbitrary units of measurement and derive from them by progressive abstractions concepts and patterns of behavior that exist between them, so-called general "laws" and "properties" of nature. The complex sciences, on the other hand, deal, with little or no abstraction, with those objects of reality that are accessible to man in the atmosphere, the hydrosphere, the lithosphere and the biosphere. Their work comprises two types of inquiry. One is concerned with abstractions to the extent of dealing with types rather than individuals—that is, with such things as plants, animals, protoplasm; clouds, streams, gla- ciers; volcanoes and mountain ranges. It comprises the search for general properties and patterns of behavior or "laws" that characterize the objects and their reactions to each other. These properties and laws apply always, everywhere. They are independent of the stream of time. We may call the results of this sort of inquiry timeless knowledge. The other type of inquiry is concerned with the objects themselves—that is, with this animal and that plant; this river system and that mountain chain; this glacier and that valley. Like all concrete objects in nature, they are subject to change with the passage of time, especially when it is measured in years, centuries, eons. The characteristics by which we recognize them —indeed, their very existence—are dependent on their position at this point in the stream of time. This we may call time-bound kntowledge. The so-called descriptive sciences are all bound to the past of which the objects of their study are the product and through which alone their present properties call be understood. They are historical sciences. This obvious fact is easily overlooked, which leads to serious misunderstanding, as we shall see later. Dynamic Geology With this broad picture in mind, let us now examine the nature of geological inquiry, defining, for the purposes of this discussion, geology as the science of rocks. Air is not a rock; water is. Meteorology and climatology are, correspondingly, gen-

Jan 1, 1946

By Walter H. Bucher

This symposium is designed to lay the basis for a general discussion of the place of geophysics in the training of geologists. As there is danger that in the ensuing debate individual interests may be given emphasis out of proportion to their place, we shall do well to view the whole field of geological inquiry in order to see the problem in true perspective. The Nature of Geological Inquiry "Basic" and "Complex" Sciences It is convenient to divide all science into two major divisions, the basic and the complex sciences. The basic sciences separate out from reality such entities as "substances" and "movements," describe their behavior in terms of arbitrary units of measurement and derive from them by progressive abstractions concepts and patterns of behavior that exist between them, so-called general "laws" and "properties" of nature. The complex sciences, on the other hand, deal, with little or no abstraction, with those objects of reality that are accessible to man in the atmosphere, the hydrosphere, the lithosphere and the biosphere. Their work comprises two types of inquiry. One is concerned with abstractions to the extent of dealing with types rather than individuals—that is, with such things as plants, animals, protoplasm; clouds, streams, gla- ciers; volcanoes and mountain ranges. It comprises the search for general properties and patterns of behavior or "laws" that characterize the objects and their reactions to each other. These properties and laws apply always, everywhere. They are independent of the stream of time. We may call the results of this sort of inquiry timeless knowledge. The other type of inquiry is concerned with the objects themselves—that is, with this animal and that plant; this river system and that mountain chain; this glacier and that valley. Like all concrete objects in nature, they are subject to change with the passage of time, especially when it is measured in years, centuries, eons. The characteristics by which we recognize them —indeed, their very existence—are dependent on their position at this point in the stream of time. This we may call time-bound kntowledge. The so-called descriptive sciences are all bound to the past of which the objects of their study are the product and through which alone their present properties call be understood. They are historical sciences. This obvious fact is easily overlooked, which leads to serious misunderstanding, as we shall see later. Dynamic Geology With this broad picture in mind, let us now examine the nature of geological inquiry, defining, for the purposes of this discussion, geology as the science of rocks. Air is not a rock; water is. Meteorology and climatology are, correspondingly, gen-

Jan 1, 1946