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By D. K. Deardorff, Earl T. Hayes

An improved technique is described for the accurate determination of melting points of metals in the temperature range 1500' to 2500°C. The improvements consist of gradient heating and refinements in cavity preparation to obtain true black-body conditions. The melting point of hafnium, as determined by this method, is set at 2222°±30°C. This is over 200°C higher than one of the values reported earlier. Discrepancies in the previously reported values for the melting point of hafnium are explained. The melting points of zirconium and titanium are found to be 1855O±15OC and 1668°±10°C, respectively. Reproducibility of results was ±3OC. PRIMARILY, this report is being made to correct a 1975o±25oC1 value for the melting point of hafnium, and to present an improved method for melting point determination. As a matter of interest, the technique was also applied to determining the melting point of zirconium and titanium. There is a wide difference in the melting point of hafnium as reported by competent investigators. DeBoer and Fast' reported a value of 2230°±500C, and later work of McPherson, as reported by Aden-stedt, placed the melting point at 1975o±25oC. Zwikker" calculated that the melting point was 2430°C. In resolving this discrepancy, improvements were made in the procedure for determining the melting points of refractory metals in the range 1500" to 2500°C. Special techniques are necessary to determine the melting point of these metals accurately. Since the metals oxidize in air above 900oC, the determinations must be carried out in an inert gas or vacuum. Also, every known refractory contaminates them to some extent. In addition, the attainment of true black-body conditions is always difficult. DeBoer and Fast actually determined the melting point of Hf-Zr as-deposited iodide process alloys and extrapolated to 100 pet Hf. McPherson employed a tungsten wire suspension similar to that described by Schramm, Gordon, and Kaufmann,1 and used hafnium metal produced by the iodide process. There was no apparent reason for the wide spread in melting points, since the quality of the metal was very good and the work was under the direction of highly competent investigators. Retracing some of this work revealed one understandable error in the case of hafnium, and led to development of an improved technique for determining melting points of reactive metals in the range 1500" to 2500°C. Material Crystal bar hafnium, zirconium, and titanium were used for this work, with analyses as shown in Table I. The hafnium was of the highest purity that has been prepared, though not as pure as the zirconium and titanium. At the instigation of the Pittsburgh Area Office of the AEC, a special lot of Hfo2 was purified, converted to the tetraflouride, and bomb-reduced with calcium, all at the Iowa State College Laboratories. This crude hafnium metal was then refined by the iodide process at the Foote Mineral Co. All specimens were cut with a Sic wheel, ground, pickled, and dried carefully before use. Procedure General Tungsten Suspension Method—In this method, a small specimen is suspended by a fine tungsten wire in a slender, induction-heated tungsten or tantalum cylinder, all under vacuum. The melting point is determined by heating the specimen slowly while observing it with an optical pyrometer focused upon a portion of the specimen that radiates as a black body. This means that there should be no reflected radiation, either from colder objects near the pyrometer or from hotter surfaces. The induction heater would be the only hotter object and, if it is slender enough, the specimen will attain the same temperature. Often a slender hole is drilled into the specimen as a source of black-body radiation. This was the general method used by McPherson in obtaining his value of 1975°C for the melting point of hafnium. In trying to repeat this work, it was found that the points of contact between the

Jan 1, 1957

By E. V. Potter, E. T. Hayes, H. C. Lukens

Large volumes of hydrogen are liberated at the cathode during electrolytic precipitation of manganese. Most of the gas escapes from the electrolyte, but a considerable amount may be entrapped in the manganese plate. Gas has been observed to escape from manganese melts in puffs that bite at the surface. It has been reported that castings made with electrolytic manganese tend to rise in the molds; for this reason the manganese is often treated to remove hydrogen before the melt is made or it is premelted and used as cast manganese in making the alloys. The effect of hydrogen on the properties of manganese and its alloys is not known, but its effect on iron and iron alloys has been studied extensively.l.2 The close relationship between iron and manganese suggests that hydrogen may have a similar effect on the properties of manganese and its alloys. The purpose of this investigation was to determine the amount of hydrogen or other gases in typical commercial electrolytic manganese sheet and to investigate ways of removing it most conveniently. Apparatus The apparatus used is shown schematically in Fig. I. It consists of a chamber A in which the metal sample is placed, a vacuum or pressure gauge B, volume gauge C, vacuum pump D, hydrogen container E, auxiliary gas chamber F, and furnace G. The specimen chamber was made of two concentric quartz tubes. The outer one, a, connects with the closed gas system and is surrounded by the furnace G. A second tube, b, fits closely inside a and has a small end that projects into the space for the specimen and holds the thermocouple for measuring the temperature of the sample. The inner tube is joined to the outer tube outside the furnace, with rubber tape and sealing wax, to prevent gas leakage into or out of the closed system. This type of specimen container is loaded very easily and can be used several times if molten metal does not come in contact with the quartz. An ordinary mercury manometer B is used to measure the pressure in the system. The volume gauge C is essentially another mercury manometer, but the volume of the column is much larger than normal and the height of the mercury can be varied by raising or lowering the well H. In this apparatus the tube had a volume of IOO C.C. for a 60-cm. length. For larger changes in gas volumes, auxiliary containers F were used to increase the volume of the system by known amounts. Valves were arranged so that these auxiliary containers could be filled from the system and evacuated by the pump as often as necessary to accommodate the increases in the volume of gas in the system. The furnace G, used to heat the samples, was equipped with an automatic temperature controller, which maintained the desired temperatures within ± 5°C.

Jan 1, 1945

By Gregoire Gutzeit

THE development reported in this paper was begun by the author a number of years ago, while he was a lecturer on complex chemistry and metallurgy at the University of Geneva, Switzerland, and in charge of that institution's research laboratory. Completion of the development and reduction to practice did not occur until last year at the Westport mill, laboratories and testing plant of the Dorr Company, where this method is now in general use for identifying and localizing the mineral constituents of both metallic and nonmetallic ores. It has proved to be a practical tool of the metallurgical staff at the Westport mill, devising unusual milling flowsheets for complex and refractory ore bodies. In a number of instances the findings have been successfully used as fundamental factors in the design and specification of complete metallurgical plants. Seven examples of the use of this method in solving practical milling problems are included in this paper. GENERAL OUTLINE The microscopic study of an ore, at first only of scientific interest, has proved extremely useful both in practical geology and in ore dressing. The binocular magnifying lenses for rough observation of the products of an ore-dressing plant have been in use for a long time; but only within the last few years has a systematic microscopical examination of ore samples become a normal tool of any research laboratory dealing with ore-dressing problems. Such an investigation avoids considerable loss of time as well as empirical trials and useless experimentation. It will generally indicate the correct grinding and often will suggest the proper method of treatment. The petrographic determination of transparent minerals in thin sections, or even in grains, has been perfected, and very accurate methods have been devised to meet any requirement, such as Feodorof's rotating stage on the petrographic microscope. Almost all transparent minerals can be positively identified by their optical properties; i.e., isotropism, anisotropism, color, pleochroism, refractory index, cleavage, crystal form, birefringence, and others. The identification of opaque minerals is a much more difficult problem and can be done only by using polished specimens. Unfortunately, most of the valuable metallic ores, and even some of the nonmetallic ones, are not transparent; therefore it has been necessary to develop a special technique for the determination of these minerals. Some optical properties-for instance, isotropism, anisotropism, color, cleavage, reflecting power-are often adequate in roughly classifying the mineral. Only "reflecting power" is a measurable value, provided special photometric equipment (ocular photometer or Orcel's photoelectric cell) is available. The other optical properties mentioned are more or less relative,

Jan 1, 1942

By L. C. Glenn

IN the preparation of this paper the writer has drawn freely upon the writings of Orton, Munn, Shaw, Mather, Miller, Hoeing, St. Clair, Jillson, and others, as well as upon his own personal knowledge of the fields of both states. It is to be regretted that certain data gathered by him and his assistants last fall are not available for publication. OIL IN TENNESSEE A few wells drilled for brine for salt making in Tennessee between 1820 and 1840 obtained oil, but no definite search was made for oil until just after the close of the Civil War. Active drilling was then begun in Overton and counties southwest of it on the eastern half of the Highland Rim. A number of strikes were made at shallow depths in the basal part of the Mississippian but the wells were soon exhausted and abandoned. Drilling was revived, about. 1892, when the Spurrier district in Pickett County was developed and was followed by the Riverton district in the same county in 1896. A pipe line was laid from the Wayne County, Ky., fields and about 60,000 bbl. of oil were run before a very heavy slump in the production, a failure to find an extension of the field, and excessive local taxation caused the removal of the pipe line in 1906. There was then no production in Tennessee until the discovery, in 1915, of oil near Oneida, Scott Co., at about 950 ft. (289 m.) in fissures in the Newman or St. Louis limestone. This field, however, soon failed and was abandoned. In 1916, oil was found at Glen Mary, Scott Co., in the Newman limestone at a depth of 1232 ft. (375 m.) A number of wells have since been drilled there, some of which were dry while others, close by, were producers. The largest one yielded, at first, about 340 bbl. per day and produced for several months, when it suddenly went dry. Several of the first wells began at 6 or 8 bbl. per day and are still maintaining that

Jan 1, 1920

By Edwin R. Phelps, Charles W. Porterfield

BACKGROUND OF SURFACE MINING Surface mining refers to the process of removing the material (over- burden) overlying a coal seam and exposing the coal so that it can be loaded out and conveyed by trucks or other methods to the preparation plant or other facility. Surface mining has not always been important in the coal industry. In the early 1900s, almost all of the coal mined in the United States was mined by underground methods. In 1900, about 192 Mt (212 million st) of bituminous coal mere mined and less than 1% was mined by surface methods. The development and use of larger equipment has allowed surface mining to gain prominence throughout the years. Table 1 shows the total production of coal by mining method in the United States for ten-pear periods since 1920 and indicates the growth of surface-mined coal production. Surface mining will undoubtedly continue to account for a large percentage of the coal production in the US for many years because: 1) The capacity of surface mining excavators has continued to increase. Today, mining companies are using shovels (see Fig. 1) which are able to move up to 137.6 m3 (180 cu pd) in each bite and draglines (see Fig. 2) which move up to 168.2 m3 (220 cu pd) in each bucketful. 2) Increasing tonnage from the thick western coal seams is being produced by surface mining methods. 3) Surface mining has normally had lower costs and a better safety record than underground mining. 4) Surface mining normally recovers a much higher percentage of the coal reserve than can recovered by underground mining. 5) Some coal measures call best be extracted by surface mining

Jan 1, 1981

By Chas. H. Behre, Arbiter. Nathaniel

Two outstanding factors characterize most undertakings in the mineral industries: (1) mineral deposits are not equally distributed over the earth but are localized by natural processes, and (2) the mineral industries are largely based upon wasting assets. Neither of these factors is invariably true, for a few mineral materials, such as water, are essentially world-wide and others are replaced periodically by processes not unlike crop production. Indeed, with some, such as the salts in the sea, the supply is cyclic in short or long periods, whereas others, like water, though locally or periodically in short supply, are essentially inexhaustible. But to the extent that most minerals are limited to certain areas and are "permanently" consumed, any industry founded upon them, by implication, demands great care in planning for the most effective extraction-the essence of wise and conservative expenditure. Several less unusual yet also truly fundamental factors in the economics of the mineral industry are those involving (1) the various kinds and properties of mineral materials, which influence their use; (2) their geo- logic and geographic availability; and (3) the techniques unique to their discovery, exploration, and utilization. This chapter is designed primarily as a brief background for later ones and as a summary of the several un- usual or at least special factors and of their effect upon the economics of the mineral industry. The social and political and especially the economic aspects of the industry are the main subjects of this volume and are dealt with in extended fashion in subsequent chapters. Fundamental Characteristics of Mineral Deposits DEFINITIONS Minerals are naturally occurring compounds of nonliving matter, each technically defined as having (1) a chemical composition that may vary

Jan 1, 1959

THE Copperton mill in reality was a sort of proving ground. It was. designed to serve three purposes: (1) to verify the accuracy of the mine sampling by actually treating substantial tonnages of ore, (2) to demonstrate on a reasonably large scale the percentage of the copper in the ore that could be recovered, and (3) to permit the testing of various kinds of machines and devices for crushing and concentrating the ore, so as to guide the engineers in designing the proposed 6000-ton milling plant at Garfield. As a matter of fact, it contained a lot of second-hand equipment sent by MacNeill and Penrose from the works of the United States Reduction &Refining Co. in Colorado; and it was by no means a model installation. Probably it would have been even less efficient, except for the skillful work of George O. Bradley and-Frank-G, Janney, both of whom had worked with Jackling at Mercur. Bradley was a mechanical engineer employed to design the plant. Later he directed the design of the concentrator at Garfield and remained as consulting mechanical engineer to the company until 1915. Janney, who afterwards became manager of mills, a position that he retained until his death in 1916, was a skilled mechanic at the Golden Gate mill at Mercur when Jackling built the plant in 1897. His flair was making machinery do what it was intended to do. He was not an ore-dressing engineer in a technical sense; but Jackling him- self was a specialist in this respect as well as in designing and construction and Janney's mechanical aptitude made him a particularly valuable man in the Utah organization. John McDonald, another of Jackling's Mercur associates, was the first mine superintendent. With practically all of the available funds earmarked for construction of the Copperton

Jan 1, 1933

By M. A. Mahtab, J. D. Dixon

The results of a parametric study of the influence of natural features (stress field, rock strength, and strength and orientation of fractures) as well as the influence of induced features (undercut span, boundary slot, and other boundary-weakening measures) on the cavability of an undercut block of ore in mining by the block- caving method are presented. The two-dimensional finite-element analysis technique was used for this study. A coarse "mesh," along with linear homogeneous assumptions for rock properties, was used to model the problem of initiation of caving in a block of ore. Interpretation of the test results suggests that weakening the "abutments" of the block as well as certain orientations of natural fractures exercise significant influence on cavability. These findings hold promise for immediate application to known situations in block-caving mines.

Jan 1, 1977

By F. R. Brotzen, L. D. Whitmire

Single crystals of high-purity molybdenum were de-formed at temperatures from 195°to 473°K, and the effect of deformation on the electrical resistivily was deler-mined. To separale the resislivity components of point and line defecls some cryslals were annealed at 473°K. The vale of resislivily increase wilh strain was nearly linear and was strongly dependent upon the deformation temperature. Point dejects are annealed out without any effect on the flow stress. At low temperatures the flow stress is a linear function of the square root of the resistivity increase attributable to dislocations. ELECTRICAL-resistivity measurements have been used successfully to gain information on structural changes in metallic materials. During plastic deformation the electrical resistivity rises because of electron scattering from newly created lattice defects. Such measurements lend themselves, therefore, to corroborating results from direct observation of lattice defects and, to a certain extent, to correlating defect densities and distribution with mechanical properties. Published information on research with single crystals of the bcc metals of Group VI, particularly molybdenum, is still limited. Yet, molybdenum single crystals of relatively high purity can be readily prepared by electron-beam-melting techniques. Furthermore, some valuable information on the defect structure of deformed crystals by direct observation is available. Lawley and Gaigher,1 for example, have examined dislocation configurations in deformed molybdenum crystals by means of transmission electron microscopy. Their results revealed that the dislocation density and distribution were strongly dependent upon the deformation temperature. These findings differed from those by Keh and weissmann,2 who found that the average dislocation density in polycrystalline iron deformed between 138° and 298°K depended only on the degree of strain and not on the deformation temperature. Martin3 and peiffer4 showed that point defects introduced in polycrystalline molybdenum by cold work can be eliminated by annealing at a relatively low tempera-ture. In view of their work it became apparent that resistivity measurements of suitably annealed crystals could disclose changes in their dislocation structure and contribute to the understanding of the work hardening of molybdenum crystals. EXPERIMENTAL PROCEDURE Crystals were grown by electron-beam zone melting5,6 of 0.062-in.-diam molybdenum rods (99.99 pct) supplied by General Electric Lamp and Wire Division, Dover, Ohio. The crystals, about 4 in. long, were prepared by using five zone-refining passes at a speed of about 6 mm per min in a vacuum of about 5 X l0-6 Torr. The resistivity ratio of the crystal, p(4.Z°K)/p(273°K), was generally near 10-3. These crystals were used as tensile specimens of uniform diameter in the "as-grown" condition. They were oriented for maximum shear on the (011)[111] slip system (Schmid factor >0.49). The specimens were held in spherically seated Templin-type grips so as to minimize bending. Samples were deformed on an Instron machine at a strain rate of about 5 X 10-5 sec-1 in an isopentane bath with dry ice at 195°K, in ice water at 273°K, and in a vegetable-oil thermostat at 373° and 473°K. The temperature in the latter was maintained constant within +2°K. Resistance measurements were carried out with a Kelvin double bridge. The resistance of the potential leads was kept low by using large-diameter wires outside the low-temperature bath. Many of the resistance data were checked by measurements made with an ac bridge. Current and potential leads were spot-welded to the specimens. The distance between the potential leads, about 3 in., was also considered to be the gage length for the strain measurements. Diameter and gage length of the samples were measured optically with an error of less than 2 pct. These measurements were used also to insure that the deformation had been uniform over the gage length of the specimen. Resistivity changes were then determined from the resistance measurements at 4.2°K assuming constancy of volume. In the course of a test, the crystal diameter, gage length, and resistance at 4.2°K were determined first in the initial state and subsequently for various amounts of elongation.

Jan 1, 1968

By K. K. Clark, W. H. Somerton

The feasibility of reducing pressures needed to fracture formations by heating the borehole intensively has been investigated on a laboratory scale. Reductions in fracture pressures of heated Bandera, Berea and Boise sandstone cores were observed at various confining pressures, simulating reservoir stress conditions to a depth of 5,000 ft. Both permeable and impermeable borehole boundary conditions were tested. Three heating conditions were used in the tests. One group of samples was heated in a furnace to a temperature of 600C, cooled to room temperature., and then tested for fracture pressures. Two other groups of samples were heated with a borehole heater to maximum borehole wall temperatures of 625 and 792C, then cooled and tested. In all cases, heated samples showed substantial reductions in fracture pressures compared to unheated samples. The higher temperature borehole heated samples showed the greatest reduction, amounting to 70 per cent in the extreme case. In actual application to wells, it was concluded that fracture pressures may be reduced by 20 to 50 per cent by intensive borehole heating before fracturing. INTRODUCTION Hydraulic fracturing of oil and gas wells is an accepted and effective technique for increasing well productivity in many areas, but is notoriously unsuccessful in other areas. The technique becomes less interesting for production stimulation purposes when excessive fracture pressures are necessary. Formations which do fracture but require high pressures, probably form horizontal fractures. There is good evidence to indicate that some formations do not fracture at all, but yield plastically under high pressure. Thus, any technique which will make formations easier to fracture or will reduce fracture pressures is potentially interesting to petroleum producers. Horizontal fractures generally occur in planes of weakness, such as bedding planes, and at pressures equaling or exceeding the effective overburden stress. In the unusual case where planes of weakness do not exist, a slightly higher pressure must be applied to overcome the tensile strength of the rock. In general, high fluid-loss fracturing fluids are conducive to the formation of horizontal fractures.1 Vertical fractures, when they do occur, are initiated at pressures generally lower than overburden pressure and are favored by low fluid-loss fracturing fluids or impermeable boreholes. The pressure necessary to create a vertical fracture in an impermeable, elastic medium can be predicted from the so-called "thick-walled cylinder" equation: Pf = 2 or+ st.............(1) where pf = fracture pressure or = radial stress st = tensile strength of medium. This equation indicates that to fracture it is necessary to overcome a tangential compressive stress, induced by and equal to two times the radial confining stress, plus the tensile strength of the medium. If the above equation held strictly true for rocks, very little could be done to reduce fracture pressure. The tensile strength of the rock might be reduced somewhat, but any change in st would be small compared to the magnitude of the tangential stress at reasonable subsurface depths. Laboratory tests have shown that actual fracture pressures exceed values predicted from Eq. 1 by factors of 1.4 to 28.6.1,2 Eq. 1 thus does not properly describe the

Jan 1, 1966

By M. R. Geer, H. F. Yancey

With the exception of pneumatic processes and a few special beneficiation methods of comparatively limited application, all mechanical coal-cleaning and mineral-dressing processes involve the admixture of solid particles with a liquid, generally water. Upon completion of the beneficia-tion process the solids must be reclaimed from the water. With coarse particles separation of solids from water is accomplished readily by the simple expedient of screening, but recovery of fine solids presents a much more difficult problem. Thickening and dewatering are practiced so generally, both within the mineral industry and elsewhere, that they have been the subject of study through the years and a number of processes for making the solid-liquid separation have been developed. Dorr-type thickeners have been standard equipment lor many years, and more recently driers employing centrifugal force have gained in popularity.' A cyclone device employed to thicken the loess suspension is a novel feature of the loess heavy-medium coal-cleaning process developed by the Netherlands State Mines in the thirties. The cyclone thickener was first mentioned by Driessen2 in 1939 in a paper describing the loess process and has been the subject of two more recent reports by the same author.3 The cyclone does not differ greatly from cyclone dust collectors used in this country for years, except that it is operated wet rather than dry. Advantages of the cyclone over other thickening devices are its simplicity of construction, high capacity, and the fact that, having no moving parts, it is simple and inexpensive to operate. The Bureau of Mines became interested in the cyclone after one of the present authors observed it in operation in the Netherlands in 1945. The first experimental work with the cyclone conducted by the Bureau of Mines was an investigation of the unit functioning as a heavy-medium cleaner for fine coal—a use for the cyclone that was conceived long after it had been perfected as a thickener. The results of this investigation were published last year.4 The present investigation deals exclusively with operation of the cyclone as a thickener. Object and Scope of Investigation Although the cyclone thickener has been dealt with in three reports by Driessen, its use as a thickener was not the principal subject of any of these reports and therefore neither the cyclone itself nor its operation was described completely. The design of the cyclone was described only in a very general way, only limited operating results were given, and virtually nothing was disclosed about the influence of the various possible operating variables. Moreover, the Netherlanders apparently had employed the cyclone exclusively for thickening loess and had not employed it On coal 'lurries. One English colliery has used a cyclone to thicken coal slurry,5 and as it appeared that

Jan 1, 1949

By Harold A. Linke

THE following article presents notes and data compiled and computed by the writer for use in the determination of: size and slope of mill launders, details of junction boxes and downspouts, and distribution of pulp. It also includes pulp formulas, volume of discharge through bushings, paths of discharging streams, banking of turns and curves. In the design of a concentrating mill, the draftsman usually considers launders to the extent of providing ample "head" for transmission of pulp from one department of the mill to another. The superintendent of construction aims to build his launders wide and deep, and on a slope steep enough to ensure positive flow. So launders are laid generally on too steep a slope, with the result that the repair gang works to maintain launder bottoms and sides against the erosive action of the conveyed pulp. To this end many kinds of liners have been devised: concrete, mastic, white iron, glass, rubber. True, the reduction of slope to the point where a pulp will flow with minimum wear, will minimize labor and expense; but when the desired slope is not predetermined, the millman hesitates to readjust his launder slopes by cut-and-try methods. To the end that the desired size and slope may be found readily, the writer has: (1) conducted experiments with pulps of different specific gravity, screen analysis and dilution; (2) gathered a few graphic data from standard reference works (such as Peele's Mining Engineer's Hand- book and Taggart's Handbook of Ore Dressing); (3) computed several tables; and compiled results that have proved dependable for Utah Copper ore. It is quite possible that the following tables and graphs may not be applicable to all ores, but it is hoped that they may prove helpful, even in slight degree, in alleviating a portion of the trouble and migraine of some other millman.

Jan 1, 1939

By Hiroshi Kato, Shin’ichi Nagashima, Hiroshi Takechi

The preferred orientations detleloped during cold rolling, annealing, and hot rolling of low-carbon steel sheets have been investigated by means of an inverse pole figure technique. And X-ray line profile meas-urerrlents were made for the study of the factor which causes the textural changes between cold-rolled and recrystallized sheets. From ND (sheet normal divection) and RD (rolling direction) inverse Pole figures tlze axis detisity change with increasing cold reduction was measured and the Preferred orientations were analyzed. These results can be explained by crystal rotation due to slip during rolling deformation. The ND axis density change during annealing of cold-rollitig sheets is contrary to the change observed in the case of rolling. It was found that the orientation dependency of stored strain energy resulting from cold rolling apparently corresponds to the textural changes during recrystallization. The texture in hot-rolled sheets was found to be influenced by finishing tenlperatltre. In a sheet kol-rolled below the Ar, temperature a significant differernce in texture between the surface and central layers was obtained, the former having {hkl}(111} and {110 )(uvw) orientations and the latter having {pqr}( 110) orientation. A large number of investigations1 6 have been made on the textures of iron and low-carbon steel sheets, and, since it was shown7 13 that preferred orientations are closely related to deep drawability of steel sheets, studies14" 7 on the influence of production processes upon textures have been made from the standpoint of industrial interest. Generally, the textures in low-carbon steel sheets have several components of preferred orientations, but the overlapping of poles makes it difficult to analyze texture quantitatively from pole figures. On the other hand, an inverse pole figure directly expresses quantitative values of components of preferred orientations as the density of a certain sample axis with respect to the crystallite coordinates. Such a texture representation is desirable for a study of deep drawability. The purpose of the present work is to use both inverse and conventional pole figures, with emphasis on the former, to clar~fy the textural changes ~n low-carbon steel sheets by the production processes of hot rolling, cold rolling, and annealing. And the factor causing the textural changes during annealing is studied using an X-ray diffraction line profile technique. EXPERIMENTAL PROCEDURE Sheet specimens for study of cold rolling and annealing textures were taken from a hot-rolled strip of rimmed steel 2.7 mm thick. The chemical composition is shown in Table I. Although the study of cold-rolling textures requires a suitable material with random orientation, it is difficult to produce a perfect random one. But the used specimens, obtained from the hot-rolled strip with a finishing temperature higher than Ar3, were nearly random, such as shown in Fig. 15. These were cold-rolled to various reductions by a 4-high rolling mill with 150-mm-diam work rolls and 300-mm-diam backup rolls. The influence of hot-rolling conditions such as finishing and coiling temperatures on textures of hot-rolled strips was studied. The chemical compositions of these hot coils are given in Table I1 and the hot-rolling conditions are given in Table 111. inverse Pole ~i~ure -~easurement. Two methods for determining inverse pole figures with high precision have been proposed. The first, by Jetter et a1.,18 consists of obtaining mean densities of divided regions in a unit stereographic triangle by solving simultaneous linear equations to approximate the integral relation between conventional and inverse pole figures. The second, proposed by ~oe'~-'~ and Bunge,22'23 consists of determining an expanded series of spherical surface harmonics which express axis densities from several sets of pole distribution data. Both methods require laborious numerical calculations which make them unsuitable for practical use. However, the axis densities of the locations corresponding to low Miller indices in a unit stereographic triangle can be obtained

Jan 1, 1969

By J. L. Lamon, W. Crafts

P. Coheur and L. Habraken—We read this paper with great interest and are glad to congratulate the authors for their valuable work, supplying an important contribution to the mechanism of tempering on the carbides in vanadium steels. We are in a good position to appreciate this work since we have been studying, for more than a year, Cr-Mo steels of a composition similar, but less highly alloyed (namely 0.1 pct C, 3 pct Cr, 1 pct Mo). Our results are quite in concordance with the authors', however, we wish to point out that it is very interesting to use equally the electron microscope in order to observe the variations of microstructure in steels. We have studied simultaneouslv the evolution of the carbides in situ with the electron microscope, and, after extraction, again with the electron microscope, and then with X-rays. The first results which we have obtained have been communicated at the Congress of Delft (July 1949) and at the "Journbes de la Metallurgie" in Paris (October 1949). These may be summarized as follows: After tempering with varying either the tempering temperatures or the tempering times, the carbides show two evolutions. The first one is connected to the carbides existing in the steels, principally in the boundaries of the grains. For some groups of steels these carbides may coalesce and for other groups they may

Jan 1, 1951

By R. A. Meussner, C. T. Fujii

Chromium solution in wustite depresses the oxygen activity in a nonideal manner and expands the lattice slightly. Gravimetric measurements of the equilibrium compositions of wustite containing 0.00 to 1.38 wt pct Cr define the oxygen potential (CO2-CO atm) and the limits of the phase field at 1000°C. These data extrapolate to a maximum solubility of 2 wt pct Cr. The lattice parameter data, room-temperature measurements of quenched samples, differ significantly from those in the literature. Both pure and chromium wus-tites contract at uniform and equal rates as the oxygen content (metal deficit) increases. The a. US metal deficit relationships are straight lines showing none of the curvature previously reported. At constant metal deficit, the a. expands by 0.002? on alloying with 0.4 to 0.5 wt pct Cr but is insensitive to further chromium additions: a small expansion rather than a marked contraction. These results require a modification of the accepted alloying mechanism. IN the high-temperature oxidation of Fe-Cr alloys in Ha-H,and CO2-CO atmospheres the vapor transfer of oxygen from the continuous wustite outer scale to the porous inner scale/alloy interface sustains the high oxidation rates.1"3 The driving force for this transport is the difference in the oxygen activity of the outer wustite and that at the inner scale/alloy interface. In pure CO2, as well as in CO2-CO atmospheres, carburization of the alloy accompanies this oxidation. Current efforts to evaluate the parameters controlling this carburization have shown that the process is not simple; i.e., the carbon concentration in the alloy initially increases rapidly, reaches a maximum, and then decreases slowly as the oxidation time is extended. This is the same pattern reported by McCoy for the more complex oxidation-carburization of stainless steels and an Fe-Cr alloy in CO2 at lower temperatures.4 These changes in the carburization process occur while the overall oxidation rate and the lattice parameters of the scale layers remain constant. If this invariance of the lattice parameter is assumed to indicate a constant scale composition and thus a constant oxygen potential, the carburization results are not easily explained. Electron microprobe traces across the thickness of these outer scales, however, have revealed distinct chromium gradients penetrating 10 to 50 µ from the inner surface where the chromium concentrations were estimated at a few tenths percent. The variation of the chromium cmcentration on the inner surface of the scale, and the resulting change of the oxygen activity, during the oxidation process is considered to be important in defining the carburization process. Thus, to gain an understanding of the complex oxidation-carburization proc- ess, it was necessary to measure the properties of wustite containing known amounts of chromium (chromium wustite). Although the general features of the Fe-Cr-0 equilibrium diagram between 900° and 1300°C have been fairly well established by Richards and white: Wood-house and White,6 Seybolt,7 and Katsura and Muan,8 there have been no detailed studies of the limits of the chromium wustite phase field or the properties of these alloyed wustites. The recent results of a limited study of chromium wustite by Levin and wagner9 indicate that more than 0.67 wt pct Cr is soluble in wustite above 850°C and that this alloying is accompanied by a substantial lattice contraction. This change in the lattice parameter was not evident in the X-ray diffraction patterns of wustite layers from the oxidation experiments;1,3 the lines were sharp even though a chromium gradient existed in the scale. The present paper describes gravimetric equilibrium experiments which delineate the boundaries of the chromium wustite single-phase field at 1000°C and define the changes in the oxygen activity and the lattice parameter of wustite as functions of chromium and oxygen contents. The lattice parameter data of chromium wustite obtained from these equilibrium and special quenching experiments differ considerably from those reported.9 Those for pure wustite show significant differences from the widely accepted data of Jette and Foote.10 Since the causes of these differences are not easily assignable, and since the literature contains many sets of data on wustite which if not in conflict are at best not in harmony, the experimental procedures are discussed in the present paper. EXPERIMENTAL Oxide Preparation. The specimens used in these studies were porous pellets compacted from high-purity (Fe,Cr)2O3 or Fe2O3 powders. These powders were prepared from electrolytic chromium (99.8 pct purity) and electrolytic iron purified by consumable-electrode, vacuum arc-melting processing (299.9 pct purity).11 The oxides were produced by standard analytical procedures: solution of the metals in acids (HC1, then HNO3 added), coprecipitation of the hydroxides (NHaOH), and filtering and washing these precipitates. Initial dehydration of the coprecipitated hydroxides was done in a porcelain evaporating dish heated by a Meker-type burner, final dehydration by firing in a recrystallized alumina crucible at 1000" to 1050°C for 20 hr in an electrically heated furnace. Spectrographic analysis detected the following impurities: silicon, 0.01 pct or less; aluminum, 0.001 pct to trace; manganese and copper, 0.0001 pct to none. Each of these levels is at least one order of magnitude lower than in commercially available CP grade ferric and chromic oxides. Fluorescence analy-

Jan 1, 1969

By R. P. Smith

The diffusivity of carbon in iron, cobalt, and alloys of 89.7 and 79.3 wt pct Co has been determined by a decarburization method for the temperature range 850° to 1100°C. The Plots of log D us 1/T for the two Fe-Co alloys are linear through the region of the Curie temperature, showing that, unlike some cases of substitutional diffusion, carbon diffusion in these alloys is not affected by electron spin order. RECENT investigations1-' have shown that for substitutional diffusion in iron the change in diffusivity with temperature does not follow an Arrhenius equation, at temperatures near the Curie temperature. Data on the diffusivity of carbon in a iron5"9 indicate that this anomaly does not exist for interstitial diffusion; however, this has not been definitely established. Since cobalt and Fe-Co alloys, 80 to 100 pct Co, have Curie temperatures in a temperature range convenient for carbon-diffusion measurements they are suitable systems for studying the relation of interstitial diffusion and the Curie temperature. EXPERIMENTAL The carbon diffusivity, D, was determined by a decarburization method. The diffusion cylinders, made from small vacuum melts of electrolytic cobalt and plastiron, were about 0.76 cm diam and 6.3 cm long. A small amount of carbon was added to each melt to keep the oxygen content as low as possible. The cylinders were first treated with a hydrogen-3 pct water vapor mixture at 1100°C to constant weight, then carburized to the desired initial carbon content with a suitable CO-C02 gas mix-

Jan 1, 1964

By K. E. Brown, J. P. Brill, T. C. Doerr

A wide range of intermittent gas-lift tests way conducted in a 1,500-ft experimental well through 11/4- and 11/2-in, nominal size tubing. The well was equipped with two gas-lift valves, four Maihak electronic pressure transmitters and surface facilities to measure casing and tubing pressures, temperature, liquid production and the rate and volume of gas injected. For each tubing size, tests were conducted varying the slug length, gas volume injected and liquid viscosity and surface tension. From these tests, an empirical "fallback" or liquid loss correlation has been developed. No general fallback correlation could be obtained, and the correlation is presented in the form of one curve for each slug length of a given liquid and lubing size. A conceptual model has been developed which combines the fallback correlation with equarions which govern liquid slug pow. A mathematical simulation of the model in the form of a digital computer program is used to calculate total recovery, gas volume used and clearance time for a given test. Tubing pressures at the gas-lift valve and at the gm-slug interface are calculated as a function of time. Tubing pressures at the surface during slug clearance ore also calculated. The results compare favorably with the test data and verify the conceptual model. The extent to which the model can be used for other tubing sizes, depths, liquids and gas-lift valves can only be determined with additional experimental data. Data are also necessary so that a fallback curve can be constructed for the particular test conditions studied. INTRODUCTION The flow of liquid slugs in vertical conduits has long been an established production method in the petroleum industry. Under the name "intermittent gas lift", many advances have been made in engineering design. However, the unsteady-state nature of liquid slug flow has discouraged attempts to describe the problem analytically. The result has been that intermittent gas lift is dominated by rules-of-thumb engineering practices developed over many years. The advent of slim-hole completions has increased the demand for a more rigorous solution to the intermittent problem. Small-diameter conduits offer more frictional per intermittent cycle. Small-diameter conduits are defined to be 1%-in. nominal size tubing or smaller. When oil is produced from the reservoir in which it is found, and transported to surface tanks by intermittent gas lift, three separate flow stages are encountered: flow of the fluids to the wellbore through a porous medium, vertical flow of a liquid slug from the point of gas injection to the surface, and horizontal flow of the liquid slug through the surface flowlines from the wellhead to the surface tanks. The three stages are depicted schematically in Fig. 1. The present study deals with liquid slug flow in both the vertical and horizontal conduits, ending when the bottom of the liquid slug reaches the surface. Due to the large number of variables involved, the analytical study of intermittent gas lift is extremely complex. The possibility of flow regimes other than slug type, the nature of the force fields acting on the system, the interfacial instabilities involved, the varying operational principles of existing gas-lift valves and the complete unsteady-state nature of the physical phenomena occurring in an intermittent gas-lift cycle relate some of the difficulties encountered.

By George W. Bain

Methods of mining building stone of any sort are planned to produce as few fractures as possible, and present a strong contrast to methods of mining metallic ores, which must be crushed eventually and have fractures produced in as great profusion as possible. Shocks transmitted to a stone invariably make it more porous and more permeable and reduce its effective life, therefore methods of mining building stone involve as This building illustrates the fine detail of workmanship, unprotected sharp corners and thin edges, and tall narrow columns characteristic of marble structures. These features require exceedingly coherent stone, and preservation of these features for decades or centuries demands many special quarrying precautions to keep absorption to 0.14 per cent or less, a detail not essential to stone for coarser architectural types. few shocks as possible. This is singularly true for marble because marble structures are intended to have long life, greater delicacy of line, more gracefulness and fineness of sculpture than those made from any other structural material (Fig. 1). So that delicate lines may remain in almost perfect preservation for decades, or even centuries, it is important

Jan 1, 1938

By George W. Bain

Methods of mining building stone of any sort are planned to produce as few fractures as possible, and present a strong contrast to methods of mining metallic ores, which must be crushed eventually and have fractures produced in as great profusion as possible. Shocks transmitted to a stone invariably make it more porous and more permeable and reduce its effective life, therefore methods of mining building stone involve as This building illustrates the fine detail of workmanship, unprotected sharp corners and thin edges, and tall narrow columns characteristic of marble structures. These features require exceedingly coherent stone, and preservation of these features for decades or centuries demands many special quarrying precautions to keep absorption to 0.14 per cent or less, a detail not essential to stone for coarser architectural types. few shocks as possible. This is singularly true for marble because marble structures are intended to have long life, greater delicacy of line, more gracefulness and fineness of sculpture than those made from any other structural material (Fig. 1). So that delicate lines may remain in almost perfect preservation for decades, or even centuries, it is important

Jan 1, 1938

By M. Cohen, R. T. Howard

It has long been realized among metallurgists that a fast, reliable method for the quantitative determination of the percentage of microconstituents in an alloy would be of great benefit in studies of equilibrium and transformation in the solid state. For example, Polushkinl has shown that the compositions of two coexisting phases in a binary system at a given temperature may be calculated very simply with the aid of two alloys lying in the two-phase field if the relative amounts of the two phases in each alloy can be determined. Recently, Grange and Stewart2 have traced the course of the austenite-martensite reaction in a series of commercial steels by making visual estimates of the percentage of martensite formed as a function of cooling temperature. The correlation of mechanical properties with structure, a subject of wide-spread current interest, is likewise dependent upon quantitative microanaly-sis. Yet, there are very few investigations described in the metallurgical literature, wherein methods of quantitative microscopy are employed. Usually, the relative amounts of the microconstituents are estimated in a qualitative or semiquantita-tive way. The authors were faced with this problem some time ago in studying the kinetics of austenite decomposition. Several aspects of this research could not be treated satisfactorily by other quantitative tools, such as specific volume,' magnetic,6 dila-tometric, electrical resistance7 or x-ray measurements.a It became necessary to find an impersonal quantitative method that could be applied to microstructures. Fortunately, it was noted that geologists and petrographers had coped with quantitative microscopy to a considerable degree in their attempts to evaluate the mineral contents of rocks. A number of excellent articles were found on this subject, and since they appear to be unknown generally to many metallurgists, the first part of the present paper is concerned with a review of the literature in some detail. With this survey as a background, the authors have adapted the so-called methods of point-counting and lineal analysis to metallography, as described in the second part of the paper. Austenite-martensite structures were selected for illustration not only because they are important in many ways, but because such fine intermixtures are notoriously difficult to estimate visually. Literature Survey Perhaps the earliest work on quantitative microscopic analysis goes back to Delesse9 (1848) who proved mathemati-

Jan 1, 1948