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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 Henry Lewelling

An experimental investigation of the relative effectiveness of standard bullets and "shaped charges" in perforating dense, hard formations is reported. A method is described which simulates the conditions under which a shot is normally fired. Results are evaluated on the basis of depth of penetration, extent 01 Fracturing. extent and nature of formation damage, and other physical characteristics. INTRODUCTION A study was made of the relative merits of bullets and "shaped charges'' as applied to well completions in hard, dense formations such as those encountered in the Permian Basin. The planning of the laboratory program stipulated that core samples should be prepared and mounted in such a way that perforation shots of either kind"" could be fired into them, keeping the factors pertinent to good shooting practice similar to what they would be in a well. The shooting was done in a buried tank. with the sample and shooting equipment covered with water. The depth of water was calculated to he sufficient to simulate the inertial effects of well fluids for the duration of an explosion (a few micro-seconds). Flow measurements were attempted on the specimens after perforation. Due to the lack of uniformity of the limestone, shale breaks. etc., these measurements proved to be of little value to the study. The mounting materials were removed. so that the character of the penetration. fracturing, etc., could be observed. METHOD Laboratory samples were selected from the hard. dolomitic sand cores from Block 31 Field. Core pieces having a 3 3/4 in. diameter and a useful length of 10 to 12 in. were used. Selection was aimed at those pieces having a minimum of shale streaks and other irregularities. The ends were cut off square Manuscript received in the Petroleum Branch office June 28, 1951. Paper presented at the Petroleum Branch Fall Meeting in Oklahoma City, Okla., Oct. 3-5, 1951. with the diamond saw. Prior to lbeing mounted. the cores were soaked in water to prevent them from absorbing water out of the wet concrete, thus weakening it. A set of steel capsules was fabricated for holding the core Samples. Seven-in. casing was cut in two-ft lengths. of which one end was closed by "orange-peeling" and welding, and the other was threaded to accept a standard bull plug. The bull plugs were fitted with copper tube connections .so that pressure could be applied when the capsules were made up. The cores were mounted in the capsules by means of wire centralizers whose function was to hold the Core in proper position while concrete was poured and set. A special aggregate was prepared wing a graded sand and gravel mixture

Jan 1, 1952

By Charles E. Mann, Douglas J. Lootens, Rufino B. Bomasang

INTRODUCTION The economy of the Philippines, like that of many other developing nations, has been severely strained by the rapid escalation of imported crude oil prices over the past decade. In an effort to reduce its dependence on imported crude, significantly increased emphasis, both in the public and private sectors, is being placed on the rapid development of Philippine coal resources. This paper is designed to present an overview of the Philippine coal industry, its historical development, present status, and future potential. COAL RESOURCES AND RESERVES In 1977, a British consulting firm collated all available data on Philippine coal resources and estimated the total coals potential at about 0.9 to 1.4 billion metric tons (mt). In 1981, using more recent data the Philippine Bureau of Energy Development (BED) estimated the potential at 1.7 billion mt. The BED estimated the proven coal reserves at 257 million mt. These coal resources are scattered throughout the major islands comprising the Philippine archipelago. However, about 52 percent of the currently proven reserves are located in the tiny island of Semirara between the islands of Mindoro and Panay. About 25 percent is located in the Cagayan Valley in northeastern Luzon while 13 percent is located in Mindanao. The remaining 10 percent is scattered in the islands of Cebu, Samar, Mindoro, Negros, Polillo, Batan, and Catanduanes. The bulk of Philippine coal is sub-bituminous in rank. Some bituminous coal with coking properties has been reported in Malangas, Zamboanga del Sur in western Mindanao, and in Catanduanes, but the exact tonnages have not been accurately established. It is believed, however, to be at most 5 million tons. A little semi-anthracite coal exists in Malangas with the remaining unmined reserves estimated at a little more than one million tons. Table 1 shows the quality ranges of Philippine coal deposits.. Figure 1 shows the distribution of known Philippine coal resources PHILIPPINE COAL PRODUCTION In 1981, total coal production was 330,720 mt. Though modest by world standards, this was the highest production figure in Philippine coal mining history. This came from 25 mines, mainly small scale underground mines of capacities varying from 10 to 100 tons per day (tpd). The actual production capability was about 800,000 mt in 1981, but the producers had to scale down production to the level of local demand. Even then, some 50,000 tons of coal remained unused by year-end. The 1981 production came from the following areas: Cebu 224,751 mt (68%) Zamboanga del Sur 57,095 mt (17%) Semirara 13,222 mt (4%) Polillo 17,132 mt (5%) Cebu has always been the main source of Philippine coal production. Coal mining has been carried out in Cebu for the last 50 years, although it has been characterized by a very crude mining technology. Due to the limited size of coal deposits and complicated geology, however, Cebu's share of the total national production is expected to go down to only 10 percent by 1985. Except for Semirara's open-pit production, the balance of Philippine coal production comes from underground mines. These underground mines generally use room-and-pillar methods, except for those at Zamboanga del Sur and Polillo which use modified longwall methods patterned after those used in Taiwan. Due to the much higher mining recovery, most underground mines are now planning on switching to longwall. At Semirara, an open pit mine is now being developed for a one million ton per year capacity by 1984, and will then be the largest Philippine coal mine. While present earthmoving work is done with bulldozers, loaders, and trucks, the main coal extraction equipment will be bucket wheel excavators imported from Austria. PRESENT COAL UTILIZATION Existing coal production is sold mainly to coal- fired cement plants and power plants. The balance is sold to a sugar central, a coconut oil mill, a food processing plant, and two plants producing carbide and ferro-silicon alloys.

Jan 1, 1982

By Walter Kauzmann

All viscous or plastic flow of incompressible matter is the result of shear strain; the changing shape of any body that is being plastically deformed can be completely described in terms of the shear strain occurring at each point in the body.† Furthermore, the relative amounts of shear strain occurring in different parts of a body under stress depend upon the relative rates of shear strain at those different points, so that if the dependence of the shear rate of any material on the temperature, shear stress, previous history, etc., were understood, the principles of plastic deformation would be known, and we could calculate how a body made of a given material, having a given shape, and subject to a specified system of forces, would change its shape with time. It may be said, then, that the problem of plasticity resolves itself into, first, the problem of the rates of pure shear processes, and second, the application of what is known about pure shear to actual cases. It is the purpose of this work to investigate the former problem —i.e., the dependence of shear rates on temperature, stress, etc.—from the standpoint of .recent developments in the field of chemical-rate theory and with particular reference to the phenomena occurring in the creep of metals and in the plastic flow of crystalline solids in general. It is left for the mechanical engineer, and perhaps the expert in hydrodynamics, to deal with the problem of app1ications.l Resolution of Macroscopic Shear into Microscopic Movements; Resemblance to Chemical Reactions Just as any large body is made up of many small units, or atoms, so macro-scopically observable shear is the result of many microscopic unit shear processes; just as the understanding of the behavior of large bodies demands the understanding of the atoms of which it is made, so the understanding of macroscopic shear demands the understanding of these fundamental unit processes. The study of shear from this "atomistic" point of view has made considerable progress. There has been fairly complete understanding of shear processes in gases for a long time, at least for non-turbulent flow, as a chapter on gaseous viscosity in any text on the kinetic theory of gases will prove' In recent years Andrade2 and Eyring3 have presented important theories for the flow of liquids and amorphous solids. Becker14 Orowan,5 Taylor,6 Burgers,7 and Kanter8 have considered the plastic flow of crystalline solids from this

Jan 1, 1941

By Harry H. Angst, Reuel A. Cochrane

THE successful exploitation by opencut methods of the low-grade porphyry copper deposits is due to the economical handling of large tonnages. Large tonnages are possible only if the rock material is broken so that the large power shovels can operate with minimum delays. This is particularly true at the New Cornelia mine, where the dense, hard, tough rock material creates problems not encountered in most of the porphyry copper mines. The introduction of churn drills at the New Cornelia for primary drilling, in 1936, necessitated a complete change in the methods of breaking ground as formerly air drills had been used. The blasting operations are of particular interest because of the handling of great quantities of high explosives in safely and efficiently fragmenting the hard rock material. ROCK FORMATIONS At the New Cornelia mine the rocks are quartz monzonite with a diorite border facies intruding a rhyolitic series. Overlying these formations is a fanglomerate formation composed of boulders of monzonite, diorite, rhyolite, and other types of rock of unknown derivation. (The word "fanglomerate" is used in this paper in referring to the local conglomerate type of rock formations.) The ore body is approximately 4800 ft. long and 2800 ft. wide, and is of the disseminated type. Mineralization occurs principally the quartz monzonite and to some extent in the adjacent diorite and rhyolite. The principal ore minerals are chalcopyrite, bornite, and a small amount of chalcocite. Over a considerable area the quartz monzonite is extremely hard and siliceous in character, owing to pegmatitic zones of alteration. The hardness of the ground depends on the intensity of the silicification. In a small area in-the pit, the monzonite contains an abundance of pyrite accompanied by sericitization and is soft and easily fragmented. This is true also in the remaining oxidized portion of the ore body. The diorite and rhyolite formations, like the monzonite, vary from extremely hard to very soft material, but on the whole are easier to fragment than the monzonite. jointing is prevalent in all the rock formations and plays an important role in the blasting efficiencies. In the fanglomerate formation, numerous well-defined joints, widely spaced, tend to make the ground blocky when blasted. This is a deterrent to good fragmentation. In the other rocks the joints are more numerous and are closely spaced, except in localized areas where the formations are extremely hard. These descriptions indicate that the lowest blasting efficiency will be obtained in the harder formations, from which the major portion of the mine production is obtained; namely, the monzonite and rhyolite. All rock formations mined at the New Cornelia pit are so hard that excavation

Jan 1, 1941

By S. F. Shaw

In 1913, the Tiro General mine, at Charcas, S.L.P., Mexico, which had been making from 125 to 150 gal. of water per min., was allowed to become flooded, after all the pumps had been removed, and in 1918 the problem of unwatering it came up for solution. There are two vertical shafts, the Tiro General, 1390 ft., and the San Fernando, 1225 ft. in depth, with five connecting levels between them. The San Fernando shaft had been partly retimbered, while the Tiro General had been newly timbered from the collar to 1090 ft. in depth. It had been possible to place guides in only one compartment of the Tiro General, from the collar to the seventh or 850-ft. level, to which it was necessary to lower the water before station pumps could be installed. Soundings indicated that compartments in the Tiro General were open to 1082 and 428 ft., and in the San Fernando shaft to 471, 488, and 586 ft. The water had risen to a point 140 ft. below the collar of the Tiro General shaft.. Pumping Equipment The steam plant at the Tiro General shaft includes one 300-hp., one 150-hp. and one 100-hp. Erie City water-tube boiler, and two 160-hp. Heine water-tube boilers. All but one of these boilers were supposed to be in good shape, but it was soon discovered that six years of idleness in a climate that is foggy for several months of the year had left them in poor condition. The compressed-air plant comprises one Nordberg cross-compound compressor with piston displacement of approximately 2500 cu. ft.of free air compressed to 96 Ib. per sq. in.; and another Nordberg cross-compound with piston displacement of 1235 cu. ft. of free air, to the same pressure. The main pump station is on the seventh level where had been installed a Prescott pot-valve plunger pump with capacity of 200 gal. per min.; also a Gould triplex plunger pump with capacity of 135 gal. per min., driven by a 6 1/2 by 10 by 12 in. steam engine. From the lower levels, the water had been raised to the seventh level by small station pumps and sinking pumps.

Jan 1, 1920

By P. Hazebroek, C. S. Mathews, E. E. Allen, H. C. Lefkovits

A rigorous study was made of the behavior of reservoirs composed of horizontal layers, unconnected except at the well and filled with a compressible fluid. The report is presented in two parts. Part I deals with the practical implications of the results obtained; Part 11 contains the mathematical derivation of the solution. The main portion of Part I is concerned with application of the results to reservoirs composed of two layers. Relative rates of depletion of the layers are studied, and it is shown that differential depletion between layers exists in the transient stage of the reservoir, which generally is of an order of magnitude longer than the transient stage in a single-layer reservoir. In the transient stage, the more permeable layer is depleted faster than the less permeable. However, the reservoir approaches a steady-state situation where both layers contribute equally to production. Theoretical build-up curves from such reservoirs are presented, and the influence of a skin effect and flow into casing and tubing are also evaluated. The build-up curves are predicted to have, first, the familiar logarithmic straight-line section and, subsequently, a rising and flattened section. The results found are compared with an extension of an approximate theory, and it is found that this simplified theory is applicable over most of the life of the reservoir. Extensions to reservoirs containing more than two layers are indicated, and examples of the performance and build-up curves for three-layered reservoirs are presented. The theoretical results on build-up curves were applied to field examples of such reservoirs, and satisfactory results were obtained. From the build-up curve, the pemeability-thickness product, the wellbore damage and the static pressure are obtained. However, it apparently is not possible to determine the properties of the individual layers from the combined build-up curve. A large number of reservoirs have been found where the producing formation is composed of two or more layers of differing physical characteristics, such as permeability and porosity, and where also the thicknesses of the layers differ. Since in general a differential depletion should exist between the layers of such reservoirs, it would be advantageous to know the amount of the differential depletion under a given production history. It also would be valuable to know the pressure behavior, because it could be undesirable to produce a reservoir in such a manner that the pressure in one of the layers would have fallen below the bubble point of the oil at a time when another layer might still be virtually undepleted. The determination of static pressures in shut-in wells with slow build-up is another feature of importance in layered reservoirs. If the behavior of the reservoir differs appreciably from the predicted behavior of a single-layer reservoir, the type of analysis for build-up curves suggested for single-layer reservoirs is not applicable. Several authors have treated the problem of finding the pressure and production characteristics of multilayer reservoirs. Horner treated the problem of n layers in an infinite field, the layers being connected only at the well. Tempelaar-Lietz2 has presented an approximate treatment of the characteristics of a bounded reservoir composed of two layers of different permeabilities and equal thicknesses. Homer gave no information on differential depletion between layers, and the treatment of Tempelaar-Lietz was not applicable for prediction of pressure build-up behavior. In addition, it was thought that a more rigorous treatment than the one by Tempelaar-Lietz would be valuable in determining the range of validity of this solution. The present study, therefore, was made of a bounded reservoir composed of two or more layers,

By S. Le Fevre

The application of electricity to the mining and beneficiation of the magnetic iron ores of the Mineville, N. Y., district, on Lake Champlain, has resulted,in economies and enhanced quality of product, without which only a comparatively small quantity of the present output could be marketed. The output of the Witherbee, Sherman & Co. mines is about 700,000 tons per annum, and of this about four-fifths is treated by magnetic separation to increase the iron content and reduce the phosphorus. The use of electricity for the magnetic separation of the ore from the gangue is therefore of primary importance, and makes possible the application of electric power for mining and preparing the ore for concentration. The fact which speaks loudest in favor of the application of electricity is this: It is possible for about 25c. per ton of shipping ore to furnish all the power required to put the ore on cars. This includes mining a hard ore underground, from a depth of 900 ft., hoisting to surface, crushing to $ or 8 in. in size, and separating from the gangue. This also includes lights about the works, and all miscellaneous power, such as about the shops. The first plant for the generation of electric power for use at Mineville was completed in 1903, and was one of the first for the application of electricity to mining iron ore. This was a Nordberg compound condensing steam engine, direct connected to a 750-kw. alternating-current generator, 3,300 volts, 3 phase, 25 cycles. All the plants added later use the same current but with higher voltage. The map, Fig. 1, shows the power plants and the transmission system; Figs. 2 and 3 are views of the shaft houses and the mills. The power from the first plant was distributed to Mills 1 and 2, one 2,500 cu. ft. compressor, and to the Harmony hoist, which was driven by a 300-h.p. motor operating four 10-ft. drums. Our experience with the hoist covers largely the development of electric hoisting from 1903 to date, and in some cases improvements were worked out to satisfy our needs. The motor is still operating as installed, but the control apparatus has been radically changed several times. When installed, the iron re-

Jan 1, 1915

By R. L. Loofbourow

Trends in the metal mining industry were definitely down in 1954. With a record in 1953 of $1.8 billion output, the last year dropped to $1.5 billion, the lowest value since 1950. The decrease in iron ore production alone accounted for at least 10 pct of the decline. PROBABLY more than any previous year, political debates of 1954 marked a new high for the mining industry. Lead and zinc prices gave forth with minor rallies producing no real improvements. An anticipated drop in copper prices never came to be. Early in the year arguments for more free trade versus tariffs to restrict imports were voiced eloquently by Charles P. Taft, president, Committee for a National Trade Policy, and Andrew Fletcher, president, St. Joseph Lead Co.

Jan 3, 1955

By C. F. Cockrell, H. E. Shafer, J. W. Leonard

A significant technological development is discussed for the processing of certain power plant flyashes that are a problem because they contain a high water-soluble mineral content and yield inferior flyash-based brick. This development is based on the addition of hydrochloric acid to the flyash-bottom ash-sodium silicate blends used for the production of flyash-based structures. Favorable changes are evi-dent in sodium silicate consumption, where about half the amount used for making brick from normal flyash is required, processing costs, and strength and appearance of the resulting freshly formed green and fired structural products. In some high cost in-stances (above the $30 or less per thousand brick estimated for normal flyash), hydrochloric acid additions can replace or reduce other costly additives normally required for problem flyashes. This results in savings of as much as $9 per thousand brick. These developments offer promising possibilities for utilizing problem flyashes as well as flyashes which may come into contact with water soluble sulfur as a result of the eventual application of certain experimental air pollution control processes. Much of the research datal-6 accrued through work by the Coal Research Bureau of West Virginia University for the Department of Interior's Office of Coal Research on converting waste power coal ash to valuable brick and other structural products, can be categorized as follows: (1) general ash-to-brick tech- nology; (2) specific ash-to-brick optimization; (3) pilot plant progress; (4) production cost estimates. A summary of the progress on bench-scale experiments indicates that coal ash can yield two types of brick. An acceptable brick is obtained by mixing 73.6% fly-ash, 23.5% bottom ash and 2.9% sodium silicate solution (dry basis). Depending on the flyash and bottom ash used, optimum brick can be manufactured by mixing 72-77% flyash, 20-25% bottom ash and 2.3-3.0% sodium silicate (dry basis) with Na2O : SiO2 ratio varied according to the composition of the flyash used. These blends are thoroughly mixed and mechanically formed into green brick shapes at pressures ranging from 1000 to the more usual 3000 lb per sq in. The green shapes then are dried and fired at temperatures ranging from 1975-2150°F using clay brick cycles that are shorter than standard. Other findings reported to date indicate that when making optimum brick, it is necessary to carefully control the top size of the moisture-releasing bottom ash so that it falls between 8 and 30 mesh, depending on the flyash used. Moreover, the chemical composition of bottom ash and flyash have been found to be of little significance with the exception of a few problem flyashes which are the subject of this paper. Finally, the pilot plant, which was previously reported under construction, is now in operation. This will indicate, among other things, the cost of brick production, which was earlier estimated for non-problem flyashes at $30 or less per thousand brick. The foregoing bench-scale technology is applicable to all the initially tested ashes as well as to the majority of ashes examined during the course of research. However, a few of the ashes yield green and fired products that may be structurally inferior or unacceptable, necessitating excessive and diverse reagent addition, and/or may be coated with unsightly surface deposits. These problem ashes generally originate in certain areas of Illinois, western Ken-

Jan 1, 1969

By S. K. Tarby, W. O. Philbrook

Limited experimental data and a critical review of the literature are given to indicate that the true equilibrium distribution of manganese between carbon-saturated iron and blast-furnace type slags has not yet been satisfactorily established as a function of the composition, temperature, and pressure of the system. THE distribution of manganese between carbon-saturated iron and blast-furnace type slags has been studied by a number of investigators.1-7 Generalization of the results of these works indicates that the weight percent distribution ratio, (%Mno)/[%Mn], decreases with increasing temperature and slag basicity, in accord with thermodynamic data and practical observation. However, where comparisons among these studies can be made for similar slag compositions and temperatures, the reported values of the manganese distribution ratio are discordant. The variations are attributed to failure of the experimenters to bring their systems completely to equilibrium with graphite and CO at 1 atm, as judged by departures from silicon equilibrium. Even in the most recent work,5-7 this problem was recognized but the authors made the questionable assumption that equilibrium could prevail for manganese distribution even though other reactions were still in progress. Manganese equilibrium values for three particular slag compositions were required incidental to a kinetic study8 and were determined experimentally. Special pains were taken to approach concurrent equilibrium with respect to silicon. Although the results were not completely definitive, they indicate that the true manganese equilibrium distribution ratios are lower than have heretofore been reported. The data are presented together with a brief commentary on the literature to suggest the need for further work in this area. EXPERIMENTAL METHOD Equilibrium runs were carried out in a stationary, induction-heated graphite crucible closed by a graphite lid and flushed continuously by a slow flow of carbon monoxide at 1 atm pressure. Temperature was controlled manually within ±3 deg C with the aid of immersed thermocouples in mullite tubes protected against slag attack by graphite sleeves. The desired temperature was established by a calibrated Pt vs Pt-10 pct Rh thermocouple and control was then maintained using a more stable W-Mo couple. Runs were made at 1500º and 1575ºC for durations of 7.5 to 10.5 hr. The charges were calculated to yield 400 g of metal and 100 g of slag. The primary slag compositions and designation numbers were as follows:

Jan 1, 1963

By G. Derge, W. Peifer, J. H. Richards

A WIDE Variety of metallurgical defects in steel have commonly been attributed to the presence of excessive amounts of hydrogen. These defects include flakes in rails and forgings, cracks in welds, and blisters in enameled ware, They have been related to hydrogen largely by circumstantiat evidence because the proper sampling and analysis of steel for hydrogen has been known to be difficult and because no general agreement has existed with regard to the relative suitability and accuracy of available methods. The need for a direct approach to these problems has been widely recognized. This general situation has been well described in the publications of the British committee on the Heterogeneity of Steel Ingots,' and current approaches to the problem were reviewed in a recent symposium of the AIME.I2 The plans described by the present authors at that meeting have now matured satisfactorily and will form the basis of this paper. The principal object of this paper will be to describe the methods of sampling and analysis which have been developed and to illustrate the usefulness and limitations of these methods by citing their application to a specific problem, The first problem selected for investigation was the behavior of hydrogen in rail steel. This was chosen because the occurrence of shatter cracks in rails has received a great deal of study over a long period of time. The defect can be controlled by the expensive procedure of slow in However, it may be hoped that a better understanding of the factors influencing the hydrogen content of rails will lead to a more efficient control of this problem. Rails provide a good starting point for a more general study of hydrogen in steel because they provide a cross-section large enough to develop cracks, Yet small enough for convenient handling and sampling. Rails were also selected because they arc made from plain carbon steel and it was felt that the initial work should not be complicated by the effects introduced by alloying elements. The considerations which determined the original planning of this study should be reviewed. The inherently complex nature of most hydrogen problems requires that a large amount of data must be collected for any particular case. This in turn means that any analytical procedure should be as rapid and simple as possible. The same objective of speed is indicated by the fact that it may finally become desirable to use hydrogen analysis in process control. It is also known that hydrogen is highly fugitive and that any procedure which facilitat~s early analysis of the sample without prolonged or irregular storage has distinct advantages. The most important previously reported methods of analysis may be classified into three general groups: (I) Vacuum fusion, (2) Vacuum extraction (without melting), (3) Total combustion.

Jan 1, 1949

By T. B. Counselman

PROBABLY the earliest concentration of iron ore in this country was carried on in the northeastern magnetite areas. Magnetic concentration was relatively simple and gave a concentrate that, after agglomeration, and in spite of being high in phosphorus because of the dry concentrating methods then in use, was satisfactory blast-furnace feed. Production from the northeastern magnetite area languished after the discovery and development of the Lake Superior ores, where there was seemingly an unlimited tonnage of high-grade ore, first the Michigan ores, and subsequently the still larger deposits of Minnesota. For years only the higher grade, direct shipping ores of the Lake Superior district were mined. Those of Michigan, and of the Vermilion Range in Minnesota, were hard ores and came principally from underground mines. The softer ores of the Mesabi came partly from underground mines, but mostly from the enormous deposits that could be worked by open-pit methods. The costs of ore from these open-pit deposits, even with the high initial cost of stripping, were so low that the underground mines of the Mesabi could hardly compete. The so-called Old Range ores, of Michigan and of the Vermilion Range of Minnesota, were hard and lumpy, and opened up the burden in the blast furnace, therefore making possible harder driving with greater output. Also, some of these ores were of such grade and physical characteristics that they were suitable for charge ore in the open hearth. These ores, therefore, commanded a price premium, and could compete with the softer, finer, but cheaper, Mesabi ores. The big tonnage reserves, however, are on the Mesabi, and it is these big open-pit deposits that constitute our stock pile of iron ore, from which we are drawing so heavily during this war period. On the western end of the Mesabi the ore was found to be high in silica, and not suitable as furnace feed. As early as 1902, attempts were made to concentrate this so-called wash ore and by 1910 the first washing plant was put into operation. The process was very simple, consisting essentially of a sizing and washing operation, with scalping screens, logwashers, and tables, which later were replaced by classifiers. Ore particles finer than 100 mesh were deliberately wasted, because these fines were undesirable in the furnace. Fortunately, these tailings were impounded, and already are being reworked. Before long some of the low-grade ores began to require more elaborate treatment than the simple washing operation and, tables having been discarded because of their low capacity, in favor of classifiers, jigs were next introduced. These were able to discard coarser pieces of tailing than classifiers. Jigs are in active use today, various improvements having been made in their design and application. Various other machines and methods of concentration have been tried from time to time, and have in turn been discarded for more improved processes. The latest and most important process that has been

Jan 1, 1943

J. M. Wadsworth,' Okmulgee, Okla. (written discussion).—It seems to me that thc young man must first be absolutely sure that the work he has taken up is to his liking and then I would advise that he get into the practical end of it and learn as much about it as he can as fast as he can. For instance, in the refinery business the college man, graduated in chemical engineering, should ground himself by going through the various departments in a refinery and working in them until he is thoroughly familiar with the operating problems. In a short time he would be able to apply many things which appear in the abstract form in his college work and this would opcn up an opportunity for him to capitalize on them, promoting his own interest. I do not criticize the present-day college men as a class, but I have found that many of them come into your plant with the idea that mere possession of a diploma should insure rapid promotion; in a short time they are impatient and usually leave. We have found in employing men that the single attribute most difficult to find in them is a lot of energy and whole-hearted interest in the work at hand, and it seems to me that if a man combines these with a careful technical training he should be fairly well equipped to gamble on his future. They must learn that the biggest satisfaction to be gained in life is in their work. Procedure for Attaining Objective of Young Petroleum Engineer H. B. Fell,+ Ardmore, Okla. (written discussion).—Of course, the first thing to be ronsidered in any proposition is the ultimate objective that is desired to be attained. 1 presume that the desired objective of most of the young men graduating in petroleum engineering will be that of chief executive of one of the companies in the petroleum industry, or one of the allied industries, or to become an independent oil producer, or oil refiner, or possibly an oil distributor. The next phase then to be considered is the procedure which should most logically be followed to attain the objeckive of the indivitlual, since in these cases these young men will have been trained in a course in petroleum engineering and it would logically be presumed that the attainment of their objective should be through the operating end of the branch of the business with which they are connected. The operating end is, of course, the department of each branch of the business that develops the resources, or refines the products, or distributes the products, from which the profits are derived, and is a part of any business which is filled with enough interesting work to appease the desires of the most ambitious young men. In order to get the best possible training it would appear to me that the place for a young man to start after graduation would be at the bottom of that branch of the industry which he expects to follow. For example, if he is going in the producing end he can gct no better training than is secured by starting as a roustabout in the ficltl, where he romes in constant rontact with the character of work that is necessary

Jan 1, 1928

By B. H. Kear, S. M. Copley

A dynamic theory of precipitation hardening in alloys containing cohevenl, stvess-.free, ordered particles is developed. The yield stvess is predicted from the stress dependence of the plastic strain vale, which is related to a derived dislocation velocity-stress function. The theory is shown to predict the magnilude and temperature dependence of the yield stress of a commercial nickel-base superalloy as well as many details of its slip structure. GLEITER and Hornbogen have developed a theory of the yield stress in alloys hardened by coherent, stress-free ordered ptrticles based on the observation that dislocations (b = a/2 (110)) glide in pairs.' When a dislocation pair shears through an ordered particle, the glide motion of the leading dislocation is impeded since it must create antiphase boundary (APB), whereas the motion of the trailing dislocation is assisted because it annihilates APB produced by the first one. Taking into account the APB energy, the size, and spacing of the particles, G-H predict the observed yielding behavior in Ni/18.8 Cr/6.2 A1 alloys composed of a matrix phase y '(nickel-solid solution) and particles of y' (basically Ni3A1). The G-H theory, as well as all previous theories of hardening by coherent ordered particles, do not include the details of dislocation motion; the present dynamic theory is an attempt to overcome this limitation. In the dynamic theory, the yield stress is predicted from the stress dependence of the plastic strain rate, which is related to a derived dislocation velocity-stress function. This function can be evaluated if the structure of the alloy, the APB energy of the ordered phase, and the characteristic drag or frictional stresses of the matrix and precipitate phases are known. The theory is shown to account for the observed temperature dependence of the yield stress in a commercial nickel-base superalloy. 1) NICKEL-BASE SUPERALLOYS Although their compositions are complex, the nickel-base superalloys have remarkably simple structures. A detailed examination of the commercial superalloy

Jan 1, 1968

By C. W. Spencer, F. G. Hochgraf, R. F. Cheney

Columnar grained specimens of nickel, containing 0.25 pct Si and 0.22 pct Mn, have been exposed to liquid bismuth in the temperature range 670° to 1050°C. Under isothermal conditions the liquid penetration rate is constant. The activation energy for the process is 22,000 cal per g-atom. Small amounts of plastic deformation, introduced into specimens prior to exposure, increase the penetration rate. The slou. step in liquid film penetration is associated with a reaction which occurs at or near the leading edge of the film. Either transfer of nickel across the liquid-solid inteqace or diffusion in the grain boundary ahead of the liquid film is suggested. Aliquid metal, if brought into contact with the surface of an unstrained solid metal, will usually penetrate to some extent into the grain boundaries of the solid. Under isothermal conditions the extent of penetration after any particular time of exposure is related to the relative magnitudes of the interfacial tensions concerned.1,2 If the liquid-solid interfacial tension is less than one-half the grain boundary tension the liquid may penetrate at a relatively rapid rate for an indefinite distance into the grain boundary surfaces. If the liquid-solid interfacial tension is greater than one-half the grain boundary energy, liquid penetration occurs at a continually decreasing rate so that after the liquid has penetrated to a relatively short distance below the surface the process essentially ceases.3 Many observations of a qualitative nature concerning inter crystalline attack by liquid metals have been reported, for example, liquid bismuth upon copper,' liquid mercury upon brass,4 and liquid mercury upon nickel.' Scheil and Schessl determined the rate of penetration of liquid bismuth into the grain boundaries of hot rolled copper rod? At constant temperature, penetration rate was found to be independent of the depth penetrated, the rate in- creasing with increasing temperature corresponding to an activation energy of 20,000 cal per g-atom for the process. It was suggested that at lower temperatures the liquid travelled mainly along lines of three grain intersections while at temperatures greater than 1000°C essentially all grain boundary surfaces were covered. Recently, in a study of copper bicrystals having a common [loo] axis it was found that at 649°C bismuth penetrated 22, 25, and 63 deg boundaries while it did not penetrate 2, 12, 15, and 72 deg boundaries.' Elbaum reported that liquid gallium penetrates aluminum grain boundaries to a depth of 0.6 cm after 11 hr at 27°c.8 Assuming that the rate controlling step in the process was diffusion down the liquid film to the specimen surface, a diffusion coefficient of 10-5 cm2 per sec was calculated. This paper reports a study of the penetration of bismuth-nickel liquids into the grain boundaries of a nickel alloy, containing 0.25 pct Si and 0.22 pct Mn as principal alloying elements. The phase diagram

Jan 1, 1962

By M. E. de Morton

Recovery and early recrystallization of heavily deformed, 99.98 pct Cr was investigated by studying metallographic structure. X-ray line sharpening, electrical resistivity, plastic properties, internal friction, and shear modulus. Appreciable recovery of resistivity, internal friction, and shear modulus together with some hardening and relief of internal strains occurred before the visible growth of a textured substructure above 350°C (recrystallization in situ). The complex behavior of shear modulus, internal friction, and its strain amplitude dependence during annealing are discussed qualitatively in terms of the relative mobility of dislocations. BY plastically deforming fully recrystallized 99.98 pct Cr above the brittle to ductile transition temperature, at -350°C. as in wire drawing, chromium can be made very ductile at room temperature. However, this ductility is lost on annealing at high temperatures when recrystallization takes place.' The present investigation was made to determine the general pattern of the changes in a number of physical and mechanical properties during recovery and recrystallization of heavily deformed chromium as part of an effort to elucidate the reasons for lack of ductility in the fully recrystallized condition. PREPARATION OF MATERIAL Wire specimens 0.027 in. in diam were prepared from arc-melted, electrolytic chromium by extruding, hot swaging and finally wire drawing at 300" to 350°C, i.e. above the brittle-to-ductile transition temperature. The total reduction in area of the wire was 98 pct and the last 3 pct of reduction was made at 100" to 150°C before cooling to room temperature. The impurity content of the material is shown in Table I. Internal friction and modulus measurements were made on a single specimen after annealing in situ at successively higher temperatures. For all other measurements, a fresh specimen was used for each temperature and annealing of these specimens was done in evacuated (0.001 mm Hg) and sealed silica tubes for 1 hr at the various temperatures up to 700°C. EXPERIMENTAL METHODS AND RESULTS The occurrence of a. transition in some physical properties of chromium at - 40°C2 imposed limitations on the temperature region where some of the measurements could be made. The reason for this transition in chromium is at present unknown but is probably associated with an antiferromagnetic state observed below - 40°C.* Heavy deformation produces an anomalous decrease in resistivity when measured at temperatures below -40°C4 though a normal increase is observed above this temperature. On the other hand internal friction in heavily deformed chromium5 over the temperature range 40" to 50°C is invariant with temperature. Above and below this range internal friction is strongly temperature dependent, increasing with increasing temperature. A temperature in this range was therefore convenient for both resistivity and internal friction measurements and for consistency the measurements of the mechanical properties were also made at about this temperature. No structural change has, however, been observed in careful X-ray measurements6 between -195" and 50°C, i.e. departure from cubic symmetry was not greater than 3:10,000; X-ray line sharpening measurements were therefore more conveniently made at room temperature.

Jan 1, 1962

By R. Ruka, E. A. Gulbransen

ONE of the interesting questions in the understanding of the reaction of iron with oxygen is the kinetics and the mechanism of the crystal structure changes occurring in the formation and breakdown of the oxide film. In a recent work' the electron diffraction method was applied to the study of the solid phase reactions occurring internally in the oxide film on iron above 570°C and under vacuum conditions. The higher oxides which form under oxidizing conditions are reduced internally by the diffusion of iron into the oxide leaving the bulk of the oxide FeO (wüstite). This paper will ask and consider three questions. These are: (1) What is the nature of the depressed transformation temperature for the Fe3O4 + Fe ? 4Fe0 reaction in very thin oxide films?; (2) What is the mechanism of the forward transformation of Fe3O4 to FeO at or near 570°C?; and (3) What is the nature and mechanism of the slow reverse transformation of FeO to Fe3O4 and Fe below 570°C?. The composition of the oxide as well as its electrical, magnetic, mechanical, and chemical properties depends upon the kinetics of these reactions. Literature Survey The composition of the oxide film on pure iron at temperatures up to 570°C has been studied extensively by the electron diffraction method. Nelson,' Jackson and Quarrell,3 and Gulbransen and Hick-man4 have shown that Fe3O4 and a-Fe2O8 are formed in the temperature range of 225" to 570°C, while y-Fe,O, is most likely formed below 225°C for long oxidation times. In very thin films FeO (wüstite) is found to form at temperatures as low as 400°C, and its existence depends essentially upon the extent of initial oxidation. FeO is not found in the formation of thick films below 570°C. On the other hand X-ray5 and micrographic8 studies show that Fe3O4 may exist as the main com-ponent in thick films up to 650°C, well above the equilibrium temperature for the reaction Fe3O4 + Fe ? 4FeO. The kinetics of the forward and reverse trans-formations of the reaction Fe3O4 + Fe ? 4FeO have not been studied in oxide films. However, analysis of the data of Gulbransen and Hickman4 on the heat-ing and cooling of iron oxide films of known thick-nesses in high vacua shows that the forward reac-tion proceeds rapidly even for a 4000 A film at temperatures of 575" to 600°C. The reverse reaction or decomposition of wüstite (FeO) occurs at tem-peratures below 450°C. Thus, there appears to be a slow process in the decomposition which is in marked contrast to the rapid forward reaction. The decomposition of a bulk sample of FeO free from the metal has been studied extensively by Chaudron, Benard and coworkers using the micro-graphic, X-ray diffraction, and thermomagnetic methods. Chaudron7,8 first observed that the de-composition of FeO (wüstite) below 570°C occurs by the reaction 4FeO ? Fe3O4 + Fe. Later work by Chaudron and Forestier5 showed that the rate of de-

Jan 1, 1951

By Floyd C. Kelley

The literature of the last decade is rich with information relating to the cause and means of control of grain growth in pure metals, but is deficient concerning the role diffusion plays in grain growth, although during this period many new products that depend on diffusion for their properties and success have been developed. Among these are cementation products, produced by calorizing, chromizing, and carbonizing, or by mixing, pressing, and sintering powdered metals such as Syke's iron-molybdenum die material, Genelite, and Elcon Metal (copper, tungsten) etc. This is a fertile field for new developments, but before it can be utilized to the fullest extent there must be a thorough invest,igation of the processes by which diffusion and grain growth take place. Grain growth plays no small part in the process and certainly the physical properties of these products depend largely on the grain size and state of equilibtiuni produced. The field of investigation does not end here, but may be extended to the effect of diffusion on impurities, segregations and dendrites in the broad field of ferrous and non-ferrous metallurgy. A number of years ago the author investigated several of these cases and noted, with striking regularity, the pronounced effect of diffusion in promoting recrystallization and grain growth. An example of this phenomenon is given in his paper on chromizingl which contained photomicrographs of large radial or columnar crystals produced by diffusion of chromium in the solid state. Another manifestation of this effect was discussed by Austen,2 who showed the part hydrogen plays in the decarburization of steel and the effect of diffusion upon the grain structure. Diffusion of Metals in Iron It seems to be a general law, whenever two metals are brought into intimate contact at a temperature at which diffusion takes place, that a comparatively rapid, or abnormal, grain growth results. The grains

By N. A. Tiner

A study was made of the effects of temperature, type of loading, and electric polarization on the fracturing behavior of copper and zinc coated with mercury. Copper showed an em-brittlement only in cyclic loading, whereas zinc showed an em-brittlenzent in both static and cyclic loading. The embrittle-ment of zinc in static loading was prevented by sub-zero cooling to a temperatzcre of about -70°F. The emhrittlement of both metals was sliglztly reduced by cathodic polarization of mercury. The basic processes involved in fracturing were discussed in the light of these observations. When a solid metal is in contact with certain liquid metals possessing high wetting characteristics, a weakening effect is produced, and the solid metal fractures in brittle manner at a relatively low stress. This lowering of the fracture stress generally is considered different from the stress cracking caused by a corrosive liquid environment and is attributed to the lowering of the solid-liquid interface tension at the grain boundaries.1-4 The purpose of this paper is to describe a number of observations on the special features of fracturing of copper and zinc coated with a liquid mercury film, and to analyze the basic processes involved in fracturing in the light of these observations. EXPERIMENTAL OBSERVATIONS I) Effect of Type of Loading—The evidence appears to indicate that in static loading, metals usually fracture by the initiation of microcracks in the interior preferentially at the grain boundaries or at the intersection of slip bands.' In cyclic loading, cracks develop on the surface within the active slip zones, and gradually propagate with increasing num- ber of cycles.6'7 Because of this difference in the manner of initiation of cracks, a series of bare and mercury coated copper and zinc specimens was subjected to static and cyclic loading, and their fracturing behavior was examined. The specimens were machined to 0.25 in. in diam and 1 in. in length from a high-purity commercial bar stock, and annealed at an appropriate temperature. Mercury was applied to the surface of the specimens by rubbing with cotton wool soaked in a saturated solution of HgCl2 or by etching with a dilute solution of HC1 and rubbing with purified mercury and by washing in water. The static tension load-extension curves were obtained by means of a Riele Screw Power Universal Testing Machine. The room-temperature load-extension curves for copper and zinc are shown in Fig. 1. The deformation behavior of copper, as judged from the general configuration of the load-extension curve, was not affected by mercury coating. The maximum load to fracture and the elongation at the maximum load were practically the same for both specimens. The mercury coated copper, however, showed somewhat less localized necking and had smaller reduction of area than the uncoated metal. The behavior of mercury coated zinc was radically different from the behavior of uncoated metal. The load-extension curves were the same at the

Jan 1, 1962