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By S. B. Lement

THE nature of the carbides that form during the tempering of martensite is a subject of continuing controversy. The only direct methods of identification available are X-ray and electron diffraction. These methods are subject to several difficulties. Only a relatively few diffraction lines of appreciable intensity emanate from carbide phases that are formed at low tempering temperatures. Furthermore, some overlapping of carbide and matrix lines occurs. There is also the problem that numerous lines in the patterns of possible carbide phases that may be present have about the same d-spacings. Increasing the number of carbide lines and eliminating the matrix lines can be accomplished by extraction techniques. However, there is always the possibility that a change in carbide structure will occur as a result of removal from the parent matrix. Therefore, such techniques as electrolytic extraction and making extraction replicas should be checked by other methods. For identifying small amounts of carbide in a tempered martensitic matrix, electron diffraction carried out in reflection is more advantageous than X-ray diffraction. To properly prepare a specimen for reflection electron diffraction, an etchant that will selectively attack the matrix and thereby cause the carbide particles to stand in relief should be used. With an electron beam directed at a grazing angle to the specimen surface, the major contribution

Jan 1, 1960

By E. M. Wise

The practice of adding moderate quantities of nickel to a variety of bronzes has been employed by foundrymen for many years with several objects in view. In some instances it was desired to harden the alloy; in others it was to increase the fluidity or to improve the solidity of the castings, or to refine their grain. These important matters have been considered in detail by Pilling and Kihlgrenl and by numerous other workers cited by them, and with the exception of the first will not be considered in the present communication. The possibility of reducing the cost of bronze by replacing a portion of the tin with nickel received attention some years ago by Burgess and Woodward12 and, as will be shown later, offers attractive savings in cost under present conditions. The age-hardening characteristics of the nickel bronzes of appropriate compositions have been known for some time and were mentioned by Price, Grant and Phillips3 and discussed by Wise4 in connection with their paper. These matters are further considered in recent patents15 and are becoming of commercial importance in the production of high-strength castings. The equilibrium relations existing in the high-copper region of the copper-nickel-tin system have been carefully studied by Eash and Upthegrove,6 and in somewhat less detail by Veszelka.7 The observa-

Jan 1, 1934

By G. R. Speich

The distribution of carbon and the type of substructure in iron-carbon martensites containing 0.02 to 0.57pct C has been studied in the as-quenched condition and after tempering at 25" to 700°C by using electrical resistivity, internal friction, hardness, and light and electron microscope techniques. in marten-sites containing less than 0.2 pct C, almost 90 pct of the carbon segregates to dislocations and to lath boundaries during quenching; in martensites containing greater than 0.20 pct C, appreciable amounts of carbon enter normal interstitial positions located far from defects. Tempering martensites with carbon contents below 0.20 pct at temperatures below 150°C results in additional carbon segregation to dislocations and to lath boundaries but no carbide precipitation whereas -carbide precipitation occurs in martensites with carbon contents exceeding 0.2 pct. Above 150°C, a rod-shaped carbide (either Fe3C or Hagg) is precipitated in all cases. At 400°C, spheroidal Fe3C precipitates at lath boundaries and at former aus-tenite grain boundaries. At 400" to 600"C, recovery of the martensite defect structure occurs. At 600" to 700°C, recrystallization of the martensite and Ost-waW ripening of the Fe3C occur. The effects of the carbon segregation that occurs during quenching and the subsequent substructural changes that occur during tempering on martensite tetragonality, hardness, and precipitation behavior are discussed. A mathematical analysis of carbon segregation during quenching is presented. RECENT studies of the strength of low-carbon martensitel-4 emphasize the importance of carbon segregation to the martensite lath boundaries and to the dislocations contained between them during quenching. Unfortunately, very few studies of the tempering of low-carbon martensites have been conducted, so the exact nature of this segregation is poorly understood. In fact, most early tempering studies5,6 were restricted to carbon contents greater than 0.20 pct. Moreover, these studies did not determine the amount of carbon segregated to the martensite substructure during quenching so that the initial state of the martensite was not established. Aborn7 studied the precipitation of carbide in low-carbon martensite during quenching but did not establish whether carbon segregation occurs prior to carbide precipitation, nor did he study the subsequent tempering sequence in detail. In the present work we have used electrical resistance and internal friction measurements, supplemented by electron transmission microscopy to establish the carbon distribution in as-quenched specimens. Specimens thin enough to avoid carbide precipitation (but not carbon segregation) were employed. The redistribution of carbon on subsequent tempering below 250°C was followed by measurements of elec- trical resistance. Additional studies were made on specimens tempered at 250" to 700°C to elucidate the overall tempering behavior of low-carbon martensites, including the formation of cementite and recrystalli-zation of the martensite. EXPERIMENTAL PROCEDURE Eight iron-carbon alloys with 0.026, 0.057, 0.097, 0.18, 0.20, 0.29, 0.39, and 0.57 wt pct C were prepared as 8-lb ingots by vacuum melting. Typical impurities in wt ppm were 40 Si, 20 Mn, 30 S, 10 P, and 10 N. These alloys were hot rolled to 3 in. plate at 1095°C) (2000°F). The hot-rolled plates were surface ground to remove scale and the decarburized layer, then cold rolled to 0.010 in. sheet. Specimens cut from the sheet were austenitized for 30 min at 1000°C (1830°F) in a vacuum tube furnace in which the pressure did not exceed 2 x 10-3 torr. Chemical analysis of specimens after austenitization indicated no decarburization at this pressure. Immediately before quenching, the furnace was filled with prepurified helium. The specimen was then pushed rapidly through an aluminum foil gasket, which sealed the bottom of the furnace, into an iced-brine bath (10 pct NaC1, 2 pct NaOH). The quenching rate at the M, temperature is about 104'c per sec for 0.010 in thick specimens, as calculated from Newton's law of heat flow2 using a heat transfer coefficient of 25 ft-'. This quenching rate is sufficiently high so that all the alloys transformed completely to martensite throughout the entire 0.010 in thickness and no carbide precipitation occurred in the martensite. All specimens were immediately transferred to liquid nitrogen after quenching and stored there until needed. Tempering below 250°C (480°F) was done in silicone oil baths thermostatically controlled to *;"C. Tempering above 250°C was done in circulating air furnaces or lead pots with the specimens contained in evacuated silica capsules. Electrical resistance was determined by measurement of the potential drop across both a standard resistance and the specimen, connected in series. All resistance measurements were made in liquid nitrogen (77K, -196°C) to minimize thermal scattering of electrons and thus maximize the contribution of impurity scattering to the resistance. Specimen dimensions were 5.10 by 0.19 by 0.025 cm. Although the precision in the electrical resistance measurements was +0.1 pct, the electrical resistivities could only be measured with an accuracy of +5 pct because of uncertainty in the specimen dimensions. Internal friction measurements were performed in an inverted pendulum apparatus at vibration frequencies of either 1.9 or 66 Hz. The specimen dimensions were 5.10 by 0.375 by 0.025 cm. Hardness measurements were made with a Leitz-Wetzlar microhardness machine with loads of 100 g. Specimens were examined by light microscopy after etching in 2 pct Nital and by electron transmission microscopy after preparation of thin sections by electrolytic thinning in a chromic-acetic acid solution.

Jan 1, 1970

By R. C. Craze

During the past 20 years. research and development in the study of reservoir behavior have dealt principally with flow of oil through sandstones. Many reservoir studies of sand fields have proved valuable in promoting recovery efficiency. This paper discusses fundamental principles governing oil and gas production from sandstone and limestone alike and presents the results of investigations relating to the application of analytical techniques used for sandstone reservoir studies to the study of limestone reservoir performance. The characteristics of limestone porous systems, porosity-permeability relationships, distribution and occurrence of oil, and characteristics of flow through such systems are discussed. Recognition is made of the similarities or differences which these factors exhibit in limestone and sandstone systems. Comparisons between operating data for typical limestone and sand reservoirs are presented. It is indicated that the distribution and movement of fluids in and through porous limestones follow the same fundamental principles underlying such processes in sandstones. This fundamental similarity may readily be discernible in the performance of many limestone reservoirs. The volumetric balance and unsteady state radial flow equation, the fluid displacement equation, use of electrical analogue devices, and other analytical techniques to study the behavior of limestone fields appear fundamentally applicable, but do require thorough understanding of the properties of the formation, of the fluids, their behavior during flow, and adequate production operating data. Need for more complete coring and comprehensive examination of core properties is stressed. The results of "active oil" studies, and of flow and interference tests are presented. Well spacing, well completion, and efficient rates of production in limestone reservoirs are briefly discussed. INTRODUCTION Limestone and dolomite reservoirs constitute the largest source of supply of crude oil in the world. an estimated 60 per cent of present production coming from carbonate reservoirs. In many large geologic provinces such as Mexico. the Middle East, and more recently Canada, almost all the oil is found in this type of rock. In the United States, all of the major oil-producing areas except California and Pennsylvania contain oil-bearing carbonate formations. The discovery in recent years of large oil reserves in the Silurian, Devonian, and Ordo-vician formations in West Texas, in addition to the large reserves in the Permian, has accentuated the interest of operators, geologists, and engineers in limestone formations and in the many problems associated with understanding the performance of these reservoirs. The rapid increase in discovery of oil in limestone formations and the present-day position of prominence held by these fields in the production and reserve picture in all parts of the world emphasize the horizons opened to the reservoir technologist in the field of geological and production research. Pertinent to an interpretation of the behavior of limestone reservoirs are the methods of analysis which may be utilized and a possession of full knowledge of the many factors which influence the analytical procedures. During the past 20 years a well-developed science of reservoir engineering has been built upon the research of many workers who studied the fundamental nature of oil reservoirs, characteristics of the porous media, properties and behavior of the contained fluids, and the mechanics of flow. Application of these studies to production practice has resulted in greater recoveries and more efficient field operation. The major portion of this evolutionary process has been founded upon studies of sand fields. The applicability of these more thoroughly developed techniques for studying sand fields to the study of the behavior of limestone fields becomes a factor of technical and practical significance. In the light of the technological background available to the reservoir analyst, this paper discusses fundamental principles governing oil and gas production from sandstone and limestone alike and presents the results of investigations relating to the application of analytical techniques used for sandstone studies to the study of limestone reservoir performance. LIMESTONE RESERVOIR CHARACTERISTICS The characteristics of limestone and sandstone reservoirs are similar in many respects and they both may occur under similar structural conditions. Fundamentally, the distribution and movement of fluids in and through the porous limestone media follow the same basic principles which dictate such processes in sandstones. Herein lies a fundamental similarity, which may readily be discernible in the performance of many limestone reservoirs. In some limestone fields, as in many sand fields, widely varying formation properties and distribution may reveal themselves in deviations in the performance of the reservoir, in the behavior of wells, and in fluid flow through the rock, and make difficult the delineation of reservoir behavior. Only by reservoir studies, core analyses, and coordinated laboratory and field experimentation can the effects of the many influencing factors upon the nature of limestone production be determined. FORMATION CHARACTERISTICS The chief difference between limestone and sandstone, aside from their chemical compositions, is the difference in the geometry and origin of the porous systems in the two kinds of rock. In sandstone the porous system results entirely from the openings among individual sand grains which occur during deposition. The geometry of the openings between the sand

Jan 1, 1950

By R. E. Pray, M. C. Fuerstenau, J. D. Miller, B. F. Perinne

Quartz cannot be floated with potassium amyl xanthate as collector at any pH. Complete flotation is achieved with certain minimal additions of amyl xanthate and Pb from pH 5.8 to 8.5 and with amyl xanthate and Zn from pH 7.5 to 8.1. The active species of these metal ions responsible for activation are shown to be PbOH and ZnOH No flotation was effected when Cu and Mg were added as activators. Previous work1,2,3,4,5,6,7 has shown that quartz may be floated in the presence of sulfonate or soap when the following two criteria are met: 1) some portion of the added metal ion has hydro-lyzed to its first hydroxy complex, and 2) a precipitate of the metal-collector has formed. Since sulfonate and soap, two substantially different anionic collectors, conform to these criteria, this phenomenon may well be expected to be of a general nature. In this view then, it would appear that any anionic collector, including xanthates, should also float quartz when these two criteria are met. The object of this paper is to demonstrate the conditions under which quartz will respond to flotation in the presence of potassium amyl xanthate. EXPERIMENTAL MATERIALS AND TECHNIQUES Quartz was prepared by leaching the sized sample (48 x 150 mesh) with HC1 until no iron could be detected in the leach liquor. Conductivity water, made by passing distilled water through an ion exchange column, was used in the investigation. Potassium amyl xanthate was selected as collector. Purification of this reagent was effected with the following method: 1) a laboratory sample of potassium amyl xanthate was dissolved to saturation in hot ethyl alcohol and filtered several times while still hot, 2) the filtrate was cooled, during which time potassium amyl xanthate crystallized out of solution; the xanthate was then separated from the solution by filtration, 3) the amyl xanthate was dissolved in fresh hot ethyl alcohol and filtered, 4) step (2) was repeated, 5) the crystalline potassium amyl xanthate was washed with ethyl ether five times, and 6) the xanthate was dried for 24 hours under continuous vacuum. Inorganic impurities are insoluble in hot ethyl alcohol whereas dixanthogen is soluble in ethyl ether. Five-gram charges of 48x150 mesh quartz were conditioned for 3 min in 125 cc of solution containing the reagents and were floated with the small-scale cell and procedure described in previous papers.478 Reagent grade HCl and NaOH were used for pH adjustment, while reagent n-amyl alcohol was added as frother. Frother addition is necessary with this technique, but it should be mentioned that data, similar to those shown in Fig. 2 for 1 x10-4 mole per liter Pb++ and 1 X 10-4 mole per liter AX-, were also obtained with a Hallimond cell in the absence of frother. EXPERIMENTAL RESULTS Clean quartz could not be floated with amyl xanthate at any pH. Flotation was achieved under certain conditions, however, when various metal ions were added to the system. The activating ions used were lead, zinc, copper and magnesium, added as reagent grade chloride salts. Lead as Activator: The effect of Pb++ as activator was examined at five different additions of amyl xanthate (Fig. 1, 2 and 3). When 1x 10-5 mole per liter xanthate was added in the presence of 1 x 10"4 mole per liter Pb ++, no flotation was obtained at pH 6.5 or below, while a recovery of about 60% was effected at pH 7. When the pH was increased to 7.8, no flotation was again obtained, Complete depression was noted from pH 7.8 to about 10, at which point a recovery of about 30% was achieved. At about pH 11, the precipitate of lead amyl xanthate which was present below this pH dissolved and complete depression occurred. When 2.5x 10-5 mole per liter xanthate was added with the same lead addition, no flotation was obtained at pH 5.8 and below, whereas a recovery of

Jan 1, 1965

By W. M. Robertson

The rate of crack Propagation thvough a solid meta1 in the presence of a liquid metal has been calculated. The crack is assumed to propagate by solution of the solid in the liquid under the influence of an applied stress, with volume diffusion of the dissolved solute through the liquid controlling the propagation. The calculated velocities can be tens of centimeters per second or higher. THE embrittlement of normally ductile solid metals by liquid metals has been the subject of extensive study, as summarized in the book by Rostoker, McCaughey, and arkuus.' In experimental studies of liquid-metal embrittlement it is usually concluded that the observed crack-propagation rates are too high to be accounted for by diffusion processes. Diffusion is considered to be an unimportant factor and various other mechanisms are invoked to account for the experimental observations. The similarities of liquid-metal embrittlement to stress-corrosion cracking, to hydrogen embrittlement of steel, and to low-temperature embrittlement of bcc metals are frequently used as analogies for these mechanisms.1"3 The present paper assesses how rapidly a crack could propagate by a mechanism of volume diffusion through the liquid metal. We assume that the crack propagates by solution of the solid in the liquid at the crack tip under the influence of the applied stress and diffusion of the dissolved solute away from the crack tip. The model uses only macroscopic thermodynamic, kinetic, and elastic concepts. The calculations indicate that this dissolution-diffusion mechanism can give high crack velocities. In some previous treatments4'' of crack propagation in a liquid-metal environment the fundamental step has been the breaking of atomic bonds at the crack tip. The liquid greatly decreases the energy necessary to break these bonds. The present model assumes the crack is filled with liquid metal; the presence of the liquid is essential because diffusion through the liquid is assumed to control the rate of propagation. With proper modification this model could also apply to stress corrosion in a liquid environment. THEORY Consider a crack in a homogeneous elastic continuum, ignoring all the structural details of the solid. This neglects a host of metallurgical details which can be significant in the problem of liquid-metal embrittlement;' but this simple assumption is a useful approach in evaluating the role of diffusion through the liquid. The stress distribution around the crack tip establishes a gradient in the chemical potential at the tip, which causes a diffusion flux through the liquid away from the tip. The solid-liquid interfacial tension works against crack propagation, since propagation requires creation of interfacial area. From these two considerations we derive the diffusion flux, which then yields an expression for the velocity of the crack tip. The concentration of the solute in the liquid, C, is equal to the equilibrium concentration in the presence of an unstressed, flat surface, Co, plus the excess concentration due to the stress, AC(a), plus the excess concentration due to capillarity, AC(y): We calculate AC(o) and AC(y) and then obtain the diffusion flux. Consider (Fig. 1) a long flat crack of length 2L, thickness 2r, and tip radius r, where r remains constant as the crack propagates in the positive x direction. There is no stress ay in the y direction across the flat surfaces of the crack. The magnitude of the stress at the crack tip due to the applied stress, a,, is given by the relation6 ^=^[l-2^] 12] which, for long narrow cracks, becomes The stress increases the chemical potential in proportion to the strain energy.? The excess chemical potential due to the stress, Ap(a), is given by where 52 is the atomic volume of the solid and E the Young's modulus. Inserting Eq. [3] gives Now consider the crack to be filled with a liquid metal. The excess solubility due to stress, hC(a), is given by the excess chemical potential due to capillarity, Ap(y), is given by8 where y is the solid-liquid interfacial energy, and v1 and YZ are the two principal radii of curvature of any surface point. At the crack tip, r1 = -r and vz = m, so TRANSACTIONS OF THE METALLURGICAL SOCIETY OF AIME

Jan 1, 1967

By R. W. Raymond

Through the courtesy of Mr. James H. Mayo, a member of the Institute, who is in charge of the operations of the Mindrinetti Company in the Saramacca district of Dutch Guiana, I have received specimeris of certain peculiar pseudomorphs of limonite after pyrite, which occur abundantly in the auriferous deposits of that. region.* I am indebted to Mr. H. Tweddle, a geiltleman- connected with the same company, for some particulars of interest con-

Jan 1, 1899

By John W. Cloud

The delivery of blows upon roadway structures by the locomotive engine at high speed, althongh long recognized, has, perhaps, not been as generally understood in severity, relation to speed, and cause as is desirable in matters of such importance. Some points of explanation, with illustrative disgrams, are, therefore, submitted to your attention, preparatory to a note 011 " Steel for Bridges," also submitted. In order that a locomotive may run at high rates of speed with-

Jan 1, 1881

Unitization—in some form from simple agreements among operators to complete consolidation of ownerships—is a means of obviating the wastes of unrestrained competition among owners in extracting oil and gas from a common reservoir, as well as of adjusting its output to the current needs of its owners. It offers opportunity for application of improved production methods which are expected to increase recovery, decrease developing and operating costs, and assist in stabilizing output.

Jan 1, 1930

(Under this heading will be published notes sent to the Secretary of the Institute by members or other persons introduced by members.) No. 528.-Mechanical engineer, member and technical graduate, with broad experience in shopwork, the economical handling and processing of materials and in plant design construction and maintenance and with good experience in mechanical engineering problems, as occurring at mines, available about Feb. 1 for a connection having sufficient work of this

Jan 2, 1919

BESIDES air -water, sulphur, salt, coal, and lime-stone are the key nonmetallic raw materials used by the chemical industry and each came in for attention at the AIMF, Industrial Minerals Division meeting at Morgantown. W, Va., Sept. 13 to 15. West Virginia is a growing chemical producing area with sites along the Ohio and Kanawka Rivers being favored because of power, accessibility of raw materials (many in the State), water supply, and transportation.

Jan 10, 1951

By Simon D. Handelsman, Reg M. M. Rowe

The mechanism of using gold as the basis for a loan was suggested to the treasurer of a mining company operating two gold heap leach mines at a time of high interest rates. Due to the seasonal nature of cash flows from operations, and the relatively low cost of funds this scheme was attractive. The paper describes the agreement with the bank, gives an example of the transactions, and describes other types of gold loans.

Jan 1, 1985

By P. R. Kneitz, G. Yoshikado, D. Zayakov

The design and analysis of a circular, domed powerhouse for Pacific Gas and Electric (PG&E) Company's Kerckhoff 2 Project is described. Exploration, geologic stress determinations, mechanical properties, reinforcement and instrumentation are addressed briefly. The analyses of the circular, domed cavern and the comparison of predicted and field deformations are presented in somewhat more detail. The behavior of the completed powerhouse cavern has been found to be substantially as predicted by the analysis.

Jan 1, 1982

By Frank Doxey

Louis A. Turnbull (U.S. Bureau of Mines, Washington, D. C.)—This paper is a well-organized concise discussion of progress in mechanization at coal mines in Nova Scotia during the last 50 years. It shows the perseverance and resourcefulness of those responsible for the production of high-quality coal essential to steel production in the area. The development of the Dosco miner and its use in longwall mining at the Sydney

Jan 1, 1955

By John J. Van den Broek

As the established tailings disposal techniques do not meet the requirements of today, alternative methods of disposal are explored. McIntyre Mines Ltd., Coal Div. found a solution in the construction and operation of a tailings dewatering plant. The solids are recovered from the tailings slurry by means of mechanical dewatering equipment and are then dried in a unique drying system to provide an excellent thermal fuel for a power generating station.

Jan 1, 1983

H. M. BOYLSTON, Cambridge, Mass.-We should feel greatly indebted to Mr. Miller for collecting this admirable series of photographs, but I cannot quite agree with his conclusions as to their significance. He apparently concludes that these needle-like constituents which he has shown in a good many cases, in the welded material at least, are cementite; that is, as we understand it, a carbide of iron. Now there seem to be

Jan 4, 1918

Unitization—in some form from simple agreements among operators to complete consolidation of ownerships—is a means of obviating the wastes of unrestrained competition among owners in extracting oil and gas from a common reservoir, as well as of adjusting its output to the current needs of its owners. It offers opportunity for application of improved production methods which are expected to increase recovery, decrease developing and operating costs, and assist in stabilizing output.

Jan 1, 1930

By Lewis Stockett

During the year 1903, a building having machinery corresponding to ail anthracite-coal breaker was erected at the town of Stockett, Cascade county, Mont., for the purpose of breaking-up and cleaning bituminous coal. The coal is mined from a vein of the Kootenai group of the Lower Cretaceous measures having the following section: The vein is nearly horizontal in position, and each bench differs in quality as shown in Table I.

Jan 1, 1905

By T. O. Olsen, R. Henriksen

Aggregated models of a bank of flotation cells have frequently been used, assuming that a single-cell model can be used for control and estimation purposes. In this paper we investigate the feasibility of this approach, and show that single-cell aggregated models may very well be used in order to estimate the aggregated net flotation rate constants of the bank. These estimates would usually be very crucial in order to control the plant.

Jan 1, 1981

By Michael K. O’Leary, William D. Coplin

Risks from political instability and government policies restricting equity ownership, local operations and transfers of payments affect the profitability of foreign mining ventures. More than seat-of-the-pants judgments and old-boy networks are required to anticipate these risks and to take actions appropriate to offsetting them. A system for making political forecasts, called the Prince System, and a series of charts relaying risks to a production of key minerals has been developed.

Jan 1, 1985