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By E. D. Calvert

As part of its goal to minimize the requirements for critical and strategic minerals, the Bureau of Mines is conducting research to foster the use of domestically abundant materials such as molybdenum. This report describes the development of an investment shell molding technique that can be used to make castings of molybdenum and its alloys. The mold material is cubic Zr02 with a monoclinic Zr02 binder. The shell, formed by standard investment molding techniques described in the text, is prepared for molybdenum casting by firing for 6 hours at 1,550° C (2,822° F) or for 4 hours at 1,650° C (3,002° F). The resulting castings have predictable and reproducible dimensions with good detail. As-cast strength is poorer than the strength of wrought materials below 1,600° F. At and above this temperature, tensile strengths of cast and wrought materials are nearly equal. Aqueous corrosion of the castings in most media is insignificant.

Jan 1, 1982

[Admissions: Aurel E. Smith, Chairman Edmond F. Egan Lawrence S. Fennell John S. Fuller Howard J. Ritts, Jr. Gene E. Roark Kenneth W. Robbins Ben M. Gottlieb Advertising: Bernard F. Klein, Chairman Henry N. Lyle R. E. Howard H. M. Krause, Jr. Mrs. Evelyn R. Robertson]

Jan 1, 1961

By E. T. Turkdogan, J. H. Swisher

The solubility of oxygen in zone-refined iron was determined in the temperature range.from 881" to 1350°C. The solubility in a iron at 881°C ms found to be about 2 to 3 ppm; in y iron, the solubility was found to increase from about 2 to 3 ppm at 950°C to about 25 ppm at 1350°C. The permeability of oxygen in an iron -0.1 pct Al alloy was determined in the y iron range, using an internal oxidation technique. By combining the permeability and solubility data, the diffzisivity of oxygen in y and a iron was calculated. The oxygen diffusivity in solid iron may be s~immarized as follows: 8820 For 6 iron and IN a recent paper, Hepworth, Smith, and Turkdogan1 reported on the solubility, permeability, and diffusivity of oxygen in 6 iron, together with permeability data for oxygen in a iron. In the present investigation, similar measurements were made in the ? phase region. In addition, a solubility measurement was performed in the a phase region to permit calculation of the diffusivity of oxygen in a, iron. References to early work on this subject are given in the previous publication.' EXPERIMENTAL Solubility Measurements. The oxygen solubility was determined by equilibrating cylindrical samples 0.3 in. diam by 14 in. long of zone-refined iron in water vapor-hydrogen gas mixtures. The zone-refined iron was prepared by B. F. Oliver of this laboratory, using an apparatus and technique described elsewhere.2'3 Six zone-melting passes were used to achieve a total impurity level of about 30 ppm. Of this 30 ppm, the combined nickel and cobalt content was about 20 ppm, oxygen was 4 ppm, and all oxidizable impurities less than 1 pprn each. A vertical resistance furnace wound with molybdenum wire was used for the experiments. The temperature was measured before and after each experiment with a Pt/Pt-10 pct Rh thermocouple. In the gas train, flow rates of hydrogen and argon were measured with capillary flow meters, and the resulting mixtures were passed through a column containing 90 pct oxalic acid dihydrate and 10 pct anhydrous oxalic acid to obtain predetermined ratios of H2O to H2. The vapor pressure of H2O above this mixture as a function of temperature is well-known.4 The exit gas was ana- lyzed periodically for H2O, and good agreement (+3 pct) with the calculated composition was obtained. The zone-refined iron specimens were held in the furnace for a sufficient length of time for equilibration, e.g., 18 hr at 1350°C and 1 week at 881°C, then quenched in a brine solution. After removing the surface oxide from the samples by machining, duplicate analyses were obtained by a combined vacuum fusion-infrared method; oxygen analysis was reproducible within 2 ppm. Permeability Measurements. The permeability of oxygen in alloys containing about 0.1 pct A1 was determined by internal oxidation and measurement of the subscale thickness as a function of time. The experimental alloys were prepared by adding aluminum to electrolytic iron (grade 104A plastiron) that had previously been vacuum-carbon deoxidized. The resulting ingots contained about 20 ppm O, 100 pprn C, 40 pprn Si, 50 ppm Mo, 20 ppm P, 20 ppm S, and 20 pprn Zr as the principal impurities. After hot rolling the ingots to 1-in.-thick slabs, specimens were machined from the stock in the form of rectangular plates, 4 by 5 by 2 in. The general procedure for the permeability experiments was the same as those for the solubility measurements. The specimens were cooled in a reducing atmosphere rather than quenched, however, in order to maintain a clean surface for measurement of the sub-scale thickness. This measurement was made on a polished cross section of each specimen, using a microscope with a micrometer stage. The inclusions formed at the lowest temperature 1033°C were too small to be seen with an optical microscope. An electron micrograph showing the size and shape of individual particles is shown in Fig. 1. The dark band in the picture is a boundary between two subgrains. The subscale thickness in these samples was measured with an optical microscope after heavily etching in 2 pct nital, which gave contrast between the subscale and the unoxidized zone.

Jan 1, 1968

MINING ENGINEERING presents the annual membership report of the Society of Mining Engineers; see page 109.

Jan 7, 1963

By Barbee J. Scheibner

This Bureau of Mines report describes the geology and physical properties of core samples at the Sunnyside coal mine No. 1, Sunnyside, Utah, and was written in conjunction with the Single-Entry Program conducted at the mine. The objective of this program was to test the hypothesis that the single-entry system in the Sunnyside mine, supported in the center by open cribs and divided by a fire-resistant partition, is equivalent to or better than a two-entry sys-tem. Drill cores, taken underground at 15 sites in the single-entry study area, facilitated the construction of geologic cross sections of the entries. Physical property data obtained from the drill cores was used in a three-dimensional finite element analysis program to evaluate the stability of the openings, the support requirements, and the de formation characteristics of the roof and floor material. Data on 10 physical property parameters for 5 rock types plus coal are also tabulated and discussed.

Jan 1, 1979

By Roger G. Long

In May 1973, the Bureau of Mines asked Arthur D. Little, Inc. (A DL) to investigate existing industrial communication standards that may be applicable to the problem of developing standards for mine communication, considering that the standards that may ultimately be developed will require simple field procedures for the industry and the inspectorate to determine that communication systems are properly functioning. The emphasis on this study is on telephone communications as related to coal mine applications. B. TASKS The tasks agreed upon for this program were as follows: 1. "Investigate the current practices and existing standards of other industries under government regulation. 2. Determine applicable methods for industry personnel and inspectors to ascertain conformance on-site with minimal test hardware. 3. Review the Bureau's approval, testing and inspection procedure as it may impact the development of such standards. 4. From the above studies investigate the development of installation and performance standards for mine communications, including voice and telemetry. 5. Prepare a written report specifying what standards and field inspection techniques are applicable with recommendations for development of subsequent data and ultimately standards and field inspection techniques. 6. Prepare a written summary of the findings of various investigations with an appendix covering the detailed findings of each investigation. 7. Prepare a list of suggestions of additional assistance the Bureau might require in subsequent phases of developing communication standards and means of ascertaining performance."

Jan 1, 1973

By J. Burns Read

IT IS the purpose of this paper to summarize, as far as possible, the metallurgical information and experience gained by the Ordnance Department, during the War, in the manufacture of artillery cartridge cases, to describe the tests to which artillery cartridge cases were put, and to summarize the knowledge and experience gained in this testing. The authors wish to acknowledge the aid given by manufacturers, army officers, and civilian employees of the Ordnance Department in obtaining these data. Artillery cartridge cases are cold drawn from circular disks punched from strips of rolled brass. The manufacture involves from 25 to 30 main operations, which are done almost entirely on a punch press. Descriptions of the operations have appeared in various periodicals and, therefore, will not be given here. After each cupping, or drawing, operation, except the last, the cases are annealed at from 540° to 650° C. (1000° to 1200°F.), to remove all the hardening stresses set up in the metal and to allow complete recrystallization. After each annealing, the cases are pickled in niter cake or sulfuric-acid solution and then washed in water to remove all traces of acid. In some instances, the cases are then immersed in a cyanide-salt solution, and afterwards rinsed in water, to remove the thin layer of copper that forms on the surface of the cases during the acid pickle. The last cold-drawing operation is followed, by the heading operation which, by flattening the head of the case on the outside, causes the metal to flow on the inside to approximately the proper finished dimensions. The mouth, or open end, is then annealed at 430° to 480° C. (800° to 900° F.) by immersion in a salt bath or by gas flames. After being washed, the cases are tapered, when they are ready for machining, inspection, and testing.

Jan 4, 1922

The Honeymoon Well nickel sulphide deposits are located in the Agnew-Wiluna greenstone belt, about 45 km south of Wiluna. Both disseminated and massive sulphide nickel deposits are hosted by komatiitic rocks within the deformed and metamorphosed Honeymoon Well ultramafic complex. Fresh ultramafic bedrock is covered by up to 50 m of highly conductive transported material which greatly hampers both exploration and understanding of the bedrock geology. In the early-1970s, mineralisation was discovered by diamond drilling geochemical anomalies defined by wide-spaced percussion drilling over ultramafics that had been outlined by ground magnetics. Subsequent drilling has defined a resource of 158 Mt at 0.71 per cent nickel (based on 0.4 per cent nickel cut-off, 300 m below surface, December 1995) in four deposits. Over the life of the project a wide range of geophysical techniques have been used including airborne and ground magnetics, time domain clectromagnetics (EM), induced polarisation (IP)/resistivity, gravity and downhole techniques including EM, IP and physical property Measurements.

Jan 1, 1996

By E. D. Gardner

Oil shale, a long-considered potential source of motor fuel in the United States, is found over an extensive area in the Green River formation in Colorado, Utah, and Wyoming.4/ Oil has been retorted commercially from shale in Scotland for many years,5/ and work done by the Bureau of Mines and other investigators has shown that it is technically feasible to extract oil from American shales.6/ By refining, the shale oil may be converted into marketable products similar to those manufactured from crude petroleum. The present paper, which was finished in 1936, discusses methods that would be adaptable to mining certain American shales, and the treatment applies specifically to conditions iii the Green River formation on Naval

Jan 1, 1942

By D. E. Wolfson

The Bureau of Mines carbonized 35 coal samples from Logan and Mingo Counties) W. Va., at 900° C using the Bureau of Mines-American Gas Association method, and determined yields of products and physical properties of cokes. Twenty samples represented the No.5 Block, Stockton, Chilton, Cedar Grove, Lower Cedar Grove, Alma, No. 2 Gas, and Eagle beds in Logan County, and 15 samples represented the Coalburg, Buffalo Creek, Winifrede, Cedar Grove, Lower Cedar Grove, Alma, and No.2 Gas beds in Mingo County, W. Va, Chemical analyses were determined for all coals. All coals in both counties rank as high-volatile A bituminous. Most of the coals are chemically suitable for metallurgical coals. Coals with accept-able ash and sulfur contents can be used as major constituents in coking blends with higher rank coal to yield coke with satisfactory properties for blast furnace use.

Jan 1, 1967

By Ad. Breyre

Internal-combustion engines have been used in Belgian mines for a long time. As early as 1899, the use of these engines underground was considered, but the general policy was to prohibit such an application unless ministorial permission was granted in special instances. At that time only gasoline engines were available, and a few of these were installed as stationary engines, although in general they wore replaced later by electric or compressed air motors. However, the number of gasoline locomotives continued to increase. Regulations governing; the use of these locomotives seen were formulated and as early as 1920, when a new set of regulations was promulgated, these of gasoline locomotives in mines could be authorized by the Provincial Inspection Department and no longer depended on obtaining a ministerial decision. Since 1931 this authorization may be given by the Chief Inspector of Mines, Director of the Mining District. Since 1920, safe practices have been incorporated in the regulations.

Jan 1, 1940

By K. L. Paciorek

The aim of this program was to develop a reliable and meaning-ful basts for assessing certain safety aspects, namely fire and, in particular, toxicity hazards of articles employed in underground coal mining operations. This investigation was centered on the thermal oxidative degradation of "pure" ingredients used specifically in the formulation of conveyor beltings. To achieve this goal all products formed on thermal oxidative degradation of the materials studied were analyzed, identified I and the amount of each individual species present was determined quantitatively on a weight of product per weight of material basis. The weight/weight data thus obtained can then be factorized to reflect the relative toxicity of each individual species present, using for example the Threshold Limit Values adopted by the American Conference of Governmental and Industrial Hygienists, whereby an overall "toxicity index" can be arrived at which makes it possible to compare the different potential formulation components in a quantitative manner insofar as their "toxicity" is concerned. Furthermore, knowing the off-gassing characteristics of the commonly used additives I their contribution to the product mix obtained from actual belting can be postulated. Conversely, from the species obtained on thermal oxidative degradation of conveyor belts the type and to a degree the content of additives can be deduced. Based on the se data meaningful regulations governing the material selection for underground use can be developed. For these studies a quiescent system at 370°C was employed. Thermogravimetric and differential thermal analyses were performed to supplement and extend the sealed system investigations and to provide information regarding thermal oxidative behavior under dynamic conditions.

Jan 1, 1975

By C. D. Keen

In the latter part of the summer of 1913 the Conservation Commission of the State of Louisiana, under presidency of M: L. Alexander, decided to stop the waste of natural gas going on at the "burning gas-well," Located about 2 mile southeast of Oil City, La. On several occasions, both in newspapers and in reports, comment had been made on the condition of this well, its harmful effect on the Caddo gas field, and the considerable loss, estimated at several thousand dollars each month, caused by the escape of the valuable fuel., But nothing had been done to bring the well under control and prevent further waste of gas until the State Conservation Commission took the matter in hand. The gas fields of Louisiana are among the greatest in the country. So far most of the gas has been found in the Caddo field proper, although considerable development has been done in and around the city of Shreveport and near the town of Mansfield in DeSoto parish. To extend the life of the gas fields and to prevent the quick exhaustion of the supply of the natural fuel are matters of vital importance for this section of the country. Four gas companies have entered the Caddo field and supply the surrounding towns and cities With gas. The Arkansas Natural Gas Co. has pipe lines to Little Rock, Ark., and supplies gas to the following cities and towns in that State: Texarkana, Hope, Garland, Emmet, Prescott, Boughton, Beirne, Gurdon, Arkadelphia, Gum Springs, Mal-vern, Dsnaldson, Gifford, Perla, Beaton, Beauxite, Mabelvale, Bryant, Sheridan, Pine Bluff, Little Rock, Argenta, Pulaski Heights, and Hot Springs. The Southwestern Gas & Electric Co. transports gas to Mooringsport, Blanchard, Caddo, Rodessa, Oil City, Vivian, Bloomburg, Hosston, Ida, Dixie, Belcher, and Shreveport. The Marshall Gas Co. supplies gas to the town of Marshall, Texas. The Louisiana Co. has a line to Shreveport. In, the oil field the gas is used for drilling purposes, and the operators either have their own gas system or buy from the gas companies. At the present time the surrounding territory depends for its fuel supply on the Caddo field, and the importance of the conservation of the natural-gas

Jan 1, 1915

By W. A. Forbes

PAGE Introductory............357 ReasoNs for Gas Cleaning.........358 First Methods of Separation of Dust.......359 Amount of Dust Produced by the Blast Furnaces of the United States Steel Corporation During 1912.....359 Dust Content in Blast-Furnace Gas.......360 Primary Cleaning. Dry Cleaning: General Remarks..........360 Braasert- Witting Whirler........362 Brassert Modifications of Brassert-Witting Whirler....363 Dyblie Whirler..........363 Remarks on Efficiency of Dry Cleaning......366 Wet Cleaning: Zschocke System..........367 Duquesne Tower..........367 Bian Gas Washer..........369 Final Cleaning. Wet Cleaning: Theisen Gas Washer.........371 Theisen Disintegrator Gas Washer.......372 Schwerz-Bayer Disintegrator Gas Washer..... 374 Fowler & Medley Vertical Gas Washer......376 Feld Gas Washer..........377 Reco Centrifugal Gas Washer........379 Sepulchre Gas Washer.........381 Dry Cleaning: Halberger-Beth Gas-Cleaning System......382 Smith.Bagley Gas-Cleaning System,......384 Howard Dust Separator.........387 Possible Separation of Dust by Electrical Precipitation ... 389 KapnOGraph............389 Methods of Determining DUst in Gas.......389 Advantages of Clean Gas.........393 Introductory. During the early stages of blast-furnace practice. the gas formed in the furnaces by the combustion of the coke used in smelting the ores was allowed to escape into the atmosphere. The light furnished

Jan 1, 1914

The Pittsburgh (Pa.) and Spokane (Wash.) Research Laboratories are among the world?s foremost mining research establishments. Once a part of the former U.S. Bureau of Mines (USBM), which was abolished by the U.S. Congress in fiscal year 96, health and safety research at these laboratories was transferred to the National Institute for Occupational Safety and Health (NIOSH). NIOSH is the Federal agency responsible for conducting research and making recommendations for the prevention of work-related illness and injury. The Institute is part of the Centers for Disease Control and Prevention within the U.S. Department of Health and Human Services. Over the past two decades, the Pittsburgh and Spokane Research Laboratories have produced sustained technological achievements in mining health and safety, including? ? Development of novel respirable coal dust control technologies and more effective monitoring techniques to reduce worker exposure to hazardous mine dusts. ? Improved ground control technologies to warn and protect miners from the dangers of coal mine roof collapses and other hazardous strata conditions. ? Improved ergonomic design criteria and training methods to protect mine workers from injuries and fatalities associated with equipment and manual tasks. ? Development of enabling technologies that allow miners to control their mining equipment from a physically safe, protected work area away from respirable dust, harmful noise levels, and roof collapses. ? Improved mine fire detection and extinguishment techniques. ? Development of smaller, lighter, and safer emergency breathing devices.

Jan 1, 2007

By Frederick C. Trutt

This report is intended as a reference for personnel interested in the computer anlaysis of coal-mine-electrical-power systems under either normal operating conditions or fault situations. The procedures developed for this purpose are described and implementation considerations are discussed with respect to the mine-power system. Considerations for choosing a solution technique and a number of examples are included. Procedures described include the Newton-Raphson iterative technique for the analysis of normal operation as well as a non-iterative Z-bus technique for analysis of unbalanced or balanced faults. During program development, strict attention has been given to the inclusion of core and/or time saving techniques such that these algorithms may be implemented on small as well as large computers. Program languages include FORTRAN IV for batch processing applications and APL or BASIC for interactive applications.

Jan 1, 1981

By Charles B. Carpenter

In general terminology, the West Texas Permian Basin comprises the area south of the Texas Panhandle and west of the Bend Arch or Central Basin region. It is outlined mere definitely by geologists, however, as that area underlain by the south half of the Permian Salt Basin4/ and includes Scurry, Mitchell, Sterling, Howard, Glasscock, Reagan, Crockett, Upton, Midland, Martin, Gaines, Andrews, Ector, Crane, Pecos, Ward, Winkler, and Loving Counties in Texas, and Lea and Eddy Counties in New Mexico. The oil fields of the area, of which more than 70 have been discovered, are shown in fire 1. Approximately 4,200 producing oil wells have been drilled in these fields. Oil has been produced from limestones and dolomites of Permian age in most of the fields in the West Texas Permian Basin. Some of the fields produced oil from sandstone beds above the limestone, and in two fields production has been found below the limestone in formations of Ordovician age.

Jan 1, 1936

By T. Umadevi, A. Pratap Singh, R. Sah, K. Abhishek

"It was possible to beneficiate a low-grade iron ore fines sample from Bellary-Hospet, Karnataka, India assaying 56% Fe, 9.1% SiO2 and 5.2% Al2O3 and produce two concentrates, namely, a sinter-grade fines concentrate (43.7% by weight), assaying 63.6% Fe, 2.6% SiO2 and 1.7% Al2O3, and a pellet-grade concentrate (30.7% by weight) assaying 64.7% Fe, 2.9% SiO2 and 1.7%Al2O3. Rejects (25.6% by weight) assayed 32.5% Fe, 27.9% SiO2 and 15.4% Al2O3. The mineralogical characterization indicated that the sample consisted of 69.5% ironbearing minerals (56% hematite, 7.5% martite and 6% goethite-limonite), 12.5% quartz and 15.2% clay, and the rest were minor minerals. Liberation size was found to be in the size range of 25 to 100 µm. The process flow sheet consists of jigs, spirals, grinding and low- and high-intensity magnetic separation of the deslimed feed. IntroductionJSW Steel Ltd is a 10-Mt/a integrated steel plant. To produce 10 Mt/a hot metal requires nearly 16 to 20 Mt/a iron ore fines. The fast depletion of highgrade iron ore fines, increased industrial demand and an increase in iron ore prices have necessitated the exploitation and use of low-grade iron ore fines in the steel-making process after beneficiation. Thus, the beneficiation of low-grade iron ores by removing the associated gangue minerals and enhancing their grade is essential. The use of these iron ore fines in sinter and pellet making has prompted the undertaking of systematic studies on low-grade iron ores.Finely disseminated low-grade iron ores with siliceous impurities have been upgraded by gravity, magnetic and flotation-based processes (Burt, 1994; Svoboda, 1987; Houot, 1983). The processing of low-grade Indian hematite ore containing high levels of alumina-bearing minerals as impurities present separation challenges and pose special problems in martite and magnetite, in association with quartz and clay as the gangue-forming minerals. Alumina is mainly contributed by clay (kaolinite, montmorillonite, illite, alunite), lateritic material and gibbsite; some alumina occurs as solids in iron oxide minerals, namely, goethite and limonite. Silica is mainly contributed by quartz and the associated clay. achieving a high-grade concentrate (Pradip, 1994; Singh and Mehrotra, 2007). Hematite ore basically consists of varying amounts of hematite, goethite,"

Jan 1, 2015

By J. G. Croeni

The titanium-iridium alloy system was investigated to determine whether alloys of this system would merit further development as control-rod material for nuclear reactors. A study was made to determine the titanium-iridium phase diagram by using melting-point, thermal analyses, X-ray diffraction, dilatometric, electrical resistivity, and metallographic techniques. The titanium-iridium alloy system was investigated between 500° and 2,400° C. Results indicate the formation of two intermetallic compounds, Ti3Ir rind TiIr3, and one intermediate solid solution centered about the 50 atomic percent iridium composition. A eutectic reaction occurs at 1,475° C, and 19 atomic percent iridium. The Ti3Ir decomposes peritectically at 1,520° C. The intermediate solid solution exhibits a maxima of 2,140° C. at 50 atomic percent iridium. This phase is also believed to undergo an order-disorder transformation at 1,750° C. Another eutectic reaction takes place at 2,000" C. and 60 atomic percent iridium. The compound TiIr3 formed at 75 atomic percent iridium decomposes peritectically at 2,115° C. Further increases in iridium content result in the formation of an iridium-rich terminal solid solution. Information obtained below 900° C. in titanium-rich alloys indicates that iridium acts as a beta stabilizer in titanium, and the authors believe that a eutectoid decomposition of beta-titanium occurs near 500° C. and 10 atomic percent iridium.

Jan 1, 1962

By Ursula E. Wolff

The precipitation of carbides from an alloy containing 33 pct Ni, 21 pct Cr, balance iron, was investigated electron microscopically by means of extraction replicas and thinned metal foils. Annealing temperatures ranged from 565°to 870°C and up to several thousand hours. M23C6 precipitated in pain boundaries, incoherent and coherent twin boundaries in that sequence. The orientation relationship between carbides and austenite matrix was determined and correlated with the morphology of the carbides and with the type of boundary in which precipitation occurred. In large-angle grain boundaries, as well as in coherent twin boundaries, the carbides had the same orientation as one of the adjacent pains. These carbides formed sheets of individual flakes with shapes related to the orientation of the boundary. In incoherent twin boundaries carbides precipitated in ribbons composed of pavallel rods. An unidentified subcarbide was found to precede precipitation of M23C6 in these boundaries. The M 23 C6 rods had a kind of fiber texture with (110) parallel to the long dimension of the rods and ribbon, and with orientations of both of the adjacent twin-related austenite crystals Predominant in the texture of the carbide. A hard sphere crystal model has been used to discuss orientation and morphology of the carbides in terms of free volume and vacancies available in the boundaries. A number of papers have dealt with the morphology of chromium carbide (M23 C6) precipitated in austenitic stainless steels.1"7 In all these investigations, the carbides were examined in the electron microscope by means of extraction replicas. With this technique, the carbides retain the spatial distribution they had in the bulk sample. However, since the matrix is dissolved in the process, the particles can turn in an unpredictable way; and the orientation relationship between matrix and carbides cannot be established. In this paper the results of studies on extraction replicas and on thinned metal foils are reported. These studies were undertaken to determine the matrix-to-car bide orientation relationship, and to correlate the orientation of the carbides with their morphology. PROCEDURE The material used was an austenitic alloy with 33 pct Ni, 21 pct Cr, balance iron, containing approximately 0.05 pct C. Coupons of 1.25-mm sheet were first solution-annealed at 1050°C for 15 min and air-cooled. Then, to precipitate the carbides, samples were isothermally annealed in the range from 565" to 870°C for times up to several thousand hours. All further specimen-preparation procedures were carried out after the final anneal. Carbon extraction replicas from polished and etched surfaces were made with 10 pct bromine in methyl alcohol.' Thin foils were prepared from punched-out 3-mm-diam disksg which fit into the electron-microscope holder. The disks were prethinned by grinding to approximately 0.5 mm thickness, and then electro-polished in a polytetrafluoroethylene holder1' with a solution containing 5 pct perchloric acid in acetic acid to which 10 g per 1 Cro3 and 5 g per 1 nickel chloride were added (etchant modified from that of Briers et al."). This solution dissolves neither the carbides nor the austenite around the carbides preferentially. By using extraction replicas, electron micrographs and selected-area electron-diffraction patterns were taken from the same carbide arrays. By using thin foils, electron micrographs were made from a grain boundary area containing carbides. Electron-diffraction patterns were then taken from the same area and from each of the adjacent grains separately. In this manner, the orientation of each grain could be determined without interference by the carbide pattern. A peculiarity of extraction replicas should be pointed out. After the matrix is etched away, the carbide arrays float freely in the etching and washing solutions, and are held in place only at the anchoring points in the carbon replica. When the replica is picked up with a screen the carbide arrays tend to flip to one side. Thus, while the surface features are preserved, the original arrangement of the carbides may severely and unpredictably be disturbed whenever the specimen contains large amounts of interconnected carbides. Nevertheless, it is possible to correlate the different morphologies of the carbides with the type of boundary in which they have precipitated. RESULTS 1) Extraction Replicas. Fig. 1 shows that the grain boundaries usually are curved, multicornered surfaces of random orientation. The coherent twin boundaries (which are (111) planes) cut a grain into parallel slices. Incoherent twin boundaries occur at the ends and on the steps of twins and are often narrow, parallel-sided strips which are much longer than they are wide. Different morphologies can clearly be distinguished for the M23Ce carbides precipitated in each of these types of boundaries, and agree well with those observed by kinzel.2 The kinetics of this precipitation has been investigated." The first carbides precipitate in junctions of three grain boundaries and fan out from there into the adjoining boundary surfaces, Fig. 2(a). These carbides are oriented randomly, Fig. 2(b), and become coarser and thicker as annealing time increases. The large-angle grain boundaries are next to fill

Jan 1, 1967