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By Roy J. Greenfield, Charles H. Stoyer

A geophysical survey was made in Kylertown, Pa., in an area where the ground water is polluted with acid mine drainage. Since acid mine water is a good electrical conductor, both direct-current electrical and electromagnetic loop methods were examined for their ability to determine the subsurface electrical conductivity structure and from this to imply the location of the acid water. Consistent results were obtained with the two methods and the interpreted subsurface resistivities were consistent with the electrical resistivity measured for water samples. It was demonstrated that fracture traces which act as conduits for ground water flow can be located with electromagnetic surveying methods. Thus geophysical methods for measuring subsurface electtrical resistivity can be used to advantage for monitoring the environmental impact on the ground-water system of acid mine water.

Jan 1, 1977

By J. Walter Snavely

PRESENT-DAY processing in many industries, calcining, sintering, briquetting, beneficiation and nodulizing, increasingly calls for the handling of large volumes of hot bulk materials. Various types of conveyors have been employed. This discussion will cover the factors governing their selection. For temperature ranges up to 400°F, or approximately 200°C, a wide range of conveyors is available. Special constructions of rubber conveyor belts. steel conveyor belts, vibrating and shaker conveyors, apron conveyors, and drag chain conveyors, all are used successfully. As temperatures go well above 400°F, however, choice of conveyors is narrowly limited. This paper will consider the problem of handling bulk materials only where the temperatures exceed 400°F.

Jan 5, 1953

By Theodor Knutzen, Charles H. Fulton

The plant of the National Smelting Co., a corporation controlled by the Horseshoe Mining Co., was built during 1901 to smelt the dry siliceous ores of the northern Black Hills, extracting the gold- and silver-values in a matte of low copper-percentage which is shipped to Omaha and Denver for refining. Originally, the plant was designed to collect the values of the siliceous ores in an iron-matte, which mas to be resmelted with lead-ores, in a lead-furnace, the lead-bullion produced to be refined into Doré bullion in English cupelling-furnaces. However, the scarcity of lead-silver ores in the Black Hills, owing to the present non-productiveness of the Galena district, led to

Jan 1, 1905

C. P. BOWIE, San Francisco, Cal.-In my work with the U.S. Bureau of Mines, I have been detailed to report on oil storage containers, and in going around the country I have, been much interested in, the possibilities in the use of concrete for such containers. In talking with a good many people, I have discovered that concrete is being used A good deal for a wide variety of oils ranging from 14° to as high as 40° Bé., especially, by some of the western railroads:, If any member has had experience, in storing gasoline in concrete, I should like to learn of it. DORSEY HAGER, Tulsa, Okla.-Mr. M J. Munn, formerly .with the U. S. Geological Survey, acid connected with the Gypsy Oil Co., until a short time ago, has invented a invented a method for the application of concrete to the storage not only of crude oil but of refined products:. The Cosden Oil Co., of Tulsa, is now working on that plan, and, expects to store refined products in concrete tanks. THE CHAIRMAN (I.N. KNAPP, Ardmore Pa.).-I have had considerable experience in building masonry tanks for gas Holders. I do not believe it is possible to build a concrete or masonry tank of any kind. With hydraulic cement, mortar, which will be absolutely water-tight, unless the bottom and inner wall, after completion are waterproofed with some impervious material. The same will be true of oil tanks, the bottom and inner face of which must be made impervious to oil. Masonry tanks are intended to be sunk in the ground. All that the wall of the tank then amounts to is a retaining wall to keep the excavation in shape and to receive an impervious coating. The bottom of, a; tank, when empty, must be protected by a relief valve from any hydraulic: pressure acting from below. At ordinary prices, for sheets, a tank 100 ft. diam by 20 ft. deep can be built of steel much quicker and cheaper than of masonry. Several years, ago I saw very large oil storage tank under construction in California the bottom and sides being concrete. The sides were, sloped at about the single of repose for the material excavated: If you build a steel oil tank, you can get. .men for the work who do nothing else, and you, are likely to get a satisfactory job; but if you wish to build a concrete or masonry tank it is almost: impossible to find men skilled in building absolutely water-tight masonry Work. The general idea is that any laborer can mix up concrete in any old way and make a,

Jan 1, 1918

Manganese Resources in Relation to Domestic Consumption Discussion of paper by JOHN V. W. REYNDERS, presented at the Cleveland Meeting and issued, as Pamphlet No. 1656-C, with MINING AND METALLURGY, May, 1927. A. G. BETTS, Kinderhook, N. Y. (written discussion).-When a business concern hires an office boy, it takes on the first bright-appearing young chap to apply and pays him the prevailing rate of wages. One of the chief tasks the .office boy is supposed to be competent to perform, is to clean out the office. The manager of the business is highly competent in many lines, but for some reason lacks the ability to keep the office clean. To the steel man, it would seem that manganese is the office boy, and it is purchased just as found and offered to the purchasing agent. The steel mill is competent to perform many functions on a grand scale and with wonderful efficiency, but it is unable to make real steel. It is the function of the office boy, manganese, to do this. It is open to serious doubt if steel mill operators have ever taken seriously the metallurgy of the preparation of crude manganese. It has merely been found that some usable crude manganese may be obtained by running certain manganese ores through an iron furnace when not busy on anything else, or remote from iron ore, or with a lining that is about gone. It is, however, an entirely unwarranted assumption that the metallurgy of manganese has been worked out, or that the supplies of usable raw ore must be limited to materials of some specified analysis. There was a time when ores of copper, lead and zinc, for example, had to be rich and of specified analysis, to be usable, but the commercial raw materials of today bear little resemblance to such ores of the past. The discussions of manganese that I have seen are based on the assumption that the metallurgy of manganese is fully established and that the only usable manganese raw materials are of the kind used today. These discussions contain another error, not so much of statement, but of implication-that the tonnages of manganese materials in the United States are so much in this state and so much in that. When it requires a period of years and the expenditure of millions of dollars for a competent mining company to explore thoroughly a few acres of mining ground, is it not absurd to say that there are so many hundred tons of manganese ore in a certain state? This fact is not apt to be known fully in 10,000, years. I do not charge the mining engineers. who are on record, of making misstatements, because they merely say that so much

Jan 5, 1927

By Richard M. Foose

FIVE miles southwest of Mt. Holly Springs, Cumberland County, Pennsylvania, the Philadelphia Clay Co. has been mining and milling a white clay since 1896; for use in white cement, as a filler in rubber, pigment and paper, in the manufacture of insecticides, and for other minor purposes. Until late in 1942, when the mine was abandoned because of labor shortage, combined underground mining and surface stripping produced approximately 30,000 tons of clay a year, of which 10,000 tons were refined in the mill. GEOLOGY Lower Cambrian Antietam quartzite and the Montalto quartzite, stratigraphically older, trend N.55°E. and make a sharp 1600-ft. anticlinal ridge of the South Mountains. The Tomstown dolomite overlies the Antietam quartzite on the southeast flank of the anticline, which is displaced near its crest by a steeply dipping oblique fault. Erosion of the less resistant Tomstown formation has resulted in a narrow valley at an elevation of 700 ft. Directly on top of the Antietam quartzite and at the base of the Tomstown formation is a zone of sandy white clay, lenticular along the strike of the formations, ranging in thickness from 10 to 300 ft. within a mile. All of the formations dip steeply to the southeast, from 65° to vertical. The clay crops out at an elevation of about 1000 feet. ORIGIN AND CHARACTER The uppermost part of the Antietam formation is sericitic and schistose at many places, and at all these places weathering is in an advanced stage. The clay is the residual product of weathering of this sericitic quartzite or sandy schist. The crude clay has the physical aspect of a sandy kaolin, but there are large areas in the clay formation that are low in free silica, and commonly the 30 ft. adjacent to the Antietam quartzite is notably free of silica. The overlying Tomstown dolomite has been weathered almost completely to a mixed yellow and brown clay, which carries a zone of nodular and chunky limonite and manganese ore, 4 to 12 ft. thick, about l00 ft. from the contact with the white clay. In mining, this zone is an important "marker," indicating where the white clay may be expected in an advancing tunnel. The contact of the white clay formation with the yellow and brown clay of the Tomstown formation is relatively sharp, although the line of contact is irregular and therefore responsible for the lenticular character of the white clay formation. Following is an analysis of the refined clay containing less than one per cent of moisture when dried at 212°F.: Si02, 67.05 per cent; A1203, 22.27; Fe203, 0.40; CaO, 0.00; Ti02, 1.05; MgO, 0.52; Na20, 0.04; K20, 0.88; ignition loss, 7.65; total, 99.86.

Jan 1, 1944

By Waldemar Lindgren

CONTENTS. [ ] I.-CHARACTER OF THE DEPOSITS. 1. Principal Features. IN many schemes of classification and description the term contact-deposit has been somewhat loosely applied to all accumulations of useful minerals (other than those of unquestioned sedimentary origin) which are enclosed between two different rocks. As thus used, the term may include deposits of widely differing origin, and, unless qualified, is not in place in a genetic classification. The present paper deals with a special class of contact-deposits. In many geological provinces, granular igneous rocks, such as granite, diorite and syenite, have broken through and invaded sedimentary rocks. The molten magma may in part have reached the surface and there solidified with relative rapidity as a lava. The largest masses of it, however, did not reach the surface, but cooled very slowly at considerable depth under great pressure, and eventually consolidated into a rock of granitic texture. Uplifts and extensive erosion may have followed; and at the present day, in many places, thousands of feet of material have been removed, bringing to the surface the intrusive granular rocks and their once deep-seated contacts with the sedimentaries which they shattered at the time of in-

Jan 1, 1902

By J. J. Kramer, G. W. Wiener, K. Foster

The effects of the primary grain size and sheet thickness on the secondary growth rates of grains with (100) surface planes were studied in 3 pct Si-Fe sheets. This secondary grain growth was carried out under conditions in which the {100} plane had the lowest surface free energy. The value of the surface energy difference, between the (100) plane and the random matrix planes was found to he only about 3 pct of the grain boundary energy, indicating that most of the driving force for secondary growth is supplzed by grain boundary energy. A method for obtaining cube texture in 3 pct Si-Fe sheets by a secondary recrystallization process has been reported.' It has been demonstrated that a difference in surface free energy between the (100) plane and other planes is responsible for this growth, where the (100) plane has the lowest surface energy. A semiquantitative relation has been derived for secondary grain growth in sheets where primary grain growth has proceeded until the grains have grown through the sheet and the average grain diameter in the plane of the sheet is from one to two times the sheet thickness. Then, the linear growth rate, G, for the secondary grains can be given by where M is the grain boundary mobility, is the grain boundary free energy, is the average primary grain radius, A is the average difference in surface free energy between the (100) plane and planes of other orientations, t is the sheet thickness, and C is a term first proposed by zener6 which acts as a negative driving force, the effect of inclusions in holding up grain boundary motion. Since the problem of grain growth being discussed is under conditions where the matrix grain size is at least equal to the sheet thickness, the radius r is, of course, a function of the sheet thickness. The term B/r is the grain boundary driving force normally associated with inclusion inhibited or texture inhibited secondary recrystallization. Here, however, the term is modified to account for the fact that growth occurs in thin sheets. The term is the additional driving force available because of the difference in surface free energy. The purpose of the present work has been to evaluate the driving force terms of the growth equation by studying growth rates of (100) secondary grains as a function of sheet thickness and primary grain size. From these data it has been possible to determine the relative values of grain boundary energy, surface energy difference, and the inclusion term, C. EXPERIMENTAL PROCEDURE A 3 pct Si-Fe alloy was melted and cast under a helium atmosphere using electrolytic iron and a pure commercial grade of silicon as raw materials. The alloy was hot and cold rolled to a thickness of 0.6 mm, and samples approximately 5 in. long by 1 1/4 in. wide were cut from the cold-rolled sheets. Four different primary grain sizes were obtained

Jan 1, 1963

By C. F. Frey, P. J. Ahern, J. F. Wallace

THE high affinity of molten titanium for oxygen and nitrogen has resulted in considerable difficulty in developing a satisfactory melting procedure. It has been found necessary to perform melting operations either in a vacuum or inert atmos-phere, and failure to obtain a satisfactory crucible material has necessitated the use of special melting techniques. These techniques have included cold-mold arc-melting utilizing both consumable and nonconsumable electrodes, skull-melting, drip-melting, and levitation melting.' It has been recognized generally that the melting of both titanium sponge and titanium scrap would be expedited by the use of induction-melting procedures but the lack of a crucible capable of containing molten titanium without objectionable contamination thus far has prevented the use of induction-melting procedures. An extensive investigation: which included the common refractory materials was not successful in developing a satisfactory crucible for induction-melting. Some success in induction-melting has been attained with the use of a graphite crucible material, but in all instances sufficient carbon contamination was encountered to cause an appreciable reduction in the optimum mechanical properties of the titanium or titanium alloys. These investigations"" report an increase in the carbon content from approximately 0.3 to 1.0 pct. A serious reduction in the tensile and forming properties has been observed as a result of this carbon contamination. The development of a satisfactory induction-melting procedure for titanium without undue contamination undoubtedly would have considerable economic significance. Such a process would be particularly useful in melting the large quantities of low-cost scrap now available that can only be reprocessed at considerable expense and difficulty by the more elaborate techniques referred to previously. In addition, the process could provide a satisfactory method of melting and alloying of bri-quetted sponge for forging ingots.

Jan 1, 1959

By Leonard Obert

The structural stability of any mine or under- ground opening in rock is dependent on the stress field, that is, the state of stress in rock before mining, the stress distribution in the rock created by the opening, and the in situ strength of the rock. In the past mine design problems have been considered by assuming that the stress field is due only to the weight of the overlying rock, the stress around the opening can be calculated from elastic theory using laboratory-determined elastic constants, and the in situ strength of the rock can be determined from laboratory tests on small specimens. Solutions to hypothetical problems using this procedure are given in a report by Obert, Duvall, and Merrill.' Because of the uncertainties of these assumptions, this method can give only a rough approximation to the solution of actual structural problems. Obviously, this approach to determining the stability of underground openings would be greatly improved if the rock stress could be measured in situ, and it is undoubtedly for this reason that in recent years many investigators have spent considerable effort on the development of procedures for measuring rock stress. In this report a method is described for determining in situ the absolute stress in rock. The method requires the measurement of the deformation of a borehole before and after the rock is stress-relieved. The magnitude and direction of the applied stresses are calculated from the borehole deformation and modulus of elasticity of the rock. Also, the results of absolute stress determination made in the walls and pillars of underground openings in five rock types are presented. From these results a number of conclusions are drawn regarding the accuracy and limitations of this method and the problem of stress measurements in general.

Jan 8, 1962

By Arthur Baker III

The orebodies are long bedding-plane lenses of chalcopyrite and sphalerite, associated with garnetite masses. Most of the orebodies are within a 50-ft thickness of Cambrian limestone; other Paleozoic limestones and dolomites are locally metamorphosed but only slightly mineralized. Pre-mineral faults are numerous, but shallow folds were the main ore-localizing structures. JOHNSON camp is in the northwestern part of Cochise County, Ariz., about 50 miles east of Tucson. The nearest major mining districts are Tombstone and Bisbee, respectively 27 and 50 miles to the south, and the Superior-Miami-Globe-Ray porphyry copper group, about 90 miles northwest. Like many mining camps of the Southwest, Johnson camp is said to have been worked by the Spaniards. The first production on record was in the early 1880's, when an unknown amount of oxidized copper-silver ore in the Peabody mine was mined from replacement orebodies in the Pennsyl-vanian Naco formation. From 1904 to 1911 outcropping oxidized ores in the Cambrian Abrigo formation were worked, and an estimated 100,000 tons of copper ore were shipped. In 1912 the first large sulphide orebody of the district, the Republic Manto orebody, was discovered, and in the following few years some 250,000 tons of predominantly sulphide ore were shipped. The average grade of this ore was approximately 4.5 pct Cu, 6 pct Zn, 0.8 oz. Ag, and 0.001 oz Au. The Republic, Copper Chief, and Mammoth mines were the principal producers during this period. Mining ceased in the district after 1920, and until 1943 only small-scale leasing operations were carried on. In 1943 all the mines that had been productive were acquired by the Coronado Copper and Zinc Co., the present operators, and in the 10 years since that time the district production has amounted to approximately 350,000 tons of milling ore averaging 2 pct Cu and 6 pct Zn. Most of this ore was produced from the Republic and Mammoth mines, but since 1950 a large part of the production has been from the new Moore mine. The total known production from the district, then, is about 3/4 million tons of copper and copper-zinc ore of low grade. All of this ore was produced from orebodies associated with garnetite in the middle member of the Cambrian Abrigo formation. In addition to this known production, an unknown tonnage of ore was extracted from the Peabody mine orebodies that lie in the Pennsylvanian Naco formation. Published information on the geology of the district is limited. Aside from brief references in various mining journals, only three papers on the district have been published.1-3 One of these is a U. S. Bureau of Mines report on a diamond drilling program, one is a brief paper on the general geology of the district, and the third is a report on geochemical experiments, with a section on the occurrence of the orebodies. The last two are by John Cooper, of the United States Geological Survey, who has done much detailed work in the area. Stratigraphy The rocks of the mineralized area are Paleozoic sediments ranging in age from Cambrian to Penn-sylvanian. Several disconformities are present in the stratigraphic column, the most important one being between the Cambrian Abrigo formation and the Devonian Martin formation. There are no angular unconformities. Within the district, the Paleozoic sediments lie in a fairly uniform monocline, striking northwest and dipping 30" to 50" northeast. This local monocline is part of a domal struc-ture centered in the Little Dragoon mountains to the southwest. The Texas Canyon stock, a quartz monzonite body intruded probably during the Laramide revolution, lies south of the mineralized area (Ref. 2, p. 33). The Paleozoic rocks dip away from the stock, and on the surface are separated from it by at least 1500 ft of Pre-Cambrian rocks. The outcrop pattern of the northeastern edge of the stock suggests that it may dip gently northeastward, passing below the mineralized area at moderate depth. No quartz monzonite has been found in mine workings or diamond drill holes, which reach to depths of 1000 ft. The only igneous rock found in the mineralized area is a lamprophyre dike cutting the Naco limestone in and near workings of the Peabody mine. With the exception of the lowermost beds—the Bolsa quartzite and the shaly lower member of the Abrigo formation—the Paleozoic sediments are predominantly carbonate rocks, Fig. 1. The middle member of the Abrigo formation, which contains the principal ore-bearing beds, is limestone, with thin shale partings throughout most of its 250-ft thick-ness. Near the top of this member is a sandy bed some 25 ft thick. The upper member of the Abrigo formation and the lower half of the overlying Devonian Martin formation are dolomitic, with num-

Jan 1, 1954

By J. Nutting, J. W. Cahn

WITH the development of thin film techniques for the direct examination of metals in the electron microscope some new problems in quantitative metallography have become apparent. In order to obtain certain contrast effects in the electron optical image when examining thin films from alloys containing dispersed phases, it is essential to use films of a thickness at least two or three times greater than that of the mean particle diameter of the dispersed phase. From micrographs of such specimens it may be desired to obtain the volume fraction of the dispersed phase and the number of particles of the phase in a unit volume of the matrix. Under these conditions the particles sectioned by

Jan 1, 1960

By R. H. Martinson, E. Teghtsoonian

The effects of magnesium-rich surface layers of varying thickness on the mechanical properties of LiF have been studied. The yield stress, critical tensile stress, and work-hardening slope increase linearly with layer thickness, while the strain to fracture decreases yapidly with increasing layev thickness. The results of tension tests, supplemente!d by metallogvaphic evidence, indicate that the yield stress and the critical tensile stress of LiF are not determined by surface-source operation. DESPITE many studies, which have recently been reviewed,' certain fundamental aspects of the plasticity of LiF remain obscure. For instance, one question still awaiting a satisfactory resolution is: does the nucleation and/or multiplication of dislocations in LiF occur preferentially near the crystal surface? It is now well-known that mobile dislocation half-loops are readily introduced into LiF by surface damage and that the mechanical properties of LiF are affected by such surface damage. However, it is not known whether, in the absence of large numbers of artificially introduced surface sources, dislocations arise more easily near the crystal surface than in the crystal interior. It is also not known to what extent existing mobile dislocations multiply preferentially near the crystal surface. The present work is an experimental study of these matters. A short investigation of the effect of magnesium -alloyed surface layers on the deformation of LiF single crystals has been published by Westwood.~ Some relevant conclusions drawn from this research are restated here for purposes of comparison with the present work. 1) Tests on as-cleaved, chemically polished, coated and uncoated specimens show that a coating can restrict the operation of artificially introduced surface sources, thereby raising the yield stress. A coating also decreases the initial rate of work hardening of as-cleaved LiF crystals by reducing the number of active dislocation sources, so that mutual dislocation interference effects are lessened. 2) A catastrophic breakthrough of groups of edge dislocations piled up against the coating can cause stress drops in the stress-strain curve. 3) A surface coating can act as a stable barrier to the egress of dislocations, causing pile-up,

Jan 1, 1965

By E. O. Lilge, H. Siebert

A design of a multiple-bomb leaching unit particularly suited for the study of heterogeneous reactions, i.e. sol id-liquid-gas interfaces at high temperatures and pressures is presented. The component parts and overall design are described and illustrated in detail. The system has been tested by a limited number of experiments and found to work satisfactorily. Heterogeneous reactions at solid-liquid-gas interfaces, at high temperatures and pressures, are studied in either autoclaves1'4 or bombs5'9. Autoclaves are usually fairly large vessels which have a stirring arrangement incorporated in the design. Mechanical design limits the use of these vessels to relatively low temperatures and pressures. They are particularly well suited to rate or kinetic studies. Bombs can be designed to be operated at high temperatures and pressures, and are smaller vessels; because of this, stirring arrangements are not easily incorporated. In this paper a multiple-bomb system is described, that has been designed to incorporate the desirable features of both the autoclave and the bomb. The described unit has flexibility for an over all study of leaching. Most of the component units in this assemblage are standard equipment, designed and produced by well known manufacturers. No claim is made to the design of this equipment, and although described in some detail, this is done merely for clarity in the elucidation of the system presented. The general layout of the multiple-bomb assemblage is shown in Fig. 1A and 1B. The basic units in this system are: 1) 6 stainless steel 100 ml bombs (Fig. 4)

Jan 1, 1964

By O. Skiredj, J. F. Elliott

It has been necessary to collate the available data on the solubility of graphite in Fe-Si-Mn alloys for a study of slag-metal equilibria in ferromanganese production. That study will be reported later; the collation is reported here. The carbon content of graphite-saturated liquid iron above 1153ºC by Chipman and co-workers1 is: %C= 1.34 + 2.54 x 10~3t(°C) [l] For graphite-saturated manganese above 1322ºC it is: %C = 2.68 + 3.52 x 1CT3 t(°C) [2]

Jan 1, 1963

By William Brewster

DATING back some five years ago, various foundries made inquiries as to the probable total carbon content in a given specification and grade of pig iron. Up to that time we had no data, and except for a few occasional determinations of total carbon, no attempt had ever been made to set up routine determinations of total carbon. In fact, at that time, a cast analysis was considered sufficient, without examining at further length into possible variations of analysis between ladles of the same cast. In view of the various inquiries as to total carbon, we sampled all piles of all grades of pig iron, making complete analyses. Finding some variation in carbon content, we secured more samples and plotted the carbon content with respect to silicon in each grade of iron except for the higher phosphorus foundry iron, where it was necessary to divide the group into twenty-point phosphorus ranges. This is easily understood, owing to the falling off of carbon content with the increase in phosphorus con-tent, silicon in each case being the same. In addition, these curves clearly demonstrate the lowering of the carbon content as the silicon is increased. In order to insure accuracy and reliable determinations the following method of sampling and analysis was employed: Two pigs selected from each end of the car, each car containing iron from one 50-ton ladle, are drilled with a 5/16-in. drill all the way through from top to bottom in the center of one section of the pig. The drillings are collected and transferred to an 80-mesh sieve; the portion passing through and the portion retained are placed in separate envelopes and labeled accordingly. The amount of sample in each envelope is weighed to obtain the proportionate amount of coarse and fine drillings, then a factor weight of sample (1.3636 grams) made up of proportionate

Jan 1, 1936

By J. L. Taylor, P. Duwez

The phase boundaries in the ternary system Ti-Cr-Al have been established at 1800° and 1400°F for alloys containing more than 60 pct Ti. The martensite transformation temperature has been measured for the titanium-rich alloys. THE studies of binary alloys of titanium with the transition elements which have been published so far1-0 ndicate clearly that the solubility of these elements is always much greater in the high temperature body-centered cubic form of titanium (ß phase) than in the low temperature hexagonal form. In this category of alloying elements are iron, nickel, chromium, manganese, vanadium, molybdenum, tungsten, columbium, and tantalum. Although studies of the nontransition elements have been rather limited, early work on titanium binary alloys'" has shown that most of them were not very soluble in the a form, with the exception of aluminum, for which the solubility in a is about 25 pct.13, 12 In addition to this large solubility in a, aluminum is also soluble in ß titanium to the extent of about 35 pct and the transformation temperature from ß to a is raised with aluminum content. This effect is also typical of aluminum, in contrast with that found for the transition elements which lower the ß to a transformation temperature. Therefore, it may be anticipated that tprnarv titanium alloys with aluminum and any one of the transition elements will constitute a class of ternary alloys having characteristic features absent in alloys involving two transition elements. Chromium was chosen as a typical transition element for the present study because ternary alloys of Ti-Al-Cr commercially produced have been found to possess very interesting physical properties (MST-3 pct A1-5 pct Cr of Mallory-Sharon).'" Binary Systems The binary systems Ti-A1 and Ti-Cr have been established recently by several investigators. The data used in this investigation were taken from the complete diagram of Bumps, Kessler, and Hansen." This diagram agrees quite well with earlier investigations." For the Ti-Cr system, the phase boundaries at 1800" and 1400°F were taken from refs. 6 and 7. The binary system Cr-A1 has been studied recently by Bradley." This system is rather complex and contains not less than seven intermediate phases. The present study was limited to the titanium corner of the ternary system (less than a total of 40 pct Cr plus Al) and none of the phases present in the Cr-A1 binary alloys were found in the ternary alloys investigated. Experimental Technique Microscopic observation and X-ray diffraction measurements were used to identify phases and de-

Jan 1, 1954

By A. Gemperle

Electron diffraction and transmission electron microscopy on foils at room temperature were used to investigate the ordering of Fe-Si alloys containing 10 to 23 at. pct Si. A certain degree of DO3 order was found in all alloys. With the exception of the lowest silicon concentration for which the antiphase domains could not be clearly resolved, the alloys have a domain structure of two-domain type with boundaries having 1/4a01<111> displacement vectors for less than 12.3 at. pct Si and with boundaries having 1/2 a0<100> displacement vectors for more than 12.3 at. pct Si. The alloys with 12.3 at. pct Si have a domain structure consisting of fine domains with 1/2a&apos;o<100> boundaries within much larger domains with 1/4a&apos;o<111> boundaries. The development of these structures can be explained by transition of the alloy from the disordered state into the B2-type order and then into the D03-type order by the mechanism proposed previously for the FeSAl alloys. The existence of the B2 structure in the lower part of the investigated concentration range reported in some articles can be explained by fine domains with 1/2a&apos;o<100> boundaries formed by several disordered planes within large domains with 1/4a&apos;o<111> boundaries. The ordered structure predicted by the theory —with practically no domain boundaries —is found in the alloys having 12.3 at. pct Si where it develops in the B2 structure region. ORDERING in Fe-Si alloys was first studied by phragmenl who found that beginning with 13 at. pct Si the DO3 (Fe3Si) superlattice reflections appear in the diffraction patterns. The equilibrium diagrams constructed later by corson2 and Haughton3 from various measurements proposed the existence of a homogeneous solid solution (a phase) in the range from 0 to 25 at. pct Si. Jette and Greiner4 and Farquhar et al.5 measured the relation between lattice parameter and composition and they considered the break in the curve at 9 to 10 at. pct Si to be caused by the ordered solution a"(Fe3Si). Glaser and Ivanick6 Determined critical ordering temperatures of the alloys containing from 10.9 to 27.9 at. pct Si from the measurement of the electric resistivity of quenched samples. In all cases the critical temperature was lower than the melting point and it was highest for 25 at. pct Si. Lihl and Ebel7 measured the lattice parameter curves at various temperatures up to 1000°C. The region between two breaks on these curves, corresponding to 10 to 12.5 at. pct Si at room temperature, was considered by them to be two-phase (a + a"). They concluded by extrapolation of the measured values that a" in the alloy having 25 at. pct Si is stable up to the melting point. Davies8 studied superlattice reflections in the X-ray diffraction patterns of an alloy containing 8.7 at. pct Si. He found the B2 structure and short-range order in the slowly cooled samples and the DO3 A. GEMPERLE is Research Scientist, Institute of PhysicS, Czechoslovak Academy of Sciences, Prague, Czechoslovakia. __Manuscript submitted January 2, 1968. IMD structure in the quenched and annealed samples. This investigation first reports the presence of the B2 structure, phase a&apos;: in Fe-Si alloys. Meinhardt and krisement9,10 also found its existence in Fe-Si alloys by neutron diffraction. No order was detected by them in the alloy containing 8 at. pct Si. The onset of B2 order was observed at a composition of 9.2 at. pct Si. They found almost perfect B2-type order with partial DO3-type order at room temperature in the 10 to 12.5 at. pct Si range and almost perfect DO3-type order in the 12.5 to 25 at. pct Si range. They established the critical temperatures Tc of both the structures through measurement at higher temperatures. The critical temperature for the B2 structure was found to be always higher than the critical temperature for the DO3 structure of the same alloy. They extrapolated the curves of the critical temperatures and concluded that the alloys with more than 17 at. pct Si have the B2 structure up to the melting point and the alloys with more than 23 at. pct Si have the DO3 structure up to the melting point. The results of Meinhardt and krisement9,10 were confirmed by Dokken&apos;s measurement" of the temperature dependence of the electrical resistivity in the 10.8 to 15 at. pct Si range. On the other hand chessin12 detected by X-ray diffraction a considerably lower degree of order in the 12.7 at. pct Si alloy. ANTIPHASE DOMAIN STRUCTURE IN ALLOYS WITH B2- AND DO$-TYPE ORDER The ordered structures B2 and DO3 can be described in terms of a subdivision of the bcc lattice into four fcc sublattices with a parameter double that of the bcc lattice. Following Marcinkowski13 we will label them I. 11, 111, IV. The B2 structure in the AB alloy is formed by placing A atoms on sublattices I and II and B atoms on sublattices III and IV. In a non-stoichiometric perfectly ordered alloy having concentration (A) > (B), A atoms occupy sublattices I and 11. and A and B atoms distributed at random occupy sublattices III and IV. The DO3 structure in an A3B alloy is formed by placing A atoms on sublattices I, 11, and 111, and B atoms on sublattice IV. In a nonstoichiometric, perfectly ordered alloy having concentration (A)/3 > (B), A atoms occupy sublattices I, 11, and 111, and A and B atoms distributed at random occupy sublattice IV. As further shown in Ref. 13, two types of domains are possible in the B2 superlattice and the antiphase domain structure has associated with it boundaries with displacement vectors 1/4 a&apos;o<ll1> only. Four types of domains are possible in the DO3 superlattice and the antiphase domain structure has associated with it boundaries with displacement vectors 1/4a&apos;o<111> and 1/2a&apos;o<l00>. Bethe14 suggested on the basis of theoretical considerations that in a structure with two sublattices at low temperatures only one domain should be present in the whole crystal at equilibrium. Similarly Bragg15 concluded that at low temperatures the domain struc-

Jan 1, 1969

By G. Das, S. V. Radcliffe

The substructural features developed in tungsten as a function of annealing temperature (up to 2200°C) and type of material [undoped and doped powder metallurgy (PM) tungsten and electron beam melted tungsten] have been investigated by transmission electron microscopy. For doped PM tungsten wires, characteristic "par-ticulate" substructural features developed rapidly with increase in annealing temperature above 700°C. The features consisted of parallel rows of elongated or circular shapes (500 to 1000A diam) lying along the direction of the wire axis and were identified as internal voids by diffraction contrast experiments. In recrystallized doped PM rod, larger voids were observed and were identified by precision dark field analysis to be cubic in shape and bounded by (100) planes. In marked contrast with both the doped PM materials, recrystallized undoped PM rod exhibited only very occasional and randomly arranged voids. Furthermore, no voids were observed in either material after electron beam melting. The high concentration of voids in the doped PM materials is attributed primarily to vaporization of doping additions or their pvoducts situated at the original grain boundaries , whereas the few voids in undoped material are considered to be traces of microporosity which were not eliminated during sintering. A tentative mechanism is suggested for the dezlelopment of the voids in relation to the processing sequences (sintering and working) and to the subsequent annealing. In recent years, a characteristic substructural feature consisting of rows of small elongated or circular regions of light contrast lying along the direction of working has been seen in thin foil electron microscopy studies of annealed sheet, wire, and rod tungsten. These features were present in the published micrographs of sheet by Weissmann et al.1 and of wire by Meieran and Thomas2, although the authors did not draw attention to them. Wronski and Fourdeux3 observed similar features in sintered rod tungsten (it was not specified whether or not the material was doped*) and interpreted them on the basis of their ap- particles, based on extraction replica evidence from the fracture surface of the initial hot-rolled slab material from which the sheet was prepared. No diffraction contrast experiments on the features were reported in any of these studies. The present investigation was undertaken with the primary objectives of: a) identifying the nature of these substructural features in tungsten by electron diffraction contrast experiments, since the contrast for voids can be expected to differ from that for crystalline or glassy particles, and b) elucidating the origin of the features and their development. For the latter purpose, doped and undoped powder metallurgy tungsten was obtained as rod and wire to represent different stages of reduction during final processing. These materials were examined both in the as-processed condition and after annealing to successively higher temperatures. In addition, the same doped and undoped materials were examined after vacuum melting in rod form. I) MATERIALS AND PROCEDURE Doped powder metallurgy (PM) tungsten wire (commercial purity 99.9 pct W) was obtained in the as-drawn and surface ground condition (0.030 in. diam "ground seal rod"). Doped and undoped tungsten rod (0.075 in. diam) representing an earlier stage of final processing was obtained from the same commercial source (Refractory Metals Division, General Electric Co.). Lengths of both the doped and undoped rod materials were single-pass melted in an electron-beam zone refiner to examine the effect of vacuum melting on the substructure. Annealing was carried out in a tungsten crucible in a tantalum strip resistance furnace under a vacuum of l0-15 mm Hg. Longitudinal sections of the wire and rod materials were examined by light and electron microscopy. The preparation of thin foils suitable for electron transmission from 0.030 in. diam tungsten wire and the rod specimens was carried out by means of a high-precision microjet technique developed to provide lack of jet stability and precise control of the area thinned. The method is described in detail elsewhere.&apos; The foils were examined in a JEM 6A electron microscope using a goniometer stage (±20 deg tilt, 360 deg rotation) and operated at 100 kV. To minimize contamination problems a 200 µ condenser aperture was used in conjunction with a useful beam current of 50 µA. II) RESULTS AND DISCUSSION A) Diffraction Contrast Analysis. In order to determine the optimum conditions for the development of the substructural feature, a series of isochronal 30 min annealing experiments were carried out on specimens of the doped PM tungsten wire. The transmission electron microscopy analysis showed that the as-drawn wire, Fig. 1(a), consists of &apos;fibers&apos; whose long axis is closely parallel to the wire axis of (110). The fiber width averages some 0.5 µ. Dense disloca-

Jan 1, 1969

H. H. Kellogg (Columbia University)—The accurate measurements of the equilibrium gas ratios for the reaction: Pb(1) + H2S = PbS(c) + H2 [I] reported in this paper are a distinct contribution to the literature, and the authors are to be congratulated. I wish to comment, however, on the correlation of the data which is presented. The authors show a straight line correlation of log H2S/H2 vs 1/T, Fig. 1, and are satisfied with this for calculation of ?Fo even when extrapolated to low temperature (427 °C). Heat capacity data for the constituents of this reaction are available (at least to 900°K), however, and ACP for reaction [I] is finite and positive in the temperature range studied. Simplification of the heat capacity equations yields: ?CP= 2.71 + 1.65 x 10-3T (298°-900°K) This positive value of ?CP should result in a small but noticeable curvature of a plot of log K vs 1/T. That the experimental data fail to show such a curvature may be traced to another oversimplification of the author&apos;s treatment of their data. They assume that the activity of liquid lead is unity for all temperatures, so that

Jan 1, 1961