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By D. G. Westlake

THE structure observed in thin foils by transmission electron microscopy is not necessarily representative of the initial bulk material. We have shown that hydrogen, originally present in a specimen of vanadium, niobium, or tantalum, can be concentrated by the thinning operation used to prepare foils from the bulk materials.' These foils exhibited domain walls indicative of a tetragonal distortion of the bcc unit cells, probably caused by ordering of the hydrogen in preferred interstitial sites. We believe this ordering does not occur at room temperature in the bulk material which contains less than 1 at. pct H. In a continued effort to prepare metal foils whose hydrogen concentrations remain constant during preparation, we have developed some new chemical and electrothinning techniques for vanadium. Each of the procedures presented in Table I produced foils that were thin enough for transmission electron microscopy. The experiments described below were performed to test the effect of each thinning procedure on hydro-

Jan 1, 1968

By R. W. Smith, C. Schroeder, R. Haddenham

Amphoteric surfactants are heteropolar organic compounds which possess at least two functional (ionic) oppositely charged groups per molecule. The ones studied are manufactured by General Mills and possess one or more long hydrocarbon chains plus a carboxyl group (s) and an amino or imino group. Hallimond tube and M. C. Fuerstenau micro flotation cell flotation tests were performed on quartz and hematite as a function of pH using amphoteric, cationic, and anionic surfactants as collectors. For the most part, flotation could be correlated with an interaction of charged groups on the collectors with oppositely charged sites on the minerals plus association of hydrocarbon chains. The comparison of flotation in a Hallimond tube and an M.C. Fuerstenau cell shows that one should use care in using the latter if one excludes an additional frother from the system. Also, it is interesting to note that sometimes greater collector concentrations are required in the Fuerstenau cell for comparable flotation recoveries.

Jan 1, 1974

By E. S. Noe, D. S. Arnold, C. E. Polson

Reactors of today and tomorrow require a high uniformity of their fuel elements despite the wide variety of uranium raw materials from the far corners of the earth. To meet these quality standards metallurgists have been working to design production methods capable of yielding reactor feed materials whose maximum impurities are specified in parts per million, whose physical limits are expressed in thousands of an inch, and whose density variations are less than 1 pct. Such requirements are necessary to maintain normal neutron flow in the atomic reactor and to insure that the isotopic content of the feed material is maintained within narrow limits. Uranium ores and concentrates are produced in many sections of the world, including the Belgian Congo, South Africa, Australia, Canada, and the Colorado Plateau of the U. S. Ores from many of the larger deposits are relatively low grade, and these are concentrated near the mine site before shipment to refining centers, but high grade ores may be shipped directly to refineries.

Jun 1, 1956

By J. H. Faulk

An examination is made of the various factors influencing drilling rate and drill bit life in various diameter holes. It is concluded that drill bits in the size range 4% to 6 1/4 in. can be used to attain substantially the some daily drilling progress as conventional size bits in soft rock drilling operations. An examination of the most important factors influencing "hazard of losing the hole" in the different hole size results in the conclusion that the smaller hole sizes can probably be drilled at reasonably low risk. However, this risk will be somewhat greater in the smaller diameter holes, requiring that special drilling and mud engineering practices be used to make small diameter holes practicable in soft rock drilling operations. An engineering analysia is made of the power and hydraulic requirements of several drill string-hole combinations to test the feasibility of drilling .small diameter holes in soft rock areas. Large econormies in rig power requirements appear possible by drilling .smaller .size holes in these operations. INTRODUCTION The industry now is re-examining the utility of small diameter holes in the light of substantial technical advances made in recent years. Faced with increasing cost of finding reserves and with proration after developing them, the industry must either develop methods of economizing or receive a lower rate of return on investments. Small diameter holes appear to involve an attractive method of economizing. Our objective is to determine if this is technically possible in soft rock operations. Soft rock, as used in this report, refers to those formations of a "drill-ability" corresponding to that of all Gulf Coast formations shallower than and frequently including much of the Eocene rock system. An important phase of technology which we shall examine is relative drilling rate and bit footage which may be obtained with various size bits. Rig operating efficiency, particularly as influenced by hazard, is also discussed in detail. The technical conclusions resulting from these examinations are used to develop sample drill string design and rig horsepower requirements for drilling holes as smaH as 4 3/4 in. and larger. The principal criterion used for the drill string design is that approximately the same daily drilling progress would be possible in all size holes in soft rock operations. This facilitates a comparison of rig size required for drilling the hole sizes in the range between 4 3/4 and 8 3/4 in. BROAD PROBLEM OF DRILLING RATE AND BIT FOOTAGE The three factors controlling daily drilling progress are: (1) drilling rate of bit while on bottom turning, (2) bit footage, and (3) rig operating efficiency. Let us look now at the first two of these factors. Drilling technology has progressed to the point that a semi-quantitative analysis of the effect of various operating variables upon these factors can be made. Those factors which apparently limit both drilling rate and bit footage for bits now in use are: (1) bit design, (2) weight on bit, (3) hydraulic cleaning capacity for bit cutting surfaces and hole bottom, and (4) rotary speed. (We neglect the effect of mud and formation properties because these factors arc the same for the various size bits.

Jan 1, 1957

By B. F. Buie

For over 200 years meerschaum has been a significant item of trade between the Near East and countries to the west. Best-known for its use in making smoking pipes and cigar and cigarette holders, it is also used in making a variety of decorative and ornamental items. It is easily carved, and is given an attractive, lustrous finish by rubbing. No published specifications are known, but compact form, purity, uniform whiteness or light color, and uniform, porous texture appear to be requisites. Fig. I a shows the appearance of a piece of crude meerschaum from Turkey; Fig. lb a carved item; and Fig. lc, d, and e show the fibrous and porous texture as revealed by the scanning electron microscope. Neither a major industrial mineral nor a precious stone, meerschaum nevertheless holds a record of long-and continuing-association with art and personal affairs of man. It is also a mineral to which modem methods of exploration and production probably could be profitably applied. An interesting account of the preparation and use of meerschaum in the early part of this century is given by Sterrett (1907). Geology and Mining Mineralogy Meerschaum is recognized now to be the compact variety of sepiolite, the claylike variety of which is one of the minerals included in the chapter on clays. The word meerschaum, from the German meaning "sea foam," was in earlier times used synonymously with sepiolite, a word of Greek origin suggestive of the resemblance of the compact variety-then the only variety known-to cuttlefish bone. At one time meerschaum was used as the commercial name, and sepiolite for the scientific name. However, to think of meerschaum as the name by which sepiolite is known commercially is no longer valid, in view of the recent emergence of the earthy variety as a competitor of bentonite and other clay materials. Present tendency is to restrict the term meerschaum to the compact variety, and to use the term sepiolite as a more general name to include both the compact and earthy varieties. This is the terminology followed in this publication. Meerschaum typically is white to light gray, has a hardness of 2 to 2 ½ , conchoidal to irregular fracture, and specific gravity varying with porosity from about 2 to less than 1. The composition is somewhat variable,- but is near that determined by Schaller (1936) for sepiolite as 2MgO.3SiO2.4H2O. A more modern for mula based on X-ray determination of the crystal structure is given by Caillére and Henin (1961) as (Site) (Mg9)030(OH)6(0H2)46H20. The reason for the firm, compact nature of meerschaum, in contrast with the earthy variety of sepiolite, is not fully understood. It may be due to the presence of a very minor amount of some bonding material such as silica. Scanning electron microscope (SEM) photographs of a specimen from Turkey (Figs. lc-le) indicate that the meerschaum is composed predominantly, if not entirely, of crystalline fibers which merge into sheetlike forms in a complex, intertwined mass. Detailed X-ray and crystal structure data, as well as some data on thermal stability range, are given by Caillère and Hénin (1961) for the sepiolite family of minerals. Mode of Occurrence and Origin Most authors have attributed the origin of meerschaum to alteration of serpentine or other magnesian minerals. The occurrence in alluvium and other surficial deposits does not necessarily indicate that the alteration was supergene. In fact, hydrothermal origin appears more likely for some deposits, though not for all.

Jan 1, 1983

By J. A. Ede

THE object of the writer is to call attention to a rather unique aggregation of economic products distributed over a line of succeeding formations about 3 mi. long, to be seen within a few miles of La Salle, Ill. Fig. 1 is an ideal section of the stratification exposed and exploited along a distance of 3 1/5 mi. in a southwesterly direction from the quarry of the Utica Hydraulic Cement Co. located near the historic site of Kaskaskia village to the Oglesby, shaft at Oglesby. No attempt has been made to cover the whole field, special mention only being made (with the exception of two places) of the operations found along the course or parallel to the direction assumed in the ideal section. I have used Fig. 2, after J. H. Bent and De Witt Kelly, to locate the relation of the La Salle anticline to the coal mines of this district and to show the operation of No. 1 and 3 mines of the Illinois Zinc Co.

Jan 9, 1919

By G. P. Hulst

THE Parkes process lead refinery of the International Lead Refining Co., at East Chicago, was built by the International Smelting & Refining Co. to treat the lead bullion produced by its Tooele plant, at Tooele, Utah. The plant was designed and constructed under the direction of the writer. Ground was broken Apr. 16, 1912, and exactly six months later the plant was in operation and lead was being cast. The capacity of the plant, running 25 days per month, is 5,000 tons. The four products of the plant are common lead, corroding lead, antimonial lead, and Doré bullion. The site is an area, 64 acres in extent, lying north of 151st Street, between McCook Avenue and the Canal. The Indiana Harbor Belt Railroad, Baltimore & Ohio Chicago Terminal, and Pennsylvania Railroad enter, the yard at the plant. There are five, storage tracks and space for storing 100 cars in the yard. The main lead to the storage tracks passes over a 100-ton track scale on entering the yard...

Jan 8, 1914

By Shosei Serata, Bruce Gardner

A system of three new field instruments has been developed to measure, in situ, the three basic classes of geomechanical parameters: material properties, stress state, and creep deformation. The significance of this development is that it represents a successful adaptation of recent computer technology to underground rock mechanics work, opening up new possibilities in underground mining methods. The system was developed to meet the application requirements of the stress control method of mining, a method which is based on the actual geomechanical conditions of the underground, rather than upon conventional linear-elastic, idealizations of ground conditions. These instruments enable in situ measurement not only of elastic, but also post-elastic, yielding, and failure conditions of geological materials, establishing the stress control method on a truly scientific foundation. In order to evaluate the present status of this field instrumentation system, case examples of underground mine openings designed with the stress control method are reviewed and analyzed, in terms of the effectiveness of the three instruments for informing and guiding the site-specific application of stress control design.

Jan 1, 1984

By C. D. Broadbent

Open pit blasting can be a low cost routine or a high cost bottleneck depending on geology, environment and the operator's ability to master site conditions. Because blasting is a repetitive operation, there should be ample opportunity to optimize the process; but ordinarily this optimization is rarely achieved and then only if conditions remain consistent and predictable. Often, however, and particularly with porphyry coppers, hidden differences in rock characteristics nullify the operator's best efforts. At a porphyry copper deposit being mined by Kennecott Copper Corporation, all of the following rock types occur; oxidized and fresh porphyry, altered and silicified limestone, explosion breccia, rhyolite, sandstone, shale and several others. The units can cover large areas or be limited to a few tens of feet in maximum dimension. They are rarely visible on the bench surface and often do not show up in the bench slope. Even though the blastability of these rocks varies substantially, a generally-uniform blasting pattern was formerly used with disappointing results. Secondary blasting was often required and high bottoms occurred frequently, overblasting wasted drilling time, and explosives caused excessive throw.

Jan 4, 1974

By G. P. Hulst

The Parkes process lead refinery of the International Lead Refining Co., at East Chicago, was built by the International Smelting & Refining CO. to treat the lead bullion produced by its Tooele plant, at Tooele, Utah. The plant was designed and constructed under the direction of the writer. Ground was broken Apr. 16, 1912, and exactly six months later the plant was in operation and lead was being cast. The capacity of the plant, running 25 days per month, is 5,000 tons. The four products of the plant are common lead, corroding lead, antimonial lead, and Dore bullion. The site is an area, 64 acres in extent, lying north of 151st Street, between McCook Avenue and the Canal. The Indiana Harbor Belt Railroad, Baltimore & Ohio Chicago Terminal, and Pennsylvania Railroad enter the yard at the plant. There are five storage tracks and space for storing 100 cars in the yard. the main lead to the storage tracks passes over a 100-ton track scale on entering the yard.

Jan 1, 1915

By Cyril Stanley Smith

BeTa brass (consisting of approximately equal atomic proportions of copper and zinc) exists as a random solid solution at high temperatures, hut at low temperature< an ordered structure is stable, with the copper and zinc atoms occupying alternate sites on the body-centered-cubic lattice. On cooling, ordering commences at a temperature of 450° to 470°C., depending on the composition. The degree of ordering progressively increases at lower temperatures until it becomes virtually complete at about 100°C. The electrical resistivity of the alloy illustrates the changes clearly (Fig. I). This type of reaction has been a favored subject for study by physicists. An excellent summary of the theory is to be found in a paper by F. C. Nix and W. Shock1ey.l All published data on electrical conductivity, specific heat and other properties agree in indicating that the ordering reaction in beta brass takes place so rapidly that it cannot be prevented or even retarded by quenching&apos; With most ordered alloys, cold-working induces disorder and

Jan 1, 1943

By Cyril Stanley Smith

BeTa brass (consisting of approximately equal atomic proportions of copper and zinc) exists as a random solid solution at high temperatures, hut at low temperature< an ordered structure is stable, with the copper and zinc atoms occupying alternate sites on the body-centered-cubic lattice. On cooling, ordering commences at a temperature of 450° to 470°C., depending on the composition. The degree of ordering progressively increases at lower temperatures until it becomes virtually complete at about 100°C. The electrical resistivity of the alloy illustrates the changes clearly (Fig. I). This type of reaction has been a favored subject for study by physicists. An excellent summary of the theory is to be found in a paper by F. C. Nix and W. Shock1ey.l All published data on electrical conductivity, specific heat and other properties agree in indicating that the ordering reaction in beta brass takes place so rapidly that it cannot be prevented or even retarded by quenching&apos; With most ordered alloys, cold-working induces disorder and

Jan 1, 1943

By Cyril Stanley Smith

BETA brass (consisting of approximately equal atomic proportions of copper and zinc) exists as a random solid solution at high temperatures, but at low temperatures [ ] an ordered structure is stable, with the copper and zinc atoms occupying alternate sites on the body-centered-cubic lattice. On cooling, ordering commences at a temperature of 450° to 470°C., depending on the composition. The degree of ordering progressively increases at lower temperatures until it becomes virtually complete at about 100°C. The electrical resistivity of the alloy illustrates the changes clearly (Fig. I). This type of reaction has been a favored subject for study by physicists. An [ ] excellent summary of the theory is to be found in a paper by F. C. Nix and W. Shockley.1 All published data on electrical conductivity, specific heat and other properties agree in indicating that the ordering reaction in beta brass takes place so rapidly that it cannot be prevented or even retarded by quenching. With most ordered alloys, cold-working induces disorder and

Jan 1, 1942

By S. G. Dixit, A. K. Biswas

The flotation and adsorption behavior of ilmenite, monazite and zircon have been studied with sodium oleate as the collector and pH as the principal variable. The maxima in the flotation and adsorption properties of any of the above minerals fall within similar pH ranges. The bell shaped pH versus adsorption magnitude (r) curve is explained on the basis of collector concentration (Co and the concentration of hydroxyl ion (COH-) acting as the depressant. An equation of the type: 1 =KiCor~K2 Coh-/Coi-is proposed to account for the experimental data. The beach sand deposits along the sea coast in Southern India contain ilmenite, monazite, zircon, rutile and sillimanite as valuable minerals while quartz, garnet, shells and traces of hornblende form the gangue. A typical composition of the deposits is reported to be as follows:&apos; Ilmenite 75%, Zircon 4-6%, Rutile 3-4%, Monazite 2 - 4%, Garnet 2 - 5% and the rest 8 -10%. Selective flotation of beach sand constituents has been reported by many workers.2-4 The fatty acid soaps have been invariably used as collectors. It is seen that all the valuable constituents of the beach sand are efficiently floated by soap collectors such as sodium oleate. In order to selectively float the beach sand constituents, it is necessary to use some depressants such as sodium silicate.3 The physicochemical parameters that govern the flotation of these minerals are yet to be studied in detail. In the present article, the findings on the parallel studies on the flotation and adsorption of the systems — ilmenite-sodium oleate, monazite-sodium oleate and zircon-sodium oleate — are being reported. In these correlative studies on adsorption and flotation of beach sand minerals, ilmenite (FeTiO3), monazite (Ce, Dy, Nd) PO4 and zircon (ZrSiO,) have been selected because they represent three important

Jan 1, 1970

By G. P. Marino

The "conductivity ", Kr, of a spherical void in a linear temperature gradient due to radiation is calculated by integration of the general expression for diffuse radiation between two gray surfaces of arbitrary orientation. The spherical geometry allows an exact evaluation of the phenomenon without resorting to up-proximate expressions for the radiant heat flux. The resulting expression for Kr is three quarters of the approximate value obtained by Loeb. IN the determination of the thermal conductivity of porous materials such as sintered UO2 and ThO2 fuel pellets, the magnitude of the thermal conductivity in the pores due to radiative heat transfer across the pore, Kr, may be important in assessing the total conductivity of the pellets. Loeb&apos; has calculated Kr for various pore geometries by approximating the net flux of heat between two surfaces of temperature difference AT as 4eT~AT and obtained: K,=4yoet3odp [1] where a is the Stefan-Boltzmann constant, E is the emissivity of the radiating surface, To is the average absolute temperature of the region across which radiation occurs, dp is the largest dimension of the gap in the direction of heat flow, and y is a geometric factor. That is: y = 1 for laminar pores and cylindrical pores with axes parallel to the heat flow direction, y = 2/3 for spherical pores, y = /4 for cylindrical pores with axes perpendicular to heat flow direction. It was the purpose of this work to obtain an exact expression for K, in spherical pores by integration of the general expression for the net heat transfer between two incremental areas on the surface of a spherical pore. This procedure yields a value of Kr 3/4 of that obtained by Loeb. I) CALCULATION OF Kr Fig. 1 illustrates the general geometry which defines the problem. The total emissive power for a gray body is given by: E = EoT4 [2] where E is the radiated energy per unit area of the radiation surface per unit time, T is the absolute temperature, o is the Stefan-Boltzmann constant (o = 5.67 X lo- &apos;&apos; watt per sq cm-"K1), and E is the emissivity of the surface. Although Eq. [2] gives the exact expression for the total emissive power of any gray body, all practical problems involve the net exchange of thermal radiation between a body and surrounding bodies. The two major considerations in the solution of such problems are a) shape and relative position of the surfaces and b) the emissivities of the surfaces. In this work it shall be assumed that all incremental areas on a pore have the same emissivity and, further, that little or no reflection occurs (i.e., the radiation hitting a surface is either absorbed or transmitted). Thus, the solution of the stated problem requires only that consideration a be satisfied. Consider two incremental surface areas dA 1 and dA2 of the same material in a general orientation to one another. Let dAl be at temperature TI and dAz be at T2. Fig. 2 illustrates the geometrical parameters involved. That is, 71, is the normal of dA, n2 the normal of dA2, r the line connecting the centers of each area, 81 the angle between nl and r, and Q2 the angle between 7,2 and r. Using Eq. [2] and the Lambert cosine law of diffuse radiation it is easily shown that:293 WdAf- dA, = ecr T*------^fpi------" dAidA2 [ 3a 1 and

Jan 1, 1970

By Cyril Stanley Smith

BETA brass (consisting of approximately equal atomic proportions of copper and zinc) exists as a random solid solution at high temperatures, but at low temperatures [ ] an ordered structure is stable, with the copper and zinc atoms occupying alternate sites on the body-centered-cubic lattice. On cooling, ordering commences at a temperature of 450° to 490°C., depending on the composition. The degree of ordering progressively increases at lower temperatures until it becomes virtually complete at about 100°C. The electrical resistivity of the alloy illustrates the changes clearly (Fig. I). This type of reaction has been a favored subject for study by physicists. An [ ] excellent summary of the theory is to be found in a paper by F. C. Nix and W. Shockley.1 All published data on electrical conductivity, specific heat and other properties agree in indicating that the ordering reaction in beta brass takes place so rapidly that it cannot be prevented or even retarded by quenching. With most ordered alloys, cold-working induces disorder and

Jan 1, 1942

AT the meeting of the Board of Directors on Jan. 28, 1927, the tentative budget of this Institute for next year was discussed, and in connection with the evident necessity for a larger income to meet increasing demands for service, the advisability of in- creasing the dues of members, was brought up. W. Spen- cer Hutchinson advocated an upward revision of the dues "believing it necessary that the Institute have a larger income, in order that it may carry on necessary work and render adequate service to its membership." Since this is a matter that directly affects every member, .President Taylor was directed to appoint a committee, which he did, consisting of George D. Barron, W. H. Bassett, and R. H. Sweetser, with T. T. Read as secre- tary, to bring in a tentative outline of the main factors in the problem for discussion at the annual meeting, on Feb. 15, and to prepare, after they have had the benefit of the discussion at that meeting, a report for the board. The amount of the annual dues is fixed by the con- stitution and can only be changed by proposing an amendment to the constitution. This amendment would have to be submitted to the members by letter ballot at the time of the election of officers for 1928, so that no change can be made in the dues for 1927 in any case. WHY THE INSTITUTE NEEDS MONEY At the annual meeting past-president Reynders, as chairman of the executive committee made the follow-ing report, which since it admirably sets forth the rea-sons why an increase in the dues has been suggested, is included here. "The report of the president has covered the situation so fully that little is left for me to say. However, a word in regard to the functions of the executive com-mittee may not be out of place.

Jan 3, 1927

By J. B. Umpleby

PRoduction engineering in 1927 may be characterized by a great. clarification of fundamental conceptions, and many improvements in technique. During the year the profession has received tnarked recogni-tion by the industry and to an extent never before attained has become an integral part of it. History Petroleum production engineering is a new profession. Prior to 1925, when this Institute undertook the work, no forum existed for the open discussion of its technical problems. There was no attempt at a handbook of the subject prior to "Petroleum Production Methods by J. R. Suman, in 1921, and no textbook prior to Petroleum Production Engineering" by L. C. Uren, in 1924. As late as 1926, only six schools and universities offered special courses in petroleum production engineering. Prior to about 1923, engineers engaged by oil companies were used almost exclusively for construction and location work. Two of the leading production engineers in the Mid-Continent field, although with their respective companies more than twelve years, were not definitely assigned to production work until 1924. Both men now head large departments giving almost their entire time to production problems. Because of the newness of the profession, the leading production engineers of today have had their fundamental training in mining, civil, mechanical and electrical courses. Not unlikely this diversified training is in considerable part responsible for the amazing growth of the profession. I believe, however, that recognition is due principally to economic pressure within the industry which has directed attention more and more sharply on costs and efficiency. After all, the justification for the growth and continued development, of the profession is to recover more oil from a given unit of sand at less cost per barrel. In this new profession, it seems to me that greatest progress will result from focusing thought and effort on this single objective, and if I might offer one suggestion to the com-

Jan 1, 1928

By F. C. Farnham

THERE has been very little, if any, uniformity in the reference datum used for magnetometer surveys. It has been the practice to choose a base station at which the magnetic field is assumed to be normal and call the difference in field strength between a given station and this base the anomaly at the given station. For small-scale surveys latitude and longitude corrections may or may not be applied, but for large-scale surveys such corrections usually are applied. The United States Coast and Geodetic Survey maps showing lines of equal magnetic intensity are commonly used to determine the normal latitude and longitude variation by scaling values from the map for given points and computing the change per mile north and the change per mile east. This method has been quite satisfactory for isolated surveys, but when two surveys originating at different base stations were extended until they joined, difficulty arose, not only because of discrepancies between base-station values, but also because of differences between the latitude and longitude correction factors used for the separate surveys. It is the purpose of this paper to describe a reference datum for magnetometer surveys which, it is believed, will eliminate most of the difficulty arising from this source. In order to be satisfactory, a general datum for magnetometer sur-veys should be as close as possible to the observed field and still he based on some assumed distribution of magnet poles, in order that the "normal" value of any component of the field for any given point may be computed to as many significant figures as desired. Such a field has been com-puted, and a comparison of the intensity of its vertical component with the average vertical intensity for the United States as shown by the U.S.C.G.S. map of lines of equal intensity for 1935 is shown in Fig. 1.

Jan 1, 1939

By S. S. Lisnyak, B. D. Lichter

An important question in the study of the "hot corrosion" phenomenon (i.e., accelerated oxidation of Ni-Cr-base and Co-Cr-base "superalloys" in the presence of sulfur) is the condition of formation and physico-chemical properties of different sulfides in the system Ni-Co-Cr-S. seyboltl has observed the presence of ((chromium-rich" sulfides of compositions M3S4, and M2S3 in the scales of superalloys after hot corrosion; however, as he points out, much confusion exists as to the identity of sulfides found on Ni-Cr and Co-Cr alloys. According to the literature,&apos; ternary sulfides, e.g., NiCr2S4, (monoclinic structure) and CoCr2S4 (spinel structure) exist in these systems. Therefore, it is likely that these compounds are found in the scale of alloys undergoing hot corrosion. At present this possibility has not been discussed in the literature. Accordingly, we have begun investigation on the properties of ternary sulfides and their mutual interaction. The magnetic and electrical properties of pure NiCr2S4 and pure CoCr2S2 have been previously determined."-&apos; In the present work we have studied the interaction between these sulfides at high temperatures by means of X-ray diffraction and magnetic susceptibility. The measurements were carried out at room temperature after appropriate thermai treatment of samples at high temperatures. For alloys containing the three elements nickel, chromium, and cobalt this interaction may be of importance in the study of the hot corrosion phenomenon. The compounds NiCr2S4 and CoCr2S4 were prepared from stoichiometric amounts of the elements and CoS in the case of CoCr2S4. Samples were mixed and sealed in evacuated silica tubes, slowly heated to 900&apos; to 100O°C, and held at temperature for a total of 120 hr (NiCr2S4) or 80 hr (CoCr2S4) with intermediate re-grinding~. X-ray diffraction showed a pure spinel structure for CoCr2S4 and a monoclinic structure for NiCr2S4. Samples of mixtures of the two ternary sulfides were prepared with different compositions, see Table I. Samples were heated for a total of 80 hr at 900&apos;C in evacuated silica tubes, with one intermediate regrind-ing. The capsules were slow-cooled to room temperature in the furnace. Samples for X-ray diffraction were prepared by placing powder on a glass slide with vaseline. Dif- fractometer traces were obtained on a G.E. XRD-5 diffractometer using a chromium tube and vanadium filter (40 kv and 31 ma). The size of the spinel unit cell was determined from the eight highest angle peaks (80 deg < 2b < 160 deg). Calculated lattice parameters were plotted vs cos B . ctn 0 and extrapolated to 6 = 90 deg. Measurements of the magnetic susceptibility were carried out at room temperature using the Faraday method in a magnetic field of 3000 G and using a Cahn RG automatic microbalance. The system was calibrated from the well-established susceptibilities of platinum and palladium: (Xpt = 0.968 x 10-6 g-1 and Xpd 7 5.04 x 10~6 g-1). The weight of samples were approximately 0.200 g. X-ray diffraction patterns for unsintered mixtures showed Bragg peaks from both the spinel (CoCr2S4) and monoclinic (NiCr2S4) structures. After sintering no monoclinic peaks were observed in samples containing up to 40 mol pct NiCr2S4. However, the spinel peaks were displaced to higher angles with increasing

Jan 1, 1970