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By D. V. Doane, G. A. Timmons, W. G. Scholz

Molybdenum of high purity can be produced by direct dissociatiott of commercial molyhdenm disulfide in vacuo at 1600° to 1700°C (2910° to 3090°F). The Product is lower in oxygen than commercially available molybdenzdm powder. Analyses of ingots arc-cast from commercial molybdenum powder, hydrogen-re-cluced from animonium molybdate, and from thermally dissociated molybdenum disulfide indicate that the levels of chemical impurities in these ingots are similar. Equipment now in operation will produce 100-lb hatches of powder product. The paper describes development of processing equipment, control of processing varzahles, handling of the product, and evaluatiotl of the melal produced. MOLYBDENITE (molybdenum disulfide) can be decomposed by heat in the absence of oxygen to produce elemental molybdenum and sulfur, which is evolved as a gas. The temperatures required for the dissociation are above 1370°C (2500°F); the sulfur must be continuously withdrawn to permit the reaction to proceed to completion. This is accomplished by continuous evacuation of the thermal dissociation chamber and condensation of the gaseous sulfur in another part of the system. Cognizance of the fact that the dissociation takes place in two steps is important in controlling the process. Basically, the molybdenite dissociation process has two potential advantages as a method of produc- ing pure molybdenum: 1) The materials entering into the process contain little or no oxygen. Since the process is carried out in vacuum at high temperature, the quantities of interstitial oxygen, nitrogen, and hydrogen in the product should be very low. 2) The process is more direct than the commercia1 method of producing high-purity molybdenum. In the conventional process, molybdenite is roasted to molybdic oxide, the oxide is purified first by sublimation, then by conversion to ammonium molybdate, and finally, the molybdate is reduced in a hydrogen atmosphere (usually in two steps) to the metal lic molybdenum powder. This paper presents a description of the stages in scaling-up of the dissociation equipment and an account of attempts to evaluate the molybdenum produced by thermal dissociation, rather than a report of a fundamental study of the dissociation reaction. Since little has been written on the subject, it is appropriate, before detailing the development of the process, to review briefly the research that has been conducted over quite a period of years. LITERATURE SURVEY The first accounts of the possibility of thermal dissociation of the mineral molybdenite were re-

Jan 1, 1962

By O. B. Ellis

Although thousands of tons of stainless steel have been used successfully for many types of equipment, there have been few cases of failures due to the phenomenon described as stress corrosion cracking. During the past seven years only six cases of such failures have been drawn to our attention and investigated in the Research Laboratories with which the author is associated. These failures oc¬curred in two coffee urns, two wool con¬ditioning units, one dyeing machine, and another in a part of a steam-jacketed stock pot. In each case the equipment failed in a comparatively short time after exposure to conditions of high humidity at tempera¬tures in the range of 100 to 200 F. The failures in all cases were characterized by general embrittlement and cracking of the stainless steel, with only slight indications of general corrosion except at the cracks. The first failure of this type was a coffee urn returned for investigation in 1937. The top and bottom sections showed a general corrosive attack and embrittlement and cracking of the stainless steel. The chemical analyses of these sections were as follows:

Jan 1, 1945

By Mehl, Robert F.

IT has been shown by numerous studies that the orientations of new metal crystals are determined by the orientations of the crystals in the original matrix, whether these new crystals are formed by recrystalliza-tion, by precipitation from solid solutions, or by transitions in the solid state. The orientations of crystals formed by recrystallization of cold-worked worked metals that bear preferred orientations are occasionally simply related to the initial preferred orientation; often, however, the relation-ship is not simple, but complicated and obscure in origin.1 The orientations of crystals formed by precipitation from solid solu-tions have been shown by many studies in this and other countries to be determined by the orientation of the crystals of the solid solution stable at the higher temperatures, though here again complicated cases have been found and no general theory is available .2 Related to this latter class

Jan 1, 1934

By E. T. Turkdogan, L. S. Darken, R. G. Olsson, H. A. Wriedt

Several aspects of the calcination of Michigan limestone were investigated: the rate of calcination of limestone spheres with diameters from 1.8 to 14 cm at temperatures from 800° to 1200°C by a thermogravimetric method; the temperature profile across limestone during calcination; the excess pressure developed in the interior of the stone during calcination; the pore surface area, pore volume, and effective gas diffusivity in burnt lime; and the microstructure of polished and fracture surfaces. It is found that, over a wide range of experimental conditions, the difference between the surface and center temperatures remains essentially unchanged during the latter half of calcination. From the rate of weight loss after about 50% calcination, the value 0.00126 cal per cm sec degree is found for the effective thermal conductivity of burnt lime. From the excess internal pressure measurements, i.e., 0.4 to 6 cm Hg at 800° to 1200°C, the permeability of burnt lime is estimated to be within the range 8 X 10-' to 5 X 10' sq cm. With increasing temperature and time of calcination, the pore structure of burnt lime coarsens as indicated by a decrease in the pore surface area, pore volume, and an increase in the average pore size. For the temperature range 600° to 835°C the ratio (effective gas diffusivity/molecular diffusivity) is about 0.18.

Jan 1, 1974

By Alexander R. Troiano, Eugene P. Klier

SINCE the very early work on quenched structures, where the products of the martensite transformation had been recognized, this transformation has provoked much interest and study. Theoretically it was desirable to account for the extreme changes in physical properties resulting from the formation of martensite, as that information might lead to results of practical importance. Desirable information, therefore, was on the kinetics of transformation from austenite to martensite as well as on the physical constitution of the martensite. It has been known for years that certain steels quenched to room temperature will contain persistent austenite as well as martensite. Other important and now well- established features of the martensite reaction are the progress of the reaction on cooling only and the independence of Ar" with cooling velocities exceeding the critical velocity. These facts have been experimentally determined by various methods and investigators. Notable among the early investigators were Tammann and Scheill and Wever and Engel.2 Unfortunately, all investigators did not fully interpret their results, which, coupled with several investigations that yielded conficting results, caused a state of confusion that was not clarified until quite recently. X-ray investigations of martensite in steels3-6 indicate it to be a supersaturated solid solution of carbon in alpha iron. This supersaturation is evident from the appearance of a body-centered tetragonal structure with the addition of sufficient carbon. The dimensions of this tetragonal structure are alinear function of the carbon content within the limits of accuracy of the determinations. Slight tempering of tetragonal martensite leads to the destruction of the tetragonal structure, which is converted to a body-centered cubic structure. This phenomenon has precipitated a controversy concerning the nature and mechanism of the tempering of martensite. The facts in the case have been outlined by Epstein7 and more recently by Antia, Fletcher, and Cohen.8 The significance of Ar" on theoretical grounds is not clear, however, although considerable study has been devoted to its determination. The precise position of Ar" as a function of carbon content was first stated by Greninger and Troianos for steels covering a range of approximately 0.7 to 1.8 per cent carbon. The effect of alloying elements on Ar" has recently been the subject matter of investigation by various methods.

Jan 1, 1945

By Daniel Martin

THE dendritic pattern of steels shown by deep etching is used exten-sively as a guide in the inspection and control of the great majority of steels used in ordnance construction and for many applications in indus-try. The value of macroexamination lies in the fact that it enables a qualified observer to make deductions concerning the general quality of relatively large pieces of metal. Not the least of these general character-istics is the nature and extent of the dendritic segregation in the steel, either in the cast condition or after mechanical or thermal treatments. PREVIOUS WORK Detailed methods for macroetching were outlined by Yatsevitch1 and have been standardized by the American Society for Testing Materials. A comprehensive study of the occurrence, origin, and the chemical and crystalline nature of the dendritic structure was given by Keshian.2 The marked persistence of dendritic segregation in nickel steels is fully recognized and has been discussed by Sauveur and Reed' and by others. Very little, however, has been written on the effect of the various elements on the macrostructure of steels, and the purpose of this report is to submit evidence concerning the influence of chromium, nickel and molybdenum on the macrostructure of some 4 by 4-in. ingots cast and treated under closely controlled conditions.

Jan 1, 1939

By Stirling Huntley, L. G. Huntley

THE controversy regarding the ,'probable future of the Mexican oil fields, and its relation to the oil industry of the United States, has led to the preparation of this paper. As has been predicted by several writers in recent papers, certain of the producing areas in the so-called "southern fields" in the Tampico Embayment have only a limited oil reserve. These areas are being pulled on by every pipe line in that region, and the length of time that they will continue to produce is a direct factor of the daily oil shipments of these companies. However, this is not the whole story, and in the following paragraphs an attempt will be made to show that the life of Mexican oil production will be a long one, and Mexican oil will continue to be a large factor n the market for an indefinite time after the areas mentioned above have been drained. The past and present producing fields will be discussed separately, in order-to establish a basis for comparison, the ,only method by which underground reserves 'can be estimated in these fields.

Jan 1, 1921

By Max Heberlein, R. P. E. Hermsdorf

The electrolytic refining of metals for the removal of undesirable impurities has become a recognized necessity in the nonferrous field. Copper, lead, zinc, nickel, silver and gold have been produced in this manner for years. The United States Metals Refining Co., realizing that considerable quantities of lead and tin could be made available to the trade if a satisfactory method of purification of these metals could be established, decided to investigate the possibilities of electrolytic solder. In cooperation with Dr. Edward F. Kern, of the School of Mines at Columbia University, the company developed a process of electrolytic refining of lead-tin alloys using a tin-lead fluosilicate electrolyte. A pilot plant was installed in November 1927, and the commercial unit was put in October 1929. Since that time thousands of tons of electrolytic solder have been produced in this plant and consumed by all branches of industry that use solder. Older Methods of Producing Solder In the early days practically all solder was made by melting together virgin lead and tin in the proper proportions to meet specifications; then the solder was cast into the commercial shapes required. Today the base of most solders comes from scrap or secondary materials. Ordinarily solder is produced from secondary materials either by sweating solder-bearing scrap or by smelting lead and tin-bearing drosses, residues and similar materials. When solder is produced from scrap by sweating, clear solder is collected directly. It is then given some kind of kettle refining and usually blended to specification with virgin metals before it is cast into finished shapes. In producing solder from drosses and residues, the materials are usually first given a reducing smelting treatment from which a crude solder is obtained. This crude solder may be refined in several ways, but usually the first step is a furnace liquation to remove the bulk of the copper, which is followed by one of the more or less complicated methods for the removal of antimony and other impurities.

Jan 1, 1937

By Pope Yeatman

In my experience, perhaps the most interesting problems came up during the testing, prospecting, developing and equipping of the Chuquicamata and Braden Copper Mines in Chile, and it is proposed in this article to give as briefly as possible what some of those problems were, their solutions, and the decisions made as to the different methods to be employed. The romance of mining is still a great lure to the young man who is making a choice of a profession to follow. The thought of travel to strange and out-of-the-way places, the glamor of pioneer life, the excitement of discovery, the constructive work of building something, entirely "from the grass roots up," or of reconstructing a played-out property and making a success of it-all of these phases have a strong appeal and often influence the young man in the choice of mining as a profession. That great engineer, Col. Seeley Wintersmith Mudd, whom we are endeavoring to honor, while having too much common sense to have been materially influenced by the romance of mining, certainly experienced all of the

Jan 1, 1932

The function of a preposition is to show the relation of one thing to another; it is necessary therefore for the writer to select the preposition that indicates the particular relation, otherwise he will fail to express himself clearly. Is it against common sense &o suggest that a Government is justified, morally as well as constitutionally, in preventing the decay of an industry by insisting upon the amalgamation of the prosperous with the needy? All these seven prepositions are used correctly. With the first dredge introduced in Russia, of Werf Conrad, Haarlem, make, this method of alluvial mining became important. Here the prepositions "with", "in", and "of" are used wrongly. He means: "This method of alluvial mining sprang into importance shortly after the first dredge, made at the Werf Conrad, Haarlem, was introduced into Russia." The statement itself is not true, but for that I am not responsible. Once, while I was serving with him, we were frozen in out of sight of land in the Gulf of Pichili in the North of China. Admiral Fisher wrote thus. He has used nine prepositions in making this brief statement. The sequence of three prepositions "in out of" is particularly awkward. Lounsbury says : One might fairly infer from the way in which it [newspaper English] is often spoken of that with the steadily increasing circulation of this sort of periodical literature there is no hope whatever for our speech. "Of that with" is lamentable. The construction is thoroughly bad, and it is bad mainly because the misplaced prepositions have tangled the meaning. I suggest:

Jan 1, 1931

By H. A. Wheeler

History ILLINOIS has so recently attained the third place in the oil production of the United States that few realize its great importance, or are aware of its highly profitable character. Since 1907 Illinois has furnished about 15 per cent. of the United States output and about 10 per cent. of the world's production. The value of the output in 1913 is estimated at $30,000,000, of which about $20,000,000 is profit. The present prosperity dates from 1905, but efforts have been made since 1865 to develop production and geologists have been very sanguine as to its future for over 25 years. Had the oil operators been as confident as the geologists, the field would have been opened at least 30 years earlier. For the rich Eastern Illinois oil field is located along the La Salle anticline, that was mapped 46 years ago by Professor Worthen in the

Jan 5, 1914

By J. F. Breedis

The morphology and crystallography of marten -site formed during quenclzing were examined by transmission electron microscopy in alloys whose compositions lie between Fe-19 wt pct Cr-11 wt pet Ni and Fe-33 wt pet Ni. Depending upon composition, four types of transformation products were observed in this portion of the Fe-Cr-Ni system. Three of these products are denoted as lath, plate, and surface martensite. The hcp structure found in association with martensite it? certain higlz-clzromium stairzless steels does not influence the transformation crystallogyaphy and cannot he Considered to act as a transitional structure in the transformation from austenite to martensite. DISTINCT changes in the characteristics of mar-tensitic transformations are produced by the partial replacement of nickel by chromium in austenitic iron alloys. Large, discrete martensite plates form in Fe-30 pct Ni, while aggregates of small crystals form in sheets parallel with (111)A austenite planes in stainless steels containing in the vicinity of 18 pct Cr and 8 pct Ni. These transformation structures are termed plate and lath martensite, respectively. In addition, an hcp structure (E) has been observed in certain high-chromium stainless steels in association with martensite. It has been suggested that the E structure acts as an intermediate step in the nucleation of martensitel-' and influences the morphology and crystallography of the final transformation product. However, this structure may be the consequence of the deformation of austenite arising from the shape distortion accompanying the transformation to bcc martensite.' An hcp stacking of atoms is produced in an fcc lattice by the introduction of an intrinsic stacking fault on alternate (111)A planes. At present, the arguments behind each explanation for the E structure are based on circumstantial evidence. This investigation seeks to determine the importance of the hcp structure to the martensitic transformation, and to examine the crystallography and morphology of the structures produced in bulk samples by quenching in alloys whose compositions lie between Fe-19 wt pct Cr-11 wt pct Ni and Fe-33 wt pct Ni. These aspects of the martensitic transformations occurring in these alloys have been studied by electron metallography and selected-area diffraction of foils examined in transmission in the electron microscope. EXPERIMENTAL METHODS The alloys have been prepared from thoroughly mixed powders of pure iron (99.6+ pct, 0.06 max pct C, 0.15 max pct N), chromium (99.9+ pct), and nickel (99.9+ pct). After sintering in an Ar-H2 atmosphere, the mixtures were melted by induction heating in recrystallized alumina boats under purified argon. The ingots were cold-rolled to 0.4-mm sheets (100 pct reduction in thickness) after the removal of at least 1.5 mm from their surfaces by grinding. Three-millimeter discs were punched from the cold-rolled sheet and annealed at 1150°C for approximately 24 hr in evacuated quartz capsules. The average grain size was 40 µ Thin foils for examination in transmission in the electron microscope were prepared from discs quenched to liquid-nitrogen temperature. A depression was first jet-machined into the center of a disc and a thin area (less than approximately 3000A in thickness) was produced at the base of the depression by electropolishing. Electron-microscope studies utilized the RCA EMU-3 and the Philips EM-100B microscopes operating at 100 kv. X-ray examination of the polycrystalline alloys was performed either in a diffractometer or in a

Jan 1, 1964

By David M. Cregger

The performance of the nation's first geologic repository for Commercial High Level Waste will be evaluated in a variety of ways which will involve the use of the state-of-the-art thermomechanical computer codes. Elastic properties of the host rock and the materials surrounding the repository are required for this numerical modeling effort to assess both near- and far-field effects. Only limited laboratory testing is possible, however, making it extremely beneficial to expand the data base by calculating dynamic elastic properties from available geophysical well logs. Elastic theory dictates that for an isotropic solid there are only two independent variables in addition to mass density, namely the compressional velocity, the shear velocity, and Poisson's Ratio. Compressional velocity and density are readily measured by geophysical well logs or in the lab; the crux of the solution requires measuring or determining either the shear velocity or Poisson's Ratio. Examination of acoustic propagated shear waves measured during confined compression testing demonstrates that Poisson's Ratio is a fundamental lithology-dependent parameter. Once a rock mass is appropriately classified, application of the laboratory derived dynamic Poisson's Ratio will yield a continuous and reasonable in situ modulus from acoustic and density logs. For preliminary characterization and assessment of the mechanical properties of rocks within the subsurface, and for studies of rock quality, this method is sufficiently accurate. The general availability of acoustic and density logs from wells logged for other purposes has made the application of this method desirable.

Jan 1, 1984

By COURTNEY DE KALB

IRON ore is the cause of the present trouble in Morocco. At least three nations are interested in the outcome and private syndicates have been active. The iron deposits are found in that mountainous northern coast line known as the Rif. This is an uplift that has been cut through, by the northward drainage, representing an ancient land surface. Erosion has produced .a fiordlike coast, which circum- stance has aided contraband' traffic to the tribes dominated by Abd-el-Krim, the chief of the clan of the Beni Urriaguel, near the center of 'the north coast, opposite Alhucemas. The iron deposits are extensive in the territory of the Beni Urriaguel. They were "located," if such a term is permissible, many years ago. The first arrangements, through direct contracts with the tribal chieftains, have been reinforced by compliance with the subsequent code under the Spanish protectorate in 1914. Under those terms, the location had to be made through the Arbitral Commission sitting in Paris. These locations, or "denouncements," were made by the I-louse of Mannesmann, of Hamburg.

Jan 1, 1925

By Langtry E. Lynd

The predominant tonnage use of titanium is as a white pigment, in the form of rutile or anatase, which are allotropic modifications of titanium dioxide. Because of its whiteness, high refractive index and resulting light scattering ability, titanium dioxide is unequaled as a white pigment for paints, paper, rubber, and a wide variety of other materials. Consumption of titanium dioxide pigments for these uses has been rising steadily for many years, United States consumption in 1956 amounting to about 486,000 tons, worth $250,000,000. Production was off a little in 1957 and 1958. An outstanding development in the titanium field in recent years is the expansion of titanium metal production. Virtually nonexistent before 1948, United States production of pure titanium metal sponge reached a high in 1957 of about 17,200 tons, worth about $77,000,000. United States titanium sponge metal production in 1958 was cut back to about 4,600 tons because of reductions in military requirements. Another major use of titanium, in the form of the mineral, rutile, is for welding rod coatings. United States consumption of rutile for this purpose in 1958 amounted to about 11,000 tons, worth $1,100,000. Titanium-Bearing Minerals Although several minerals contain titanium as a major constituent, only a few of these occur in sufficient quantities and concentrations to be of commercial importance. These are ilmenite (FeTiO3), rutile (TiO2), and alteration products of ilmenite which have been referred to as weathered ilmenite, leucoxene, or arizonite. The other polymorphs of titanium dioxide, brookite and anatase, occur in a few deposits, of which only one has been of even minor importance. Considerable concentrations of titanite or sphene (CaTiSiO5) and perovskite (CaTiO3) are known, but do not compete with ilmenite and rutile deposits in grade or size. Rutile is very widely distributed as an accessory mineral in most rocks, but large deposits of commercial importance are rare. A few rock deposits have been worked for rutile but only one, in Virginia, is in operation (1959). Development of one in Mexico was discontinued recently. At present, the main sources of rutile are the beach and dune sands of Australia and Florida. A major use of rutile is for the manufacture of titanium tetrachloride, which is the intermediate compound universally used in titanium metal manufacture. Another main use of rutile is for welding rod coatings. Although the whiteness and brightness of titanium dioxide pigment is due to the high refractive index of rutile or anatase, natural rutile is too impure to be used directly as a white pigment, is too expensive to use for manufacturing pure oxide pigment, and is too scarce to provide the required tonnages. Instead, the cheaper, more abundant, mixed oxide of iron and titanium, ilmenite, which is readily decomposed by sulfuric acid, is used for manufacture of rutile and anatase pigments. Ilmenite is mined from both rock and sand deposits. Rock deposits contain ilmenite in massive or heavily disseminated form along with magnetite or hematite and are almost invariably associated with anorthositic and gabbroic rocks. Ilmenite also occurs as an accessory mineral in a great many igneous and metamorphic rock types. Concentrations of

Jan 1, 1960

By E. H. Sellards

Phosphate rock like other mineral substances is found in nature in varying degrees of purity.

Jan 1, 1915

By Charles W. Carter, Alfred H. Bell

In 1943, Illinois produced 82,256,000 bbl. of oil, or 5.5 per cent of the total for the United States, and ranked sixth in the nation in oil production. This represents a decline of 23 per cent from 1942, when the total Illinois production was 106,ggo,o~~ bbl. and Illinois ranked fifth. The daily average production for 1943 was approximately 225,000 bbl. Daily averages by months were as follows: Jan......... 238,000 July......... 218,000 Feb......... 240,000 Aug......... 216,000 Mar......... 237,qoo Sept........ 220,ooo Apr......... 230,000 Oct......... 220,000 May....... 221,000 Nov......... 223,000 June......; . 222,000 Dec......... z18,ooo This shows that most of the decline during the year took place between March and May, and that for the last eight months of 1943 production has been essentially steady. This means that there has been enough production from new wells drilled to balance the natural decline of the Older wells. The trends of drilling and production are shown in Fig. I and Table 3.

Jan 1, 1944

By Bruce N. McIver, Leo Casagrande

Similarities are noted in the practices and problems of constructing dams to impound mine tailings, fly ash, and chemical wastes. The comparison of a typical tailings dam with a conventional water-retaining earth dam shows that the former is inherently less stable and can be susceptible to cracking, liquefaction, erosion, and frost action, as illustrated by examples. Several methods are presented for building safe tailings dams using either the coarse fraction of the tailings or local soils, the important factor in each method being proper compaction of the material. The safety of existing tailings dams can be improved by flattening the overall slope, preferably by adding berms, or by decreasing the height. Where neither remedy is possible, the installation of electro-osmotic tie-backs is suggested. Dumps of mine spoil can be stabilized economically by compacting the material in layers along the toe to form a dam.

Jan 1, 1971

By H. O. Hofman

In the blast-furnace smelting of lead, copper and other non-ferrous metals, the largest part of the product obtained is slag. Its formation consumes more of the heat-energy of the fuel charged than any other chemical reaction that takes place. It is therefore of importance to know at what temperatures the different slags will form, so as to be able to choose in a given case the slag that will form at the right point in the operation, will keep the products thoroughly fluid, so as to insure a satisfactory separation, and will permit the consumption of fuel to be reduced to the lowest practicable point. While practical experience has brought out in a general way the leading differences as to the formation-temperatures of Rome silica—iron —lime slags, accurate details are still wanting. The object of the investigation here described was to supply some of these.* Prominent among the men who have worked on the fusibility of silicates are Lampadius, † Sefström,‡ Berthier,§

Jan 1, 1900

By Alfred H. Bell, Charles W. Carter

In 1943, Illinois produced 82,256,000 bbl. of oil, or 5.5 per cent of the total for the United States, and ranked sixth in the nation in oil production. This represents a decline of 23 per cent from 1942, when the total Illinois production was 106,ggo,o~~ bbl. and Illinois ranked fifth. The daily average production for 1943 was approximately 225,000 bbl. Daily averages by months were as follows: Jan......... 238,000 July......... 218,000 Feb......... 240,000 Aug......... 216,000 Mar......... 237,qoo Sept........ 220,ooo Apr......... 230,000 Oct......... 220,000 May....... 221,000 Nov......... 223,000 June......; . 222,000 Dec......... z18,ooo This shows that most of the decline during the year took place between March and May, and that for the last eight months of 1943 production has been essentially steady. This means that there has been enough production from new wells drilled to balance the natural decline of the Older wells. The trends of drilling and production are shown in Fig. I and Table 3.

Jan 1, 1944