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By M. E. Steidlitz

FABRICATION of semiconductor devices.requires the formation of electrical contacts, often involving the use of lead, tin, and lead-tin solders. In several recent instances when germanium had been bonded to nickel with lead, a new metallic phase appeared, unattached to either germanium or nickel, but rather suspended as a continuous foil wholly contained within the lead matrix. Since such metallic structures do not form in nickel-lead or lead-germanium systems under identical conditions, a brief study was made of the characteristics and possible formation mechanisms of this material. EXPERIMENTAL Specimens were prepared by placing single crystal, transistor-grade germanium discs, 30-mils in diam by 6-mils thick, into a depression in a graphite boat. =A* nickel washers, 125 mils in diam by 5-mils thick, containing a center hole of 10-mils diam, and coined into a soup bowl shape, were loaded on top of the discs, so that the bottom of the

Jan 1, 1959

By Stanley J. LeFond

Brazil is one of the most outstanding examples of economic development of our time. Its amazing growth record is substantiated by a GNP which has increased at an average rate of 92% for the period 1968-1970 and estimates for 1971 range from 11.7-12.5%. Hence, this growth, coupled with a more relaxed attitude of the Brazilian government towards foreign participation in business opportunities and the remittance of profits out of the country, has caused many exploration companies to reevaluate the potential of Brazil. Despite recent press notices and publicity, Brazil is still not a mining country in the tradition of Canada or Australia. It is still basically an agriculture and manufacturing country.

Jan 11, 1973

By H. M. Otte, A. G. Crocker

SLIP, twinning, stacking faults, and precipitates on well-defined planes in a crystal produce traces that are visible on either a polished or an etched surface. The purpose of this note is to establish the usefulness and limitations of the information obtained from such traces when determining the orientation of single crystals or grains in a polycrystal. Attention will be confined specifically to traces produced by octahedral planes in cubic crystals, though most of the remarks can be taken as more generally valid. The problem of determining the crystal orientation is completely solved in principle' and in particular for the special case under consideration.1'2 Tables are available3 in which the orientations can simply be looked up when given the two or three angles between the traces. Thus a quick and simple method is available for obtaining the orientation of a crystal from surface traces. In this note two examples will be given from recently published papers and will show the use of the method with the aid of the Tables, as well as some of the precautions that should be taken in the procedure. As part of an analysis of X-ray Kossel lines, Peters and Ogilvie 4 determined from them the crystallographic orientation of the specimen. They chose a Cu-5.10 wt pct Si alloy that had been partly transformed from the a (fee) phase to the k (hcp) phase. The latter formed as very straight platelets along the octahedral planes of the a phase, and a photograph (Fig. 7 of Ref. 4) was reproduced in the paper4 of the region for which the orientation had been determined from the Kossel lines. Apart from a very small area (about 0.15 mm diam) near the top center of the photograph, the region shown was clearly all of one orientation. Traces in four different directions were readily identified. Starting with the smallest angle and proceeding counterclockwise, the angles between the traces were measured to be 27° 43', 55° 16', 64 3 43 1, and32"26'. These add up to 1802 08 1, indicating a cumulative error of 8'. The correct values should, of course, be taken from the original glass plates, or at least from prints on distortion-free paper, so the precision of the quoted values is actually greater than their accuracy. The solutions can be looked up in the Tables3 in four ways, depending on how the angles are paired, tion for the minutes of arc is required and the solution obtained will be identical for all the four pairs if the values of the angles are not in error. In a practical situation, such as this one, there are several sources of error, so that the four solutions obtained will all be slightly different. An arithmetic average of the four solutions is mathematically incorrect, but may, in special cases, give an answer close to the correct one. A rigorous procedure for refining the orientation has been described by Mackenzie;5 he gives a least-squares method that can be applied, if necessary, to this type of problem. The orientation thus determined can be compared with the one from the Kosel lines and discrepancies larger than the experimental error assigned to nonor thogonality of the X-ray or electron beam to the specimen. Here the example will only be used to illustrate the general procedure for making a very rapid rough check. From measurements on the stereographic projection, Fig. 9 of the paper,4 we can determine that the surface normal is approximately (0.434, 0.704, 0.562). From the Tables3 we find, using 28°, 55" as a good approximation to the first pair (27°43', 55°16'), that the surface normal is (0.453, 0.678, 0.579).* These two values are within 2 deg of each

Jan 1, 1967

By Frank B. McKune

This is something new in my life. A lot of you men here today I do not know, and some I do know. So if you have any remarks to make, I wish you would give your name and the name of your company. This is the first Acid Meeting which has been held under the auspices of the National Open-Hearth Steel Conference, and I hope it is a success. Whether it is a success or not depends entirely upon the support we get. If it does get good support, I have the idea it will be continued as a regular feature of the National Open-Hearth Steel Conference. We all think we have pretty good practices. But we can all learn and I hope that you, gentlemen, who take issue with the things someone else has said will stand up and give your opinions. Otherwise, the meeting will fall rather flat, and we won't get a great deal out of it; and there will not be enough interest shown by the National Committee to continue to place the meeting on the regular yearly program.

Jan 1, 1940

Discussion of the paper of Robert Henry Lee, presented at the New York Meeting, October, 1913, and printed in Bulletin No. 82, October, 1913, pp. 2515 to 2522. J. E. JOHNSON, JR., New York, N. Y.:-This subject is of great and increasing importance, as the exhaustion of the deposits of ore of ideal character compels the iron industry to turn more and more to those which are less desirable on account of physical structure as well as analysis. Thus there has come about the use of the Mesabi ores in this country and also of the Minette ores in Europe, which produce far greater percentages of flue dust than did the lumpy ores first used. It is a matter of common knowledge that the utilization of this flue dust, containing commonly 50 per. cent. or more of metallic iron, has been a problem very difficult and tedious of solution. The number and variety of the solutions now offered is a sufficient proof of this. . I have no intention of going into the merits or demerits of any of these processes as such, but there are certain considerations concerning the effect of their product on the operation and fuel economy of the blast furnace which I believe to be new and which I desire to bring out. There are two methods, so different as almost to be direct opposites of each other, whereby an ore may exercise an unfavorable effect on the economy of the blast furnace. The first of these is well known and results from the ore being refractory and highly resistant to the action of the reducing gases of the blast furnace. This results in its being incompletely reduced when it reaches the zone of fusion and in the reduction being finished by the direct action of carbon in the lower portion of the furnace. This is so well understood as to need little elaboration or comment. There is, however, another action which may be equally as fatal to the economy of the furnace as the foregoing, and as this point is, to the best of my knowledge, not generally appreciated, it is one upon which I desire to lay particular stress. This consists in the ore being, in a sense, too reducible.

Jan 12, 1913

By John V. Beall

During the last quarter of 1948, two new machines, which may revolutionize the coal mining industry, made their first public appearance within two months of each other. Both are designed to mine and load coal continuously. On Oct. 27, the "Colmol," invented by C. H. Snyder and A. E. Lamm, president and executive vice-president, respectively, of the Sunnyhill Coal Co., was demonstrated at the No. 8 mine of that Company at New Lexington, Ohio. The "Joy Continuous Miner," invented by H. F. Silver, president of the Silver Engineering Works, Denver, and developed and manufactured by the Joy Manufacturing Co., was demonstrated at the Mathies mine, near Finleyville, Pa., in the Pittsburgh coal seam.

Jan 1, 1949

By F. F. Poland

The purpose of this paper is to describe a new process for the refining of secondary copper-base metals and a specially designed high-temperature electric-resistor furnace used in the process for the distillation of zinc from these metals. The process was used for the conversion of nickel silver to cupronickel and to recover the zinc content in metallic form. It also proved applicable and economical for the treatment of scrap brass for separating and reclaiming the copper and zinc. The relatively large furnace developed for the distillation of zinc is described in detail, for it made economically possiblc the direct recovery of metallic zinc from scrap brass, which is a new step in the processing of such material. Considerable interest has been shown in the utilization of the distillation furnace for other metallurgical processes, where it is of advantage to operate in a controlled neutral or reducing atmosphere, or to avoid having the processed metal in contact with refractories other than carbon, or to operate at temperatures between 3000 and 4000°F. Purpose of Development It was recognized early in the war effort that nickel would become a critical metal. therefore all nickel stock and alloys containing relatively high percentages of nickel were frozen immediately. Among these alloys were considerable quantities of various grades of nickel silver, an alloy containing copper, nickel, zinc, and in some grades lead, also minor amounts of iron, manganese and other constituents. At the time there was no existing plant or process to eliminate the zinc, lead, and minor constituents so as to convert this metal to cupronickel, one of the important alloys needed by the U. S. Navy for condenser parts. Therefore the Bureau of Industrial Conservation of the War Production Board requested the executives of the leading nonferrous metal companies to have their metallurgical staffs study the problem of converting this metal to cupronickel conforming to U. S. Navy Specification 44T40. The composition specified therein is as follows: nickel, 29 to 32 per cent; zinc, 1.00; iron, 0.00 to 0.60; lead, 0.05; tin, 1.20; manganese, 0.00 to 1.00; total of other elemcnts (maximum). 0.50; copper, remainder. The problem in converting these alloys to cupronickel was the elimination of zinc, lead, iron, manganese, and other elements without appreciable loss of nickel to slags or other by-products. Revere Copper and Brass Incorporated, through its Research and Development Department, undertook to solve this problem. A Government-owned plant was built at Rome, N. Y., and there the conversion was made successfully.

Jan 1, 1949

By Harold M. Feder, Robert V. Schablaske, Irving Johnson, Ewald Veleckis

The stoichiometry, structure, and stability of the internzediate phases formed between zinc and some of the rare earth (RE) metals were systematically exarnined by means of a recording effusion balance and X-ray diffraction analyses. In the La-, Ce-, PY-, Nd-, and Y-Zu systems, at or below about 600 C, the following sequences of phases (REZnx) were found: La, x = 1, 2, 4.0, 5.25, 7.3, 17/2, 11, and 13.0;' Ce, x = 1, 2, 3, 11/3, 4.3, 5.25, 7.0, 17/2,* and 11; Pr,x = 1,2, 3, 11/3 ,* 4.3, 5.3(?), 7.0, 17/2,* and 11; Nd,x = 1,2, 3,* 11/3,* 4.3, 6.5, 8.5,* and 11; Y,x = 1,2,3, 11/3, 4.5, 5.0, 17/2,* and 12.* The structure types of all these phases were classified. In addition, lattice parameters were obtained for the first time for the pluses denoted by asterisks. In the absence of de tectable valency or electronegativity effects the systesnatic trends in the results have been ascribed to the effects of' the lanthanide contraction. For example, the maximum number of zinc atoms in the coordination polyhedron surrounding the RE atom decreases from twenty-four to twenty-two to twenty as the size of the RE atom decreases. THE structures and compositions of a great many intermetallic phases (e.g., the Laves phases) are known to be based primarily, but not exclusively, on the space-filling efficiency of various modes of packing together atoms of different sizes. The valencies and electronegativities of the constituent atoms are, however, also influential. In extreme cases hypothetical intermetallic phases which fulfill the efficient spacefilling requirements may not be present in the constitutional diagram because of thermodynamic instability brought about by the operation of valency or electronegativity factors. Hence, for a detailed study of the influence of atomic size on alloy structure and composition, it would be desirable to minimize variations of valency and electronegativity. The intermetallic phases formed by the rave earths (RE) with some common partner offer an excellent opportunity for isolating the effects of size from those of valency and electronegativity. The rare earths exhibit a large, but smooth, decrease in size (the lanthanide contraction) in the series from lanthanum to lutetium when inter comparison is made for a common valence state, e.g., isolated atoms or trivalent ions. The elements yttrium and scandium are frequently included as pseudo rare earths; their sizes place them in the vicinity of dysprosium and lutetium, respectively. The electronegativities of RE elements vary by less than 10 pet. The trivalent state is the most common; however, the well-known tendency of cerium, praseodymium, and terbium to achieve higher valencies, and of samarium, europium, and ytterbium to seek lower valencies, requires that caution be exercised in the assumption of equal valencies. In the present study the existence, constitution, and structure of each of the numerous intermediate phases formed by zinc with lanthanum, cerium, praseodymium, neodymium, or yttrium were examined systematically and in detail. The investigation was conducted by a recording effusion balance technique and by X-ray diffraction analysis. The results enrich our knowledge of the phase diagrams of these systems. In addition, they present some clear-cut evidences of the operation of the size factor alone. EXPERIMENTAL PROCEDURE Apparatus. The mode of operation of the recording effusion balance and its application to phase studies have been discussed in detail elsewhere.' In this work, an effusion cell containing a finely divided alloy was suspended within an evacuated tube from the beam of an analytical balance. The tube was immersed in a massive molten salt bath whose temperature was controlled to within 0.5o C during each experiment. The loss in weight of the alloy owing to effusion of zinc* was continuously recorded. Two effusion cells, 1/2 in. diam by 1 in. high, were machined from tantalum rods. Two orifices were drilled laterally into the walls of each cell. The orifice areas were determined by calibration with pure zinc: cell A had a total orifice area of 6.5 x 10-41 sq cm, and cell B an orifice area of 9.8 x 10-3 sq cm. By appropriate choices of orifice area and temperature the wide range of volatilities from pure zinc to pure rare earth metal could be investigated. X-ray diffraction powder photographs were made at room temperature with a 114.6-mm Debye-Scherrer camera with both filtered CuKa radiation and filtered CrKa radiation. Lattice parameters were refined by a computer-programmed least-squares analytical treatment which incorporated appropriate extrapolation techniques.2 Frequent use was also made of a special computer program3 designed to generate a powder pattern from an assumed structure in order to verify structural assignments. Materials. Lanthanum, neodymium, and yttrium were purchased from the Lunex Co., cerium from the Cerium Metals Corp., and praseodymium from the St.

Jan 1, 1968

By Thomas H. Leggett

IN speaking of the mining and economic conditions prevailing at the present time on the Rand, it is not my intention to go into the details of the mining-practice, since this has been already well described both in the Transactions1 and elsewhere,2 but rather to take a more comprehensive view of the industry and its surroundings as a. whole, marking its general development and the lines of its future progress. In a. paper entitled Deep-Level Shafts on the Witwatersrand, with Remarks on a Method of Working the Greatest Number of Deep-Level Mines with the Fewest Possible Shafts,3 presented to this Institute in August, 1900, I drew attention to the great cost of sinking the very deep vertical shafts that were then being seriously proposed as necessary for the development of the deeper areas, pointing out the strong advisability of working this ground by means of inclines to be sunk from the existing shafts of from 3,000 to 4,000 ft. in vertical depth. In this paper it is stated (1:). 975): "In short, practice upon the Rand now tends towards fewer vertical shafts and more underground inclines, especially for the very deep mining about to be undertaken." In consequence, the 6,000-ft. vertical shafts, at one time so much discussed, have never been started, and they do not now seem likely ever to be. The necessity of placing all deep shafts further apart in order to make them control and exhaust larger areas was also dwelt upon. This economy was vitally necessary for both 1 Gold-Mining in the Transvaal, South Africa, John Hays Hammond, xxxi., S17 to 855 (1901). R Engineering and Mining Journal, vol. lxxxv., p. 53 (1908). ' Trans., xxx., 947 to 987 (1900).

Jan 5, 1908

By M. N. Shetty, A. C. D. Chaklader

RECENTLY, it has been demonstrated that a considerable densification and interparticle bonding can be achieved if a pressure is applied to a powder compact while the material of the compact is undergoing either a decomposition reaction' or a polymorphic transformation.' The term "reactive hot pressing" has been coined to identify this process in which a phase change is combined with pressure to achieve interparticle bonding. This process is based on a principle which postulates that there is an enhanced reactivity and mobility of the molecular species at the phase-transformation temperature and this effect is utilized for interparticle bonding in powder compacts. This note summarizes the results obtained in an attempt to utilize this technique to produce ceramic-metal composites. In this case, a decomposition reaction of a compound (which after decomposition yielded an oxide) was used to achieve interparticle bonding in ceramic-metal composites. The reactive hot pressing was carried out in a Phillips induction heating unit, using either a graphite or a high-temperature steel die which functioned as both the susceptor and the hot-pressing component. The die was heated to the desired temperature in a helium atmosphere. All cermets produced by this technique were based on alumina as the ceramic phase. Different metal phases such as iron, copper, and chromium were used to study the effect of varying the metal phase on the properties of the composite. a Mono-hydrate (Boehmite) was mixed with different proportions of metal powders (-325 mesh) in dry condition in a mortar and pestle. No special precautions were taken for proper mixing. The mixtures were then compacted into a cylindrical form having an approximate dimension of 1 cm in diameter and 1 cm in height. For this compaction an ordinary

Jan 1, 1965

By John T. Eastlick

The Banner mining district is about 70 miles northeast of Tucson in the southern part of Gila County, Arizona. Production from the district, valued at about $26 million, is chiefly from copper-silver-lead zinc ores. The stratigraphic section consists of Precambrian conglomerates, quartzites, dolomites, and limestones, Cambrian quartzites; Devonian limestones; dolomites, and shales; Mississippian limestones; Pennsylvanian limestones and shales; and Cretaceous volcanic and sedimentary rocks. Deformation of these rocks presumably started near the end of the Cretaceous, and extended into the late Tertiary. The sedimentary rocks were folded, faulted, and intruded by fine grained diorite, quartz mica diorite, and dacite porphyry. At least four distinct stages of mineralization are recognized. In the first stage of contact metamorphism and the second stage of hydrothermal alteration, favorable zones were prepared for ore deposition. Metallization occurred in three of the mineralizing stages. Magnetite, pyrite, and hematite were deposited near the end of the second stage of hydrothermal alteration. The third stage included the main deposition of sphalerite, chalcopyrite, bornite, and galena. In the fourth and final stage, minor amounts of sulfide minerals were deposited with a late anhydrite and quartz gangue. The ore deposits in the form of veins and veinlets, pipes, irregular massive replacements, and bedded replacements are localized by the extent and distribution of metamorphic and hydrothermal alteration, by the proximity to the intrusive contacts, and by the effects of structural development. Oxidized ores of copper, lead, and zinc constituted the principal production of the district prior to 1940, but, for the most part, supergene enrichment was of minor economic importance. The ore bodies of the district are in the mesothermal class of deposits, occurring as normal metasomatic replacement and vein types.

Jan 1, 1968

By Herbert Clark Hoover, Lou Henry Hoover

As stated in the preface, the nomenclature to be adopted for weights and measures has presented great difficulty. Agricola uses, throughout, the Roman and the Romanized Greek scales, but in many cases he uses these terms merely as lingual equivalents for the .German quantities of his day. Moreover the classic language sometimes failed him, whereupon he coined new Latin terms adapted from the Roman scale, and thus added further confusion. We can, perhaps, make the matter dearer by an illustration of a case in weights. The Roman centumpondium, composed of zoo librae, the old German ceniner of 100 pfundt, and the English hundredweight of 1112 pounds can be called lingual equivalents. The first weighs about 494,600 Troy grains, the second 721,900, and the third 784,000. While the divisions of the centumpondium and the centner are the same, the Libra is divided into 12 unciae and the pfundt into 16 unizen, and in most places a summation of the units given proves that the author had in mind the Roman ratios. However, on p. 509 he makes the direct statement that the centumpondium weighs 146 librae, which would be about the correct weight if the centumpondium referred to was a ceniner. If we take an example such as " each centumpondium of lead contains one uncia of silver", and reduce it according to purely lingual equivalents, we should find that it runs 24.3 Troy ounces per short ton, on the basis of Roman values, and 18.25 ounces per short ton, on the basis of old German. If we were to translate these into English lingual equivalents of one ounce per hundredweight, then the value would be 17.9 ounces per short ton. [ ]

Jan 1, 1950

By Harrison Everett Ashley

(Pittsburg Meeting, March, 1910.) Slimes are usually defined as all material passing a certain-sized sieve, which is invariably the finest sieve employed by each metallurgist in his tests; 100-mesh and 200-mesh have been taken as the limits by different writers in recent volumes of the Transactions ; 150-mesh is common practice. The reader of the first two volumes of Richards 1 is impressed by the inflexibility with which all grinding-arrangements are praised or condemned according as they make little or much slime. Until recently, one of the principal aims of the mill-man was to keep down the slimes. He was obliged to have separate apparatus for sand- and slime-treatment. The latter was sometimes puzzling and erratic. Often it was found most .economical to omit treatment of the slimes entirely, or to store them in immense basins or heaps, waiting for possible future improvements in methods of treatment. Recently, improved processes of agitation and filtration have made possible the successful extraction of values from many slimes. The tendency, when the metal is exceedingly finely disseminated, is to cut out all sand-treatment and to slime everything. These processes have been almost entirely mechanical in their conception, and it is the object of the present paper to show that certain chemical considerations may greatly hinder or assist their successful operation. It has long been a source of dissatisfaction to chemists that their analyses fail to be of much help to the clay-worker; that it is a matter of common occurrence for clays of closely identical ultimate chemical constitution to show the widest possible divergence in physical properties. * Published by permission of the Director of the U. S. Geological Survey. Ore Dressing (1903).

Aug 1, 1910

By W. S. Tower

STEEL is the basic metal, the main metallic prop of the modern industrial world, a good gage for measuring the state of our complex economy. Any who had doubts on that score should have had them dispelled by the many evidences of public concern over the affairs of the steel industry in recent months. I do not need to relate the various criticisms of the industry, nor the questions about its policies and performance which have come in a rising flood, especially from unthinking and irresponsible sources. But judged from the standpoint of production, or from plans to improve and expand facilities, or from technical progress, the facts about the steel industry are proof of

Jan 1, 1948

By J. O. Betterton, W. K. Noyce

I~JTI HE work on the indium-zirconium system is part A of a larger investigation of zirconium-phase diagrams with solute elements, silver, cadmium, indium, tin, and antimony, which is intended to provide information about the metallic valency of zirconium. The system is an ideal example since the sizes of indium and zirconium atoms are nearly the same, and the solute and the solvent occur in the same row of the periodic table. The only solute from Group III B which had previously been added to zirconium was aluminum' and it was of interest to determine whether indium would dissolve appreciably in alpha zirconium and stabilize this phase in the same manner. Experimental Procedure The experimental methods used in the indium-zirconium work are similar to those described earlier for the silver-zirconium system.' Reactor Grade 1 iodide zirconium of 99.95 pct purity* and indium of 99.99 pct purity were arc cast, and then annealed in silica capsules with protective foils of zirconium and molybdenum. Annealing temperatures and times varied from 1 day at 1300°C to 43 days at 550°C. The compositions of the alloys were detcrmined by an individual chemical analysis of the actual metallographic specimens after two or more sides were examined to insure the absence of solute segregation. Calibrated thermocouples were used throughout, and the uncertainty in the temperatures reported, owing to calibration error, furnace control, and measurement of the small temperature gradients near the capsules, is believed to be well within ±2°C. Typical impurities in the alloys were found by a neutron-activation analysis of four different alloys. The results are given in Table I where the ranges of values will be seen to compare favorably with the usual values for iodide zirconium. With respect to oxygen, nitrogen, and carbon the absence of any unusual amount of these elements compared to iodide zirconium was indicated by the alloy hardness values, since hardness is increased sharply by the presence of these elements. The value for 0 pct In, obtained from the alloys by extrapolation, is 58 2 7 VPN which is in the low part3 f the normal range of hardness found in iodide zirconium. Results of the Experiments The zirconium-rich portion of the indium-zirconium phase diagram from the annealing experiments is shown in Fig. 1. Indium was found to

Jan 1, 1959

THE IRON HUNTER. By Chase S. Osborn, pp. 316, Ills. 10. The MacMillan Company, New York. 1919. An autobiography, the story of a Hoosier boy who fought his way to manhood and power through early misfortune and poverty, from street urchin and newsboy, to editor and author; from lumberjack and dock walloper to statesman and Governor of Michigan. The reader has the measure of the man in the first chapter, a dramatic recital of how the fighting boy editor cleaned up a lawless mining camp of 40 years ago. The thread of the narrative is the author's life-long devotion to outdoor living, ex-ploration and travel. Residing in Sault de Sainte Marie, Mich., in the heart of the Lake Superior country, he took his delight and, incidentally, found his fortune in prospecting the north woods for iron ore; eventually, extending his travels to the continents and many of the islands of the world, he discovered what, he believes-to be a great iron range in Madagascar. In this book there is plenty of anecdote, a great deal of wholesome social and po¬litical philosophy and some interesting sidelights on the characters of some of the author's prominent contemporaries in the political life of Michigan. The style is direct and animated, flavored and illuminated with the vernacular of Hoosierdom and the woods country of the North. The author levies on the vocabulary of the sciences and the classics for many a noun and adjective and, with Rooseveltian license, now and then coins a word. The reader's interest will be gripped from cover to cover, albeit he may occasionally need a dictionary. R. C. A.

Jan 11, 1919

By E. A. Gulbransen, W. S. Wysong

The behavior of molybdenum and its surface oxides in oxidizing and reducing gas atmospheres and in high vacua at elevated temperatures is a question of scientific and technical importance. The use of molybdenum as a metal or as an important component in alloys in oxidizing atmospheres at elevated temperatures has been limited because of the unprotec-tive nature of its oxide film and the volatility of this oxide at moderate temperatures. This communication will present results of a vacuum microbalance studyl, 2 of the following problems: (I) the oxidation kinetics in the temperature range of 250°to 450°C; (2) the reduction with pure hydrogen of thin oxide films formed on molybdenum; (3) the volatility of the thin oxide films; and (4) the vacuum oxidation of molybdenum at high temperatures. Molybdenum is an interesting metal to study for the following reasons: (I) although the oxide-to-metal-volume ratio is greater than one, the metal is not considered protective; (2) the metal oxidizes readily at temperatures of 2 50°C and higher; (3) the oxides of the metal are reduced at temperatures as low as 500°C by pure hydrogen; (4) the oxide Moo3 melts at 795°C; and (5) the oxides of molybdenum are volatile at moderate temperatures. The following variables are studied in the oxidation kinetics: time, temperature, pressure, surface preparation, surface area, concentration of inert gas in the lattice, cycling procedures in temperature, vacuum effect and high temperature vacuum oxidation. The general interpretation of many of these factors has been previously discussed. Literature The oxidation of molybdenum has not been studied critically. Although many studies have probably been made on the kinetics of the oxidation process, none has been reported in the literature available to us. The crystal structures found in the oxidation of molybdenum have been studied by Hickman and Gulbransen." Their results showed that Moo2 is the oxide which is stable in contact with the metallic substrate throughout the temperature range 300 to 700°C. As the film thickens in the low temperature range, MoO3 becomes predominant on the surface. Above 400°C, Moos is no longer observed, MoO2 being the only oxide found. Hagg and Magneli6 have shown from an X ray study that the a-phase, orthor-hombic Moo3 is stable up to 1050°C. Two other phases, ß and ß with compositions close to MoO2.90 are also obtained. The formula for the 0 phase is not given but that of the ß phase is defined as Mo9O26 The 0' phase is found to be built upon a monoclinic unit cell. A ?-phase is isolated from a preparation MoO2.75 heated for 17 hrs at 670°C. This phase is

Jan 1, 1949

By R. E. Ray, J. W. Stevenson, J. A. Berry

Conventional concrete block plastered with a cementitious coating is the most common material used in the construction of permanent stoppings to direct airflow in underground mines in the US. All mines experience various degrees of strata convergence depending on depth of overburden, geological conditions, and type of roof support employed. Strata convergence will cause cracks and joint openings in masonry stoppings, resulting insignificant air leakage losses. Where strata convergence is severe, complete structural failure of the stopping can ultimately occur. Reconstruction of damaged or destroyed stoppings adds expensive overhead to mining operations, and even greater expenses are incurred from the additional fan horsepower required to overcome leakage losses. Ideally, a stopping should maintain high resistance to airflow while yielding to strata convergence. By properly incorporating a polyisocyanurate rigid foam material within the masonry block structure, stopping service life can be increased in mines experiencing strata convergence problems such as floor heave, roof loading, and lateral rib movement.

Jan 1, 1986

By N. O. Taylor

THE failure, by swelling, of several cast aluminum-zinc, spiral, pump rods, used to circulate water in a constant-temperature bath, brought up the question as to whether the presence of tin in varying quantities would have any appreciable influence in controlling this action. Previous workers had found the same difficulty with aluminum-zinc alloys, due to their swelling in water or solutions of electrolyte^.^ It was known that pure aluminum was practically insoluble in concentrated sulfuric and nitric acids, presumably due to the formation of an oxidized film on the surface. Concentrated sulfuric acid had little or no effect on pure zinc and tin and concentrated hydrochloric acid would attack all three metals. These facts aroused curiosity as to the probable reaction of the ternary alloys of these metals, and tests were made to determine their resistivity to the action of common laboratory reagents. Samples, covering the entire range of the ternary series of aluminum, zinc and tin alloys, were made up from good grades of the commercial metals.2 The materials were melted, at as low temperatures as possible, in graphite crucibles in a gas-fired crucible furnace. Graphite crucibles were used in preference to clay, to prevent the absorption of silicon by the aluminum, as found by previous workers. The melted materials were stirred thoroughly with pine sticks in order to ensure complete mixing and the greatest possible freedom from oxidation, and were cast in sectional, iron molds giving bars % in. in diameter and 5 in. long.

Jan 1, 1927

By Harry C. Gatos, Frank J. Bachner, Mario D. Banus

The portion of the Nb-Sn phase diagram between 75 and 79 at. pct Nb at temperatures near the liquidus has been investigated by melting alloys of known composition and examining the microstmc-tzlres resulting when these melts were quenched. The Nb-Sn samples were contained in magnesia sleeves, and were mounted in a high-pressure apparatus. It was shown that Nb3Sn me1ts by a peri-tectic decomposition and that the composition of the compound Nb3Sn at the peritectic horizontal lies between 77 and 78 at. pct Nb. Analysis of the phases present in the samples was accomplished by anodic staining techniques and an electron-microbeam analyzer. DURING the past several years a great deal of work has been devoted to the Nb-Sn system, and the bulk of this work has been primarily concerned with the intermetallic phase Nb3Sn. However, the melting characteristics of Nb3Sn have not been investigated because of the difficulty in maintaining known compositions due to tin losses by vaporization, and the added difficulty of containing Nb-Sn alloys without sample-container reaction at the high temperatures involved. This paper reports on the development of a technique for containing Nb-Sn alloys under pressure high enough to prevent tin losses at temperatures in excess of the liquidus. Using this technique, melts of known composition were made and a phase diagram near the liquidus is proposed based on the microstructures resulting when these melts were quenched. EXPERIMENTAL The Nb-Sn alloys weighing 0.7 g each were prepared in the form of cylinders. Niobium powder, -200, +325 mesh, and tin shavings with a minute amount of tin powder for a binder were mixed in the desired proportions and cold-pressed at 50,000 psi in a 0.150-in. die. This cylinder was then enclosed as shown in Fig. 1, and the entire arrangement mounted in a 2.6-in. pyrophyllite tetrahedron.' The desired temperatures (-2500°C) presented several problems in high-pressure container materials. Boron nitride, the usual sample holder, was found to react with niobium to form the nitride. However, MgO cans and plugs machined from refractory rods did not melt nor react with the sample. Thick tantalum contact disks were used to carry the large currents (~450 amps) to the graphite heater, since tantalum did not melt and had enough strength to prevent extrusion of the sample. It was further observed that the graphite heater and tantalum disks could not be in direct contact with the pyrophyllite because it melts and decomposes at these temperatures to kyanite and coesite (SiO2),2 the former reacting with graphite and the latter with tantalum to form the silicide. The use of a MgO outer sleeve

Jan 1, 1965