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By Charles L. Hosler

My function here today is not to illuminate any particular subject but simply to welcome you to Penn State and to the College of Earth and Mineral Sciences. Our college is, of course, dedicated to the same thing to which most of you have dedicated your lives--the exploration of the earth, the extraction of materials from it, and the production of useful things from those materials. We have about 2,000 students engaged in studying in preparation for service in these activities at the present time. Like other colleges of our type, we've undergone a great expansion just at a time when university budgets are contracting. This creates an interesting situation as to how we can best use our resources. This, of course, is the thing a lot of you are going to be talking about here--how we can best use the world's resources. As you well know, the expectations of the people of the world are rising, and, with the numbers of people increasing and with finite resources, there never was a time in history when it was more important that we become "quantitative" in our discovery, estimation, extraction, and utilization of those resources. I think it is admirable and very timely that you are gathered together to discuss your various approaches to this particu¬lar problem of quantifying and making most efficient use of the resources of the world. Yours is sort of a hidden profession, not just because you actually go underground, but because the public in general is not aware of where the materials they use come from. If you are successful in your professions the public will continue to be unaware. Only if you fail will your essential function become patently obvious. I wish you success both in your professional pursuits and in this particular meeting.

Jan 1, 1977

By Reich G. Gaertner

Almost every mining engineer who has had charge of extensive underground workings will have observed how often directions as to course and levels, deduced from careful theodolite measurements, have been slighted or disregarded by mine-foremen and shift-bosses, and how often these tedious measurements had to be repeated, even for minor works, such as ventilation-drifts or winzes, in order to carry them on with the required or desirable regularity. Besides the time and care absorbed by theodolite surveys, there is still another inconvenience, namely, the interruption of transportation during the time of observation, and, in heavily producing mines, the loss consequent upon such interruption. In proposing a subsidiary instrument to the theodolite, it is my purpose not to present a new one, but simply to recommend to the consideration of American mining engineers one which has been in use in nearly all the prominent mines of Europe for many decades, and has there fulfilled its purpose admirably. I refer to the mining or hanging compass (Fig. 1). At my urgent request, the firm of Keuffel & Esser, of New York, have lately constructed this instrument in a form which adapts it better to use in this country. By the addition of the trigonometer, the banging compass becomes at once an instrument which will prove of value even in the hands of foremen and practical miners, who have little or no knowledge of trigonometrical calculations. Probably many will say that me have no use for needle-instruments ; that our modern theodolites are of such perfect description, and leave so little to be desired, that the introduction of a compass would look like a step backwards compared to the fine results obtained by angle-instruments. I concede all that, and do not pre-

Jan 1, 1886

By P. K. Weimer

Coinpletely integrated thin-film circuits inco?,porating more than 1000 active and passive elements have been fabricated reproducibly in the laboratory by evaporation of- all components. A 180-stage modified shift register comprising 540 CdSe TFT's, 360 resistovs, and 180 capacitors was deposited upon a glass substrate during one pump-down of the vacuum systeitl. Experimental units have been operated for more than 5000 hr at temperatures uP to 85°C without failure of any slages. The present pupper reviews the charvactevistics of evaporated thin-film transistors (TFT's) and discusses their application to integrnted circuils. INTEGRATED circuits most widely used today are based upon silicon technology, with the circuits formed on the surface of a block of single-crystal silicon1 or on a block of sapphire 2,3 upon which a thin layer of silicon has been deposited. Transistor patterns and interconnections are defined by photographic procedures using photoresist masking. Large groups of transistors are produced in batches which undergo many processing steps, some of which are carried out at elevated temperatures. Passive elements are formed by treatment of the semiconductor surface or are deposited by evaporation alongside the active elements. The size and complexity of the circuits are limited by defects in the devices and by the size of the available single-crystal chips. Capacitative coupling to the semiconducting substrate may also limit useful size and frequency response of the circuits. An alternative approach to integrated circuits is based upon the deposition by evaporation of all circuit components upon a noncrystalline, insulating substrate such as glass.4 Thin-film field-effect transistors,1'6 known as TFT's, can be deposited in large arrays on glass or plastic substrates at the same time the associated passive elements are being deposited. Although still in the research stage the all-evaporated approach is expected to offer certain advantages for many applications. In particular, the use of thin films upon a noncrystalline substrate offers the prospect of producing complex, large-area circuits not now feasible with single-crystal silicon. Important applications of this type include memory arrays for computers and imaging devices for television. The ease with which the evaporated TFT's can be deposited may permit continuous, automated production methods not possible with high-temperature batch processing. Recent advances7'8 in the fabrication of thin-film transistors have led to greatly improved reproduci-bility and life of the TFT's. Experimental circuits having over 1000 active and passive elements deposited upon a common glass substrate are currently being produced in the laboratory. The present paper reviews recent progress in the development of the TFT and in its application to integrated circuits. I) DESCRIPTION OF THE THIN-FILM FIELD-EFFECT TRANSISTOR The TFT is a field-effect transistor of the type having the control gate separated from the semiconductor by a thin insulating spacer. Although its operation resembles that of the silicon MOS transistorg its construction is based entirely on thin-film techniques. Fig. 1 shows a cross-sectional view of an evaporated TFT deposited upon a glass substrate compared with a silicon MOS transistor deposited upon single-crystal sapphire.3 The semiconductor in the TFT is a poly crystal line layer, of a material which can be readily evaporated, such as cadmium sulfide, cadmium selenide,l0 or tellurium." Silicon monoxide layers have usually served as the gate insulator, but other oxides, sulfides, and fluorides may be used. Film thicknesses range from a few hundred to a few thousand angstroms. The source, drain, and gate electrodes in the TFT are of metal. Qpical source-drain gap dimensions are 0.0003 x 0.030 in., with a gate strip whose width slightly overlaps the source and drain. The source and drain electrodes should make low impedance contacts to the semiconductor. With cadmium sulfide films, gold is a satisfactory material for underlying electrodes, while aluminum is preferable for overlying electrodes.12 Considerable variation in design of the TFT is permissible, with the electrodes being

Jan 1, 1967

By W. W. Stephens, W. J. Kroll, H. P. Holmes

THE only two methods for producing commercial quantities of malleable zirconium, up to now, have been using magnesium reduction of the anhydrous chloride under a neutral gas, and using purification of raw zirconium by the iodide dissociation method on a hot filament. The purity of the metal obtained by the latter process is about the same as that resulting from the chloride reduction, with the exception of the oxygen content, which may be about 0.05 pct lower in the iodide metal. Even traces of oxygen have a strong hardening effect on zirconium. Since, in the iodide process, the impurities, Si, Al, Fe, Ni, and Mg in the raw zirconium used, are carried over, it would appear uneconomical to use this method of refining solely to eliminate the traces of oxygen, unless very soft metal is desired. One important step to improve the iodide method, namely, dissociating pure iodide made from carbide and recycling the iodine, which would change this refining process into a method for extracting zirconium from the ore, has not yet been made. The Bureau of Mines, by using the chloride reduction, wanted to produce quantities of a reasonably pure and malleable metal at low cost for large-scale industrial use. This aim has been achieved, and a pilot plant permitting production of 600 lb of malleable zirconium per week will be described (fig. 1). Briefly, the Bureau of Mines process consists of reducing purified gaseous anhydrous zirconium chloride with fused magnesium under a noble-gas atmosphere. The reaction product, magnesium chloride, and any excess magnesium metal present are removed from the sponge zirconium in the next step by fusion and evaporation in a good vacuum at about 925°C. In this process, care is taken to keep air out of contact with the hot metal, which otherwise would contaminate the product with oxygen and nitrogen. Both these impurities embrittle zirconium even when present in an amount as low as 0.1 pct. A number of previous reports1-3 describe the method and the various improvements that finally led to a workable process. The major steps made were the production of large quantities of carbide, which is the raw material for producing the chloride, its chlorination with reasonable efficiencies, and the elimination of iron trichloride contained in the raw chloride, as well as that of the zirconium oxide which is always present in this product. The physical nature of the anhydrous chloride, which sublimes at 331°C at atmospheric pressure and melts at 420°C under a pressure of 25 atm, made it necessary to provide a special safety device on the purification and reduction vessels in the form of a lead-alloy seal, permitting escape of excess gases if pressure tended to build up. The main difficulties encountered in the reduction and in the following step, salt separation in a vacuum at elevated temperature, were caused by the material from which the reaction pot was constructed—iron. This metal reacts with zirconium at about 940°C with formation of a eutectic. The last step, salt separation by evaporation of the magnesium and magnesium chloride in a vacuum, is quite unconventional and has not been used before on such a scale. It is only due to the improved construction of high-vacuum pumps, especially oil-diffusion pumps, that such a method could be used. The various steps of the Bureau of Mines process, as described in the general outline above, may be summarized as follows: (1) production of the carbide, (2) chlorination of the carbide, (3) purification of the raw chloride, (4) reduction of the pure chloride with fused magnesium, (5) separation of excess magnesium and magnesium chloride in vacuum at elevated temperature, and (6) melting of the sponge obtained. Production of Carbide The arc furnace, described in a previous report,' was improved both to reduce the graphite consumption caused by the burning of the bottom plates and to concentrate the heat in order to obtain better power efficiency. This was achieved by providing the bottom with graphite plates entirely embedded in refractory bricks, the contact with the current being made with three water-cooled copper plugs. Figs. 2 and 3 show the arrangement. The crucible, made

Jan 1, 1951

With the signing of the armistice on Nov. 11, the direction of the main concentration of effort of the United States was changed. In order to win the war, all industrial efforts had to be organized and centralized. With the war won and peace in sight, this centralization of effort stopped and the full play of individual initiative was allowed to resume its sway in the community. During this period of reversal of direction of effort, there was a natural loss of momentum and the United States, as well as the rest of the world, is in for a period of readjustment. The immense progress that was made in one direction under the stress of the necessities of war, which focused the energies of a nation in one direction, is an outstanding example of what can be accomplished if a community with many varying interests can be united on one objective which it desires to attain. The realization that the fusing of many interests into one stream of effort is difficult should not prevent us from taking the long view ahead that is necessary in order to be able to measure the progress made. If we don't have a mountain peak to guide us, we are very likely to run in circles in the plain without reaching the goal to which we strive. The most efficient development of natural resources is an ideal that, from a material point of view, appeals to the engineer. This ideal includes giving of opportunities to everyone to take a share in the development of these resources.. It also contemplates rewarding foresight

Jan 4, 1919

By H. W. Gudenau, R. S. Chatty, W. Wenzel, M. Ponthenkandath

During several experimental programs conducted at the Institute of Ferrous Metallurgy, Technical University, Aachen, whisker formation was observed when iron ores were reduced at low as well as at high temperatures. Thus, in an attempt to find the reason for the volume change taking place during reduction, iron whisker growth was observed. Whisker growth appears to be one of the important reasons for the swelling of pellets. One set of experimental observations determined that when iron forms as needles rather than as a crust on the surface of oxide, the pellets became very porous. In related experiments, the beneficiation of finely disseminated iron ores, in which the metallic iron is separated from the gangue in granular or nodular form, was achieved by a reduction-concentration method. In this process, which is conducted at sufficiently high temperatures, oxide whisker growth, resulting from the formation of volatile suboxides and a gas transport mechanism, plays a vital role in the joint deposition of SiO, and iron from the vapor stage.

Jan 1, 1973

By R. R. Angel

Drilling rate is a parameter that should be considered in determining the volume requirements for air and gas drilling. The use of past methods which ignore the effects of the solids content upon the pressure and velocity of the annulus flow stream can result in undercalculation of the required volurne by as much as 50 per cent. A vertical-flow equation is presented for determining volume requirements. This equation includes the effect of the solids that are transported up the annulus in the flow stream by incorporating the drilling rate as one of the parameters. The effect of down-hole temperature on required circulation rates is also ana-lvzed. A simple approximate method of determining volume requirements is presented. This method is more accurate than the methods used in the past. Hole cleaning difficulties are analyzed for a recent air drilling job where past methods indicated that - excess air was being used. Sample curves of calculated boitom-hole pressures are presented for air and gas drilling in several hole sizes. INTRODUCTION In certain areas the use of air or natural gas as a circulating medium for drilling oil and gas wells is becoming a common practice. Large increases in penetration rate and bit life are achieved through the use of these media in preference to mud or water. Drilling rates as high as 90 ft/hr have been obtained in shales. The importance of maintaining adequate circulation rate is generally recognized; however, much disagreement exists among drilling operators as to what constitutes "adequate" circulation rate. In quarry drilling, where annular velocities can be accurately determined, an annular velocity of 3,000 ft/min of standard air is required for best results in rocks having approximately the same density as those commonly penetrated in drilling oil or gas wells'. Although this standard air velocity has proven satisfactory for quarry drilling, some oil and gas well drilling operators believe that an equivalent annular velocity of more than 4,000 ft/min is required; others believe that as little as 2,000 ft/min . is sufficient. Much of this disagreement results from determining the required circulation rates with methods which fail to incorporate the drilled solids in an equation which is applicable to vertical flow. Hughes Tool Co. Bulletins No. 23' and 23-A3 present data for determining circulation rates based on the Weymouth formula. These data do not include the drilling rate as a parameter and, therefore, neglect the effect of the solids being transported up the annulus. In spite of this apparent defect and the fact that the Weymouth formula is not applicable to vertical flow, the Hughes data have well served the drilling industry in many areas and are important and timely contributions to the science of air and gas drilling. The Hughes data purposely omit a correction for increasing down-hole temperature. At slow drilling rates this effectively compensates for the use of a formula which is not valid for vertical flow; however, volumes determined by the Hughes method are not sufficient to support rapid drilling rates at moderate and great depths. For example, Phillips Petroleum Co.'s Cauthorn "D" No. l in the Vinegarone field for Val Verde County, Tex., was air drilled from 1,500 to 9,300 ft using a compressor delivering 1,400 cu ft/min. The 8 3/4-in hole was drilled with 5-in. drill pipe, and drilling rates as high as 90 ft/hr were obtained between 7,000 and 9,300 ft. No water or caving hole was encountered. At 7,728 ft it was necessary to wash-out 60 ft of cuttings to reach bottom after a trip to change bits. At 8,130 ft a twist-off occurred and the drill col-lars were stuck in drill cuttings. These difficulties indicate that the 1,400 cu ft/min of air was not sufficient to keep the hole clean. Hughes data indicates that 1,180 cu ft/min is sufficient to produce an annular ve-

Jan 1, 1958

By E. C. van Reuth

FIFTY-three alloys have been examined in the Fe-W and Co-W alloy systems in an attempt to verify the finding of o phases in these systems as reported by Goldschmidt.' The alloys were examined metallographically and by X-ray diffraction. The 10-g specimens were made by powder metallurgy techniques. Very fine, high-purity powders were compressed in a double-acting die at 120,000 psi after hydrogen reduction. All compacts were then sintered for 200 hr at 950°C in a helium atmosphere. Metallographic investigation and X-ray diffraction proved this time to be sufficient to allow complete homogenization before the subsequent high-temperature anneal. Each specimen was then sealed into an evacuated silica capsule and annealed at 1400"or 1500 C (except two) for 25 hr. (The 60 pct Fe and 55 pct Co alloys taken to 1610"and 1680°C respectively were held at these temperatures for 1hr. However, since these structures were at equilibrium before the anneal, and in view of their resultant structures, it is assumed that they reached equilib-

Jan 1, 1960

By D. R. Bomberger, M. Deul

An automatic microscope has been developed to measure the size and populations of macerals and minerals in fine coal particles. Differentiations are made on the basis of reflectance. This study is concerned with the size distribution of pyrite inclusions. Most fine coal cleaning processes do not remove pyrite as completely as a straight density separation. Consideration of the pyrite size distribution is suggested as a more accurate method of predicting sulfur reduction by a cleaning process. Analyses of float-sink results and Deister Table operation in terms of pyrite particle sizes are made. Other potential applications of automatic microscopy are also discussed. In the study of coal cleaning by pseudo-gravity methods (tables, cyclones, hydrotators, etc.), it is customary to express the deficiency of the process relative to float-sink measurements in some form of "percent efficiency". These have been calculated in many different ways in order to provide a means of extrapolation of test data to untested coal feeds. This works quite well with coarse coal (here defined as larger than one-eighth in.). Large, heavy pieces of refuse are rejected rather thoroughly by many cleaning processes, and the efficiencies relative to float-sink results approach 100%. In coarse coals, the difference in the sizes of fine pyrite is masked by the averaging effect of the large coal envelopes. The existence and fate of fine pyrite is often hidden in the larger numbers representing coarse (and easily removed) pyrite. There are cases where it is desirable to subject fine coal (here defined as smaller than one-eighth in.) to cleaning processes. This is true of naturally occurring fie coal streams and in cases where comminution followed by cleaning is necessary to provide the quality desired. It is in this area that the use of process efficiency relative to float sink fails. Percent efficiencies decline to very low figures, and equivalent separation densities become a matter for conjecture. The net result is that an attempt to estimate product quality from float-sink data and a process efficiency figure often results in large errors. This work represents a new approach to the problem by observing the fate of pyrite particles, grouped by sizes, in a cleaning process. Examples are given which relate pyrite size measurements to float-sink washability and to a Deister Table operation. EXPERIMENTAL WORK The automatic microscope used here has been previously described.' Briefly, it is an instrument which measures the diam of particles (as defined by a range of reflectance) exposed on a polished specimen. The instrument scans a sample briquet, measures diam of exposed pyrite inclusions and records the data by size intervals. Preparation of the briquet is critical, due to the automatic nature of the process. The principal requirement is for an optically flat surface, so that focus will be maintained as the motorized stage moves the specimen under the lens. The various substances present must be polished to the same level in spite of the wide difference in hardness between coal substance and minerals. The polishing method must not pluck out small grains, which might be rather loosely held by surrounding coal. The procedure below was successful in producing all of these results. The coal sample (8 mesh or finer) was riffled (a micro vibrating riffle is essential) to obtain 15 g. One volume of Lucite powder (thermosetting plastic mounting medium) was mixed with three volumes of coal and mixed thoroughly. A briquet was formed using a cylindrical die (1 1/4 in. diam) at 3000 lb per in.* pressure and 150°C. Preparation of the optical surface was accomplished on automatic polishing equipment, according to the following schedule: 1) Grinding: 3 stages, using successively fine Carborundum grits of 180, 320 and 600 mesh. 2) Rough polishing: 2 stages, using 3µ alumina on cast iron, followed by 1µ alumina on lead. 3) Fine polishing: 2 stages, using 0.5µ alumina on napless broadcloth over bronze, followed by 0.1µ alumina on silk filament cloth over bronze. Raw data were corrected for the fact that the chords

Jan 1, 1964

By T. S. Plaskett

A striated structure perpendicular to the growth axis was observed by the copper-decoration tech-nique in dislocation-free, .float-zoned silicon crystals. The striations, which were spaced about 100 p apart, fitted the relationship d = f/u , where d is the spacing, f is the growth rate, and u is the crystal rotation rate. Each stria was resolved into an UNDOPED silicon crystals pulled from quartz crucibles by the Czochralski technique usually exhibit a striated structure perpendicular to the growth axis.'-' This structure has been attributed to oxygen segregation, with the oxygen being introduced from the quartz crucible. If the crucible is rotated, the level of oxygen contamination has been reported as high as 10° atoms per cu cm.10 These striations are similar to solute striations commonly observed in doped Czochralski-grown crystals. The periodic nature of the striations is caused by a periodic variation in the growth rate",12 which is attributed mainly to thermal gradients in the melt.13 A finer striated structure14 attributed to constitutional supercooling is sometimes observed between the coarse striae. The oxygen striations have been observed by infrared transmission techniques,' by the copper-decoration technique,' by X-ray diffraction microscopy,6-8 and by 9 p absorption measurements3 on crystals pulled from the melt both with and without dislocations. In this investigation float-zoned dislocation-free crystals were examined by the copper-decoration technique. The level of oxygen for float-zone material is less than 1016 atoms per cu cm the lower limit of detection by 9 p absorption measurement. EXPERIMENTAL TECHNIQUE The crystals were grown by the float-zone process with the rf heating coil outside of the quartz envelope containing the silicon. All float zoning was done under an atmosphere of purified helium. The Dash technique15 was used to grow the crystal dislocation-free. This involves growing the crystal initially with a diameter between 2 and 3 mm and at array of starlike precipitates of copper. The strucLure was not .found at the surface tor a depth of about 1.5 mm, or in a region of similar width ahead of a dislocation network. The structure is postulated to consist of vacancy clusterings or dislocation loops. very rapid rates, about 20 mm per min, for a distance of about 3 cm. The diameter of the crystal is then increased to the diameter of the source of silicon, which in this case was about 19 mm. Because of the arrangement of the apparatus, the zone was passed downward rather than upward, contrary to the standard float-zoning practice. Also, the source was rotated rather than the seed. ziegler17 has made dislocation-free crystals by a similar technique but has passed the zone upwards. The starting material was zone-refined and had a p-type resistivity of 150 ohm-cm. The major impurity was boron; the total impurity excluding the boron was reported by the supplier (Dow-Corning) to be typically less than 2 x 1013 atoms per cu cm. The crystals were examined by the Dash copper-decoration technique18'19—a method in which about 10" atoms per cu cm of copper are diffused at a temperature between 900" and 1000°C into silicon which is then quenched to room temperature. On quenching, the copper precipitates on crystalline defects which are then visible when viewed by transmission infrared microscopy. The photomicrographs shown were taken either of the infrared image tube screen or directly on infrared film. All sections prior to decorating were chemically polished and, for some sections, given a sirtlZ0 dislocation etch-pit examination. After decorating, the samples were mechanically polished. RESULTS A photomicrograph, taken in transmission of a decorated cross section, is shown in Fig. 1. The portion of the section shown is near the surface of the crystal. The entire cross section showed no dislocation etch pits after being given a Sirtl etch treatment. It is seen that the copper precipitated randomly. Each precipitate, as has been reported by others, was found to have a starlike structure.

Jan 1, 1965

By F. F. Schmidt, H. R. Ogden, E. S. Bartlett

Continuing tantalum alloy development studies have been concerned with a more detailed investigation of promising binary, ternary, and more complex tantalum alloys containing Groups IV-A, V-A, VI -A. VII-A, and VII-A metal additions. A primary objective of these studies was to improve the elevated temperature strength of tantalum with minimum degradation of fabricability and low-temperature ductility by alloying. Several alloys were found to exhibit hot tensile strengths in the excess of 25, 15, and 10 ksi at 2700°, 3000°, and 3500°F, respectively, combined with excellent cryogenic toughness and ductility. Particularly outstanding in this respect are alloys in the system Ta-Mo-W. Ternary parameter curves describing hot-strength, low-temperature ductility, recrystallization temperature, weld ductility, and fabricability are presented for the Ta-Cb-V, Ta-Hf-W, Ta-Mo-Hf, Ta-Mo-V, Ta-Mo-W, and Ta-V-W systems. At present, only four metals qualify for large scale structural applications at temperatures above about 1800°F. These are tungsten, tantalum, molybdenum, and columbium. Research and development work on these refractory metals has progressed to the point where efforts are now primarily directed toward the improvement of high- and low-temperature mechanical properties through alloying. High melting point combined with excellent low-temperature ductility, fabricability, toughness, weldability, and high solubility and tolerance for both substitutional and interstitial solutes are important attributes of tantalum. Conversely, its high density and relative scarcity compared with other refractory metals are the major deterrents to the use of tantalum. Early studies in the Battelle alloy development program established base line data on the mechanical and metallurgical properties of high-purity tantalum.' These studies were extended to include a preliminary investigation of the effects of various alloying elements on the established base properties.2,3 Recent studies involved a more detailed investigation of promising binary alloys containing Cb, Hf, Mo, Os, Re, Ru, and W, and ternary Ta-Cb-V, Ta-Hf-W, Ta-Mo-Hf, Ta-Mo-V, Ta-Mo-W, and Ta-V-W alloys. Results of major importance obtained are given in this article. EXPERIMENTAL PROCEDURES Electron-beam-melted tantalum (Wah Chang) and high-purity alloying elements were consolidated as 150-g ingots by multiple nonconsumable arc melting under a partial atmosphere of helium. Homogeneity of the button ingots was checked radiographically. Alloy buttons measured about 1-1/2 to 1-3/4 in. in diam by about 0.35 and 0.50 in. thick. Nominal alloy compositions were checked on each alloy button by weighing after arc melting. In most instances, weight losses were within 3 pct of the total weight charged. Subsequent chemical analyses on a number of selected alloys showed interstitial contents to range as shown below: Range of Interstitial Content, ppm 0 C N H 25-75 50-100 10-50 1-5 Metallic alloying additions were found to agree well with nominal compositions based on weight change data. Fabrication directly from the cast button to sheet was conducted at low (75° to 900°F), intermediate (1800° to 2000°F), or high (3000°F) temperatures, depending upon alloy content and hardness. Evacuated stainless steel or molybdenum packs were used for fabrication at intermediate and high temperatures, respectively. The temperature required to complete recrystal-lization in one hour was determined by hardness measurements and metallographic observations (longitudinal test sections) after vacuum annealing at 180°F intervals in the range 2010° to 2910°F. All mechanical property evaluations were conducted on recrystallized sheet, nominally 0.04 in. thick. Weldability of the various alloys was screened using manual TIG welding techniques. Bend ductility (bend axis perpendicular to weld axis) was the criterion used for evaluation. Tensile specimens employed 0.200 by 1 in. gage lengths, and bend test specimens measured about 1 by 1/4 in. Low-temperature tensile tests were conducted using a crosshead speed of 0.02 in. per min up to the point of yielding, and 0.05 in. per min to fracture. High-temperature tensile tests were conducted in vacuum using a crosshead speed of 0.01 in. per min

Jan 1, 1963

By C. H. North, L. E. Lynd, W. W. Anderson, H. Sigurdson

CONSIDERABLE uncertainty is revealed in the literature regarding the nature of the titanium minerals which make up the bulk of the heavy, opaque fractions of numerous beach sand deposits of the world. An investigation was made, therefore, of beach sand concentrates of North Carolina, Florida, Brazil, and India. Magnetic concentration, X-ray, and microscope data were obtained which show that these concentrates consist essentially of ilmenite and its alteration products. The alteration, brought about by oxidation and leaching of iron values, has resulted in upgrading the ores to a range of 56 to 64 pct TiO2, as compared with 52.7 pct in ilmenite of theoretical composition. Conclusions drawn regarding the nature of the dominant titanium-bearing mineral in beach sand deposits have been based mainly on chemical composition, specific gravity, and petrography. This material has usually been referred to as ilmenite or weathered ilmenite. It has also been referred to as arizonite because in chemical composition it resembles an occurrence in Arizona which was described by Palmer1 in 1909.

Jan 8, 1954

The Fifth Annual National Exposition of Chemical Industries will be held in Chicago at the Coliseum and First Regiment Armory during the week of Sept. 22. It was decided to hold the exposition in Chicago, this year, for two reasons: The U. S. Army commandeered the Grand Central Palace Exposition Building in New York, immediately on the close of the last exposition and converted it into a receiving hospital, the use for which is now, happily, nearly ceased; and it was thought that the Exposition would succeed in bringing about a greater development of chemical industries in the Chicago district and the adjoining states. The Advisory Committee of the Exposition consists of: Charles H. Herty, Chairman, Editor Journal of Industrial and Engineering Chemistry; Raymond F. Bacon, Director, Mellon Institute; L. H. Baekeland, Member Naval Consulting Board; W. D. Bancroft, President, American Electrochemical Society; Henry B. Faber, Industrial Filtration Corpn.; Ellwood Hendrick, President, The Chemists' Club; Bernard C. Hesse, Chemist, General Chemical Co.; A. D. Little, President, Arthur D. Little Inc.; Wm. H. Nichols, President, American Chemical Society; R. P. Perry, Vice-president, The Barrett Co.; H. C. Parmelee, Editor Chemical &; Metallurgical Engineering, G. W. Thompson, President, American Institute of Chemical Engineers; T. B. Wagner, Vice-president, U. S. Food Products Corpn.; M. C. Whitaker, President, U. S. Industrial Chemical Co.; and Charles F. Roth and Fred W. Payne. There is also added a special Chicago committee consisting of L. V. Redman, W. D. Richardson, A. V. H. Mory, Carl S. Minor, F. W. Willard, and Wm. Hoskins; the managers, as in the past, are Charles F. Roth and Fred W. Payne.

Jan 6, 1919

By Norman F. Schulz, Emert W. Lindroos, Strathmore R. B. Cooke

DURING the course of an investigation of the effects of various starch products on hematite and quartz in regard to their separation by flotation, it was found that whereas most starches flocculated suspensions of hematite in water, they did not flocculate similar suspensions of quartz. However, a derivative of whole corn starch containing approximately one tenth aminoethyl group (-—CH,CH2NH2) per glucose unit proved to be an exception. This aminoethyl starch was a very good flocculant for both hematite and quartz, and also possessed the property of depressing both minerals in cationic flotation tests. In view of the widespread use of starch as a flocculating agent of solids in tailing water, pulps, and for coal slimes, ore and various other purposes in sulphide and nonsulphide flotation, attention is called to the effective surface activity of aminoethyl starch in flocculating suspensions of the two minerals investigated. Test Materials The starch products employed included Globe Pearl starch No. 144 and fresh aminoethyl starch, both supplied by the Corn Products Refining Co. Dr. A. L. Elder" has kindly furnished a description The minerals used in the various tests are listed in Table I. Their specific surfaces were determined by the air permeability method, which gave results reproducible to within plus or minus 3 pct. Surface areas obtained by krypton adsorption were greater than the air permeability values by a factor of 2.0 for quartz and 62.4 for hematite. Starch Adsorption on Mineral Surfaces Starch adsorption data were obtained by agitating for 1 hr measured volumes of neutral starch solutions of known concentrations with weighed quantities of finely divided mineral of measured specific surface. The mineral then was separated from the pulp liquor by centrifugation and the residual starch content determined by chemical analysis. The analytical procedure consisted of oxidizing the starch with an excess of dichromate in acid medium at elevated temperature and titrating the excess dichromate by the ferrous ammonium sulphate—potassium permanganate method. Analytical results were reproducible to within less than 1 pct. Adsorption data obtained in unbuffered solutions near the neutral point are plotted in Fig. 1. The adsorption on either mineral was far greater for the aminoethyl starch than for the Pearl starch. Flocculation The degree of flocculation was determined for a given pulp by measuring the time required for the supernatant liquid to reach a certain degree of clarity. This was accomplished by passing a standard light beam through the pulp, contained in a glass settling tube, and measuring the time required after agitation ceased for the intensity of the transmitted beam to reach a predetermined value. Starch reagent was added to each pulp in small uniform increments, and the settling time was determined after each such addition. Increase in pulp liquor volume due to the added starch reagent was ignored in these tests. Pulps were maintained at or near neutrality. of the preparation of the aminoethyl starch: "Three hundred and sixty grams of powdered unmodified corn starch was slurried in 3 liters of water and stirred during gelatinization. Eighty-six grams of ethylenimine was added slowly during reflux which was continued for 4 hr. The yellow solution set to a gel upon cooling. This was broken up and neutralized with HC1. The thick paste was dried on hot rolls. Adsorbed polyethylenimine and salts were removed from the yellowish products by washing first with acidified aqueous '60 per cent' alcohol. The white product contained nitrogen corresponding to about one aminoethoxy group per ten glucose residues." Only laboratory samples of this starch derivative have been prepared. The starch reagents for use in flocculation, flotation, and adsorption tests were made up by dispersing the appropriate quantities of air-dry starch in cold water, adding boiling water, and heating for 30 min at 120°C under pressure. When used ip adsorption tests, the starch solutions first were cleared of insoluble matter by centrifugation.

Jan 1, 1953

By Strathmore R. B. Cooke, Emert W. Lindroos, Norman F. Schulz

DURING the course of an investigation of the effects of various starch products on hematite and quartz in regard to their separation by flotation, it was found that whereas most starches flocculated suspensions of hematite in water, they did not flocculate similar suspensions of quartz. However, a derivative of whole corn starch containing approximately one tenth aminoethyl group (-—CH,CH2NH2) per glucose unit proved to be an exception. This aminoethyl starch was a very good flocculant for both hematite and quartz, and also possessed the property of depressing both minerals in cationic flotation tests. In view of the widespread use of starch as a flocculating agent of solids in tailing water, pulps, and for coal slimes, ore and various other purposes in sulphide and nonsulphide flotation, attention is called to the effective surface activity of aminoethyl starch in flocculating suspensions of the two minerals investigated. Test Materials The starch products employed included Globe Pearl starch No. 144 and fresh aminoethyl starch, both supplied by the Corn Products Refining Co. Dr. A. L. Elder" has kindly furnished a description The minerals used in the various tests are listed in Table I. Their specific surfaces were determined by the air permeability method, which gave results reproducible to within plus or minus 3 pct. Surface areas obtained by krypton adsorption were greater than the air permeability values by a factor of 2.0 for quartz and 62.4 for hematite. Starch Adsorption on Mineral Surfaces Starch adsorption data were obtained by agitating for 1 hr measured volumes of neutral starch solutions of known concentrations with weighed quantities of finely divided mineral of measured specific surface. The mineral then was separated from the pulp liquor by centrifugation and the residual starch content determined by chemical analysis. The analytical procedure consisted of oxidizing the starch with an excess of dichromate in acid medium at elevated temperature and titrating the excess dichromate by the ferrous ammonium sulphate—potassium permanganate method. Analytical results were reproducible to within less than 1 pct. Adsorption data obtained in unbuffered solutions near the neutral point are plotted in Fig. 1. The adsorption on either mineral was far greater for the aminoethyl starch than for the Pearl starch. Flocculation The degree of flocculation was determined for a given pulp by measuring the time required for the supernatant liquid to reach a certain degree of clarity. This was accomplished by passing a standard light beam through the pulp, contained in a glass settling tube, and measuring the time required after agitation ceased for the intensity of the transmitted beam to reach a predetermined value. Starch reagent was added to each pulp in small uniform increments, and the settling time was determined after each such addition. Increase in pulp liquor volume due to the added starch reagent was ignored in these tests. Pulps were maintained at or near neutrality. of the preparation of the aminoethyl starch: "Three hundred and sixty grams of powdered unmodified corn starch was slurried in 3 liters of water and stirred during gelatinization. Eighty-six grams of ethylenimine was added slowly during reflux which was continued for 4 hr. The yellow solution set to a gel upon cooling. This was broken up and neutralized with HC1. The thick paste was dried on hot rolls. Adsorbed polyethylenimine and salts were removed from the yellowish products by washing first with acidified aqueous '60 per cent' alcohol. The white product contained nitrogen corresponding to about one aminoethoxy group per ten glucose residues." Only laboratory samples of this starch derivative have been prepared. The starch reagents for use in flocculation, flotation, and adsorption tests were made up by dispersing the appropriate quantities of air-dry starch in cold water, adding boiling water, and heating for 30 min at 120°C under pressure. When used ip adsorption tests, the starch solutions first were cleared of insoluble matter by centrifugation.

Jan 1, 1953

By Donald M. Hausen

Microscopic evaluation of trace quantities of metalliferous phases in flotation products requires counting large numbers of particles. Particle counts of many thousands may be required for precision, but cannot be obtained practically by conventional microscopic techniques. A less tedious microscopic method for evaluating trace sulfides in mill tailings was developed for the O'okiep Mining Co. in South Africa. Hundreds of thousands of particles were evaluated by this method called "gross-counting." Gross-counting consists of counting microscopic fields rather than point-counting individual particles. Total counts are calculated by multiplying the average number of particles per field by the total number of fields examined over the entire mount. Total gross-counts range from about 20,000 particles for +200 to 100,000 or more for -400 mesh size material in lucite mounts. Sulfides and metallic particles in each field are identified and tallied along with field counts. Totals for each type of metallic particle are divided by the total gross-count to give volume percent which is corrected to weight percent by specific gravity factors.

Jan 1, 1973

By B. J. Kochanowsky

TO improve blasting methods it is necessary to know how the explosive force acts and how rock resists this force. Because of the tremendous power developed within milliseconds and the great number of other factors directly affecting the technical and economic results, an analysis of the fundamentals of blasting theory is difficult. But since the rules used for layout design and for calculations of size of explosive charges are based on theoretical assumptions, complete knowledge of blasting theory has great practical importance in mining. Analysis of Blasting Theory: It is interesting to note the opinion of blasting experts with respect to contemporary blasting theories. F. Stussi; Professor of the University of Zurich, stated: "We do not have enough experience yet to change our army engineering regulations in blasting and base it on new fundamentals. It is our duty to collect more practical data and to do more research in blasting to close this gap." K. H. Fraenkel,2 editor of the Manual on Rock Blasting published in 1953 in Sweden and written by well-known Swedish, German, Swiss, and French blasting and explosive experts, said: "To the best of our knowledge no suitable formulas for civil blasting work are to be found in the American, French or German literature." Present blasting theory is based upon two assumptions. 1) The blasting force of explosive acts in concentrical and spherical form. 2) Rock resistance against the explosive force is directly proportional to the strength characteristics of the rock. The first classical formula based on theoretical fundamental in blasting theory for explosive charge calculation was introduced by Vauban, a military engineer who lived 300 years ago. It was Vauban who proposed the famous formula L = w3 q, where L is the explosive charge, w = line of least resistance, and q = specific explosive consumption proportional to the weight of rock. Later engineers used q as proportional to the strength of the rock. Since Vauban's time different suggestions concerning blasting theory have been proposed. However, the principles stated at that time so affected the thinking of later generations that his formula is still in use and practically unchanged. The first controversy concerned the form of crater. It was found that geological features of rock affected its form. The factor q was analyzed thoroughly by Lares3 and later by Ohnesorge," Weichelt,5 Bendel,6 and others, but the assumption remained that resistance against explosive force is directly proportional to the strength of the rock blasted. The greatest controversy, which has not yet been settled, concerned w. It was noted that w3 is more appropriate for long lines of resistance and w2 for lines of resistance less than 15 ft. Based on the assumption that the explosive force acts concentrically and spherically, spacings between charges were limited to distances not greater than the length of line of least resistance. Sometimes larger spacing is recommended, but this is due to the advantageous geological and physical properties of rock and not to the action of an explosive force as such. In addition to the classical formula, empirical formulas are used widely. These state that the explosive charge is directly proportional to the volume of blasted rock in cubic yards, and the amounts of explosive required are usually expressed in pounds of explosive per cubic yard of rock. Empirical and classical formulas are contradictory. In the empirical formula, but not in the classical formula, explosive charge is taken proportional to all three space axes: line of least resistance, spacing, and bench height. In spite of this contradiction, both formulas give good results. This is possible because as now practiced the explosive charge calculation for heavy burdens need not be highly accurate. Each, open pit or quarry, usually works with a certain relation between bench height and line of least resistance and between charge spacing and line of least resistance. When these relations are changed, however, the specific explosive consumption q changes greatly. This is one of the reasons why the principles on which the formulas are based appear to be incorrect. In addition to the formulas discussed, others exist and are based more or less on the same theoretical

Jan 1, 1956

By Louis A. Mattson, Winthrop A. Rowe, John T. Cumberlidge, Victor M. Mejia

The parent ultramafic of Nickel Mountain is an alpine-peri-dotite. Compositional layering and late stage dunites suggest the intrusive crystallized in the upper mantle or lower crust. The ultramafic mass was fault emplaced in the upper crust, probably during upper Jurassic time. Soil, saprolite and silica boxwork nickeliferous ores were formed over the Nickel Mountain peridotite during the development and later destruction of the Klamath peneplane. A complex fault pattern was produced by irregular gravity displacements along fault surfaces during the relative uplift of Nickel Mountain. The majority of the ores occur in the fractured hanging wall of these gravity faults. Consequently, structure mapping is important for mining purposes. Ore types at Riddle are classified on the basis of MgO, Fe, and Si02 contents as well as textures. The chemical, mineralogical and textural differences of the various ore types reflect differences in weathering histories. Satellitic ore bodies occur peripherally to Nickel Mountain. These are erosional remnants of landslides and large gravity fault blocks from Nickel Mountain.

Jan 1, 1976

By J. Gurland

The effect of four different second-phase additions on the strength of composite alloys with a common matrix was investigated. The four compositions each consisted of 85 pct by volume of silver with additions of 15 pct of either tungsten, molybdenum, tungsten carbide, or nickel. These particular additives were chosen because of their low mutual solid solubilities with silver at room temperature, the alloys consisting essentially of a dispersion strengthened silver matrix in which the second phase is distributed randomly. Test specimens were prepared by a powder metallurgy procedure consisting of ball milling the mixed powders, compacting, and sintering at 920°C for 1 hr in hydrogen. The constituent powders were of CP quality and of particle size between 2 and 10 ?. The compacts were subsequently hot pressed at 1000 psi and 1400° in an Inconel die, coined at room temperature at 60,000 psi and finally annealed and outgassed in vacuum at 800°F. The microstructures of the alloys are shown in Fig. 1, and the microscopically observed porosity grade was A-2 or better as evaluated by ASTM Recommended Practice B 276-54. The properties of the sintered compacts are listed in Table I, and the load-deformation curves in bending are shown in Fig. 2. The samples, of rectangular cross section, were loaded at the center of 58 in. span, and the reported stress was calculated on the basis of linearly elastic behavior in order to allow the comparison of specimens of slightly different dimensions. It is apparent that the tungsten, molybdenum, and tungsten carbide alloys exhibit very similar deformation curves. The moduli of elasticity were determined from the slopes of the stress-deflection curves at small loads. The measured values agree quite well with those calculated by the strength of materials approximation proposed by Paul1 for the elastic constants of mixtures, the calculated values being 15.0, 15.0, 17.4, and 13.4 million psi, respectively, for the tungsten, molybdenum, tungsten carbide, and nickel combinations with silver. The strength of the Ag-Ni composition is appreciably lower than that of the other three alloys. The discrepancy between the two groups is accounted for by the following characteristics of deformation and failure which were observed microscopically during the tests: A) The deformation of the W, Mo, and WC alloys did not involve the second phase particles to any appreciable extent. Slip and fracture took place in the silver-rich matrix alone, although the fracture path generally skirted the particles by favoring the phase boundaries. The deformation proceeded according to the following sequence: 1) formation of small, discontinuous microcracks in areas of the matrix adjacent to a particle, 2) general slip in the matrix and extension of cracks, 3) failure of specimens by propagation of cracks through matrix. The near coincidence of the 3 load-deflection curves suggests that the nature of the second phase particles does not decisively influence the plastic behavior of composite alloys of this composition as long as the particles do not undergo any considerable deformation themselves. B) A markedly different behavior was exhibited by the Ag-Ni composition where the relatively low flow strength is associated with the low yield strength of the nickel grains. Slip in the nickel grains was first observed at a stress of approximately 10,000 psi, although failure, at a later stage, took place by the propagation of cracks through the matrix. The ductility of this aggregate, in which both components deform plastically, is appreciably greater than that of the elastic-plastic composites. In summary: 1) The measured values of the moduli of elasticity of the composite alloys under discussion are in good agreement with the "strength of materials" approximation proposed by Paul.' 2) The overall plastic behavior of these particle-strengthened alloys is unaffected by the nature of the second phase particles, if the latter remain elastic. This work was supported by the Office of Naval Research. The experimental results are presented

Jan 1, 1962

By J. Chipman, N. J. Grant, J. H. Walsh, T. B. King

WITH the development of adequate sampling and analysis techniques, much information has been obtained concerning the behavior of hydrogen in the steel bath during the course of steelmak-ing operations. From studies of this type it has become clear that the slag has an important role to play in determining the hydrogen content found in commercial products. A knowledge of the behavior of hydrogen in slags is necessary to round out our knowledge of hydrogen in steelmaking practice; with this information we are better able to assess practical methods of control. In this paper a method developed for analyzing slags for hydrogen content, studies of the solubility of hydrogen in synthetic slags, and studies of the variation of hydrogen content in slag and steel in industrial heats will be described. Previous Work—While very little has been done in the past to determine the hydrogen content of metallurgical slags, measurements have been made on such slag-like materials as geologic magmas and glasses. Goranson as made extensive studies of the solubility of water in natural and synthetic granites. Many workers have investigated the solubility of gases in synthetic and commercial glasses, but the recent work of Russell" is the most extensive. Russell found that the solubility of water in glass was proportional to the square root of the water vapor pressure in water vapor-oxygen mixtures. It was found that the solubility could either increase or decrease with temperature depending on the glass composition. Wentrup, Fucke, and Rief,' and Piper, Hagedorn, and Backes' have extracted hydrogen by holding a slag at 1300" and 800°C respectively in vacuum. Wentrup et al. reported hydrogen and water vapor as evolved together while Piper et al. passed the evolved gases from the hot extraction treatment over hot ferromanganese to reduce the evolved water vapor to hydrogen and, therefore, reported the analyses in terms of total dissolved hydrogen. Yavoiskii has reported hydrogen and nitrogen analyses on steelmaking slags. Dobrokhotov, Povol-skii, and Khan have studied the hydrogen content of basic open hearth steel under slags of varying viscosity. These authors reported that the hydrogen content of the steel bath increased as the fluidity of the slag was increased by the addition of bauxite. They recommended that a viscous slag be used and the steel tapped without deoxidation in the furnace to ensure a low final hydrogen content. Analysis of Slags for Hydrogen Development of Apparatus—The vacuum fusion analysis equipment described by Shields, Chipman, and Grant" was modified for the analysis of slags." This method depends upon the reduction of water in the slag to hydrogen, which is readily determined by the method used for hydrogen in steel. Preliminary experiments were made with a eu-tectic ferrosilicon melt as the reducing agent. Other experiments included the use of graphite and molybdenum crucibles. The ferrosilicon alloy bath was found to produce a thick coating on the furnace tube which could adsorb hydrogen. Graphite produced CO by the reduction of FeO, MnO, and SiO2 in such quantities that analysis for hydrogen was virtually impossible. Molybdenum, while giving a low blank value, could reduce the slag sufficiently to produce a volatile oxide which again was found to adsorb hydrogen. The arrangement finally adopted is shown in Fig. 1. The molybdenum sheet served as the induction-heated susceptor, and was separated from the escaping gases by alumina guide tubes. An outer jacket of alumina protected the quartz furnace tube, and alumina and quartz stools completed the assembly. The falling sample is shown wrapped in aluminum foil, 0.002 in. thickness, which acted as the reducing agent' This foil was careful'~ washed in acetone and an d and then dried in hot air before wrapping the weighed slag sample for charging into the apparatus. Investigation of the hydrogen content of the aluminum foil itself showed that a small quantity of hydrogen was released in vacuum, but had no relation to the weight of the aluminum charged. This quantity of hydrogen was

Jan 1, 1957