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By A. S. Grove, C. T. Sah, E. H. Snow, B. E. Deal

A summary of- several recent investigations in to the properties of the metal-oxide-silicon system is presented. A major portion of these studies makes use of the MOS capacitance-z)oltage method of' analysis. The particular areas of investigation which are reported include: 1) a general survey of the electvical properties of thermally oxidized silicon surjbccs; 2) a study of ion migration through silicon dioxide films ; 3) measurements of electron and hole mobilities in surface inversion layers; 4) a study of impurity redistribution due to thermal o.ridatiotz; and 5) measurements of the rates of oxidation oj-heavily doper7. silicon. THE importance of the metal-oxide-semiconductor (MOS) system in the semiconductor industry is well-known. In addition to its importance in the "planar" device technology,' the MOS structure is now also used in the fabrication of active solid-state devices. Consequently, extensive efforts have been made recently to obtain a better understanding of the characteristics of this system. A summary of some studies of the MOS system conducted in our laboratories during the past year is presented. For the most part these studies used silicon as the semiconductor, along with silicon dioxide and aluminum as the other two components of the system. Since the MOS capacitance-voltage method of analysis was used extensively in these studies, we will first briefly describe its nature and consider some of the possible causes of deviation of experimental observations from the simple theory. We will then outline the various related areas of investigation carried out in our laboratories and will briefly indicate some of the results. It should be noted that the purpose of this paper is merely to provide a brief summary of MOS studies. More detailed discussions of the various areas of investigation are given in the references cited. PRINCIPLES OF THE MOS C-V METHOD OF ANALYSIS' A sketch of the MOS structure is shown in the upper portion of Fig. 1. In this case the insulating film is Si02 and the semiconductor p-type silicon. If a large negative bias is applied to the metal field plate, holes are attracted to the silicon surface. The silicon then behaves much like a metal and the capacitance measured is that of the oxide layer alone, Co. If a small positive bias is applied to the aluminum, holes are repelled and a region depleted of majority carriers is formed at the silicon surface. This depletion I-egion adds to the width of the dielectric and the measured capacitance begins to drop. With increasing positive bias, the width of the electrical depletion region increases. At some large positive bias an inzevsion regiotr is formed at the surface and additional charges induced in the silicon appear in the form of electrons in this narrow inversion region. Thus the depletion-region width approaches a maximum value and, consequently, the capacitance reaches a minimum value and then either levels off or rises again depending on the measurement frequency and the rate of equilibration of the minority carriers in the inversion layer.3 Band diagrams, along with the corresponding charge distributions, are shown in Fig. 1 for the above bias conditions. If minority carriers cannot accumulate at the surface to form an inversion region, the depletion-region width continues to increase with increased positive bias and the capacitance drops toward zero as in a reverse biased p-n junction. The effect of a work-function difference $hs between the metal and the silicon, and of surface charges per unit area Qss located at the oxide-silicon interface, is simply to attract charges in the silicon much like the applied bias. It can be shown that this results in a parallel shift of the capacitance-voltage characteristic along the voltage axis by an amount corresponding to AV = -$bIs + Qss/Co. Theoretical curves have been calculated4 giving the capacitance of the MOS structure C normalized to the oxide capacitance Co vs the quantity VG here VG is the voltage applied to the metal field plate. In Fig. 2 such calculations are shown as points for a particular oxide thickness and bulk impurity concentration for a p-type semiconductor. (For an n-type semiconductor the curves would be mirror images of these.) All three cases, i.e., low frequency. high frequency, and depletion, are indicated. Also shown in the figure are recorder tracings of the characteristics of actual devices. These characteristics have been shifted along the voltage axis to compensate the effect of surface charges and work-function difference. It is evident that agreement between experiment and theory is good. The nature of this shift along the voltage axis is

Jan 1, 1965

By A. B. Cox, L. W. Wark

In an earlier paper1 measurements of contact angles due to the effect of xanthates on mineral surfaces were reported. The solutions in which these measurements were made differed widely from those of modern flotation circuits. It is intended, however, by introducing, one at a time, the other principal reagents of flotation, to approach gradually the solution composition of flotation liquors. The work now described is an attempt to determine the effect of one of the most important of these reagents—namely, sodium cyanide—on the establishment of air-mineral contact. The work has been carried out for the following companies: Broken Hill South, North Broken Hill, Zinc Corporation, Electrolytic Zinc of Australasia, Mount Lyell Mining and Railway, and Burma Corporation. Since the effect of cyanide is inseparably connected with the alkalinity, the results cited below deal with the mutual effects of alkalis and cyanide. Alkalis alone exert a significant effect on the air-mineral contact but comparatively large amounts are required. Since the addition of a small amount of cyanide greatly decreases the degree of alkalinity necessary for the suppression of contact at surfaces of any of the minerals experimented with (except galena) and since alkalis are rarely used alone in practice, little attention has been paid to cyanide-free solutions. It was shown in the previous paper that, excluding the dixanthogen effect, whenever contact was practicable at all in an ethyl xanthate solution the angle of contact was 60". There is, therefore, less necessity to measure equilibrium contact angles; in fact, the experiments herein described have generally been conducted with a view to determining whether contact is possible and not to measuring the actual value of the contact angle. The separations which have generally to be effected in dealing with complex sulfide ores are: (1) galena from sphalerite, pyrite, etc.; (2) sphalerite from pyrite and/or gangue minerals; (3) copper minerals from pyrite and gangue minerals; (4) pyrite from gangue minerals; (5) chal-

Jan 1, 1935

By Richard S. McCaffery

A Research on iron blast-furnace slags has been in progress since 1922 in the metallurgical department of the University of Wisconsin, supplemented by observations, tests and critical examination of operating records at 10 furnaces. From the data thus collected information has been put into forms suitable for use by furnace operators and is given in this report and the three accompanying papers.' In the viscosity results reported, it is estimated that temperatures were measured within 5" C. and that the viscosity determination of the particular slag investigated is accurate within ± 4 per cent. In the viscosity diagrams in the various papers, the equal viscosity lines were drawn in such a manner that in all cases they are located correctly with respect to the actual experimental results, but when determining a viscosity for a particular composition from the diagrams, the viscosity may. be slightly less accurate than the experimentally determined viscosity for the same slag, for the reason that the iso-vis lines interpolated between the experimental results may be shifted slightly without violation of the experimental data. The viscosity diagrams represent our judgment of their position under the above conditions, and we believe the relative accuracy of viscosity data taken from the diagrams is more than sufficient for any use to which the data may be put. Hundreds of samples of slags synthetically produced in the laboratory and of actual furnace slags have been studied in various ways. The ranges of compositions of slags used for viscosity measurements are: silica 25 to 55 per cent.; alumina 0 to 35 per cent.; lime 25 to 55 per cent.; magnesia 0 to 20 per cent. These measurements were made at temperatures of 1250°, 1300°, 1350°, 1400°, 1450°, 1500°, 1550°, 1600" and 1650" Centigrade. Descriptions of apparatus, methods used and statements of the problems investigated have been published in the papers listed in the bibliography beginning on page 120.

Jan 1, 1932

By M. O. Holowaty, C. M. Squarcy

Blast furnaces are the tools of men, and it is men who have made them great. Here is presented the story of the Ironmakers-the men who first poured hot metal into what would someday be the sinews of a nation. W HEN the Jacobean merchant adventurers bade farewell to the first ship of colonists sailing for the new land, they instructed them to direct all their skill and energy to grow silk worms in Virginia. The adventurers felt sure that they could flood the market with highly priced and much desired goods like silk, sugar, tea, and indigo. They were also convinced that they would fill the needs of the mother country for iron. Early iron production in the colonies The merchants certainly had a wonderful imagination, for silk and indigo were just as exotic in Virginia as they were in England. The settlers found it more profitable to raise tobacco on the vast stretches of the free, fertile land. Thus the plans of settlers clashed with those of The Virginia Co.; and only point of agreement was the desire to produce iron. But, even there the motives of the settlers and those of The Virginia Co. of London were worlds apart. The settlers wanted to produce the tools badly needed in the colony, while the Company desired to cash in on the rising demand for iron which the home industry could not satisfy. Both the settlers and the Company lost no time trying to find iron ore. Locations of the early mines are not known. If, however, the reports of the Irishman, Francis Maguel, can be trusted, as early as 1609 a ship sailed for England with a load of 17 tons of crude iron which the East India Co. purchased at £ 4 per ton. The iron was of excellent quality and considered the best iron made of non-English ore that was ever purchased.

Jan 1, 1961

By Morris Cohen

Within the past two years, a number of publications have called attention to the double peaks, or stages, that appear in the hardness and strength curves of certain aging alloys. The author has shown the existence of double hardness peaks during the aging of a high-purity silver-copper alloy;' and on the basis of electrical resistance, microscopic, dilation and lattice-parameter measurements, hc concluded that the initial hardness peak occurs prior to precipitation while the secondary hardening is due to precipitation. It was suggested that the general mechanism of age-hardening involves two consecutive processes, the first consisting of nucleus or knot2 formation, and the second consisting of actual precipitation and particle growth. It was further held that the two stages are interdependent, but because of nonuniform precipitation they may overlap each other to an extent that increases as the aging temperature is raised. At high aging temperatures, the effect of the first stage cannot be detected because of the rapid occurrernce of precipitation. The general theory of age-hardening recently presented by Dr. M. L. V. Gayler3 is in close agreement with the picture outlined above. With reference to work done on duralumin, copper-beryllium and copper-silver alloys, Dr. Gayler also concluded that age-hardening takes place in two consecutive steps: first, diffusion (in which the solute atoms migrate to certain crystallographic planes), and then precipitation. However, W. L. Fink and D. W. Smith4 have shown that the double aging peaks that appear in the strength curves of high-purity aluminum-copper alloys may be explained without recourse to pre-precipitation phenomena. By means of very careful metallographic technique, Fink and Smith demonstrated that during aging the precipitation takes place at an accelerated rate along the grain boundaries and slip planes as a result of the plastic deformation caused by the drastic quench from the solution heat-treatment temperature. The general precipitation occurs at a

Jan 1, 1939

By Morris Cohen

Within the past two years, a number of publications have called attention to the double peaks, or stages, that appear in the hardness and strength curves of certain aging alloys. The author has shown the existence of double hardness peaks during the aging of a high-purity silver-copper alloy;' and on the basis of electrical resistance, microscopic, dilation and lattice-parameter measurements, hc concluded that the initial hardness peak occurs prior to precipitation while the secondary hardening is due to precipitation. It was suggested that the general mechanism of age-hardening involves two consecutive processes, the first consisting of nucleus or knot2 formation, and the second consisting of actual precipitation and particle growth. It was further held that the two stages are interdependent, but because of nonuniform precipitation they may overlap each other to an extent that increases as the aging temperature is raised. At high aging temperatures, the effect of the first stage cannot be detected because of the rapid occurrernce of precipitation. The general theory of age-hardening recently presented by Dr. M. L. V. Gayler3 is in close agreement with the picture outlined above. With reference to work done on duralumin, copper-beryllium and copper-silver alloys, Dr. Gayler also concluded that age-hardening takes place in two consecutive steps: first, diffusion (in which the solute atoms migrate to certain crystallographic planes), and then precipitation. However, W. L. Fink and D. W. Smith4 have shown that the double aging peaks that appear in the strength curves of high-purity aluminum-copper alloys may be explained without recourse to pre-precipitation phenomena. By means of very careful metallographic technique, Fink and Smith demonstrated that during aging the precipitation takes place at an accelerated rate along the grain boundaries and slip planes as a result of the plastic deformation caused by the drastic quench from the solution heat-treatment temperature. The general precipitation occurs at a

Jan 1, 1939

By Morris Cohen

WITHIN the past two years, a number of publications have called attention to the double peaks, or stages, that appear in the hardness and strength curves of certain aging alloys. The author has shown the existence of double hardness peaks during the aging of a high-purity silver-copper alloy;1 and on the basis of electrical resistance, microscopic, dilation and lattice-parameter measurements, he concluded that the initial hardness peak occurs prior to precipitation while the secondary hardening is due to precipitation. It was suggested that the general mechanism of age-hardening involves two consecutive processes, the first consisting of nucleus or knot2 formation, and the second consisting of actual precipitation and particle growth. It was further held that the two stages are interdependent, but because of nonuniform precipitation they may overlap each other to an extent that increases as the aging temperature is raised. At high aging temperatures, the effect of the first stage cannot be detected because of the rapid occurrence of precipitation. The general theory of age-hardening recently presented by Dr. M. L. V. Gayler3 is in close agreement with the picture outlined above. With reference to work done on duralumin, copper-beryllium and copper-silver alloys, Dr. Gayler also concluded that age-hardening takes place in two consecutive steps: first, diffusion (in which the solute atoms migrate to certain crystallographic planes), and then precipitation. However, W. L. Fink and D. W. Smith4 have shown that the double aging peaks that appear in the strength curves of high-purity aluminum-copper alloys may be explained without recourse to pre-precipitation phenomena. By means of very careful metallographic technique, Fink and Smith demonstrated that during aging the precipitation takes place at an accelerated rate along the grain boundaries and slip planes as a result of the plastic deformation caused by the drastic quench from the solution heat-treatment temperature. ? The general precipitation occurs at a

Jan 1, 1938

By T. E. Watkins, M. D. Nelson

INTRODUCTION Deeper drilling for oil is becoming more and more the rule rather than the exception. With deeper drilling come additional problems, perhaps the greatest being those brought on by the higher temperatures encountered down the hole. particularly in the Gulf Coast region of Texas and Louisiana. Temperature gradients of the order of 1.8° to 2.0°F/100 ft are not unusual, and a gradient of 2.3"F.'100 ft is found in some areas of Texas. With a mean surface temperature of 74oF, the following temperatures could be expected for a geothermal gradient of 2.0°F; 100 ft: at 10,000 it. 271°F. 12,000 ft, 314°F: 14,000 ft, 354,oF; and 16.000 ft. 394°F. Severe gelation of lime-base drilling fluid in wells that have high bottom hole temperatures has become perhaps the most serious difficulty enconntered in drilling under such conditions. Lime-base drilling fluids have been very succesefully and widely used in the drilling of wells in the Gulf Coast region because of their inherent stability toward contaminants. their ability to suppress the swelling dispersion of bentonitic shales, and their ease of maintainance. The gradual recognition: during the past few years, that these muds were. in themselve. the cause of many difficulties experienced in drilling has led to wide-pread efforts by the drilling industry. to determine the reasons for the failure of these mud systems and to develop mud systems capable of performing satisfactorily under high-temperature conditios. MANIFESTATIONS OF HIGH-TEMPERATURE GELATION it is generally possible to recognize the symptons of high-temperature gelation early enough that advance predictions can be made of serious difficulties. in mud control, and the useful life of the drilling fluids can be extended by proper treatment. Following i.; a list of the manifestations of high-temperature gelation: (1) The drill string 'takes weight' while going in the hole after a trip. In early stages of high-temperature gelation it is possible to notice a slight reduction in drill string weight as the drill pipe is lowred near the bottom of the hole. (2) Excessive pump pressure is required to .tart the circulation of drilling fluid at or near the bottom of the hole when going hack to bottom after a trip. As the severity of the gelation increases it may be necessary to break circulation a number of times when going in the hole. (3) The drilling fluid from the bottom of the hole is thick and often granular or lumpy when pumped up after making a round trip. In a severely gelled drilling fluid system such a condition may be irreversible; that is, it cannot be stirred or chemically treated to produce a satisfactory drilling fluid. (4) Completion tool.. such as logging tools or perforating guns will not sink to the bottom of the hole. On some occasions completion tools will become stuck and require a fishing job to retrieve them if the wire line attached to them is broken. It is often difficult to determine whether the condition of the drilling fluid is responsible for sticking the tool or whether the wire line becomes key seated in a crooked hole and causes the allow difficulty. When there are 110 other symptoms of high-temperature gelation. then the difficulty may usually be attributed to the latter cause. (5) In extreme cases of high-temperature gelation it is necessary to "wash" and "ream" when going back to bottom after coming out of the hole. (6) In many -instance. it has been found to be extremely difficult and expensive to 1111 production packers 2nd tubing in moderately deep oil wells which had been drilled with a lime-base drilling fluid. In such instances-the original mud had apparently "set" to a consistency approaching that of a weak cement. CAUSES OF HIGH-TEMPERATURE GELATION Extensive test; have indicated that a lime-base mud does not develop a highly gelled condition at temperatures below 250°F. whereas above that temperature such condition often develops rapidly. (Fig. 1) concurrently. the following changes are evident ill the mud: (1) The alkalinity of the mud decreases to a very low value. with both caustic soda and lime being consumed. (2) The quartz content of the mud decreases sharply. (3) The bentonitic content of the mud decreases or di-appears, with concurrent decrease or loss of base exchange capacity of mud solids. (4) New compounds formed in the mud have been found to be cal-cium silicate, calcium aluminum silicate, and calcium sodium aluminum silicate. (5) The mud loses the ability to form a filter cake of low permeability. The above characteristics have been discussed, in part. by other authors

Jan 1, 1953

By N. A. Gokcen

The construction and operation of a simple and accurate vacuum-fusion apparatus are described in detail. Absolute accuracy of the oxygen analysis has been determined by the reduction of oxides weighed to 20.01 mg. The Bureau of Standards steel samples have been analyzed repeatedly, and their inadequacy for the acceptable range of oxygen is presented. The limits of interference of manganese, aluminum, and titanium, and the effects of tin and water-cooling of the furnace tube have been investigated in detail. ANALYSIS by the vacuum-fusion method consists of melting a sample in a degassed graphite crucible under high vacuum and extracting oxygen as carbon monoxide, and nitrogen and hydrogen as gaseous elements. The resulting gas mixture is analyzed for its constituents, from which oxygen, nitrogen, and frequently hydrogen may be determined within 1/2 hr or less. The history and summary of methods1-4 and extensive reviews of literature'.' for the determination of gases in metals have been published in detail. The foundation of the modern vacuum-fusion method of analysis was laid by Jordan and Eckman,11 and Oberhoffer and his associates.1, 10 Diergarten,11, 12 Meyer,13 Thanheiser et al.,14, 15 Ericson and Benedicks,16 Ziegler,17, 18 Sloman,16-23 Thompson et al.,24 and later many others contributed to the improvement, accuracy, and limitations of the method. In some investigations, however, the limitations of the procedure and the errors involved in the analysis require further critical examination and evaluation. In many apparatuses, lunnecessarily complicated and cumbersome features and elaborate precautionary measures do not have conclusive advantages. The purpose of this invest:igation was, therefore, a) to construct a very simple and accurate apparatus, b) to determine the absolute accuracy of results, c) to establish the limits of interference of manganese. aluminum, and titanium, d) to reexamine critically the reduction and recovery of oxygen from oxide powders of various sizes, and e) to evaluate critically the eight steels of the Bureau of Standards."' Apparatus The apparatus used in this investigation is shown in Fig. 1. It has been used for over three years, during which several modifications were made. A brief description of the apparatus is as follows. The transparent silica or Vycor tube, E, is joined to the Pyrex head, B, by mean of a face to face ground joint sealed with mercury. A similarly sealed ball and socket joint would also have been satisfactory. A standard tapered ground joint, successfully used by some investigators, was tried, but in the absence of grease or vacuum cement it was very difficult to disassemble the joint. The graphite crucible, G, 15/16 or l 1/8 in. OD, 2 1/2 or 3 in. high, 1/10 in. wall, shown enlarged in Fig. 3a, is made from the rods containing less than 0.08 pet ash. Two baffles, overlapping sufficiently to prevent spattering, are inserted in two opposite slots cut on a band saw. Two small holes in the baffles permit the temperature measurement of the melt. A second type of crucible, Fig. 2, G, shown enlarged in Fig. 3b, is also satisfactory, though not as convenient as the crucible shown in Fig. 3a. Somewhat similar but more elaborate crucibles with baffles were first tried by Ericson and Benedicks,'" but were abandoned in favor of a crucible with a stopper and a peripheral graphite powder filter. Various versions of their crucible with a stopper have later been used by other analysts, 10-27, 27-30 The crucible is packed directly in E, Figs. 1 and 2, with —35 + 48 graphite powder for shielding and insulation. A minimum layer of 7 mm of powder is necessary for keeping E cool and minimizing the blank. The first use of graphite powder was made by Sloman,10-23 Who found that —200 mesh was the most satisfactory. The author tried various size powders from +20 to —100 mesh and found that a) particles of 28 mesh or larger were not sufficiently insulating and were heated by the induction current, b) the powder finer than 60 mesh packed too much and did not readily permit the escape of gases even when the crucible was heated very slowly; hence, the powder was occasionally blown out of the side in the crucible and in the mercury pump. The optimum size powder is, therefore, 35 to 48 mesh size or 0.4 mm in average diameter. The furnace is designed to eliminate excessive amounts of

Jan 1, 1959

By H. R. Hanley, C. Y. Clayton

One of the most important contributions to the art of electrolytic zinc production has been the aluminum cathode. This has been used in all major production since its commercial developmerit in 1916. The literature is replete with important contributions, some of which may have been replaced by better ones, but thus far there appears no other metal to take the place of aluminum as cathode material. Credit for this innovation goes to Sherard Cowper Coles, of England. When experimenting on the extraction of zinc from Broken Hill ore at Hayle, Cornwall, in 1893, he introduced the aluminum cathode, and in 1895 obtained . British Patent No. 20073. The reason for this dominant position of aluminum as cathode material in zinc sulphate electrolytes is its unique surface, to which electro-deposited metals usually do not tightly adhere. The metal must be of high purity for best results. It is possible to develop a starting-sheet method by which thin electro-deposited sheets of cathode zinc are made and stripped from a smooth aluminum plate. Such thin sheets of cathode zinc may be used as are the copper sheets in standard electrolytic copper-refinery practice. However, complications arise because of extreme warping of the zinc starting sheet after a few hours of deposition, and thus special arrangements must be made to compensate for this abnormality. Reasons advanced for the ease with which deposits may be stripped from the aluminum surface are: (1) presence of a permanent oxide coating on the metal, (2) failure of aluminum to alloy with the deposit, (3) differences in coefficient of expansion, (4) high position of aluminum in the electromotive series of metals. Of these reasons for nonadherence, which may have some application in general deposition, probably the oxide coating has the greatest bearing on the subject of zinc deposition. Adherence of zinc deposits has occasionally had serious effect on tonnage and production costs. Opinions have differed as to the specific

Jan 1, 1944

By R. A. Wood, R. I. Jaffee, H. R. Ogden, D. N. Williams

The tensile properties, creep resistance. and thermal stability of highly alloyed Ti-Al-Zr alloys were examined. On the basis of these studies, the Ti-7Al-1ZZr composition was selected for more complete evaluation. The alloy was found to be weldable and free from excessive directionality. In addition, it developed maximum properties without requiring heat treatment other than an annealing operation in the alpha field. The alloy was recommended for scale up and is presently being investigated on a production-level basis. One of the more attractive properties of titanium alloys is their ability to withstand stress at moderately high temperatures, and a considerable amount of effort has been devoted to increasing the maximum service temperature of titanium alloys. This work has suggested that the optimum alloys for high-temperature service will be single-phase a (close-packed hexagonal) alloys containing significant amounts of aluminum. However, the maximum amount of aluminum which can be alloyed with titanium is between 6 and 8 pct,l since at high-aluminum contents an embrittlement reaction occurs in the anticipated service temperature range, 800" to 1100°F. It has been shown that the embrittlement reaction involves decomposition of the high-aluminum a phase to one or more new phases.' Since this reaction does not occur at intermediate or low-aluminum contents, it was felt that intermediate Ti-A1 alloys might be strengthened by a-soluble ternary additions without inducing the embrittlement reaction. The first alloying addition considered was tin, which shows extensive solubility in a titanium and has moderate strengthening tendencies. Unfortunately, it was soon apparent that tin also promoted the embrittlement reaction, and that to obtain a stable alloy, the aluminum content had to be reduced as the tin content was increased. The second alloying addition considered was zirconium, which is similar to tin in its effects on titanium. This element did not contribute to the embrittlement reaction and, in fact, appeared to increase the maximum amount of aluminum which could be alloyed with titanium without inducing instability. This paper describes an investigation of the Ti-A1-Zr a alloy region. Alloys containing from 4 to 12 pct A1 and from 6 to 15 pct Zr were examined. The properties of these alloys are described and the bases for selecting an optimum composition is outlined. This composition, Ti-7A1-12Zr, is presently being scaled up in tonnage quantities, and is being evaluated extensively throughout the industry. In addition to presenting the basis for its selection, this paper presents a description of the properties developed in laboratory material as determined during the alloy investigation. These properties suggest that this alloy can fill an important position in applications requiring light weight, fabrica-bility, weldability, and strength to 1000oF or higher. EXPERIMENTAL PROCEDURES Titanium alloy ingots were prepared by inert electrode arc melting under an argon atmosphere. Alloying elements used were 110 Bhn titanium sponge, high-purity aluminum, and reactor-grade zirconium. Pancake-shaped ingots were prepared weighing approximately 300 g. The composition of the ingots was checked by weight measurements before and after melting. The pancake ingots were forged at 2000°F to approximately half their original thickness to give a flat plate roughly 1/2 in. thick. This plate was then rolled at 1800' to 1600°F to 0.250 in. thick. All of the alloys examined fabricated well. However, alloys containing 15 pct Zr tended to overheat due to exothermic oxidation, and scaling was excessive. As might be anticipated from its effect in decreasing the ß transus, increased zirconium appeared to improve fabricability somewhat, especially during rolling at lower temperatures. Except for a limited study of heat-treatment response, all alloys were examined in the a-annealed condition. Prior to heat treatment the a and ß tran-sus temperatures were determined by metallo-graphic examination of samples quenched after annealing at 50-deg intervals in the transformation region. These data are shown in Fig. 1. Recrystal-lization appeared to occur in about 1 hr in the range 1300º to 1500ºF. Therefore, alloys were annealed for 1 hr at 1550ºF (4 and 5 pct Al), 1600ºF (6 through 7-1/2 pct Al), or 1650°F (8 or more pct Al). This produced an equiaxed a grain structure. In most alloys, a "ghost" structure was visible after the a-annealing treatment, as shown in Fig. 2. This structure apparently resulted from the acicular

Jan 1, 1963

By Alexander L. Holley

THE 400-ton testing machine, ordered in June, 1875, by the United States Board appointed to test "iron, steel, and other metals," has lately been completed at the Watertown Arsenal, thoroughly proved and accepted by the Board. The excellence of the machine in every respect is more than satisfactory, and its accuracy is at first sight astonishing, although an investigation of its principles must show that if the weighing apparatus will weigh at all, it must do so with perfect accuracy, because all its movements are absolutely without friction. The proof experiments were numerous, and the effects of recoil after sudden ruptures at maximum loads, were watched with great care, but without much anxiety, because the weighing parts affected are by no means delicate in structure, and their motion is almost infinitely small. Among the tests were the following : A forged link of hard, wrought iron, 5 inches in diameter between the eyes, was slowly strained in tension, and broke short off with a loud report at 722,800 pounds. The diameter before breaking at the point of fracture was 5.04 inches; after breaking, 4.98 inches. In order to see if the weighing parts had been disturbed by the recoil, which was obviously near the greatest recoil the machine will ever suffer, a horse-hair was next tested ; it was 7-1000ths of an inch in diameter; it stretched 30 per cent., and broke at 1 pound. Other horse-hairs vary in tenacity between 1 and 2 pounds. Of course, the accuracy of the machine on such delicate specimens, and indeed on specimens having some hundreds of pounds tenacity, has been checked and proved by other weighing machines. A 5-inch round bar, turned down to 3 5/8 inches diameter along the centre, was pulled apart at 430,200 pounds tension. Then some more horse-hairs were tested ; also copper wires 19 1/2-1000ths of an inch in diameter, which averaged 25 pounds tenacity..

Jan 1, 1879

By T. T. Quirke, L. C. McCabe

The object of the present investigation was to discover a physical basis for rank differentiation of coals, particularly the coals of the Illinois basin. Vitrainl was selected as the most appropriate coal material to use in the investigation, because of its homogeneity and ease of acquisition and handling. Previous Investigations.—Hoffman and Jenker2 have shown that their index of reflection is a characteristic of coal rank and that the Leitz slit microphotometer may be used in determining the different intensities of reflection. Zhemchuzhnikov3 measured the luster of several Russian coals with a color analyzer and found that the degree of luster was indicative of rank. Luster-volatile matter curves based on data from Sucan and Donetz coals were satisfactorily used for determining the rank or volatile content of other coals after the luster strength was determined. In 1934 Fisher4 reported refractive indices of 1.76 for bituminous vitrain and 1.87 for semibituminous vitrain. Investigation of Angle of Polarization.—Early in the present investigation several determinations of the refractive indices of the vitrains were made by immersing the minus 150 plus 200-mesh powder in oils. It was found that all the samples fell within the range 1.6 to 1.8. However, difficulty was encountered in securing oils in this high index range that were closely enough spaced to separate some of the coals. The writers made a number of determinations of the angle of maximum polarization from the polished surfaces of the vitrains and derived their refractive indices by the procedure described in the following paragraphs. Johannsen5 states the fundamental concepts underlying this procedure as follows: In general, in an isotropic medium light vibrates in all directions at right angles to the direction of propagation, and when it meets with another isotropic medium at an angle, part of the light is reflected and part refracted. It has been found that after reflection or refraction, the vibrations do not move with the same freedom in every

Jan 1, 1938

By T. T. Quirke, L. C. McCabe

The object of the present investigation was to discover a physical basis for rank differentiation of coals, particularly the coals of the Illinois basin. Vitrainl was selected as the most appropriate coal material to use in the investigation, because of its homogeneity and ease of acquisition and handling. Previous Investigations.—Hoffman and Jenker2 have shown that their index of reflection is a characteristic of coal rank and that the Leitz slit microphotometer may be used in determining the different intensities of reflection. Zhemchuzhnikov3 measured the luster of several Russian coals with a color analyzer and found that the degree of luster was indicative of rank. Luster-volatile matter curves based on data from Sucan and Donetz coals were satisfactorily used for determining the rank or volatile content of other coals after the luster strength was determined. In 1934 Fisher4 reported refractive indices of 1.76 for bituminous vitrain and 1.87 for semibituminous vitrain. Investigation of Angle of Polarization.—Early in the present investigation several determinations of the refractive indices of the vitrains were made by immersing the minus 150 plus 200-mesh powder in oils. It was found that all the samples fell within the range 1.6 to 1.8. However, difficulty was encountered in securing oils in this high index range that were closely enough spaced to separate some of the coals. The writers made a number of determinations of the angle of maximum polarization from the polished surfaces of the vitrains and derived their refractive indices by the procedure described in the following paragraphs. Johannsen5 states the fundamental concepts underlying this procedure as follows: In general, in an isotropic medium light vibrates in all directions at right angles to the direction of propagation, and when it meets with another isotropic medium at an angle, part of the light is reflected and part refracted. It has been found that after reflection or refraction, the vibrations do not move with the same freedom in every

Jan 1, 1938

By H. R. Hanley, Charles Y. Clayton

One of the most important contributions to the art of electrolytic zinc production has been the aluminum cathode. This has been used in all major production since its commercial development in 1916. The literature is replete with important contributions, some of which may have been replaced by better ones, but thus far there appears no other metal to take the place of aluminum as cathode material. Credit for this innovation goes to Sherard Cowper Coles, of England. When experimenting on the extraction of zinc from Broken Hill ore at Hayle, Cornwall, in 1893, he introduced the aluminum cathode, and in 1895 obtained British Patent No. 20073. The reason for this dominant position of aluminum as cathode material in zinc sulphate electrolytes is its unique surface, to which electro-deposited metals usually do not tightly adhere. The metal must, be of high purity for best results. It is possible to develop a starting-sheet method by which thin electro-deposited sheets of cathode zinc are made and stripped from a smooth aluminum plate. Such thin sheets of cathode zinc may be used as are the copper sheets in standard electrolytic copper-refinery practice. However, complications arise because of extreme warping of the zinc starting sheet after a few hours of deposition, and thus special arrangements must be made to compensate for this abnormality. Reasons advanced for the ease with which deposits may be stripped from the aluminum surface are: (1) presence of a permanent oxide coating on the metal, (2) failure of aluminum to alloy with the deposit, (3) differences in coefficient of expansion, (4) high position of aluminum in the electromotive scries of metals. Of these reasons for nonadherence, which may have some application in general deposition, probably the oxide coating has the greatest bearing on the subject of zinc deposition. Adherence of zinc deposits has occasionally had serious effect on tonnage and production costs. Opinions have differed as to the specific

Jan 1, 1943

By H. R. Hanley, Charles Y. Clayton

One of the most important contributions to the art of electrolytic zinc production has been the aluminum cathode. This has been used in all major production since its commercial development in 1916. The literature is replete with important contributions, some of which may have been replaced by better ones, but thus far there appears no other metal to take the place of aluminum as cathode material. Credit for this innovation goes to Sherard Cowper Coles, of England. When experimenting on the extraction of zinc from Broken Hill ore at Hayle, Cornwall, in 1893, he introduced the aluminum cathode, and in 1895 obtained British Patent No. 20073. The reason for this dominant position of aluminum as cathode material in zinc sulphate electrolytes is its unique surface, to which electro-deposited metals usually do not tightly adhere. The metal must, be of high purity for best results. It is possible to develop a starting-sheet method by which thin electro-deposited sheets of cathode zinc are made and stripped from a smooth aluminum plate. Such thin sheets of cathode zinc may be used as are the copper sheets in standard electrolytic copper-refinery practice. However, complications arise because of extreme warping of the zinc starting sheet after a few hours of deposition, and thus special arrangements must be made to compensate for this abnormality. Reasons advanced for the ease with which deposits may be stripped from the aluminum surface are: (1) presence of a permanent oxide coating on the metal, (2) failure of aluminum to alloy with the deposit, (3) differences in coefficient of expansion, (4) high position of aluminum in the electromotive scries of metals. Of these reasons for nonadherence, which may have some application in general deposition, probably the oxide coating has the greatest bearing on the subject of zinc deposition. Adherence of zinc deposits has occasionally had serious effect on tonnage and production costs. Opinions have differed as to the specific

Jan 1, 1943

By H. R. Hanley, Charles Y. Clayton

ONE of the most important contributions to the art of electrolytic zinc production has been the aluminum cathode. This has been used in all major production since its commercial development in 1916. The literature is replete with important contributions, some of which may have been replaced by better ones, but thus far there appears no other metal to take the place of aluminum as cathode material. Credit for this innovation goes to Sherard Cowper Coles, of England. When experi¬menting on the extraction of zinc from Broken Hill ore at Hayle, Cornwall, in 1893, he introduced the aluminum cathode, and in 1895 obtained British Patent No. 20073. The reason for this dominant position of aluminum as cathode material in zinc sulphate electrolytes is its unique surface, to which electrodeposited metals usually do not tightly adhere. The metal must be of high purity for best results. It is possible to develop a starting-sheet method by which thin electrodeposited sheets of cathode zinc are made and stripped from a smooth aluminum plate. Such thin sheets of cathode zinc may be used as are the copper sheets in standard electrolytic copper-refinery practice. However, complications arise because of extreme warping of the zinc starting sheet after a few hours of deposition, and thus special arrangements must be made to compensate for this abnormality. Reasons advanced for the ease with which deposits may be stripped from the aluminum surface are: (1) presence of a permanent oxide coating on the metal, (2) failure of aluminum to alloy with the deposit, (3) differences in coefficient of expansion, (4) high position of aluminum in the electromotive series of metals. Of these reasons for nonadherence, which may have some application in general deposition, probably the oxide coating has the greatest bearing on the subject of zinc deposition. Adherence of zinc deposits has occasionally had serious effect oil tonnage and production costs. Opinions have differed as to the specific

Jan 1, 1938

By B. B. Zavoico, J. G. H. Crump, P. P. Gregory

West Texas was the scene of greatly increased oil activity during 1937, producing 75,743,000 bb1.l in that year as compared with 61,901,-000 bb1.2 in 1936, an increase of 22.36 per cent. The annual total of wells completed increased from 15863 in 1936 to 28062 in 1937, an increase of 76.92 per cent. Of the total completions in 1937, 2464 were oil wells,2 11 gas wells2 and 331 dry holes.2 The marked increase in the number of oil wells completed in West Texas during 1937 had a substantial effect upon the daily average production per well, which decreased 20.84 per cent from December 1936, when a total of 5310 wells3 produced 5,236,467 bbl.3 for an average of 31.81 bbl. per well per day to December 1937, when 7571 wells2 with a total production of 5,910,257 bb1.2 averaged 25.18 bbl. per well per day. Drilling blocks and checkerboard acreage were being acquired following geophysical work in the northern end of the Permian Basin area, composed of Bailey, Cochran, Hockley, Yoakum and Terry Counties, presaging extension of active development northward. During 1937, at one time 30 geophysical crews were working in West Texas, and an average of 15 to 20 crews was active in this area throughout the year. Discoveries Wasson-Denver Field.—Wasson-Denver field in Gaines and Yoakum Counties was the outstanding field discovery of the year. Production is from porous limestone found at about 5000 ft., and an average well is good for from 300 to 500 bbl. of crude oil per day through 3/4-in. choke. The discovery well was drilled by A. G. Carter and others on the Wasson Ranch, Gaines County, and the field has since been extended into Yoakum County. At the year's end 21 wells had been completed, producing

Jan 1, 1938

Executive Committee. ROBERT H. RICHARDS, Chairman. ALBERT SAUVEUR, Vice-Chairman. TIMOTHY W. SPRAGUE. HENRY A. WENTWORTH. AUGUSTUS H. EUSTIS, Secretary, 131 State St.., Boston, Mass. The twelfth meeting of the Boston Section was held at the Engineers' Club, 2 Commonwealth Ave., Boston, on Monday evening, May 5, 1913, fifteen members and three guests being present.. The meeting Was called to order by Vice-Chairman Albert Sauveur, Who introduced the speaker of the evening, Utley Wedge, of Ardmore. Pa. Mr. Wedge read a, paper on the chloridizing roasting of copper ores, Which lie illustrated With a stereopticon, and Which will be published in full by the Institute. After Mr. Wedge had closed his paper, Which was received with great interest by all the members. the following discussion took place: Professor Hofman said that iron was formerly thought to bo essential to the Henderson process, but that it is not absolutely essential. Mr. Wedge said that., as far as he knew, the presence of some sulphates Was an absolute necessity, and that lime ores can be worked satisfactorily, although lime has an effect on the subsequent leaching. He added that the low fuel consumption of the latest Wedge furnace is a result of direct application of the combustion gases to the ore. Ten per cent. of fuel Was needed with the muffle furnace. By direct firing lie has been able to reduce the fuel needed to from 2 to 4 per cent. In the latest types of furnaces the uses from the upper hearth are not used. There is doubtless some tem-perature at Which the loss from copper chloride volatilization becomes serious, but in practice on Rio Tinto ores troublesome losses are not experienced.. The copper apparently does not become volatile at the temperatures where we would expect that it would. There are doubtless ores in which there would be serious danger from losses from this source. The latest furnaces do not use the high temperatures that Were needed in the former single-hearth Wedge furnaces.

Jan 7, 1913

By Alexander L. Holley

The 400-ton testing machine, ordered in June, 1875, by the United States Board appointed to test "iron, steel, and other metals," has lately been completed at the Watertown Arsenal, thoroughly proved and accepted by the Board. The excellence of the machine in every respect is more than satisfactory, and its accuracy is at first sight astonishing, although an investigation of its principles must show that if the weighing apparatus will weigh at all, it must do so with perfect accuracy, because all its movements are absolutely without friction. The proof experiments were numerous, and the effects of recoil after sudden ruptures at maximum loads, were watched with great care, but without much anxiety, because the weighing parts affected are by no means delicate in structure, and their motion is almost infinitely small. Among the tests were the following : A forged link of hard, wrought iron, 5 inches in diameter between the eyes, was slowly strained in tension, and broke short off with a loud report at 722,800 pounds. The diameter before breaking at the point of fracture was 5.04 inches; after breaking, 4.98 inches. In order to see if the weighing parts had been disturbed by the recoil, which was obviously near the greatest recoil the machine will ever suffer, a horse-hair was next tested; it was 7-1000ths of an inch in diameter; it stretched 30 per cent., and broke at 1 pound. Other horse-hairs vary in tenacity between 1 and 2 pounds. Of course, the accuracy of the machine on such delicate specimens, and indeed on specimens having some hundreds of pounds tenacity, has been checked and proved by other weighing machines. A 5-inch round bar, turned down to 38 inches diameter along the centre, was pulled apart at 430,200 pounds tension. Then some more horse-hairs were tested ; also copper wires 191/2-1000ths of an inch in diameter, which averaged 25 pounds tenacity..

Jan 1, 1879