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By C. V. Millikan

New developments in air-gas lift practices in the Mid-Continent area since our Pall meeting in Fort Worth have done much to increase the efficiency of installations, and thus bring within economic limit of air-gas lift many wells which could not have been flowed profitably before. After the gas-lift had so thoroughly demonstrated its value in the Seminole field, its use spread to other areas and many installations were made of which the economy could be questioned. In the Seminole area, when production began to decline it was necessary either to increase the efficiency of the air or gas-lift or to put the wells on the pump, and pumping was not a process of lifting oil to which any operator looked forward with confidence. These conditions have resulted in the development of many practices which increase the efficiency and permit wells to be flowed with air or gas which earlier could not have been flowed economically, and wells which have been flowing to continue to a lower rate of production. The practices which have come into more common usage in the Mid-Continent area recently are mostly revivals of and improvements on practices which have been known in air-lift work for several years. Many arc peculiar to the individual well on which they are used. Intermittent Flowing Some interesting results are being obtained in Seminole and other districts by intermittent injection of gas. Gas is introduced during per-iods iods of 3 to 5 min. at a rate considerably over that necessary to acquire the production at a steady rate of injection, and is then cut off for a period of 3 to 15 min. Two to five wells are run from the same group of conlpressors. The total volume of gas required is sometimes reduced as much as one-third of that required when it is introduced at a constant rate, without changing the amount of oil production. The maximum pressure required is usually higher, but the average equal to or lower than that required for constant rate of flow. The effect on the wells is usually an irregular rate of flowing which may cause inconvenience where recycling is practiced. It would seem that this increase in efficiency is due to less slippage when the gas is introduced intermittently than when it is intro-

Jan 1, 1928

By G. C. Bateman

THE Workmen's Compensation Act of Ontario was passed in 1915 and Miners' Phthisis was added to the list of compensable industrial diseases in 1916. Under this provision of the Act only about two cases were compensated per year. In 1924, The Department of Public Health made a survey of miners in the four principal camps-Sudbury, Porcupine, Kirkland Lake and Cobalt--and the survey indicated that an alarming proportion of the men exposed to dust had silicosis in one or other of its several stages. A number of conferences were held between representatives of the Department of Mines, the Department of Public Health, the Compensation Board and the mine operators. The operators were advised that in the earliest stages of silicosis there was no physical disability and if men in that stage were removed from underground there would be little danger of permanent disability. They were further advised that if active steps were taken at once to compensate men that had some real disability and remove from the mines men in the early stages of silicosis, the first cost would be the greatest and thereafter their liability should decrease. As a result of this advice, and having at that time no reason to doubt the findings of the survey, the operators agreed to do all that was asked of them and cooperate with the Government in the steps believed necessary to meet the situation, and to provide compensation for the men affected. Amendments In 1926 Arrangements were made for the necessary amendments to the Mines Act and the Workmen's Compensation Act and these amendments were passed in 1926. The Amendment to the Mines Act provided that all underground employees must be the holders of certificates certifying that they were free from tuberculosis of the respiratory organs and further provided that the certificates must be renewed annually. The Government, however, at that time refused to adopt a form of certificate for applicants certifying as to their physical fitness for underground work. The Amendments to the Compensation Act defined both silicosis and

Jan 1, 1937

By Robert L. Voss, Richard D. Hagni

Sparry dolomite from all of the operating mines in the Viburnum Trend of Southeast Missouri have been found by cathodoluminescence microscopy to reveal a systematic pattern of banding resulting from a growth zoning within individual dolomite rhombs. Four principal bands have been recognized throughout the entire Trend and each of the major bands contain even finer internal banding. Minor bands a few microns in width can be correlated in specimens collected ten's of kilometers apart along the trend. The first three principal dolomite bands decrease from south to north. This feature, together with the fact that the white sparry dolomite crystals decrease in abundance from south to north in the Trend, suggests that a major source for the fluids was from the south. The application of cathodoluminescence microscopy to crystalline dolomite demonstrates a strong correlation between ore grade and the intensity of internal banding and dissolution textures.

Jan 1, 1985

By R. G. Ward, P. L. Sachdev

Using an improved maximum bubble pressure technique, the densities of iron silicates at 1400°C have been measured under nitrogen. At the wiistite composition the density has been measured by bubble-blowing experments with both argon and nitrogen and calculated from the measured volume of a known mass of melt under nitrogen. The densities under nitrogen are significantly different from those measured under argon for melts containing less than 28 wt pct SiO2. THE constitution of liquid slags is not well understood, largely because no single property or parameter can be measured which gives conclusive evi- dence of the types and packing of the ions present. Of the many property measurements which can provide information leading to a picture of the constitution of slags, density gives the most direct evidence and has been studied extensively. The work reported here is part of a program of study of densities in multicomponent melts in which the iron oxide-silica system is the solvent. These melts are important as they are fundamental to basic steelmaking, and they allow the study of basic silicate compositions which have hitherto been largely neglected. As considerable disparity exists

Jan 1, 1965

By Harrison Schmitt

During the past decade the writer has studied and mapped certain ore deposits and their structural associations in the states of Chihuahua, Durango, New Mexico and Arizona, and he believes that these deposits, with the exception of the manto-chimney, are representative of the principal types in the area of the states named. In this paper the deposits are described; then generalizations are drawn so far as seems appropriate. Hanover, New Mexico The Hanover, New Mexico, zinc deposits were briefly described by Lindgren and others,' Paige2 and recently in more detail by Schmitt. These, the kind ordinarily called contact metamorphic, border the southern end of an oval area of granodiorite intrusive ¾ mile wide and 2 miles long (Fig. I). The granodiorite has intruded, folded, and metamorphosed sedimentary and igneous rocks, which range in age from pre-Cambrian to Upper Cretaceous. About 90 per cent of the ore has replaced coarse, recrystallized, pure, fossiliferous, lower Mississippian, nonmagnesian limestone (Hanover limestone) 110 ft. thick;4 about 75 per cent of it occurs in the upper 50 ft. of this horizon just below an 18-ft. lower Pennsylvanian shale bed, which lies on a locally inconspicuous unconformity representing upper Mississippian time. The orebodies show five shapes or attitudes, each dependent on a special structural situation: 1. Most of the ore occurs as podlike, thick lenslike or other "three-dimensional" shoots extending from top to bottom of the Hanover limestone and lying adjacent to the outer contact of a silicate zone largely of andradite, which follows the intrusive contact (Figs. 1 and 2).

Jan 1, 1935

By Walter Harvey Weed

AMONG the many causes of that perplexing feature of mine-exploitation, the unequal distribution of the ore, the influence of the country-rock upon the vein-contents has long been accepted as an important factor in certain districts, but the general application of the theory has not been proved. It is now possible to obtain trustworthy data with which to test the theory, and either to confirm or to overthrow this time-honored tradition. By the searching methods of modern petrography and chemistry, rock-determinations are now scientifically made, while the examination of thin sections of ores supplements field- and laboratory-study, and affords conclusive evidence of the paragenesis of the ore-minerals. In the great mass of data regarding mineral deposits accumulated during the past century, there are some facts which stand the test as to reliability; but the greater part are not available for use in this discussion. Within the last 20 years, however, many able workers have contributed careful and accurate accounts of various ore-deposits; and it is by the facts given in such papers, and by personal experience, that. I have become convinced that there is in some districts a true relation between the country-rock and the mineral contents of the veins. My own interest in the subject arose from the observation of a number of striking instances of the variation of vein-contents with the nature of the inclosing rock. Having already recorded certain observations of this kind, I venture to present in this paper further notes, together with a few facts from the literature of the subject, which seem to prove the correctness of my view. It is apparent that if the relation holds true, though in limited districts only, it will be of great practical in-

Jan 1, 1913

By C. A. Mitke

During September, 1911, the fire area in the Lowell mine continually increased and gases resulting from the fire came through the upcast shaft. These gases contained such a large percentage of sulphur dioxide that the men were unable to go up and down on cages, and, within a comparatively short time, repairs in the shaft mere found to be necessary. Since the fire was in sulphide ores and extended into certain timbered sections, the gases contained varying amounts of SO2, CO2, and perhaps, at times, CO. The temperature in the shaft was generally about 97", and the relative humidity from 97 to 99.5 per cent. The corrosive action of the fumes became apparent when the cables had to be changed more often than usual, the heads of lag screws in the guides of the shaft disappeared, and the cages needed frequent repairs. It also became necessary to repair two compartments of the shaft by putting in 150 ft. of new guides between the 600 and 800 levels and lag screws in nearly all the old guides from the surface to the 800 level. 2. Ordinary Methods of Testing Helmets which were Unsatisfactory. These conditions required all work to be done by men wearing oxygen helmets. The Draeger type was tried, and was used until all repairs were completed. At first the helmets were tested for air circulation and air tightness and the injector mas tested by water gauge according to the methods recommended by the Draeger Oxygen Apparatus Co. Six arrangements, covering these different tests, are illustrated in the catalogue and circulars of the company. After the above tests had been made on the oxygen apparatus, the men still complained about leaky helmets. Small quantities of gas entered the helmets and could not be detected by these methods. The

Jan 1, 1914

By C. S. Corbett

There is much comment at present in the ranks of the oil industry regarding unit operation of oil fields and the benefit that would accrue if it could be extensively applied. It seems certain that, as an immediate corrective of the present situation, overproduction could be effectively curtailed with all the advantages of proper conservation of petroleum resources and with no important loss to anyone connected with the industry. Unit Operation in Certain Foreign Fields Many an oil operator in America would doubtless like to have exclusive control of one or more oil-bearing structures for development in accordance with the economic position of the industry and especially in accordance with the best production practice known. A few operators now have this privilege, particularly in certain foreign fields, and are following lines of procedure which show that they are aware of the great opportunity that is theirs. We find in an article by Professor Strigeoff,1 and in a paper read by Captain Comins2 before the American Petroleum Institute, the outlines of procedure adopted, respectively, by the Soviet Government for the nationalized Russian oil fields and by the Anglo-Persian Oil Co. for its fields in Persia. Comprehensive plans for the unit operation of other oil fields may have been described publicly but no such descriptions have come to the attention of the writer. New fields are coming more and more into the hands of single operators or of a few who control large activities and who appreciate fully the need for cooperative action and are willing to forego the lure of a large quick profit from high flush production in order to secure the advantage of better stabilization in the industry and a larger though more deferred profit by operating the field as a unit. Much can be done toward efficient development of an oil field controlled by a few operators who are willing to cooperate for that purpose, but the best result can be obtained only by pooling their interests in the field

Jan 1, 1930

By William Hutton Blauvelt

Coke is the product of dry distillation of bituminous coal, by which the volatile matter is driven off, producing a hard body of cellular structure. Not all bituminous coals will coke, and there has been much discussion regarding the substance which is present in coking-coals to distinguish them from dry coals. Professor Lewes says that the bituminous matter in coal is largely derived from the spores of fossil mosses. Resins are present in all soft coals, and contribute largely to the cementing of the coke. The resinates and hydrocarbons begin to distil out at moderate temperatures and leave the pitchy residual, which at 500' C. forms a mass already well caked together, if the proportion of humus residual is not too great. This coke is soft, but if the heat be raised to 1,000° C. the pitch decomposes further, leaving carbon, and Professor Lewes is convinced that the coking bond is due to these liquid products which distil off, leaving pitch, which then carbonizes and binds the mass into coke. Professor Parr concludes that the structures of the organic compouilds of the coal Which furnish the cemeding-material for coke, and which are apparently attacked by oxygen, have not been determined and seen] to vary somesvhat in different types of coal. However, they yield, on oxidation, humic acids of varying composition which decompose into powdery residues. Because of the complex nature of these substances and the difficulty experienced in isolating and identifying them, the theory of coking is still an open problem and the explanations advanced are largely hypothetical. In the coking process the volatile matter driven off in the oven consists mainly of tar, ammonia, and gas, familiarly known as by-products. Both the quality and quantity of coke and by-products vary greatly With the composition of the coal.

Jan 1, 1913

By Rossiter W. Raymond

It is scarcely necessary to augment or amend the "Appreciation" of Dr. Douglas, from the pen of Dr. Albert A. Ledoux, which appeared in January, 1916, in Bulletin No. 109 of the Institute. The author of that admirable summary enjoyed the great privilege of expressing while Dr. Douglas was yet among us (though already marked for death) the love and esteem with which we all regarded him. But now that his earthly life has ended, the historian must still be the eulogist. No line need be added or deleted in the portrait of him already drawn; it has only to be accepted now as a true likeness, and hung in the gallery of the immortals, illuminated by the crowning glory of another world. James Douglas was born at Quebec, Canada, November 4, 1837. His father, James Douglas, was a distinguished physician and surgeon, known in many lands, especially in the Orient, and famous in his own country for his philanthropy as well as his skill, having established and directed for many years the first retreat for the insane in the Dominion. of Canada. One of the latest literary labors of the son was the editing and publishing of his father's journal and reminiscences—a fascinating volume, the review of which, though a tempting task, I must here forego. Nearly fifty years ago, I had the great pleasure of spending an hour with the elder Douglas, who guided me through his collection of Egyptian and Asiatic treasures. I might almost say souvenirs; so many of them were connected with personal experiences and exalted personages. The veteran's memory had already begun to fail with age, but his vivacity and imagination glowed all the more brightly; and his reminiscences of travel and adventure were embroidered with Oriental magnificence. I felt, after that hour, as if I had visited a stately, half-ruined edifice, overgrown with vines and flowers. The father's genius, adventurous spirit and generous philanthropy descended to his versatile, yet practical son. Like other men of such temperament, James Douglas tried many things before circumstances beyond his own control forced him into the line of his principal lifework. At the age of 18, he was sent to the University of Edinburgh, where he studied for two years. Returning to Canada, he entered Queen's University, at Kingston, Ontario, where he was graduated as Bachelor of Arts in 1858. Subsequently he studied medicine at Lava1 University, Quebec;

Jan 1, 1919

By S. W. Kennedy, M. Cohen, L. D. Calvert

A high-temperature X-ray diffraction method has been used to study the composition and the kinetics of formation of oxide scales at 800 °C on iron and pure iron-nickel alloys containing 25.6, 75, and 84 pct Ni. This technique has been combined with chemical analysis, and metallographic examination, and determination of weight-gain time curves. The 75 and 84 pct Ni alloys form a three-layer scale consisting of porous NiO next to the metal, a spinel layer, and a -Fe203 on the outside. The 25 pct Ni alloy produces a scale of spinel and Fe,O,, in which, however, traces of FeO and NiO are observed near to the metal. On all the nickel alloys the Fe20, is orieqted with the (107) plane parallel to the surfaces. The exposed surface of the Fe20, is in the form of needles whose axis is perpendicular to the specimen surface. Although the alloys show nonuniform oxidation rates as determined from weight-gain measurements, the X-ray data indicate that the total scale and individml scale layers grow uniformly and parabolically. Deep subscale formation is observed in the 25 pct Ni alloy only. This appeared to be associated with cracking of the scale and penetration of the oxygen along the grain boundaries. ALTHOUGH film formation has been investigated by high-temperature electron-diffraction techniques, for example by Gulbransenl and Hickman,' there have apparently been no investigations of scaling by methods permitting study of the scale during formation at the reaction temperature. Methods involving quenching of scales are based on the working assumption that no significant changes take place on cooling. In general, however, compounds may disproportionate, and the different thermal expansions of constituents may cause disruption of the scale on cooling. In particular, some scales cannot be quenched without spalling. These difficulties are avoided by X-ray diffraction examination at the temperature of formation. High-temperature diffraction procedures also provide a method of determining the kinetics of formation of each phase separately in a multicom-ponent scale. The scaling of binary iron-nickel alloys Containing up to 30 pct Ni at a temperature of 800°C has been studied by Benard and Moreau using cooled specimen~,~ whilst Foley, Druck, and Fryxel14 made an electron-diffraction study of cooled oxide films formed on an iron 42 pci Ni alloy. In the present work the scaling of three iron-nickel alloys containing 25.6, 75, and 84 pct by weight of nickel, at 800°C in oxygen at atmospheric pressure was investigated by X-ray diffraction techniques using a Norelco Geiger-counter diffrac-tometer. The oxidation of iron was investigated for comparison. In addition normal metallographic examinations and chemical and X-ray analyses were made, and weight-gain time curves obtained. EXPERIMENTAL Materials Used—The analyses of the alloys were as follows: Percent by Weight Nickel 25.6 pct 75.4 pct 83.2 pct Aluminum 0.004 None found 0.002 Cobalt — 0.05 0.05 Chromium — — — Silicon — 0.01 None found Carbon All less than 0.05 pct The chemical analysis of the iron was: Al— 0.002 i 0.001 pct, C—0.007 pct, Cr less than 0.001 pct, Cu—0.002 ± 0.001 pct, Mn—0.003 ± 0.001 pct, N—0.0002 pct, 0-0.013 pct, P—less than 0.0002 pct, Pb—not detected, S—0.0017 pct, Si—0.0095 pct, Sn—none detected. This iron was the same as that used to make the alloys and was obtained from the same source-Vacuum Metals Corp. One specimen of pure iron from The British Iron and Steel Research Association was used for preliminary investigation. Specimens were machined to shape from cast rod, polished (the final polish being with 600 Sic paper), degreased in trichlorethylene, washed, and etched. The etching and neutralizing procedure adopted by

Jan 1, 1960

By V. A. Phillips

Transmission-electron micrographs of electro-thinned samples of bulk-aged Cu-3.1 pet Co alloy show an aging sequence, supersaturated solid solution — coherent particles — quasi -coherent particles — noncoherent particles. Hardening is due to precipitation of coherent spherical fee coball-rich particles showing coherency strain fields, which are resolved at between 15 and 30A diameter. Loss of- full coherency did not occur until well into the overaged region, even with the assistance of deformation after aging. Different average particle diameters of 123, 92, and 149 ± 10Å were observed in samples aged to peak yield strength at 600°, 650°, and 700°C, respectively, indicating that there is no critical size for peak hardening. Noncoherent particles tended to develop (111) faces and became octahedral in shape. Dislocations tended to nucleate spherical coherent particles which eventually grew together forming large elongated particles. The surface energy of a noncoherent (low-angle) inter-phase boundary is estimated to he about 50 ergs per sq cm. A number of particle lining-up phenomena were observed. Overaging is principally attributed to increase in particle spacing, progressive loss of coherency, and increase in amount of discontinzdous precipitation. COPPER dissolves about 5.6 at. pet (5.2 wt pet) of cobalt at 1110oC1 and the solubility decreases to 0.75 at. petl (0.54 at. pet)2 at 650°C and to 0.1 at. pet or less at lower temperature.' It has been known for many years3-5 that Cu-Co alloys are capable of age hardening. Since cobalt is fee above 417°C and its atom size is only about 2 pet smaller than that of copper, precipitation of coherent particles would be expected. The equilibrium phase precipitated at 700°C and below contains about 10 pet Cu in solution which tends to stabilize the fee structure, lowering the transformation temperature to 340oc.l The alloy is known to undergo discontinuous precipitation in addition to general precipitation; while the former can be seen with an optical microscope, the latter precipitates are not visible except in the grosly overaged condition.5, 6 Extensive use has therefore been made of the ferromagnetic properties of the precipitate in order to follow the course of aging, and it has proved possible to measure the average particle size, spacing, approximate shape, and volume fraction and to determine that the particles are coherent without ever seeing a particle (see for example Refs. 2, 7, and 8). The magnetic measurements of particle size are limited to diameters below about 120Å.7 The present study was undertaken using the techniques of transmission-electron microscopy in order to check the above conclusions, to extend the previous magnetic work to larger particle sizes, and to attempt a more detailed correlation of properties and structure. A portion of this work has already been published.9-11 The present paper is concerned with the metallographic features of precipitation in relation to aging curves. Bonar and Kelly12'13 have published preliminary results of a similar study on single crystals of Cu-2 at. pet Co. EXPERIMENTAL Preparation of Alloy. A Cu-Co alloy, containing 3.12 wt pet (3.36 at. pet) Co by analysis, was prepared from 99.999 pet purity oxygen-free copper and electrolytic-grade cobalt. The alloy was melted and cast in vacuo in a high-frequency furnace using a graphite crucible and mold: Analysis showed chat 0.004 pet C was picked up during melting. The 1-1/2-lb ingot was homogenized in hydrogen for 24 hr at 1000°C. Slices were cold-rolled to 0.005 or 0.003 in. thickness, with an intermediate 650°C anneal in hydrogen at 0.080 in. thickness. Batches of six to ten strips were solution-treated in sealed-off quartz tubes in high vacuum in a vertical furnace and quenched by dropping into iced brine containing a device which snapped off the nose of the tube. Solution treatment consisted of 1 hr at 990°C or 2 hr at 965°C. The latter was employed for all mechanical-property studies, since a tendency was noted for the higher temperature to give porous material. Strips were usually aged individually in a horizontal vacuum furnace, inserting into the hot zone and withdrawing into a cold zone without breaking the vacuum. This method gave a rapid heating rate, permitting the use of short aging times. In some cases, particularly for the longer aging times at the higher temperatures, samples were sealed individually in quartz tubes in high

Jan 1, 1964

By H. F. Ramstad, F. D. Richardson

The equilibria (a) SiOz +Hz =SiO +H20 and (b) Si + SiO, = 2Si0 have beet1 studied at temperatures of 1425"to 1600°C ad 1310°to 1485°C respectively. The stattdard free energy changes for the tzrro reactions are given by the equatiotts Combination of the results for both equilibria leads to tiotz removes certain anomalies in existing high-terlzperature data for equilibria involving silica and silicon in iron. In many metallurgical processes and in many laboratory investigations silicon monoxide undoubtedly plays an important role. It is unfortunate therefore that wide differences exist between the results obtained by different investigators1-7 in their studies of such equilibria as In an attempt to put our knowledge of SiO on a surer basis, an exhaustive study has been made of equilibria [I] and [2] at temperatures ranging from 1300" to 1600°C. Reaction [I] was studied by measuring the amounts of silica which could be condensed from streams of Hz or Hz + HzO which had previously been brought into equilibrium with silica at temperatures ranging from 1425" to 1600°C. Reaction [2] was studied by measuring the material that could be condensed from streams of Hz or argon which had been brought into equilibrium with mixtures of silicon and silica at temperatures ranging from 1310" to 1485°C. EXPERIMENTAL Materials. The silicon was "superpure" grade and contained less than 0.1 pct impurities. The silica was prepared from pure mineral quartz; this was crushed and treated with concentrated hydrochloric acid to remove particles of iron, washed with water, and finally dried at 120°C. For the hydrogen + silica reaction, the silica was sized to —20+100 mesh. For the silicon + silica reaction, the two materials were ground to a fine powder in an agate mortar. The hydrogen and argon were commercial oxygen-free gases. The gas streams were controlled with capillary flow meters and the volumes were measured by wet gas meters. After passing through the meters, the gases were partially dried by silica gel. The hydrogen for the HZ + SiOz reaction was then passed through palladised asbestos at 300°C and dried with magnesium perchlorate. The efficiency of oxygen removal was checked throughout the experiments by passing the gas over an electrically heated strip of nichrome, used as an indicator as described by Rathman and de itt.' When mixtures of HZ + Hz0 were required, the partial pressures of water vapor (1.8 to 22 mm) were obtained by passing the hydrogen through oxalic acid dihydrateg' lo held at various controlled temperatures, O.l°C, by means of a water bath. The hydrogen for the Si + Si02 reaction was purified by passing it over a mixture of 3 parts of magnesium to 5 of lime heated to 600°."l1 u The argon for this reaction was passed through titanium powder (-3/16 in. + 100 mesh) heated to 900°C. The nitrogen used to prevent the reaction products escaping from the condenser (see later), was deoxidized by copper or iron at 600°C. All these gases were finally dried with magnesium perchlorate. Furnace, Temperature Contr01, and Measurement A molybdenum resistance furnace was used for both sets of experiments. The reactions were conducted inside a high-grade alumina tube, 36 in. long and 1 in. in diam as indicated in Fig. 1. With this arrangement an even temperature zone (2"C) 4 cm long was satisfactorily obtained. The temperatures were kept constant by means of a proportional controller actuated by a Pt-Pt 13 pct Rh thermocouple. This was placed between the two alumina tubes, so that the temperature at the junction was 1400" to 1450°C. Up to 1485"C, the temperatures were measured with Pt-Pt 13 pct Rh thermocouples. For higher temperatures an optical pyrometer was used, this being sighted (through the glass window 1 in Fig. 1) on the end of the alumina tube, that held the SiOz or Si +SiOz mixture, 10 in Fig. 1. The optical pyrometer was recalibrated whenever a change was made in any part of the apparatus situated in the hot zone. Successive readings with the optical pyrometer were reproducible to within 1"C. Equilibrium Apparatus and Procedure. Hydvogen and Silica Reaction. The apparatus is shown in Fig.

Jan 1, 1962

By S. Nakajima, H. Okazaki

Quantitatiue studies of the deformation texture in drawn tungsten wives were made by the X-vay dif-fractottletetr. Experimental results show that the diffraction Intensities are equal to tilose pvedicted from the (1 10). fiber lexlure but the angxla), spreads of. diffraction peaks in the pole distribution curres are different for different diffraction planes and directions. For this reason a modified (110) fiber lextuve model, in which a kind of anisotropy is assumed, is proposed to explain the results. According to this model the poles lying on a line directing front the (110) to the (110) poles in the (1 10) standard stereograpllic projection should show spreads which are different from those lyitlg on a line directing from the (001) to the (001) poles, which is confirmed by the experiments. The anisolvopy and the spveads of the pole positions are large at the outer part of the wires and decrease gradually lowards the inside of the wire. The possibilily of occurrence of such anisolropy in irrelals with fcc stvuctures is discltssed. THE deformation texture of drawn tungsten wires has been assumed by different investigators to be the simple ( 110) fiber texture.' Recently, however, Leber2,3 has shown that a swaged tungsten rod has a cylindrical texture. It changes gradually to the (110) fiber texture by drawing through dies. However, even after drawing to 0.25 mm in diam, the cylindrical texture can still be found in wires together with the (110) fiber texture. This was deduced from the pole figures obtained from the longitudinal section of these wires. Use was made also of quantitative measurements of the pole distribution curves. Leber stated that the angular spread of the pole distribution curves (henceforward called dispersions) are quite different for (400) 45 deg and (400) 90 deg: the former is always larger than the latter. This inequality is accompanied by deviations of the diffraction intensities from the theoretical values for the ( 110) fiber texture. Bhandary and cullity4 have reported similar results on iron wire and explained them by assuming a cylindrical texture. Both Leber3 and Bhandary4 used only the results of the (400) reflection for the determination of the dispersion. The pole figures found by Leber3 and by Rieck5 are largely different. The model given by Leber to explain the effects is in the authors' opinion in some respects unsatisfactory, especially if one looks at other than the (400) reflections. Intensities and dispersions of diffraction peaks are conclusive factors for the determination of the fine structure in wire textures. For this reason we studied them extensively to come to a model which is more suitable to fit the facts. In the following, after giving the experimental set-up, we report about measurements of X-ray diffraction on drawn tungsten wires. Different models to describe the experimental results will be discussed. EXPERIMENTAL GO-SiO2-A12O3 doped tungsten wires drawn to 0.18 mm in diam were used for the measurements. The wires were chemically etched to various diameters down to 0.03 mm. Measurements were carried out for the different wires in order to determine the dependence of the texture on the radius. The wires were cut to pieces of 10 mm length and fixed with paste closely against each other on a flat, polished glass plate. Parallelism of the wires with the surface of the glass plate should be adequate. For the diffraction studies three different X-ray sources were applied, respectively, giving the CuK,, FeK,, and FeKp emission. The measurements were carried out with a diffrac-tometer with a GM counter. The latter was fixed to a certain diffraction angle 20hkl and the diffraction intensity was recorded as a function of the angle of rotation of the specimen around the axis, lying in the specimen surface and perpendicular to the wire axis, as shown in Fig. 1. Measurements were also done with the detector at angles slightly deviating from the diffraction maxima The measured intensities in this case were taken to be equal to the background level. The deviations were chosen as small as possible but large enough to eliminate the influence of the diffraction maxima. The useful range of the rotation angle x of the specimen is generally limited by the wavelength of the X-rays. We have: where and cp is the angle between the wire axis and the normal of the diffraction plane. Intensity measurements were made to find the necessary corrections for counting loss of the GM counter and for distortion resulting from such effects as absorption of X-rays and from inclination of the reflection plane under study with respect to the surface of the specimen. The counting loss was esti-

Jan 1, 1968

By Jacques Steininger, Robert E. England

Single crystals of ZnTe and ZnTe1-,Sex with x up to 0.13 have been grown from the elements by temperature gradient solution zoning using excess tellurium as a solvent. Best results have been obtained with charges with the compositions 45/55 at. pct Zn, Te, for ZnTe and increasing amounts of selenium for ZnTe1-xSex. The temperature in the molten zone was maintained at about 1070°C with a gradient of about 10°C per cm. Chemical analyses of quenched ZnTe ingots show tellurium concentrations in the molten zone as high as 70 pct with concentration differences across the zone of 1 to 2 at. pct Dark dots which are observed by transmitted light microscopy in as-grown crystals can be removed by annealing in zinc vapor at 900 C. INTEREST in wide band gap semiconductors has led to a new study of ZnTe and ZnTel-xSex crystal growth. ZnTe is the only II-VI compound with a wide band gap (2.3 ev) that can be made p type with low resistivity. Attempts to make it n type with low enough resistivity to be useful for p-n junctions have so far been unsuccessful.1 ZnSe has a band gap of 2.65 ev but can be made n type only. However, ZnTel-xSex solid solutions with x as low as 0.36 have been made both highly n and p type2 with a minimum band gap around 2.12 ev3 at room temperature and appear to hold the best promise for efficient injection electroluminescence in the visible. ZnTe has the lowest melting point of the zinc chal-cogenides (1295°C) and consequently attempts have been made to grow crystals from both the liquid and the vapor phase.4 Complicated apparatus is required for growth from stoichiometric melts because of the high vapor pressures of the elements at the melting point of ZnTe and because of the problem of quartz devitrification. Small crystals have thus been grown in high-pressure equipment by Fischer5 and by Narita et a1.6 with pressures of the order of 50 atm of argon to prevent excessive evaporation from the melt. Large crystals of ZnTe can be obtained by growth from the vapor phase4 but they often present numerous dislocations and inclusions. An improvement in the quality of vapor- grown ZnTe crystals was reported by Albers and Aten7 by equilibration of mixtures of small crystals with compositions lying on either side of the solid single-phase field at fixed temperature. The same technique was later applied by Aten8 to the growth of ZnTe1-xSex crystals with less than 1 pct inhomo-geneity. Because of the higher liquidus temperatures of the solid solutions and the high vapor pressure of selenium, previous attempts to grow ZnTel-xSex from the melt have been limited and unsuccessful.9 The phase diagram of the Zn- Te system is reproduced in Fig. 1, based on data from Kobayashi10 and Kulwicki.11 Carides and Fishher12 have reported lower liquidus temperatures on the tellurium-rich side, but their data would require confirmation. The liquidus temperature on the tellurium-rich side decreases rapidly with increasing tellurium concentration and the Te2 vapor pressure over the liquidus also decreases accordingly.'3 The decrease in liquidus temperature and vapor pressure therefore makes it possible to use conventional apparatus if there is a sufficient excess of tellurium in the melt. Single crystals of ZnTe have thus been grown by Kucza,14 in a modified Bridgman technique, from solutions containing up to 60 at. pct of Te by lowering unsupported quartz ampoules through a temperature gradient at about 1200°C. Under these conditions, the phase diagram indicates that the entire charge is initially molten. Crystal growth can therefore proceed by normal freezing and rejection of excess tellurium into the melt. The modified Bridgman technique has several major limitations. Because of the rejection of excess tellurium into the melt during freezing, the melt composition and the temperature at the growth interface vary continuously. They tend to follow the liquidus until the eutectic which is very close to pure tellurium (447°C, >99 pct Te). Since the solidus composition also varies with temperature,15 crystals grown by this method are inhomogeneous. They present small variations from stoichiometry which may affect their structure and physical properties. The simultaneous increase in tellurium content and decrease in melt temperature also combine to reduce the rate of diffusion of tellurium away from the growth interface, thereby causing constitutional supercooling and possibly dendritic growth. To minimize these effects, the initial melt composition is in practice kept relatively close to stoichiometry (less than 60 pct Te). This however limits the possibilities of operating at low temperatures and pressures. This paper describes a modified method of crystal growth by temperature gradient solution zoning (TGSZ) which is an adaptation of the temperature gradient zone-melting technique developed by pfann16 and of the traveling solvent method of Mlavsky and weinstein.I7 The TGSZ method now applied to the growth of ZnTe and ZnTel-xSex crystals is characterized by its very simple experimental arrangement and sample preparation technique. Unlike the modified Bridgman technique, there is no increase in the tellurium concentration in the melt and therefore it is possible to operate at lower temperatures and pressures. This method is also suitable for maintaining a constant temperature at the growth interface.

Jan 1, 1969

By Michael Tenenbaum, T. L. Joseph

In a previous investigation1 the authors studied the effect of pressure on the reduction of iron ores by hydrogen. With hydrogen as a reducing agent, the rate of reduction was increased substantially by increasing the pressure from 1 to 2 atmospheres. The results with hydrogen prompted the present study of the effect of pressure on reduction with carbon monoxide and with mixtures of carbon monoxide and nitrogen. Features of Reduction Process The gas stream in the lower part of the blast furnace always contains sufficient concentrations of reducing gases to complete reduction provided sufficient time is allowed for the reaction to proceed. Reducing gases react immediately with the iron oxide on the surface of lumps of ore. However, as the unreduced surface recedes from the easily accessible exterior of the lump, the reaction proceeds by virtue of the diffusion of the gases into and out of individual pieces. The rate of diffusion of gases, which undoubtedly plays an important role in the reduction of iron ores, depends on several factors, most important of which are: (1) molecular weight or density, (2) pressure, (3) temperature, (4) concentration gradient. Thus, the rate of reduction of a lump of iron ore at any temperature will depend not only on the specific reaction rate but also upon: (1) available surface of unreduced iron oxide, (2) rate of diffusion of the reducing gas to the reacting surface, (3) rate of effusion of the gaseous products of the reaction from the reacting surface, (4) adsorption of the gases on the reacting surface. The various features of the reduction process were discussed in previous work and need not be reviewed. However, in order to explain

Jan 1, 1940

By H. N. Mills

The glass industry is a major user of many industrial minerals in the manufacture of its product. It is the intent of this chapter to: (1) acquaint the reader with the glass industry by including a few production statistics, and (2) cover the various aspects of the major raw materials used to make glass. The matter of glass compositions, properties, and batches is considered beyond the scope of this chapter which deals only with raw materials. For more details on the particular minerals and rocks used in glassmaking, the reader is referred to chapters in the commodity section of this book. Glass Industry Statistics Glass manufacture in the United States can be divided into three major product classifications as follows: 1) Glass containers 2) Pressed and blown glass 3) Flat glass Glass containers include bottles and jars for the packaging of food and beverages, as well as drugs, chemicals, and cosmetics. Pressed and blown glass includes table, kitchen, art and novelty ware, lighting and electronic glassware, and fiber glass. Flat glass covers sheet or window glass, plate, laminated, and safety glass. The US Department of Commerce statistics, as recorded in the 1977 Census of Manufacturers, compares the dollar value of glass shipments for each product category. These statistics are shown in Table 1 (Anon., 1980) and are self-explanatory. A comparison of the tonnage output in each product classification is difficult, as production data is reported in "gross" for glass containers, "pounds" for fiber glass, "pieces" for glassware, [ ] and "square feet" for flat glass. In the case of glass containers, an average "pounds per gross" factor can be applied to the total production figures reported in thousands of gross in Bureau of Census industrial reports. Table 2 presents the calculated annual production tonnage for glass containers for the years 1974-1979. Except for 1979, there was a yearly increase in production. The tonnage figures of Table 2 are further influenced by decreasing weight per gross which has occurred in the glass container industry since 1975. This reflects the gradual shift to lighter weight containers for beverages. Other segments of the glass industry have experienced growth, but the figures in tons are not published information. Fiber glass growth has been influenced by the heavy demand for insulation as part of energy conservation efforts on a national basis. The production of flat glass by the float process has continued to grow with several new plants entering production. All portions of the glass industry experienced the effects of the general economic decline of 1979-1980, but the outlook for the future is bright. Batch Materials For Glass Use Materials and Function Soda-lime-silica glass represents the largest proportion of glass manufactured for commercial use. It is produced by the fluxing and

Jan 1, 1983

By P. C. Kapur

An approximate but simple and practical solution to the discretized batch grinding equation has been obtained. The solution is based on a new grind function, a combination of selection and breakage parameters and particle-size distribution of the feed. The grind function, which is readily computed from limited experimental data, has significant implications for analysis of the particle-size reduction processes. Using the practical solution, three ball-mill comminution systems—dry dolomite, wet quartz, and limestone—have been simulated with acceptable precision. The application of the discretized batch-grinding equation1 to routine comminution analysis is frustrated by two principal difficulties. First, the selection and breakage parameters of the grinding equation must be computed separately. This is usually a difficult and uncertain task although, recently, a number of experimentally and computationally efficient strategies have been proposed for determination of these parameters?" Second, for actual computation, the solution to the batch-grinding equation becomes progressively tedious and unwieldly for finer particle-size range.1,2 The purpose of this part of the report is to present an approximate solution to the batch-grinding equation, which is practical in that it seems to overcome the aforementioned obstacles. The solution involves the concepts of a new grind function, a lumped parameter of the selection-breakage functions, and particle-size distribution of the feed, which is readily computed from a limited amount of experimental data.

Jan 1, 1971

By O. W. Ellis

CERTAIN alloys1 that, as a result of quenching, are retained in the form of homogeneous solid solution are known to increase in hardness and strength on standing at room temperature or on heating at slightly elevated temperatures. Other alloys" that, on rapid cooling, are held in the form of homogeneous solid solution (as, for example, certain steels) behave in like manner on heating to somewhat higher temperatures. The observed increase in the hardness and strength of these alloys, referred to as "aging" or as "secondary hardness," is widely accepted as being occasioned, either in whole or in part, by the precipitation in submicroscopic form of such constituents as were held in supersaturated solid solution as a result of cooling in excess of a certain critical rate. In earlier discussions of the cause of age hardening or secondary hardness, the question of the hardness of the precipitated particles does not appear to have been raised. At present, however, the general opinion appears to be that age hardening and secondary hardness are occasioned by the precipitation of hard particles within the supersaturated solid substance.3 The authors may be wrong in their belief that the last is a prevailing opinion. Nevertheless, it is thought that the following experiments,

Jan 7, 1924

By R. S. Botsford

SPECULATION as to when and under what conditions mining may be resumed in Russia by foreign interests is becoming more interesting. Circumstances have changed so completely that all new projects must give careful consideration to the conditions as they exist at this time. For example, it is now estimated that a certain copper company in Russia can produce copper and put it on board ship at seaboard for 8 1/2c. per lb., crediting the copper with the value of precious metals contained. It is further estimated that in some places gold can be produced at a cost of about one-half of its value; platinum can be produced even more advantageously. Transportation, which is absolutely necessary for mines of coal, iron or manganese ore, as well as for an industry consuming either coal or coke, is not so essential for the operation of a gold or platinum dredge when the dredge has once been put into operation; after that, food is the principal material for which transportation must be provided. During 1922 the operators in the Urals, who had combined in a so-called platinum trust, expected to produce about 2340 lb. of crude platinum but the amount actually recovered during that season was reported as only 1620 lb., most of which came from hand workings; Nicolo Pavda had the principal dredges in operation during that year. In preparation for 1923 operations, about $400,000 worth of repair parts were obtained in England. At least two American-built dredges and one Putiloff dredge are reported in operation at Nicolo Pavda and it is supposed that most of the better dredges in the platinum district are now working.

Jan 12, 1923