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By E. W. Davis

The: mysterious Lake Erie price for iron ore, established each spring, determines the maximum price that will be paid during the following season for ore of Mesabi Non-Bessemer base grade. This price is important to the ore producers, hut since most of the ore in the Lake Superior district is owned or controlled by consuming interests, the really important question to them is not the price of ore but how much it will cost them to mine and transport their season's requirements to their furnace plants. However, a few million tons are actually sold each year, and considerable quantities are traded for mixing purposes, and the negotiations lor these sales and trades usually begin with some reference to the Lake Erie price. There is no difficulty with the Lake Erie price itself or with the manner in which it is established, but the system prescribed for determining the values of ores that are not exactly base grade is incomplete. The Lake Erie price takes into consideration only the iron and phosphorus contained in the ore, but when the ore producer is negotiating a sale or trade, he is confronted by the fact that his ore must he studied and the price adjusted, not only on the basis of the iron and phosphorus analyses, as specified by the Lake Erie price, but also on the basis of silica! alumina, manganese, structure, etc. The vague and unsatisfactory methods used in making these adjustments bear some relation to the manner in which the ore is supposed to act in the blast furnace. The ore producer may not understand all of the idiosyncrasies of the blast furnace, but if the smelting-plant operators have a system more accurate than the Lake Erie price method for determining the relative values of different ores, why not pass this information on to the ore producers, so that they can make use of it and perhaps modify their practice in such a manner as to benefit both themselves and their customers? There is a lack of understanding and appreciation between these two groups that may, to some extent, be unavoidable, but in the interests of efficiency and conservation rules that are more accurate and complete than the Lake Erie price method in use at the present time should be established for the guidance of the ore producers. Recently a paper was read before the Eastern States Blast Furnace and Coke Oven Association, by Mr. G. W. Hewitt, Manager Production, Blast Furnace and Coke Oven Department, Wheeling Steel Corporation, in which he explained how his company determines the relative values of different grades of Non-Bessemer ore. This is a very important paper, perhaps not so much on account of the actual calculation methods described as because of the fact that premiums and penalties are shown on Non-Bessemer ores for silica, alumina, phosphorus, and manganese. As pointed out by Mr. Hewitt, the premium and penalty system described may not apply without adjustments to other smelting plants. However, if the various ore

Jan 1, 1941

By E. W. Davis

The: mysterious Lake Erie price for iron ore, established each spring, determines the maximum price that will be paid during the following season for ore of Mesabi Non-Bessemer base grade. This price is important to the ore producers, hut since most of the ore in the Lake Superior district is owned or controlled by consuming interests, the really important question to them is not the price of ore but how much it will cost them to mine and transport their season's requirements to their furnace plants. However, a few million tons are actually sold each year, and considerable quantities are traded for mixing purposes, and the negotiations lor these sales and trades usually begin with some reference to the Lake Erie price. There is no difficulty with the Lake Erie price itself or with the manner in which it is established, but the system prescribed for determining the values of ores that are not exactly base grade is incomplete. The Lake Erie price takes into consideration only the iron and phosphorus contained in the ore, but when the ore producer is negotiating a sale or trade, he is confronted by the fact that his ore must he studied and the price adjusted, not only on the basis of the iron and phosphorus analyses, as specified by the Lake Erie price, but also on the basis of silica! alumina, manganese, structure, etc. The vague and unsatisfactory methods used in making these adjustments bear some relation to the manner in which the ore is supposed to act in the blast furnace. The ore producer may not understand all of the idiosyncrasies of the blast furnace, but if the smelting-plant operators have a system more accurate than the Lake Erie price method for determining the relative values of different ores, why not pass this information on to the ore producers, so that they can make use of it and perhaps modify their practice in such a manner as to benefit both themselves and their customers? There is a lack of understanding and appreciation between these two groups that may, to some extent, be unavoidable, but in the interests of efficiency and conservation rules that are more accurate and complete than the Lake Erie price method in use at the present time should be established for the guidance of the ore producers. Recently a paper was read before the Eastern States Blast Furnace and Coke Oven Association, by Mr. G. W. Hewitt, Manager Production, Blast Furnace and Coke Oven Department, Wheeling Steel Corporation, in which he explained how his company determines the relative values of different grades of Non-Bessemer ore. This is a very important paper, perhaps not so much on account of the actual calculation methods described as because of the fact that premiums and penalties are shown on Non-Bessemer ores for silica, alumina, phosphorus, and manganese. As pointed out by Mr. Hewitt, the premium and penalty system described may not apply without adjustments to other smelting plants. However, if the various ore

Jan 1, 1941

Henry D. Hibbard, New York City (communication to the Secretary): The title of Mr. Sargent's paper is somewhat misleading, since the paper itself relates chiefly to various kinds of annealing and their effects, and in very small part only to heat-treatment proper. This term has a well-defined meaning in steel metallurgf, and always includes a rate of cooling faster than the material treated would have in the open air. In bringing about this accelerated rate of cooling, some medium other than air at rest is brought into contact with the heated steel. Usually a liquid (almost always either oil or water) is employed ; but for certain steels a blast of air, and for others an easily fusible or soft metal, such as led (either solid or melted), may be used. Heat-treatment usually includes also subsequent moderate heating, followed, it may be, with another accelerated cooling.

Jan 1, 1902

By Mungo Park, C. Baring Horwood

This paper is intended, in the light of recent investigations, to call attention to some of the essential features of good practice in sampling and mine-valuation. Mine-sampling may be divided broadly into two classes: (1) development-sampling and cornputatioll of ore-reserves; and, (2) stope-sampling and estimation of stope-values. Development-Sampling. It is with development-sampling only that this paper deals— the term development being taken to mean the opening-up of a mine by cross-cuts, drives, connections, etc., preparatory to actual extraction of the ore for milling. In development-sampling the work of the sampler and the consequent estima-

Jan 1, 1909

By George A. Morrison

THE Columbia Chemical Division of the Pittsburgh Plate Glass Co. is at Barberton, Ohio, 35 miles south of Cleveland. For many years large tonnages of limestone have been brought to the Barberton plant from distant points. The stone is here burnt in vertical kilns, the resultant product then hydrated and the hydrated lime used in chemical processing. To eliminate the expense of these shipments, the company decided to investigate a limestone bed known to exist on company property at Barberton, where the stone is used. The bed lay at a depth of more than 2000 ft. and was known locally as the "Deep Lime." Chemical analyses of sludge from churn-drill holes made some years ago proved that the limestone was of sufficient purity to warrant diamond-drill exploration. Four diamond-drill holes were put down at well-spaced intervals, to represent fairly an area of four miles by one mile. Cores logged as to chemical and physical conditions were found to compare closely, and to corroborate the earlier evidence that the limestone was of superior quality for chemical use. A plant of 300 tons per hour was subsequently decided upon. SITE The yard at the chemical plant was already so congested that location of the projected mine within its area could not be considered. Eventually a site was selected 2 miles northwest of the plant, near the main line of the Erie Railroad. Here 412 acres were owned outright by the company and stone rights were obtained on 250 additional acres. This location required a transportation line of nearly 2 miles (8800 ft.), crossing two major highways, and to avoid interruption of deliveries to the plant, overpasses were planned. GEOLOGY The limestone in the immediate vicinity lies about 2200 ft. below the surface. Geologists* identify this stone as Delaware of Devonian age. It is overlain by 18 ft. of unconsolidated (sand and gravel), 100 ft. of water-bearing sandstone, and finally 2080 ft. of shale into which sandstone in thin layers is interbedded. The contact of shale and limestone is abrupt, flat-lying and very pronounced. Berea sandstone, often found at 520 ft., is absent, but Euclid sandstone was encountered, together with a seepage of oil and a small amount of methane gas. The limestone bed itself is 345 ft. thick, and overlies 200 ft. of gypsum. The lower part becomes dolomitic as it approaches the gypsum. A detailed study of the drill cores indicates that the upper 50 ft, are highest in lime and reasonably low in silica. The physical make-up shows several separating cherty layers. These occur at definite horizons and cause distinct partings, which become horizontal planes of

Jan 1, 1943

By W. F. Vietti

Operations in the Texas Gulf Coast during the past year have resulted in the discovery of a number of new fields arid the extension of a few of the older fields, both by deeper drilling and by lateral development. Twenty-six new oil and gas-producing areas and discovery of oil or gas in three subsequently abandoned wells have been recorded for a total of 29 new fields of varying importance. Producing areas at Conroe, Manvel, Greta, Pierce Junction, Hastings, Dirks, Thompson, Batson, Mykawa, Tomball, Raccoon Bend, Samfordyce arid Saxct have been increased. Primary geologic studies followed by geophysical mapping or straight geophysical prospects have been responsible for the more important discoveries. These methods have further proved themselves an aid to limiting wildcatting to the more prospective areas and as the chief means to discover reserves in the future. Production for 1935 totaled 69,560,720 bbl. as compared with 60,850,-360 bbl. for 1934. Strict proration has been in force throughout the discovery of more oil than has been produced. The number of producing oil wells has steadily increased to 4851 at the end of 1935, as compared with 3858 at the end of 1934, owing in part to the prolonged life, because of proration. There were 1272 oil and gas wells completed during 1935, as against 835 in 1934. New Fields Pertinent data on the new fields discovered during 1935 are includrd in Tables 1 and 2. Hence, the discussion of these discoveries will be limited. Bee County.—Three new gas fields were added during the year: Beeville, discovered by G. M. Church in No. 1 Wood on Sept. 21; Foley, discovered by Dirks Bros. in No. 1 Foley on Feb. 8; and Plummer, discovered by Hynes and Fisher in No. 1 T. M. Plummer on Sept. 2. The three new oil fields added are: Hartzendorf, drilled on fee land by Hartzendorf and completed on May 17 as a small pumper; Ray, southwest of Tuleta, and discovered by Jameson and Burns in No. 1 Campbell

Jan 1, 1936

By W. F. Vietti

Operations in the Texas Gulf Coast during the past year have resulted in the discovery of a number of new fields arid the extension of a few of the older fields, both by deeper drilling and by lateral development. Twenty-six new oil and gas-producing areas and discovery of oil or gas in three subsequently abandoned wells have been recorded for a total of 29 new fields of varying importance. Producing areas at Conroe, Manvel, Greta, Pierce Junction, Hastings, Dirks, Thompson, Batson, Mykawa, Tomball, Raccoon Bend, Samfordyce arid Saxct have been increased. Primary geologic studies followed by geophysical mapping or straight geophysical prospects have been responsible for the more important discoveries. These methods have further proved themselves an aid to limiting wildcatting to the more prospective areas and as the chief means to discover reserves in the future. Production for 1935 totaled 69,560,720 bbl. as compared with 60,850,-360 bbl. for 1934. Strict proration has been in force throughout the discovery of more oil than has been produced. The number of producing oil wells has steadily increased to 4851 at the end of 1935, as compared with 3858 at the end of 1934, owing in part to the prolonged life, because of proration. There were 1272 oil and gas wells completed during 1935, as against 835 in 1934. New Fields Pertinent data on the new fields discovered during 1935 are includrd in Tables 1 and 2. Hence, the discussion of these discoveries will be limited. Bee County.—Three new gas fields were added during the year: Beeville, discovered by G. M. Church in No. 1 Wood on Sept. 21; Foley, discovered by Dirks Bros. in No. 1 Foley on Feb. 8; and Plummer, discovered by Hynes and Fisher in No. 1 T. M. Plummer on Sept. 2. The three new oil fields added are: Hartzendorf, drilled on fee land by Hartzendorf and completed on May 17 as a small pumper; Ray, southwest of Tuleta, and discovered by Jameson and Burns in No. 1 Campbell

Jan 1, 1936

By F. A. Forward, J. Halpern

A new process for extracting uranium from ores with carbonate solutions is described. Leaching is carried out under oxygen pressure to ensure that all the uranium is converted to the soluble hexavalent state. By this method), alkaline leaching can be used successfully to treat a greater variety of ores, including pitchblende ores, than has been possible in the past. The advantages of carbonate leaching over conventional acid leaching processes are enhanced further by a new method which has been developed for recovering uranium from basic leach solutions. This is achieved by reducing the uranium to the tetravalent state with hydrogen in the presence of a suitable catalyst. A high grade uranium oxide product is precipitated directly from the leach solutions. Vanadium oxide also can be precipitated by this method. The chemistry of the leaching and precipitation reactions are discussed, and laboratory results are presented which illustrate the applicability of the process and describe the variables affecting leaching and precipitation rates, recoveries, and reagent consumption. THE extractive metallurgy of uranium is influenced by a number of special considerations which generally do not arise in connection with the treatment of the more common base metal ores. Perhaps foremost among these is the very low uranium content of most of the ores which are encountered today, usually only a few tenths of one percent. A further difficulty is presented by the fact that the uranium often occurs in such a form that it cannot be concentrated efficiently by gravity or flotation methods. In these and other important respects, there is evident some degree of parallelism between the extractive metallurgy of uranium and that of gold and, as in the latter case, it has generally been found that uranium ores can best be treated directly by selective leaching methods. It is readily evident that this parallel does not extend to the chemical properties of the two metals. Unlike gold, which is easily reduced to metallic form, uranium is highly reactive. It tends to occur as oxides, silicates, or salts. Two ores are of predominant importance as commercial sources of this metal: pitchblende which contains uranium as the oxide, U3O51 and carnotite in which the uranium is present as a complex salt with vanadium, K2O-2UCV3V2O5-3H2O. These ores may vary widely in respect to the nature of their gangue constituents. Some are largely siliceous in composition, while others consist mainly of calcite. Sometimes substantial amounts of pyrite or of organic materials are present and these may lead to specific problems in treating the ore. Further complications may be introduced by the presence of other metal values such as gold, copper, cobalt, or vanadium whose re- covery has to be considered along with that of the uranium, or whose separation from uranium presents particular difficulty. In general, there are two main processes for recovering uranium in common use today.'.2 One of these employs an acid solution such as dilute sulphuric acid to extract the uranium from the ore. A suitable oxidizing agent such as MnO, or NaNO, is sometimes added if the uranium in the ore is in a partially reduced state. The uranium dissolves as a uranyl sulphate salt and can be precipitated subsequently by neutralization or other suitable treatment of the solution. The second process employs an alkaline leaching solution, usually containing sodium carbonate. The uranium, which must be in the hexavalent state, is dissolved as a complex uranyl tricarbonate salt, and then is precipitated either by neutralizing the solution with acid or by adding an excess of sodium hydroxide. The latter method has the advantage of permitting the solutions to be recycled, since the carbonate is not destroyed. This is essential if the process is to be economical, particularly with low grade ores. With each of these processes, there are associated a number of advantages and disadvantages and the choice between using acid or carbonate leaching is generally determined by the nature of the ore to be treated. In the past, more ores appear to have been amenable to acid leaching than to carbonate leaching and the former process correspondingly has found wider application. With most ores, acid leaching has been found to operate fairly efficiently and to yield high recoveries. One of the main disadvantages has been that large amounts of impurities, such as iron and aluminum, sometimes are taken into solution along with the uranium. This may give rise to a high reagent consumption and to difficulties in separating a pure uranium product. Excessive reagent consumption in the acid leach process also may result

Jan 1, 1955

By Shiou-Chuan Sun

Most previous work on sedimentation of coal1 and mineral2,3 suspensions has been conducted in graduated 1-liter glass cylinders of 6-cm diam. With this type of large container it is often difficult to see through the suspension and tedious to perform a large number of tests. Furthermore, the heavy glass walls and the graduation lines of glass cylinders cause internal and stray reflections, respectively. To obviate these difficulties, an Atlab Emulsion Viewer from Arthur H. Thomas Co. was adopted as an alternative apparatus. Equipment: The viewer,4 shown in Fig. 1, consists of: 1) a stainless steel frame rack holding 21 flat-bottom Nessler tubes or an ungraduated replica 1.64 cm ID and 1.80 cm OD, 2) a movable masked 150-w lumaline lamp behind the tubes, and 3) a scaled glass panel with 100 vertical divisions in front of the tubes. The tubes are snugly held by springs in slots formed by spacer bars, which also serve as shields to eliminate stray light. The lumaline lamp is mounted behind a slit in a movable housing so that it can be positioned behind the suspension to be examined. The lowest or 100-division line on the front glass plate is leveled with the upper side of the bottom of all tubes. The scaled portion of each tube, roughly 19 cm high and 40 ml in volume, is used to study coal and mineral suspensions.

Jan 1, 1959

By J. Q. Ehrgott

INTRODUCTION The U. S. Army Engineer Waterways Experiment Station (WES), under sponsorship of the Defense Atomic Support Agency, has recently developed a unique dynamic high-pressure triaxial testing device (DHT). The device permits acquisition of both axial and lateral deformation data while undisturbed soil and/or rock specimens are subjected to various states of controlled impulsive-type stresses produced by varying both the axial stress and the radial stress rapidly with time. The device is used to develop controlled dynamic pressure pulses within the triaxial chamber fluid on soil or rock test specimens to 3 inches in diameter. Controlled dynamic axial pulse loads are delivered to the specimen by a piston driven by an existing pneumatic ram loader (SECO). The DHT consists of a triaxial cell and a pressure supply and decay system which permits the chamber pressure to be varied with time. Together the DHT and SECO operate in a testing program so as to provide time varying confining pressures and axial loads to test specimens at independently controlled but synchronized programmed rise, hold, and decay times. Rise time is defined as the time from zero load or pressure to peak load or pressure; hold time is the time of constant peak load or pressure; and the decay time is the time from peak load or pressure to zero load or pressure. The maximum dynamic confining pressure attainable is approximately 15,000 psi and the fastest rise and decay times are 3 millisecond (msec) and 20 msec, respectively. This paper presents a description of the DHT, the necessary support equipment, and details of the measurement system. Performance evaluation tests conducted on clay siltstone and a Cretaceous sandstone are presented since the results demonstrate some of the capabilities of the device and show some of its characteristics.

Jan 1, 1971

By Henry F. Cooper, Scott E. Blouin

Large jacking test procedures that have been applied to obtain static in-situ rock properties (Ref. 1) have shown that the in-situ rock modulus and strength can be considerably less than what would be obtained from laboratory tests on intact samples. This trend is also expected to be true for dynamic properties, but few dynamic in- situ rock property tests have been conducted. During the past several years, high explosive test procedures have been developed to simulate the airblast and direct induced ground motions (Ref. 2) produced by nuclear explosions . These test procedures load large volumes (up to 10 7 f t3) of the earth with stress levels sufficiently high to produc5 feet of particle displacement over surface areas up to l0 5 ft2. This paper discusses some of the data obtained, and the implications of these results for our understanding of the dynamic response of in-situ rock. DESCRIPTION OF TEST PROCEDURES As shown in Fig. 1, the High Explosive Simulation Technique (HEST) consists of a cavity of uniform height bounded on the sides by a soil berm, above by an overburden of uniform thickness, and below by the test bed on the earth's surface. Horizontal racks of detonating cord are placed in the cavity and detonated at one end of the test bed. This detonation produces an explosive wave that propagates across the test bed, loading the earth with an overpressure pulse that decays with time because of the compression and lifting of the overburden. Since 1964, there have been approximately 40 such tests on test bed areas ranging from a few hundred to l0 5 sq ft., simulating peak overpressure conditions between about 100 and 6000 psi and specific impulses between a few and over 100 psi-sec.

Jan 1, 1971

By Malcolm McColl, C. A. Mead

Thin films (of mica have unique attributes that are exceptionally good for studies of high-field conduction mechamisms in thin-film insulators and the quantum mechanical tunneling of electrons from metal to metal. The principal advantages of using mica films are that the films are crystalline and the cleavage planes occur every 10Å. This property results in films whose thicknesses are integral multiples of 10Å and whose surfaces are uniformly parallel over sizable areas. Hence, very well-defined metal -mica-metal structures are possible. Furthermore, the fact that the insulator is split fro??! a bulk sample allows the index of refraction, dielectric constant, forbidden energy gap, and trapping levels and their density- to be obtained directly from measurements performed on thick samples Of mica rather than requiring that these properties be interred from the conduction characterrsties alone. In the work to he described, all the cleaving was done in a high vacuum just prior to the evaporation of metal elertrodes so as to avoid air contamination at the interfaces. Results of these studies indicate that the current through the 30 and 40Å films exhibited quantitative agreement with the theoretical voltage and temperature dependence derived by Strallon for the tunneling of electrons directly from metal to metal. Thicker films at room temperature exhibited volt-ampere curves suggesting Schottky emission of electrons from the cathode into the conduction band of mica. However, the thermal activation energy was smaller than that found from other measurements, and the experimsntal Schottky dielectric constant was larger than the square of the index of refraction. These facts would indicate that the electrons were being injected into polaron stales ill the iusulator. At low temperatures and high fields, the current through the thicker films did not exhibit the Fowler -Nordheim dependence as would be predicted by a simple extention of the theory of field emission into a vacuum. THE mechanism of electrons tunneling through insulating films has received considerable attention in the last few years due to the devices possible utilizing tunneling'-4 and the success of tunneling in the study of superconductivity.5,6 Until the recent paper by Hartman and chivian7 on the study of aluminum oxide, there had been no reported successful quantitative experimental fit to the theory. Their method of fabrication necessarily results in a polycrystalline insulator, the stoichiometry of which is nonuniform from one side to the other. This structure also introduces complications to the shape of the barrier which is set up by the insulator since the insulator possesses a spatially nonuniform band structure and dielectric constant. Due to these facts an analysis of the data in terms of a pviori barrier shape is of questionable validity. The use of muscovite mica not only overcomes these disadvantages but, as an insulating thin film, provides physical properties (dielectric constant. trapping levels and their densities, forbidden energy gap, and so forth) that are identical to the easily measured values of the bulk sample. Furthermore, it is a single-crystal insulator whose cleavage planes (10Å apart8,9) provide uniformly parallel surfaces of well-known separation. This material is therefore ideally suited to the study of electron-transport phenomena. Von Hippel10 using a 6.5-µ-thick sample was the first to observe the high-field conductivity (=5 x l06 v per cm) of mica. No attempt was made to develop an empirical formula, but Von Hippel concluded from intuitive arguments that the current was being space-charge limited by trapped electrons. Mal'tsev11 in a more recent investigation at high fields observed a dependence of the conductivity a on the field F of the form exp(ßF1/2). This dependence was attributed to the Frenkel effect,12,13 a Schottky type of emission from filled traps. No mention in the English abstract was made of the thicknesses of his samples or, and more important, of how well the value of ß fit Frenkel's theory. In 1962 Foote and Kazan14 developed a technique for splitting mica to a thickness of less than 100Å and observed a dependence of the current density j on the field of the form j = jo exp(ßF1/2) on a thin sample thought to be 40Å thick. Assuming that this was a Schottky emission process and that the appropriate dielectric constant for such a mechanism would be closer to a low-frequency value of 7.6, Foote and Kazan calculated from ß an independent thickness of the mica of 36Å. No further investigation was made of the phenomenon. However, the work reported in this paper indicates that the film measured by Foote and Kazan was probably 60Å thick, the error arising from the measurement of the very small metal-insulator-metal diode areas that were used, along with the diode capacitance and dielectric constant, to calculate the thickness. In the research reported in this paper, Foote and Kazan's technique was modified to cleave muscovite in a vacuum of 10-6 Torr, immediately after which metal electrodes were evaporated creating Au-mica-A1 diodes. Aluminum was chosen because of its strong adhesion to mica, as necessitated by the

Jan 1, 1965

By C. M. EYE

IN the spring of 1905 I was employed by Messrs. Bradley and Requa, under our fellow member, Thomas Cox, on the mill plans for the Nevada Consolidated, when an opportunity came to go to the Philippines to erect a small mill on the property of the Benguet Consolidated. This I accepted, expecting to be away eight months or so, but it was seven years before I got back. .I sailed in May, on the Coptic, having as room-mate as far as Kobe, A. E. Drucker, who was going out to Korea for the Oriental Consolidated. It was the first trans-ocean trip for either of us, and we had some rather unusual experiences. This was toward the close of the Russo-Japanese war and the Russian fleet was known to be on the way from Suez to Asiatic waters, but it was a matter of doubt whether they would risk a passage between Japan and the mainland, or take the longer but obviously safer route outside of Japan. The Coptic carried much contraband of war for Japan, so naturally did not care to meet this fleet. No definite word being available at Honolulu, we went to the Midway Islands, but the cable station there had very little information to offer, so we proceeded cautiously toward Japan. On the last afternoon out, we steamed due north at half speed for several hours, and finally sneaked into Yokohama at night, to learn that ' the Russian fleet had met the Japanese the day before and had been annihilated. We sailed over the spot in the Sea of Japan a week later, and when we got to Manila we found three of the Russian boats interned and being guarded by the monitor Monadnock and a cruiser. This was only a matter of form, as the Russians were only too glad to be there for the rest of the war, and the boats could not have gone far anyway, for they were literally shot to pieces. The Admiral's flagship had a hole within 3 ft. of the water line, for ward, through which a man could enter by stooping.

Jan 1, 1929

By R. F. Mehl, R. F. Bunshah

A fast amplifier technique has been developed for the measurement of the rate of propagation of martensite in an Fe-29.5 pct Ni alloy. The time of formation of one plate of martensite is 3x10 sec and the rate of propagation is 3300 ft per sec approximately. IT has been known for some time that the plate-like structural unit of martensite forms from austenite with great rapidity. Wiester1 and Hane-mann, Hofmann, and Wiester took motion-pictures of the transformation as it occurs in a 1.65 pct C steel; they demonstrated that a single plate formed fully in the time interval between successive frames, viz., 1/20 sec, thus setting an upper limit. Forster and Scheil,3 using an Fe-Ni alloy with 29 pct Ni, recorded the sonic characteristics of the process electrically, upon an oscillograph, setting the upper time limit at 0.002 sec. Forster and Scheil,~ measuring the change in electrical resistance in the same alloy upon a cardiograph, set a limit of 0.02 sec. Forster and Scheil5 later, employing the same alloy, improved their technique, reporting an upper limit of 7.10 sec. In studying signals of such short duration, it is an important question whether the frequency response of the electrical system used is high enough compared to frequency of the pulse measured, or, put differently, whether the system is able to reproduce without distortion the signal arising, in this case, from the formation of a single martensite plate. Forster and Scheil (referring only to their last paper) obtained signals of a frequency of 30 kilocycles (hereinafter kc); this was about the frequency response of the equipment used; thus, if the signal had a frequency higher than 30 kc, it would still appear as a signal of frequency 30 kc. All of these results thus provided upper limits only. Recent developments in electronics have made available equipment with very high frequency response, very high sweep-speeds, high gain, etc. The electrical characteristics of such equipment, used in the present study, are given in Table I. Such equipment offers obvious attraction in the study of the rate of propagation of a martensite structural unit—and perhaps of other structural alterations proceeding at a very high rate. This paper reports an attempt to develop a technique employing such equipment to measure the time of propagation of a martensite structural unit and the variation of this with temperature, with the mode of formation—athermal and isothermal—in both polycrystalline and single-crystal samples; and from such measurements to obtain the rate of propagation. As will be seen, the results obtained are useful theoretically. Materials All data presented here are for an Fe-Ni alloy of the following analysis: 29.5 pct Ni, 0.027 pct C, 0.135 pct Mn, 0.094 pct Si, balance Fe. There were several reasons for choosing this alloy: 1—it is substantially the one used by previous investigators; 2—it exhibits both the athermala and the isothermal' mode of formation of martensite, both studied in detail by Machlin and Cohen; 3—the subzero temperatures of transformation in this alloy are experimentally very convenient; 4—it exhibits the "burst phenomenon";" 5—the change in electrical resistance upon the formation of martensite, a decrease, is great, approximately 50 pct.' The polycrystalline specimens were in the form of wires of 0.025 in. diameter; the single crystals were 1x1/4x1/4 in. Experimental Methods Electrical Apparatus: Fig. 1 is a schematic drawing of the electrical circuit used. The principle used in these measurements is the same as that used by Forster and Scheil." A small direct current, about 1 to 2 amp, is passed through the sample. When a martensite plate forms, the resistance of the sample changes and a high frequency signal is generated. This signal is picked up by the probes attached to the sample, fed into the bank of amplifiers and thence to the vertical deflection plates of a cathode-ray oscilloscope. The signal itself triggers the oscilloscope trace which flashes across the tube face and is photographed by means of a 35 mm movie camera at the end of a light-tight hood. The camera has no shutter. As soon as the signal flashes

Jan 1, 1954

By P. D. Hunt, B. Tani, M. G. Chasanov, R. Schablaske

The Zn-Vphase diagram was studied by thermal. metallographic, X-ray, and sampling techniques. Three ternary phase equilibria were observed: Mutual solid solubilities in vanadium and zinc appear to be negligible. The liquidus line is retrograde from 670° to 756°C. 1 HE only information in the literature relating to the Zn-V system was a study of corrosion of vanadium by liquid zinc' and an examination of the effectiveness of zinc coatings in protecting vanadium-base alloys from oxidation at high temperatures.2 Establishment of the Zn-V phase diagram was undertaken as part of a study of transition metal solubilities in liquid metal solvents. Chemical, metallographic, thermal, and X-ray diffraction analyses were used to determine the diagram. MATERIALS AND EXPERIMENTAL PROCEDURES Vanadium (99.86 pct) in the form of powder and small chips was employed. Stick zinc (99.99 pct; major impurities: 10 to 15 ppm Pb and 20 ppm Cu) was used in the liquidus determinations and thermal analyses; zinc powder (98.80 pct) was used to prepare intermediate compositions. The liquidus lines were determined by chemical analysis of filtered samples of the saturated melts. The apparatus and sampling techniques were similar to those described by Martin, et al.3 The entire metal sample was dissolved to preclude analytical errors due to segregation on cooling. Vanadium was determined amperometrically, using iron (11) as the titrant,4 to an estimated accuracy of 1 pct. Standard techniques of thermal analysis were employed to examine alloy specimens contained in alumina crucibles under helium. Heating and cooling rates were about 1°C per min. At least five heating and cooling cycles over the range 420° to 700°C were performed for each of two Zn-15 pct V alloys. A Zn-0.2 pct V alloy was used in the determination of the eutectic temperature. The separation of intermediate phases from zinc-rich alloys was carried out by selective leaching with ammonium nitrate solutions. For further investigation of intermediate phases 1/4 in. diam powder compacts were prepared by pressing at 80,000 psi and were annealed in argon at 415" to 450°C for 10 days. Larger quantities of intermediate phases were prepared in sealed tantalum capsules heated in a rocking furnace. Temperatures were determined to an estimated accuracy of 0.5°C with a Pt/Pt-10 pct Rh thermo-

Jan 1, 1963

By R. S. Wagner, W. C. Ellis

A new mechanism of crystal growth involving oapor, liquid, crnd solid phases explains many observations of the effect of implurities in crystal growth from the vapor. The role of the impuuitq is to form a liquid Solution with the crystalline tnalerial to be grown from the vapor. Since the solution is n prefevred site for deposition firorti the uapor, the liquid becorrles supersaturated. Crystal growth occurs by precipitatzon from the supersaturated liquid crt tlie solid-liquid zntevfnce. A crystalline defect, such as a screw dislocation, is not essetztial for VLS (vapor -liquid-solid) growth. The concept of the VLS mechanism is discussed in detail with reference to tire controlled growth of silicon crystals using gold, platinum, palladium, nickel, silver, or copper as an implurity agent. RECENTLY a short communication' described a new concept of crystal growth from the vapor, the VLS mechanism. In this paper we present a detailed description of the process and its application to the growth of silicon crystals and we discuss its relevance to existing concepts of .'whisker" crystal growth. Crystal growth from the vapor is usually explained by a theory proposed by Frank2 and developed in detail by Burton, Cabrera, and Frank.3 In this theory a screw dislocation terminating at the growth surface provides a self-perpetuating step. Accommodation of atoms at the step is energetically favorable, and is possible of much lower supersatu-ration than required for two-dimensional nucleation. Crystals of a unique form resulting from aniso-tropic growth from the vapor are "whisker" or filamentary ones. Such crystals have a lengthwise dimension orders of magnitude larger than those of the cross section. For most filamentary crystals both the fast-growth direction and directions of lateral growth have small Miller indices. The special growth form for a whisker crystal implies that the tip surface of the crystal must be a preferred growth site. sears4 proposed that, according to the Frank theory. a whisker contains a screw dislocation emergent at the growing tip. Such an axial defect provides a preferred growth site and accounts for unidirectional growth. The hypothesis was extended by Price. Vermilyea. and Webb," still implying the presence of a dislocation at the whisker tip. They postulated that impurities arriving at the fast-growing tip face become buried while those arriving on the surface of slow-growing lateral faces accumulate and thereby hinder growth. These considerations led to a whisker morphology. There is increasing evidence that most whisker crystals grown from the vapor are dislocation-free. Webb and his coworkers6 searched for an Eshelby twist7 in zinc? cadmium, iron. copper, silver, and palladium whisker crystals. They found unequivocal evidence for an axial screw dislocation in only one element, palladium. However, not every palladium crystal examined contained a dislocation. Observations with the electron microscope have failed to show dislocations in whisker crystals of zinc, silicon.9 and one morphology of AlN.10 Since many whiskers are completely free of dislocations, an axial dislocation does not appear to be required for whisker growth of many substances. A significant advance in understanding whisker growth has been a recognition of the need for impurities. This requirement has been clearly demonstrated for copper,11 iron,13 and silicon9-1 whiskers. For silicon, detailed studies proved conclusively that certain impurities, for example, nickel or gold, are essential. Another pertinent phenomenon which has received little attention is the presence of a liquid layer or droplets on the surface of some crystals growing from the vapor. Crystals in which this has been observed include p-toluidine,14 MoO3,15 ferrites,16 and silicon carbide.'" The liquid layers or globules were considered to be metastable phases, molecular complexes, or intermediate polymers originating from condensation of the vapor phase. The possibility has been suggested that the halide being reduced is condensed at the tip18 or adsorbed on the surface11 of a growing metal whisker, for example copper. The literature on whiskers discloses illustrations of rounded terminations at the tips. These appear. for example, on crystals of A12O3,19,20 sic,21 and BeO.22 For BeO, Edwards and Happel suggested that during growth of the whisker the rounded termination consisted of molten beryllium enclosed in a solid shell of BeO. A recent paper9 on the growth of silicon whiskers contains many observations pertinent to an understanding of the mechanisnl of whisker growth. These observations are summarized as follows. 1) Silicon whiskers are dislocation-free. 2) Certain impurities are essential for whisker growth. Without such impurities the silicon deposit is in the form of a film or consists of discrete polyhedral crystals.

Jan 1, 1965

By Oliver C., Ralston

THE following data were obtained during Tan exhaustive research into the possibilities of concentrating United Verde massive sulfide copper-zinc-iron ores by flotation. The composition of these ores approximates the following mineralogical analysis: 3 to 15 per cent chalcopyrite; 3 to 11 per cent marmatite (ferruginous sphalerite) ; 47 to 69 per cent pyrite; and 10 per cent quartz. The remainder is usually schist gangue. The sulfide minerals are finely dis-seminated; chalcopvrite and marmatite begin to be liberated on grinding at about 100 mesh, but complete liberation from gangue (pyrite in this case is considered a gangue mineral) is

Jan 1, 1935

By H. I. Aaronson, C. Wells

Configurations of ferrite crystals have been found in a plain carbon steel which appear to have resulted from the nucleation of new ferrite crystals at the interphase boundaries of previously formed crystals despite the high carbon concentrations which necessarily develop at these boundaries. This phenomenon has been termed sympathetic nucleation. An attempt has been made to reconcile the occurrence of sympathetic nu-cleation with current nucleation theory. THIS investigation is one of a series on the formation of proeutectoid ferrite from austenite. From the viewpoint of chemical composition, this reaction consists of the nucleation and diffusional growth of crystals of carbon-poor ferrite within a matrix of carbon-rich austenite. The austenite adjacent to the austenite-ferrite boundaries will be greatly enriched in carbon, approximately to the value of the y/(a + y) equilibrium curve or its metastable extrapolation at the temperature of transformation. Those areas of austenite appreciably farther removed from the growing ferrite, on the other hand, will be relatively unaltered in composition, especially at the earlier stages of transformation. Since rates of nucleation are considered to decrease exponentially with decreasing supersaturation,' the frequency with which ferrite nuclei appear at austenite-ferrite boundaries should be negligible in relation to that at which they form in other regions of the austenite. During this investigation, however, many groupings of ferrite crystals have been found which appear to have resulted from the nucleation of ferrite at austenite-ferrite boundaries. This phenomenon has been given the name of sympathetic 71.1tcleation. A number of micrographs of morphological configurations caused by sympathetic nucleation will be presented, after which an explanation for this reaction will be proposed in terms of current nucleation theory. Some of the structures to be considered are composed of bainite, an aggregate of ferrite and carbide, rather than of ferrite. Since ferrite and bainite differ only in that bainite forms under conditions which result in the nucleation of carbides behind the advancing austenite-ferrite boundaries,' it will usually be unnecessary, for the purpose of this paper, to distinguish between the two reaction products. All studies were performed on an electric furnace steel (obtained from the Vanadium Alloy Steel Co.) containing 0.29 pct C, 0.76 pct Mn, 0.25 pct Si, 0.005 pct P, and 0.007 pct S. The alloy was cast as a 150 Ib, 7x7 in. cross section ingot and forged into bars 2x2 in. in cross section. These bars were homogenized for 48 hr at 1250°C in an Endo-Gas atmosphere. The depth to which decarburization penetrated during this heat treatment was determined by chemical and microscopic analyses and the affected metal was removed by machining. Specimens for isothermal transformation studies were cut from the remaining material; most of these specimens were 1/2x1/4X1/16 in., though some with a thickness of 1/32 in. were prepared for use at the shorter reaction times and lower reaction temperatures. Specimens were austenitized for 30 min at 1300°C, isothermally reacted for various times at temperatures ranging from 775" to 475 "C, and then quenched in iced water. The austenite grain sizes within individual specimens ranged from ASTM Nos. 1 through —4. A commercial heat-treating salt which was continuously deoxidized by an immersed graphite crucible served to minimize the loss of carbon during austenitizing; thick covers of powdered graphite and immersed graphite rods effectively prevented decarburization in the lead pots employed for the isothermal reaction treatments. The heat-treated specimens were sectioned and mounted in Bakelite. Following the completion of standard grinding and mechanical polishing procedures, the specimens were electrolytically polished with a Buehler-Waisman apparatus and etched in 2 pct nital. Experimental Results Rules of Evidence for Sympathetic Nucleation—On the basis of observations made on a single plane of polish, one precipitate crystal may be considered to have been sympathetically nucleated at the inter-phase boundary of another precipitate crystal when the following conditions are fulfilled: 1) The sympathetically nucleated crystal is not in contact with a grain boundary or a subboundary in the matrix phase. 2) The shape, size, and location of the crystal at whose boundary sympathetic nucleation occurred (hereafter termed the base crystal) and the crystal formed by sympathetic nucleation substantially pre-clude the possibility that the plane of polish em-ployed may have concealed the fact that both crys-tals actually nucleated at a grain boundary or a sub-boundary in the matrix phase.

Jan 1, 1957

By S. Leber

Pole figures and pole distributions were used for the quantitative detevinination of the preferred orientations in swaged tungsten rods and the effect of subsequent wire drawing on the texture. In the swaged rod, the preferred orientation could best be described as a pseudo (111-112) [110] cylindrical texture. A secondary component was assigned the indices (110) [001]. Further reduction by swaging retained these cylindrical textures. Wire drawing caused lattice rotations about the wire axis, converting the cylindrical texture into a normal fiber texture. The conversion was initiated and proceeded lnost rapidly in the center of the wire. The (110) /001] component was converted into a (110) fiber texture by wire drawing. The effective rotations were about axes contained in the lransverse plane. The preferred orientation associated with tungsten wire usually has been assumed to consist of a (110) fiber texture. This implies rotational randomness around the wire axis. Leber1 has shown that rotation about the wire axis may be restricted resulting in a preferred orientation designated as a cylindrical texture. Specific crystal planes tended to remain aligned parallel to the wire surface. This texture seemed to be the result of the swaging operation used in the intermediate stages of fabrication. Bhandary and cullity2 detected similar textures in swaged iron wires. Peck and Thomas3 suggested that the preferential alignment of crystal planes parallel to the wire surface was the result of tangential flow, characteristic of swaging. Wire drawing, following swaging, twisted the crystals about axes parallel to the wire axis, converting the cylindrical texture into a normal fiber texture.4 In this investigation, quantitative techniques were used to more accurately characterize the cylindrical texture and to study its conversion into a normal fiber texture. PROCEDURE The material investigated was lamp-quality tungsten. Three ingots were rod-rolled and swaged to 112 mils diameter, and were then drawn to 10-mil wire. Samples were obtained after each drawing pass. (110) and (200) pole figures were obtained from samples prepared as shown in Fig. 1. To form the sample shown in Fig. l(a), l-in. lengths of wire were glued side by side to form a l-in. square. The composite was ground and electropolished to form a diametral reference surface. For certain specific tests, samples were prepared as shown in Fig. l(b). This composite was made from 10-mil-thick strips prepared by grinding on parallel longitudinal planes. The polished reference surface in this case was, in essence, the wire surface. The two forms of samples [~igs. l(a) and l(b)] were related by a 90-deg rotation around the wire axis. Because of ease in preparation, most data was obtained from the diametral samples. The X-ray data were obtained using a Siemen's pole-figure goniometer. These data were not corrected for absorption or defocusing effects, since only the angular locations of the intensity maxima were of interest. Regions of the pole figure more than 80 deg from the center were not investigated. Partial monochromatization was achieved by the use of unfiltered copper radiation and a krypton-filled proportional counter. No evidence of spurious white radiation effects5 could be detected. Therefore, more elaborate X-ray techniques were not required. Intensity levels were chosen to show all pertinent details of the orientation distributions. The reference plane for the pole figures was the diametral section. The orthogonal reference directions, shown in Fig. 1, were the wire axis, the radial axis per-

Jan 1, 1965

By W. M. McKewan

Dense magnetite pellets were reduced in hydrogen-water vapor-nitrogen mixtures over a temperature range of 400° to 500° C at a pressure of 0.97 atm. The rate of reduction per unit area was found to be constant with time and directly proportional to the partial pressure of hydrogen at a constant ratio of water vapor to hydrogen. Water vapor poisoned the oxide surface by an oxidizing reaction and markedly slowed the reduction. The enthalpy of activation was found to be + 13,600 cal per mole. THE investigation of the reduction of iron oxides has been the subject of numerous papers. Most of these papers have dealt with the evaluation of various ores, both magnetite and hematite. There have

Jan 1, 1962