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By A. Gatti

Studies were made on the system iron plus alumina. Various methods of dispersing and various amounts of alumina were used. Powder metallurgy techniques were used to produce the final product. Microstructures and some mechanical properties are presented. Alloys containing up to 16 pct alumina by weight are ductile at all temperatures tested. The ivon-alumina materials have a higher yield stress and improved creep resistance over that of pure iron. SINCE the development of SAP' an A1- Al2O3 powder metallurgy product, great interest has been shown in the development of a SAP-like structure in metals and alloys other than aluminum. The outstanding properties of this class of materials are: 1) Good creep resistance at high temperature. 2) High yield strengths and high hardness at high temperatures. 3) High recrystallization temperature. However, the lack of ductility and formability has thus far limited the applications of SAP-like materials. The following report deals with methods of dispersing A12O3 in Fe, processing of powders into rod, structures produced after processing, and mechanical properties of the iron-alumina material produced. Methods of dispersing the alumina and also the volume fraction of alumina added were varied. MATERIAL Powder Processing— Four methods of obtaining dispersions of alumina in iron were studied. 1) Oxidation-reduction of a Fe + 8 pct Al alloy. .2) Coprecipitation of Fe(OH)3 + Al(OH)3 from aqueous solution. 3) Colloidal mixing of Fe,O3 and Al2O3. 4) Colloidal mixing of Fe powder and A1,O3. Fig. 1 is a processing flowsheet which outlines the processing steps taken to produce a final extruded bar 1/4 in. in diameter and about 30 in. long. The - 100 mesh iron-aluminum alloy was oxidized by placing a thin layer of powder on an alumina plaque. The reduction step was modified to include 1/2 hr at 1000°C since the powders tended to become pyro-phoric unless sintered slightly after low-temperature reduction. Compacting was done in a 1-1/8-in.-diam pressing die. The slugs produced averaged 1 in. in length. The billets were encased in low-carbon steel cans shown schematically in Fig. 2. The blank is included for structure and property comparison purposes. TESTING PROCEDURE All tests were made on as-extruded material.

Jan 1, 1960

By N. O. Taylor

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

Jan 1, 1927

By Robert R. Walden, LeMont West

K ENTUCKY'S first acid-grade fluorspar flotation Kmill, shown in Fig. 1, was placed in operation Aug. 1, 1952, by the Pennsylvania Salt Manufacturing Co. at Mexico, Ky. During 1951 a critical shortage of acid-grade fluorspar developed and it became necessary for the company to produce part of its fluorspar requirements. In 1951 the company purchased the Crider and Lennen metallurgical fluorspar mill and an adjacent stockpile of tailing at Mexico, Ky. The tailing, assaying about 26 pct calcium fluoride, originated from log washer and jig mill concentrators in the area. As the mill did not have a fluorspar dryer or convenient rail facilities, the company leased the Burleson concentrator at Marion, Ky., where these facilities were available. At Marion, Ky., on the Illinois Central Railroad, dry acid-grade fluorspar is transported direct to the company's Calvert City, Ky., hydrofluoric acid plant. The Mexico flotation plant was reconditioned and designed to produce acid-grade fluorspar from the jig tailing stockpile. The new plant flowsheet is shown in Fig. 2. The ore feed, old tailing, which contains 10 pct of waste rock and coarse gravel assaying approximately 8 pct CaF,, is bound together by sticky clay

Jan 1, 1955

By W. O. Milligan, J. L. McAtee

THE constitution and structure of the hydrous forms of aluminum oxides and hydroxides have been studied in the laboratory of the Depart¬ment of Chemistry at Rice Institute for almost three decades. Progress reports have been made from time to time 13,17,18 summarizing and evaluating the existing state of knowledge concerning the complex inorganic system A12Oa-H2O. X-ray and electron diffraction analysis, together with dehydra¬tion isobars and isotherms, have been the most useful methods for increasing the understanding of the structure and interrelationships of the various forms of alumina and aluminum hydroxides. The purpose of this paper is to bring up to date the information now available, in the hope that a clearer understanding of the structures of these materials may prove useful in aiding mineralogists and geologists in studies of the genetic significance of the aluminum hydroxide minerals, and possibly of the closely related clay minerals. Early investigators found the system alumina-water to be confusing, since, prior to X-ray diffraction examination, it was not possible to clearly identify and characterize the various crystalline forms. One could not be certain as to whether or not different investigators were working with the same chemical individuals. In later studies, including some from the authors' laboratory, addi¬tional confusion resulted from difficulty in preparing pure samples of the various aluminum hydroxides and in obtaining relatively large crystals of dimensions above the colloidal range of particle size. Even at present, it is difficult to establish sets of interplanar spacings for the several forms of the aluminum hydroxides, as illustrated by the 29 different X-ray diffraction pat¬terns listed in a current publication. The nomenclature of the aluminum hydroxides is also extremely confus¬ing, inasmuch as two different systems are employed by large groups of in¬vestigators. Plans are being made to formulate a uniform system of nomen¬clature but in this report the designations employed will agree with previous papers from the same source.13,17,18 Four forms of crystalline aluminum hydroxides may be considered to be well defined and recognized, which, together with hydrous alumina "amor¬phous to X-rays," comprise an exceedingly complex inorganic system. Several

Jan 1, 1952

By S. D. Warriner

ONE of the most, if not the most, difficult of the problems associated with the mining and distri-bution of anthracite is to get clearly into the minds of the consumers and of the editorial and reporto-rial writers in the public press the relationship between the cost of production, the price at the mine and the price that the consumer pays for his coal, delivered in the cellar. One sees in his morning paper a statement to the .effect that out of the $12 or $13 per ton that his dealer charges him, the miner gets only $2 or even less, and he asks himself or the paper asks for him, "Who gets the difference?" Not infrequently the amount that the miner gets is given for run-of-mine bituminous coal while the price quoted is that of prepared anthra-cite, egg, stove, or chestnut, as the case may be, delivered to the bin of the consumer; and the difference stands out with all the more prominence; and it sticks in his memory with a persistency which no manner of explanation is able to efface. A recently published official report for the year. 1921 of one of the State Bureaus stated the total production of anthracite in net tons of 2000 lb., and included not only the output recovered by washeries from old culm banks and by dredges from creek and river channels, but also the colliery consumption;, i.e., the coal used by the companies in the operation of the collieries. This resulted in a total production of 90,509,075 net tons for which the labor cost was stated at $283,961,300, or $3.13 per net ton, equivalent to $3.50 per gross ton. This figure of $3.50 was immediately seized upon as representing the labor cost per gross ton of fresh-mined commercial coal. It is almost a hopeless task to try to correct such errors of statement in the first place, and, in the second place, to correct the misapprehen-sions that arise from them. As a matter of fact, the report was misleading in regard to the labor cost of the entire production shipped, as the coal used for colliery consumption should be deducted. Correctly stated, the report should have shown, calculated in terms of gross tons of 2240 lb., the legal weight in Pennsylvania, as follows: Gross production 80,607,359 tons Less colliery fuel 8,757,137 tons Commercial production 71,850,222 tons Total labor bill $283,961,300.00 Labor cost per ton...: 8 3.952 The foregoing figures" of tonnage are obtained from the State Department of Mines. Even these include the quantity recovered from calm, banks by washeries, and consequently the $3.95 arrived at as the average labor cost is somewhat less than that actually involved in the mining of fresh-mined coal. Unfortunately, the figures of washery production and the cost of producing it are not available.

Jan 7, 1922

By E. S. Rowland, J. Welchner, R. H Marshall

This paper presents results on an extension into the realm of high-carbon steels of some work recently published1 on the effects of time at temperature, quenching temperature and prior structure on the hardenability of one 0.20 and four 0.40 per cent carbon alloy steels. It was shown at that time that unless the conditions of time, temperature and prior structure are substantially the same in performing the hardenability test as in conducting hardening of parts in production, the correlation of hardenability information with the hardness and properties of production parts is often not of satisfactory accuracy. The general effects of these variables on the austenitic grain size, distribution of excess carbides and critical cooling rate have been known for many years and one or more have been investigated by Shepherd,2,3 Davenport and Bain,4 Digges,5,6 Digges and Jordan,' Post and associates8 and Roberts and Mehl,9 to mention only a few. There has been no systematic investigation, however, into the quantitative variations produced on the hardenability of commercial high-carbon steels by changes in these factors of time, temperature and prior structure. Procedure A plain carbon hypereutectoid steel, S.A.E. 52100 and Graph-Mo, a molybdenum-bearing high-carbon steel containing some graphite, were chosen for this investigation. The chemical analyses of these electric-furnace steels are given in Table I. The procedure used was exactly that reported previously,' hence the details will not be repeated here. Normalized (165o°F.) and spheroidized prior structures were utilized on all steels with hot-rolled and quenched (I600°F. oil) prior conditions added for the plain carbon steel. The end-quench test developed by Jominy10 was sclected for use in this investigation and, with the noted exceptions, the American Society for Testing Materials standard procedure was followed. The effect of time at temperature was examined at intervals of o, 10 and 40 min. and 4 hr., and a few 16-hr. tests were run. Salt-bath heating of the specimens was employed to control and minimize the

Jan 1, 1944

By R. H. Marshall, J. Welchner, E. S. Rowland

This paper presents results on an extension into the realm of high-carbon steels of some work recently published1 on the effects of time at temperature, quenching temperature and prior structure on the hardenability of one 0.20 and four 0.40 per cent carbon alloy steels. It was shown at that time that unless the conditions of time, temperature and prior structure are substantially the same in performing the hardenability test as in conducting hardening of parts in production, the correlation of hardenability information with the hardness and properties of production parts is often not of satisfactory accuracy. The general effects of these variables on the austenitic grain size, distribution of excess carbides and critical cooling rate have been known for many years and one or more have been investigated by Shepherd,2,3 Davenport and Bain,4 Digges,5,6 Digges and Jordan,' Post and associates8 and Roberts and Mehl,9 to mention only a few. There has been no systematic investigation, however, into the quantitative variations produced on the hardenability of commercial high-carbon steels by changes in these factors of time, temperature and prior structure. Procedure A plain carbon hypereutectoid steel, S.A.E. 52100 and Graph-Mo, a molybdenum-bearing high-carbon steel containing some graphite, were chosen for this investigation. The chemical analyses of these electric-furnace steels are given in Table I. The procedure used was exactly that reported previously,' hence the details will not be repeated here. Normalized (165o°F.) and spheroidized prior structures were utilized on all steels with hot-rolled and quenched (I600°F. oil) prior conditions added for the plain carbon steel. The end-quench test developed by Jominy10 was sclected for use in this investigation and, with the noted exceptions, the American Society for Testing Materials standard procedure was followed. The effect of time at temperature was examined at intervals of o, 10 and 40 min. and 4 hr., and a few 16-hr. tests were run. Salt-bath heating of the specimens was employed to control and minimize the

Jan 1, 1944

By Lawrence H. Van Vlack, Otta K. Riegger

Periclase-type oxides were examined microscopically after being exposed to siliceous liquids. The rate of grain growth was found to be inversely proportional to the grain diameter. Grain growth proceeds more rapidly at higher temperatures, but is retarded by increasing liquid contents. aMag-nesiowiistites with higher MgO contents grow less rapidly than those with higher FeO contents. The growth rate is reduced by the presence of a second solid phase. The silica-containing liquid penetrates as a film between the individual magnesiowus tite grains. This is independent of time, temperature, amount of liquid, or the MgO/ Fe0 ratio. When present, olivine and spinel-type phases can provide a solid-to-solid &apos;&apos;bridge" between magnesioustite grains. THIS paper presents the results of a study of the microstructures of periclase type oxides in the presence of a silicate liquid. The purpose was to learn more about the effect of service factors such as 1) time, 2) temperature, and 3) liquid content upon A) grain growth, and B) liquid location among the solid grains. This study was prompted by the fact that periclase refractories are known to have very little solid-to-solid contact when the phases which are present are limited to periclase and liquid. Such a micro-structure gains industrial significance because it permits fracture during service when stresses are applied at high temperatures. The details of ceramic microstructures have not received extensive attention. This is in contrast to the extensive attention given to a) the phase relationships pertaining to refractory compositions, and b) the details of the microstructures of comparable metallic materials. A brief review will be made of the pertinent phase relationships and microstructural considerations in general, as well as of refractory compositions. a) Phase Relationships. This investigation was limited to those compositions in which (Mg, Fe)O was the solid phase. MgO and FeO form a complete series of solid solutions. Pure MgO has the name of periclase. The related FeO structure is called wustite. Both have the NaC1-type structure: however, wustite possesses a cation deficiency so that the true composition is Fe<10 even in the presence of metallic iron. The phase relationships involving solid (Mg, Fe)O and a silicate liquid are shown in Fig. 1. In this case. the liquid is saturated with (Mg, Fe)o. There-fore its SiOz content is below that encountered in orthosilicate liquids. As a consequence the liquid phase specie:; are primarily the following ions: and 0-&apos; plus occasional Fe+ ions. Two features are of importance: a) the liquid contains relatively small species and b) the liquid contains large quantities of the same species as the solid. viz., Fig. 2 shows the system, FeO-SiOz, which will be used in some of the discussions that follow. This diagram is the right side, vertical section of Fig. 1. Here, as pre\iously, the composition at the FeO end of the diagram is nonstoichiometric, varying from Feo.950 when the liquid oxide is in contact with the solid iron, to about Fe 0, when the solid oxide is in equilibrium with an atmosphere of equal proportions of CO and C02 at the solidus temperature. The Fe/O ratio will be maintained in wustite in the presence of SiO,. However, the FeM/Fe++ ratio in the liquid will be lower because of the effect OIF the SiO, on the activity of the FeO. With the addition of MgO to wustite, the over-all composition (IvZg, Fe)@, has a value of x lying between 0.9 and 1.0 when the COz/CO ratio is 1.0&apos;. b) Microstructures. In general, published attention to refractory microstructures has been directed toward the phase analyses that accompany compositional variations. This is illustrated by Harvey6 in his work on silica brick and by wells7 in his work on periclase brick. In each case, a series of altered zones is encountered which provides a sequence of phase associations. If due consideration is given to reaction kinetics, such an examination reveals phases that are compatible with equilibrium studies. Admittedly, however, it is often necessary to determine more complicated polycomponent systems to account for all the phases present.8 Relatively little attention has been given to microstructural geometry in ceramic materials. Certainly less attention has been given to this aspect of ceramic microstructures than to the size, shape, and distribution of the constituent phases in metals. Burke has pointed out that the grain size of oxides follows the same growth rules as for metals, viz.,

Jan 1, 1962

By Robert D. Longyear

IN MOST diamond core drilling the primary objective is the recovery of samples to be used for chemical analysis, physical tests, or visual inspection. Unless these samples are reliable and the information systematically recorded, the time and money spent in securing them are largely wasted. A properly taken diamond-drill sample is similar to a properly moiled channel sample but more accurate. No channel sample can be moiled in as even a groove as the smooth cylinder of material normally removed in diamond drilling. More important still, sampling by the diamond drill practically eliminates that personal equation which Jora1emon4 reference numbers apply to publications listed in the bibliography at the end of this article) has aptly termed "the almost magnetic attraction of the most conscientious hand toward rich pieces of ore."

Jan 1, 1937

By H. H. Rachford

Numerical solutions of immiscible flow problems in which dispersive effects of capillarity are dominated by convection require excessively fine grid spacing with attendant high computing costs. The use of coarser spacing reduces cost but often produces oscillation or undue dispersion associated with displacement fronts, A numerical formulation is proposed here which should be applicable to two-dimensional flow problems. it is in part analogous to an approach previously tested for miscible systems. The convective transport is approximated using a change of variables to yield a coordinate system moving approximately with the local characteristic velocity. The capillarity-induced dispersive terms in the differential system describing the process are approximated with respect to a fixed coordinate system by the usual implicit formulation. One-dimensional tests of the procedure yielded results in which the saturation profiles tended smoothly to the zero-capillary pressure solution as the ratio of viscous to capillary forces was successively increased in a sequence of calculations. This contrasted favorably with solutions by other numerical procedures which would require attendant grid refinements to approach the zero capillary pressure results. INTRODUCTION Numerical solution of displacement problems has until recently relied on applying methods developed primarily for transient heat-flow problems. Such problems are classified as parabolic in type, and where the heat transport is purely by diffusion their solutions are characterized by a high degree of smoothness. It is not surprising, therefore, that for approximating these solutions available finite difference methods are quite adequate. In flow problems the transport is partly by diffusion, partly by convection or flow. Although the problem remains of parabolic type because the dispersive effects of capillary forces or diffusion play some role in every displacement, at high flow rates the problem is dominated by convection, and solutions tend toward those of equations of the hyperbolic type. Solutions of hyperbolic problems are characterized by the translation of fronts, or discontinuities, that may progressively increase in sharpness. Numerical methods for treating parabolic problems become less and less satisfactory as displacement rates increase and the role of dispersion due to concentration or capillary pressure gradients becomes small relative to transport due to flow. In computation the difficulty manifests itself as an error associated with the grid size chosen. 1-6 In summary, if the heat-flow type approximations are to include the terms arising due to convection, one of several choices may be made: (1) an upstream (to the direction of flow) approximation for the convection terms may be used; (2) a centered-in-distance (CID) approximation may be used; or (3) a recently developed approximation based on the theory of oscillation matrices may be chosen.6 The last appears to have significant promise for one-dimensional flow problems; its extendibility to two or three dimensions is an open question. In either of the first two approaches, a suitably small ratio of v&/D must be maintained, where v is the velocity, & is the grid spacing and D the effective dispersivity in the direction of flow. In the first choice, the approximation of the convective part is only first-order correct and errors introduced appear as a numerically induced dispersivity of magnitude proportional to v?x. In the CID choice, the approximation can be second-order correct, but the difference formulation fails to satisfy the maximum principle unless a condition on v?x/D is met. Practically, this means that for high flow rates oscillatory solutions may result in the neighborhood of a front unless exceedingly small grid intervals are taken. While the procedure proposed by Stone and Brian4 permits a less severe limitation to be placed on this ratio, ultimately the flow rates increase relative to the dispersivity the oscillation obtains. Further, extensions of their approach to higher dimensional systems may be attended by considerable

Jan 1, 1967

By F. D. Rosi

The slip and twinning behavior in extended titanium crystals were studied in some detail. The formation and appearance of coarse kink bands are discussed. Their crystallographic geometry was determined by X-ray analysis. A phenomenological interpretation of the complexities in kink band development is also presented. The critical resolved shear stress, coefficient of shear hardening, and plane of fracture were determined for several crystals extended at room temperature. THE slip and twinning elements observed in the room-temperature deformation of titanium were enumerated in a previous paper1 in which considerations were advanced regarding the nature and selection of these elements and their effect on the known mechanical properties of this metal. The present study concerns the crystallographic, microscopic, and mechanical aspects of flow in relation to the slip and twinning elements, and includes a prediction of slip systems, nature of slip and twin markings, inhomogeneities of plastic flow, and stress-strain characteristics. Unless otherwise noted, arc-melted titanium sponge (99.77 pct) was used in these experiments. The method of production of crystals, their dimensions, and the surface preparation for micrographic examination have been reported.&apos; For obtaining stress-strain characteristics, only those crystals which traversed the entire width of the specimen and were at least 8 mm in length were used. Tensile deformation of the crystals was performed with conventional grips for sheet specimens and a constant-stress loading beam, designed after the method of Andrade and Chalmers.&apos; The specimens were loaded by allowing sand to flow from a reservoir into a bucket suspended from the longer end of a balanced 6:1 lever arm at a rate controlled to load the specimen approximately 2 kg per min. Strain measurements were made using the Baldwin SR-4, bonded, resistance-wire strain gage, Type A-8, which permitted a reading accuracy of 2 microinches per inch. The formulas used in the evaluation of shear stress and shear strain, as in deriving the coefficient of shear hardening, are given by Schmid and Boasv n terms of the original orientation and change in length of the crystal. For calculating the critical resolved shear stress, the standard equation was used. The crystallographic nature of the unpredictable slip observed in a number of specimens was determined by the single-surface X-ray method of analysis as described in ref. 1. Experimental Results Prediction of Slip System: It was reported&apos; that room temperature slip in titanium takes place predominantly on {10i0} and in a <1120> direction, giving three potential slip systems. Hence, it should be possible to predict the operative primary system in the manner used by Taylor and Elam&apos; for alu- minum (i.e., the one with the greatest component of shear stress in the direction of slip). The stereo-graphic construction in Fig. 1 shows that this is true. In all cases, slip was found to occur initially on the (0110) plane and, in a number of cases, in the [21f0] direction. (The direction of slip was not determined for all orientations.) It follows that duplex slip can be expected when two slip systems are geometrically equally favorable for slip, as demonstrated in Fig. 2. In both crystals slip took place simultaneously on the (1700) and (olio) prismatic planes, as indicated by Fig. 2a and b. In the case of crystal B the movement of the specimen axis with increasing extension was toward the (10i0) direction, which represents the stable end orientation resulting from alternate slip on the [2ii0] and [1120] directions. This is analogous to the duplex slip process in face-centered cubic metals." Unpredictable Slip: In a number of crystals whose orientations were well within the operation of a single slip system, secondary slip occurred on planes not predicted by the criterion of maximum shear stress. Examples are shown in Fig. 3. In addition to

Jan 1, 1955

By N. K. Chen, R. Maddin

THE textures of straight-rolled and of cross-rolled molybdenum were first determined with the aid of pole figures by Custers and Riemersma.&apos; These authors have shown that for straight-rolling, the main texture was (100) [0111 with a considerable spread about the rolling direction. After cross-rolling a second texture was obtained in which there was a [111] axis perpendicular to the rolling plane, possessing a rotary symmetry. Recently Semchy-shen and Timmons2 in their study of preferred orientation of arc-cast molybdenum sheet obtained similar pole figures. In these two investigations, polycrystalline materials were used. In the main, the textures of molybdenum in these cases are qualitatively consistent with rolling textures of other body-centered cubic metals, such as iron and Fe-Si alloys." In the present investigation, single crystals of molybdenum were deformed by rolling with respect to specific crystallographic planes and directions. Since the deformation textures of polycrystalline aggregates have been related intimately to the behavior of individual grains,4 a study of possible correlations of final textures with respect to the initial orientations of the single crystals might conceivably lead to a better understanding of the textures. Annealing treatments were carried out after deformation in order to study the recrystallization characteristics as well as the recrystallization texture. Rolling of Single Crystals Single crystals of molybdenum (about 1/8 in. in diarn x 1-in. long), grown by the method previously described,5 were cold-rolled without intermediate anneals. Except for specimens MR-1 and MR-2, which were rolled at random in the preliminary test in order to find a proper rate of reduction, all other specimens were carefully documented as to their respective orientation before deformation by means of X-ray Laue back-reflection methods. A stereo-graphic projection was constructed from which it was possible to determine a particular plane and direction to be considered for rolling. Parallel flat surfaces were then polished metallographically with respect to a reference scratch on the specimen which was mounted in sealing wax. These flat surfaces contained the plane chosen for rolling. After etching, a Laue back-reflection photogram was again made of one of the flat surfaces to determine the exact plane of rolling. The initial orientations of all the specimens (specified by two elements for each crystal, direction of rolling and the pole of the rolling plane) are summarized in Fig. 1. The specimens were mounted in plasticene between two hardened Si-Fe plates. The sandwich was then rolled down, keeping the direction constant in the case of straight-rolling. In cross-rolling (MR-10, MR-11, and MR-12) the sandwich was rotated 90" after each pass so that every first and third pass contained the same rolling direction. Specimens MR-14, MR-15, and MR-16 were compression-rolled following the manner of Barrett." In these cases the direction of the sandwich through the rolls was changed by 3" to 5" for each pass until the specimens were rolled to the desired reduction in thickness. It was found that if extreme care was exercised in rolling, i. e., the amount of deformation per pass was extremely small, the specimens could be rolled to a large reduction in thickness. The rate of reduction used, with a single exception of MR-1. was generally 0.001 in. per 10 passes. Thus, it took about 800 passes to reduce a specimen to a final reduction in thickness of 87 to 98 pct. The results of rolling are shown in Table I. Cold-Rolling Textures The final orientations were determined by the conventional Laue transmission method," using molybdenum radiation, with or without a zirconium filter. Pole figures were plotted from (1101 and (200) reflections in which three degrees of intensity— heavy, medium, and light—were determined visually. Three main types of textures have been observed from the deformed single crystals. These are: 1—a

Jan 1, 1954

By Edgar C. Bain, William E. Griffiths

The results of an inquiry into the structural nature of some 70 iron alloys containing both nickel and chromium over a considerable range of concentration are briefly described in this paper. This study is a part of a comprehensive program of investigation into alloys involving chromium in progress at the Union Carbide and Carbon Research 1aboratories. All the compositions studied contained carbon in amount comparable to commercial alloys. The B Constituent In addition to locating the limits of composition for the three principal types of structure (polyhedral ferrite, martensite and austenite) and their combinations, certain other features of the system were observed. A hitherto undescribed brittle constituent (designated here as the "B constituent") was discovered. It is very hard, non-magnetic and forms in two modes from chrome-ferrite by recrystallization. It is the stable low-temperature condition for the equal-proportion chromium-iron materials containing less than 10 per cent. nickel. Although it partakes of the nature of an inter-metallic compound, yet it may exist over a considerable range of composition. It is non-existent above a temperalure zone, varying with composition, from 800° C. to 950° C., and heating above this critical temperature develops chrome ferrite persistent after average cooling rate; a few hours just below this temperature will develop the complicated brittle crystalline type. The B constituent, when found in the grain boundaries of alloys of lower chromium content, contributes a serious brittleness removable, however, by heating and cooling rapid enough to prevent its re-format&apos;ion. By suitable means of precipitution, the hard B constituent can be made to strengthen the already stiff alloy matrix in the manner of submicro-scopic particles, as exemplified in duralumin or the Sykes iron-tungsten and iron-molybdenum alloys. A possible explanation is offered for the familiar brittleness developed in chrome iron at temperatures above about 475" C. and removable by

Jan 1, 1927

By W. S. Sanner

Experiments were conducted to determine the quantity and purity of ultraclean anthracite that could be prepared in the laboratory, using conventional separating techniques. A low, a medium, and a high-volatile anthracite were studied. Specific gravity separation followed by grinding, screening, and refloating at lighter specific gravities yielded small quantities of material purified to 1.0% ash, as follows: from low-volatile anthracite, 0.7%; from medium-volatile coal, 1.0%; and from high-volatile coal, 2.3%. The reduction in ash had no appreciable effect on the volatile matter or sulfur content of the coal. The limited quantities of material containing 1.0% or less ash obtainable indicate that if ultraclean coal is desired, a practical approach should include the processing units as an integral part of a convc.ntiona1 dense-media washing plant. Anthracite preparation practices during much of the industry&apos;s history were geared to maximum recovery of the larger sizes, pea through egg, which were used in hand-fired, domestic furnaces. Those sizes were cleaned to meet trade requirements, and the smaller sizes were usually higher in ash content. The impression, thus, was that ash content of anthracite always increased as the sizes got smaller. It was presumed that it was impossible to wash the finer sizes to extremely low ash contents. Following World War 11, the classical domestic market began to decline and the finer sizes assumed an increasingly large share of the market. For example, in 1949l 61% of the production was still pea and larger. Fig. l2 shows that -by 1955 these sizes accounted for only 50%, and in 1965, they were only 39% of the total anthracite produced. With the reduction in the market, increased quality was demanded, especially in export markets, and an increasing number of dense-media magnetite washers were installed in new and existing cleaning plants. In 1965, the coarse coal prepared at 59 breakers in the anthracite fields was sampled by the U.S. Bureau of Mines (USBM); approximately 50% of these plants were equipped with dense-media magnetite washers.3 Since 1950, more attention has been focused on the use of finer sizes for numerous industrial uses, including iron-ore sintering, pelletizing, foundry coke-making, cement manufacture, production of calcium carbide, and of carbon electrodes, etc. Most industrial uses require relatively clean anthracite, such as 10 to 11% ash for sintering and foundry coke, 7% for aluminum melting-pot cathode carbon, and 5% for carbide production. Hence, cleaning methods have been improved to the extent that dense-media washers, hydraulic cyclones, and flotation cells have been introduced as fine-coal-cleaning devices. It is now possible to wash the buckwheat, rice, and barley sizes (9116 X 3132-in.) to ash contents as low as 8 to 10% in dense-media devices, but washing the -3132-in. sizes to those limits presents more difficult problems, due mainly to the fineness of the material. This USBM investigation was conducted to determine the amount and purity of ultraclean anthracite that could be prepared in the laboratory, using conventional separating techniques. The goal was to reduce the ash content to a level acceptable for industrial carbon uses, including electrode manufacture, which generally requires an ash content of 1% or less. While low-ash content is of primary importance in selecting industrial carbons, the amounts of other constituents are also important, including iron, silicon, titanium, nickel, vanadium, and sulfur. They were not considered in this work, since their occurrence in deashed anthracite has been studied elsewhere.4 The results of the present investigation were used to design a flowsheet, suggesting a method for producing ultraclean anthracite as part of conventional preparation practice, using dense-media vessels, crushers, pulverizers,

Jan 1, 1970

By P. K. Weimer

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

Jan 1, 1967

By R. M. Goldhoff, J. W. Spretnak

IN connection with establishing the mechanism by which boron enhances the hardenability of heat treatable steels, this research work has been undertaken. Spretnak and Speiser1,2 indicated the need for studying high temperature effects in boron steels and, chief among these, the possible nonhomogeneous distribution of boron in iron grains. The occurrence of this effect may be of significance in explaining the mechanism of enhancement of hardenability by boron as well as in explaining some of the observed characteristics of boron steel behavior. Primarily, then, this work was undertaken a) to establish whether or not boron is adsorbed in ? solid solutions, b) to determine the nature of any such adsorption effects, i.e., whether it is positive or negative as well as its temperature coefficient, and c) to establish the magnitude of any such effect. While past literature on this specific subject is rather sparse, a number of authors have postulated that the observed temporary loss of hardenability as well as the occurrence of the characteristic boron constituent in these steels is due to the nonuniform distribution of boron in austenite.3-0 Experimental Techniques Attempts to obtain direct evidence of grain boundary effects in boron steels have been unsuccessful, both by using the technique of Chalmers&apos; in which small concentrations of solute made radioactive by irradiation are detected by autoradiographic means, and by means of studying cleavage fractures with the electron microscope.8 The present study attempts the design of experiments to measure the effect of boron on properties which might be subject to variation because of grain boundary effects. A study of the theoretical aspects of grain growth indicates that such studies may be pertinent. Another valid type of experiment involves the measurement in polycrystalline materials of properties whose values depend on the bulk of the grain, being negligibly influenced by grain boundaries. One such property is the lattice parameter measured by X-ray diffraction. The value of the lattice parameter reflects the average conditions which obtain over a relatively large number of atoms in a fixed crystalline lattice, and is therefore mainly dependent on bulk grain material. Measurement of lattice parameter variation over the austenite range of temperature in iron with and without boron should give evidence of concentration variations in the bulk grain material if adsorption effects are significant. Finally, use is made of the Grange and Garvey3 metallographic test for boron in which a characteristic boron constituent can be developed in austenite grain boundaries. The very occurrence of this phenomenon suggests grain boundary enrichment of boron and a study of the occurrence of this constituent and its varation with austenitizing temperature should help to detect grain boundary effects. Materials One lb ingots of pure iron, an Fe-B alloy, an Fe-C alloy, and an Fe-C-B alloy were prepared. The melting technique included an initial melting of electrolytic iron under vacuum followed by remelting under hydrogen and, finally, by melting under argon with the addition of alloying elements. Each ingot was surface machined between meltings. A quantitative spectrographic analysis was obtained on the pure ingot and, in addition, oxygen, nitrogen, and carbon were determined by the vacuum fusion method. The results of these analyses are given in Table I. Semiquantitative spectrographic analyses were performed on the alloy ingots, while quantitative determinations of the alloy additions were obtained. These analyses are shown in Table 11. The cast ingots were subjected to the following sequence of fabrication treatments: forging to 5/8 in. bars, swaging to 0.300 in. rounds, drawing to 0.025 and 0.010 in. wire. Portions of each ingot were retained in the swaged condition for experimental use. For certain portions of the work typical commercial steels were used. These materials were supplied by the Republic Steel Corp., Canton, Ohio, and correspond to AISI 8640 and AISI 86B40 compositions.

Jan 1, 1958

By Hallan N. Marsh, Bruce H. Robinson

It is generally believed that the flowing of wells through tubing instead of casing results in the conservation of gas. It is further believed that use of tubing prolongs the flowing life of a well and results in greater ultimate recovery, provided either that there are no adjacent wells, or that any adjacent wells are similarly operated. Recent experience in the flowing of Buckbee zone wells at Santa Fe Springs has not only substantiated both of these beliefs but has led to the further conclusion that the use of tubing results in a greater cumulative flowing production, &apos; even in a highly competitive field like Santa Fe Springs, where the wells concerned are closely offset by wells of both the same and other companies flowing through casing. Further, gas-oil ratio has been so reduced that greater ultimate recovery can be expected. In the belief that such would be the case, the majority of the Buckbee zone wells of one company were brought in through tubing, but enough wells were flowed through casing to form the basis for a comparison. For the purpose of this comparison, wells with flow strings 2½ or 3-in. dia. are designated as tubed wells, while those having flow strings larger than 3-in. dia. are designated as untubed wells. Casing used was mostly of 5 ¾-in. dia., the remainder being of 4¾-in. dia. There were 15 tubed wells and 8 untubed wells and they were scattered over the field in such a way that neither group appears to have any distinct advantage as regards location. Locations of all wells involved in the comparison are shown on Fig. 1. All the Buckbee sand wells of the company are included in the average production curves, with the exception of eight that were unsatisfactory for reasons other than the method of flowing. Findings 1. Buckbee sand wells flowing through casing larger than 3 in. had an average maximum production rate of 4670 bbl. per day, while wells flowed through straight tubing or 3-in. casing had an average maximum production of only 3300 bbl. per day. (See Fig. 2.)

Jan 1, 1932

By H. A. Fisch, A. J. Opinsky, J. L. Bartos

Fort?-six- two-grain bounduries were studied in doped tungsten 1amp wire that had been heated to 3450°K very vapidly. Back-reflection Laue photograms were taken of the grain boundary partners and solved, using a computer. The resulting distribution of large-grain orientations was analyzed. Rotational axes were calculatedfor each grain boundary pair. The axes of least rotation show an anisotropy of rolalional angle. WhILE the orientations of large grains in straight doped tungsten wire have been studied extensively, little has been done to characterize the boundary that separates them. Rosi.1 upon seeing the jagged interlocking boundary in doped tungsten wire. inferred that the grains should have a preferred orientation, and proved it. He interprets his data as indicative of a single ideal orientation—(531)— being parallel to the wire axis. Rieck2, 3 and Mannerkoski&apos; have essentially confirmed this finding. Opinsky, Orehotsky, and Siegle argue that the data suggest that (211)—a plane-is parallel to the wire axis instead. This (211 ) contains the (531). and hence would appear to be a more general case.5 Ahlborn and wasserman6 report that their orientation data stretch from (110) through (531) to (311). This path is the locus of {211 Recently. Opinsky has suggested that the data can be interpreted as a series of ideal orientations that can be related by coincidence relationships to the (110) fiber texture. All these investigators have determined the orientations of the large grains by the back-reflection Laue technique, and they have all obtained similar results. Only Rieck5 as methodically looked at the large grains along a wire. He was apparently not concerned with the relationships of the large grains across their common boundary, but only with their individual orientations. This research was undertaken to fill this gap in the under standing of the mechanical properties of tungsten wire. Only the crystallographic aspects of the problem will be reported here. In addition, the large number of large-grain orientations, which was accumulated in this study. will also be analyzed. EXPERIMENTAL MATERIAL AND TECHNIQUES All of the data were obtained from four pieces of the same 7-mil-diam General Electric tungsten lamp wire. Twelve-inch lengths of the cleaned wire were heated in vacuum by the flick of a switch to 90 pct of the amperes necessary for fusion (a temperature of approximately 3450°K) and held for 1 min. On the basis of other data. it is estimated that the rise time is of the order of 0.5 sec. The four pieces of wire could have come from anywhere within about 18 ft of wire. Consecutive segments of each piece of wire were mounted in bakelite and polished metallographically The polishing procedure followed that described by woods. "nly boundaries between two grains that each occupied the entire cross section of the wire were photographed and X-rayed. The metallographic sample was mounted accurately with respect to the X-ray unit. Steps were taken to read the films as accurately as possible with the conventional Greninger net. The data were then entered into computer programs that solve the Laue film by precisely the same techniques that are used in the solution of the film by means of the stereographic projection. The use of the computer has probably shifted the main source of error from the stereographic plot to the reading of the film. On the basis of several experiments, it is thought that the error associated with the entire process, from mounting the sample through the computer solution, is of the order of about one-half degree. The output of the computer is the direction cosines of the fiducial direction (the wire axis) and the locations of the three cube axes. The former data were used to calculate the differences in orientation between the two grain boundary partners, and the latter were used in the calculation of the rotational axes that could bring the two grains

Jan 1, 1970

By J. W. Rutter, K. T. Aust

THE object of the experiments to be described in this report was to determine, first, which grains, out of a large number introduced into a sample in which their growth could proceed, were able to grow most successfully; and, second, the factors which control their growth selection. In an earlier study of grain boundary migration in high-purity lead,&apos; it was found that, under some conditions, the most successful grain in an experiment of this type bears a special orientation relationship to the grain into which it is growing. The present work represents an extension of the previous study, directed at the determination of the orientation relationships which appear under a wider variety of conditions. Experiments of this general type have been done using commercial aluminum2 with somewhat conflicting results. In the present experiments, in contrast to the above,&apos; the sample composition was a principal controlled variable, resulting in a considerable clarification of the phenomena observed. EXPERIMENTAL TECHNIQUE The experimental technique used in this investigation was essentially that employed previously in studies of grain boundary migration kinetics.1&apos;3 The material used was zone-refined lead with various small amounts of tin or silver added to study the effect of varying the sample composition. The specimens were in the form of single crystals, about 1/4 in. 1/4 in cross section by 3 to 4 in. in length, grown from the melt in a horizontal graphite boat. A crystal grown in this way generally contained a lineage or "striation" substructure of the type shown in Fig. 1 of Ref. 1. This substructure consists of an array of low-angle boundaries which partition the crystal into regions misoriented from each other by a few degrees. The substructure constitutes a source of driving energy, estimated to be about 4000 ergs per cc, for the migration of a large-angle grain boundary into the striated crystal. New grains were introduced by plastic deformation in compression of a localized reglon at one end of the sample. Re-crystallization occurs at room temperature in the deformed region, introducing a large number of new, striation-free grains into the specimen. These grains are able to grow into the melt-grown crystal on annealing at a suitable temperature. The stria-tions are removed by passage of the grain boundary, as the substructure energy is utilized to produce the boundary migration. Usually, only one or two of the recrystallized grains persist after growth has occurred for about 1 cm out of the deformed region. Laue back-reflection X-ray photographs were obtained to determine the orientation relationship between the melt-grown crystal and the recrystallized grain or grains which grew most successfully in each specimen. EXPERIMENTAL OBSERVATIONS Fig. 1 shows the results obtained for a series of specimens to which had been added tin in the range from 0 to 5 ppm by weight. In this figure is plotted, in the standard stereographic triangle, the single axis about which the most successful recrystallized grain or grains are related to the starting, melt-grown crystal by the smallest rotation. The range of angular rotations observed about such axes is indicated beside each stereographic triangle. The results shown in the stereographic triangle on the left, Fig. l(a), were obtained by localized deformation at one end of each specimen at room temperature, followed by annealing in a furnace which had been preheated to 300°C. The furnace atmosphere was argon. It will be seen that the orientation relationships observed between the melt-grown and recrystallized grains are quite random. On the right, Fig. l(b), are shown results for samples in which the de-

Jan 1, 1961

By Kenneth S. Ritchie

THE discovery well of the world&apos;s -deepest oil producing structure, University 1-B of Group No. One Oil Corporation, in the Big Lake oil field, Reagan County, Texas, has had a remarkable record. The well is outstanding for the following reasons: (1) It is the world&apos;s pioneer well to produce. oil in commercial quantities from a structure 8500 ft. below the earth&apos;s . surface; (2) this well was the only. producer from the 8500-ft. pay for a period of 17 months and 24 days; (3) the flow of the discovery well has been free from-the customary changes at the casinghead, with the exception of putting on a back-pressure of 185 lb.; and, (4) the well&apos;s daily production of oil and gas increased rather steadily for 17 months and 18 days from an initial of 40 bbl. per day to a maximum of 2926 bbl. per day, and then six months later, after a period of decline and self-readjustment to subsurface changes caused by six more deep producers, the well set its real record for one day&apos;s production of oil at 2950 bbl

Jan 1, 1931