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By Horace Mann

A FEW years ago, it was generally thought that from 15 to 18 per, cent. of zinc oxide was the upper limit of a workable lead blast-furnace slag. With slags above this zinc-oxide content, the furnaces gave so much trouble because of hearth, wall, and crucible accretions that the campaign was very short. The time lost in cleaning out the frozen furnaces, for it was seldom possible to blow them out, and blowing in was so great that it was considered uneconomical to attempt the running of high-zinc slags, even if this were metallurgically possible. It is true that there are, references to one or two slags much higher in zinc than the foregoing,1 but the average smelterman regarded these, as freaks and not to be considered for regular furnace work. One or two plants, notably the plant of the United States Smelting Co, at Canyon City, Colo., ran charges, higher in zinc. At this plant, the zinc-oxide content of the charge was frequently 20 per cent. and higher but the slags from these furnace's seldom ran over 10 to 12 per. cent. zinc oxide. The furnaces were run with a large volume of air under a relatively low pressure, a low smelting column, and a very hot top; as a result, a large amount of zinc was volatilized. Even with the low smelting column and hot top, accretions caused much trouble and barring, down was a daily occurrence. At the time most of the theories on lead blast-furnace work were promulgated or worked out, it was necessary to run a furnace with a cold top in order to avoid an excessive loss due to fines and fume. At the same time, the smelting conditions had to be such that the lead and silver would be reduced and would enter the bullion. The slag had to be liquid but the charge must not give excessive accretions either in the hearth or on the walls of the furnace. This forced the operators to run the furnaces with a comparatively low blast, which, in turn, caused a small fuel consumption per unit of time with the accompanying result of a low working temperature.

Jan 8, 1925

By C. M. Wayman, R. Bullough

The selection rules fir twinning in fcc, bcc, and hcp lattices as established in Part I are used to predict the positions, relative to the matrix (untwinned) reciprocal lattice, of reflections due to double diffraction from the twins. These doubly diffracted reciprocal lattice points, which often coincide with ordinary matrix reciprocal lattice points, are deduced from kinematical considerations. 1. INTRODUCTION. A Bragg diffracted beam under certain conditions may be rediffracted to produce a third beam i .e., the incident beam, the first diffracted beam, and the rediffracted beam). In such a case an initial incident beam is diffracted by a set of planes; the diffracted beam may then be rediffracted by a second set of crystallographically different planes. The initially diffracted beam acts as an incident beam for the second set of planes, thus resulting in a twice-diffracted beam. This twice-diffracted beam may be regarded as a singly diffracted beam from a set of lattice planes whose structure factor is zero. In order to find the reciprocal lattice point corresponding to the doubly diffracted beam, it is customary1,2 to combine vectorially the component reciprocal lattice vectors which head to the extra reflections. For example, hcp metals may exhibit the forbidden (0001) reflections.* As Fig. 1 shows, the (0001) reciprocal lattice point results from: (1010) + (1011) = (0001) Similarly, combination of the beams (1011) and (1010) gives rise to: (1011)- (1010) = (0001) As Pashley and stowell2 have pointed out, even if in fact the double diffraction points lie on the Ewald sphere, they may not actually represent observed doubly diffracted beams because the initially diffracted primary beam, i.e., the source, must also correspond to a reciprocal lattice point which lies on the sphere of reflection; however, the reciprocal lattice point corresponding to the planes causing the rediffraction need not lie on the sphere. A little consideration of the Ewald construction in Fig. 2 makes this argument clear. In Fig. 2 the incident beam is represented by the wave vector ko. This beam is initially diffracted by the lattice planes (hkl) which are represented by the reciprocal lattice vector r(hk1) The reciprocal lattice point (hkl) of course lies on the Ewald sphere in order that the Bragg condition be satisfied. The initially diffracted beam is represented by the wave vector kl. If now kl is rediffracted by a second set of planes (h'k'l') resulting in k2 the lattice point (h"k"l") must lie on the Ewald sphere if the double diffracted beam k2 is to be observed. It is clear that (h"k"l") is the vector sum of (hkl) and (h'k'l'), and that (h'k'l') need not in fact lie on the Ewald sphere. In the usual1,2 analysis the origin (000) of the reciprocal lattice is shifted to the point (hkl). However the translation (000)— (hkl) automatically shifts the point (h'k'l') to the Ewald sphere, i.e., (h'k'l')— (h"k"1"). It is to be seen that (hkl), the source reflection, must lie on the Ewald sphere; if it does not the translation (000) — (hkl) places the "new" origin off the sphere, not satisfying the Ewald construction and hence the Bragg condition. The point (h"k"1") of course must lie on the sphere if it corresponds to an observed doubly diffracted beam. It is to be noted that crystals having the hcp structure, as just discussed, are intrinsically capable (i.e., without lattice defects such as twins) of double diffraction, as contrasted to fcc and bcc crystals which are extrinsically capable (requiring lattice defects or reoriented lattice regions). The "allowed" bcc reciprocal lattice points (which comprise an fcc lattice) are (110), (2001, (211), (220), (310), (2221, (321), (4001, and so forth. The combination

Jan 1, 1967

By Alexander L. Field

This paper contains an account of experimental results obtained in an extensive investigation of steels containing zirconium. There recently appeared' an announcement by F. M. Becket, at whose suggestion and under whose general direction this investigation was made, a statement of the outstanding features of the work and a brief explanation of the factors that led to its inception. It is not possible, in a paper of this character, to record all of the operating and test data collected, which includes the production of more than 350 heats of steel. The difficulty of a complete presentation is increased by the fact that several lines of experimentation are too incomplete to warrant publication of the results at the present time. In addition to the methods of manufacture and test employed in the work, there is described experimental evidence on which are based certain definite conclusions regarding the remarkable effects brought about by the presence in steel of relatively small percentages of zirconium. When added to a molten steel bath, zirconium combines chemically with dissolved oxygen, nitrogen, and sulfur, in the order named, and is capable of neutralizing the embrittling effect of phosphorus in whole or in part; although in the case of phosphorus there is no evidence so far of actual chemical combination. These effects arc not in the nature of suppositions supported by theory, nor is their existence deduced merely on the basis of analytical evidence. In each phase of its relation to or reaction with the four impurities mentioned, zirconium affects beneficiauy the mechanical properties of the steel to which it is added, in a manner which it is one of the purposes of this paper to explain in terms of a tentative working theory.

Jan 1, 1923

By Gerald Edmunds

Castings of pure metals and many alloys usually have a coarse-grained structure characterized by long columnar grains throughout the main body of the casting. Frequently, the surface exhibits finer, sometimes nearly equiaxed grains, and such grains may also compose other parts of the casting. This paper deals .primarily with determinations of the grain-orientation textures of the columnar and surface grains of polycrystalline zinc castings. It includes some results upon a cadmium casting and a magnesium casting. A hypothesis is developed to account for the observations on columnar grains and to use as a basis for predicting orientations in other cast metals. A general description of the position of the columnar grains in castings is that their long axes are approximately parallel to the direction of the thermal gradient during crystallization. Thus, in cylindrical castings the columnar grain axes tend to be radial, and in large flat castings where most of the cooling is through one or both of the large mold surfaces they tend to be perpendicular to the mold surfaces. At the edges and corners the direction of heat flow and therefore the position of the grains is more cornplex. Actually observation shows that even in castings made in flat molds the cooling seems to be somewhat irregular, since columnar grains tend to emanate from certain areas of the cooling surface, indicating that thermal contact was better there than in neighboring areas. The nucleus from which a columnar grain grows may be so oriented that its direction of maximum growth rate does not coincide with the direction of the thermal gradient. In this case the long axis of the grain probably assumes an intermediate position. Notwithstanding these minor irregularities, the situation does exist that the long axes of the columnar grains are generally disposed approximately perpendicular to the mold surface. Schmid and Wassermanl and Nix and Schmid2 have determined the orientation texture of columnar grains in castings of several cubic, tetragonal, hexagonal close-packed and rhombohedra1 metals. For zinc and cadmium, they report the basal plane to be parallel to the columnar grain axes, with no preference for any particular direction in this plane to coincide with the grain axes. This texture, termed a ring fiber texture,3 is uncommon in metals; zinc and cadmium are the only ones reported to exhibit it. Generally, it is stated, a simpler texture exists in which a principal, though not necessarily the most closely packed, crystallographic direction is parallel to the direction of heat flow. In cast magnesium (also hexagonal close packed) they report a digonal axis I, [100] direction, parallel to the direction of heat flow. The writer is not aware of any other orientation-texture determinations on cast polycrystalline hexagonal metals. In view of the observations reported in the present paper it is of interest also to note that Nix and Schmid stated that a

Jan 1, 1941

By J. C. Shyne, T. D. Gulden

The steady-state creep behavior, in compression, of indium containing a dispersion of atomized glass particles was studzed over a range of temperature, stress, and composition. The observed behavior was not consistent with a simple model of dislocation climb over dispersed particles. From room temperature to about 100°C the temperature dependence could be described by an activation energy about one and a half times that of self-dijfusion in indium while at higher temperatures a much higher ternperature dependence was observed. THE value of dispersion-hardened and precipitation-hardened alloys has long been recognized. The mechanism of hardening, however, is not completely understood, especially at elevated temperatures where dispersed particles increase creep resistance. Following the suggestion of Schoeck1 that the rate of creep in dispersion-hardened materials is controlled by dislocation climb over second-phase particles, Ansel and weertman2 derived steady-state creep equations for dispersion-hardened materials. Their derivation was based on dislocation climb over non-deformable spherical particles in a metallic matrix. For low stresses they predicted a linear relation between applied stress and steady-state creep rate. For stresses large enough to cause dislocations to pinch off around the precipitate particles, the theoretical creep rate was shown to be proportional to the fourth power of stress. For very high stresses an exponential stress dependence was predicted. In all cases the theoretical creep rate is linearly proportional to the diffusion coefficient. This provided the primary temperature-dependent factor. Subsequently, Ansel and Lenel3 reported some experimental data on SAP, a composite of aluminum and aluminum oxide, that was in good qualitative agreement with the above theories. Their experimental creep rates, however, were four orders of magnitude less than the theory predicts. This was attributed to a low density of active dislocation sources in the material; somehow the dispersed particles inactivated the dislocation sources instead of merely interferring with dislocation motion. Meyers and sherby4 have recently reported on the creep behavior of SAP. Their results were inconsistent with a simple dispersion-strengthening model and led them to conclude that a continuous network of oxide controls the high-temperature mechanical characteristics of SAP. Because of the rather complex mechanical behavior of SAP and the lack of agreement about the morphology of its oxide phase, it appeared desirable to study the creep of a dispersion-strengthened material of controlled morphology. For the present work a dispersion of spherical glass particles imbedded in a matrix of indium was chosen. The microstructure of this material was similar to the idealized uniform dispersion of hard spheres in a deforming matrix assumed by Ansel and Weertman in their theoretical treatment. SPECIMEN PREPARATION For experimental convenience, it was decided to use a low melting-point metal in this investigation. It was necessary that the metal not be oxidized readily up to its melting temperature and that it wet the second-phase particles. It was desired that the material chosen for the dispersed phase be available as a fine powder with closely controlled size and shape. The material chosen to satisfy these requirements consisted of a matrix of indium metal containing a dispersion of atomized particles of a soft soda-lime-silica glass ranging from 5 to 30 µ in diam. The glass particles had a highly regular spherical shape. The composite was made by stirring the glass powder into liquid indium maintained at a temperature just above the melting point of indium, 156°C. The creep specimens were prepared by a hot pressing operation. Five to ten g of the mixture were placed in a steel die and pressed at 125°C for 5 min under a pressure of 30,000 psi. The resulting specimens were cylinders about 3/8 in. in diam and ranged from 0.4 to 0.7 in. high. By following this procedure a uniform dispersion was obtained in the creep specimens. Typical microstructures of specimens containing twenty and forty volume percent glass powder are shown in Figs. 1 and 2. Unfortunately, grain size could not be determined by the metallo-graphic techniques used. CREEP TESTING PROCEDURE Creep tests were performed in compression under constant stress. The specimens were placed in

Jan 1, 1963

By Hewitt Wilson

IN 1903, T. M. and E. H. Alvord, of Marblemount, Wash., built a soapstone-grinding mill in the Skagit River Valley and are reported to have produced "ground talc" during 1904 and 1905, shipping to the paper mills in Wisconsin. Between 1916 and 1920, the Western Talc Co. built and operated a talc-grinding mill north of Mondovi, on the banks of the Spokane River, in eastern Washington, and sold powdered talc to the Inland Empire Paper Co. of Spokane. ? The most active develop-ment in recent years has been by two companies in the Skagit Valley-the Skagit Talc Company, Inc., which has been sawing soapstone block for the soda-recovery furnaces of the pulp and paper companies, and the Asbestos-Talc Products of Washington, Inc., at Burlington, which has been mining and dry-grinding a soft serpentine for the structural filler and insulation trade. Many prospects have been opened in the northern part of the state on both sides of the Cascade Mountains, and these activities undoubtedly are the forerunner of an industry that promises to attain considerable magnitude in the North Pacific States. At the present time, talc is imported from California for use as paper filler, and soapstone block from Virginia for use in the soda-recovery furnaces. A small market has been created locally for tailor and foundry:, pencils, stove grills, and block soapstone for art objects. The results of the present study, as yet incomplete, indicate that the use as a refractory and as a ceramic filler and flux can be expanded.

Jan 1, 1936

By J. M. W. Mackenzie

The interactions between oil drops and mineral surfaces have been examined for the cetyltrimethylammonium bromide (CTAB)-quartz and sodium dodecyl sulfate (SDS)-hematite systems. The results have been interpreted using a electrical double layer interaction model, a "sweeping-penetration" model based on steric interactions and a free energy of adhesion model. The adsorption of long-chain ions at the mineral interface was also studied and found to follow a Fuerstenau-Modi model of combined Coulombic and chain-chain interaction forces. The basis of the emulsion flotation process and the feature which makes it differ from conventional flotation is: encounter, followed by adhesion, between oil drops and mineral particles which are suspended in an aqueous environment. The manner in which the adhesion between these two phases contributes to the flotation process may be through the formation of min-eral-oil drop-mineral linkages, mineral-oil drop-air bubble linkages, or a combination of both. Possible flotation mechanisms derived from these adhesion processes are shown schematically in Fig. 2 while Fig. 1 shows an example of the first mechanism for quartz particles which have been floated using a cetyltrimethyl-ammonium bromide (CTAB)-Nujol emulsion as collector. In Fig. 2 the three phases, mineral, oil, and air, for convenience have been shown as having approximately equal size. This would not always be the case in an actual emulsion flotation operation. For the flotation of sand-sized particles of approximately 0.5 mm diam, the mineral particles would be at least ten times the size of the largest emulsion drops present in the system, while in the flotation of —10u slime particles, the mineral phase may be of the same order of size as the oil phase. The air bubbles in a flotation cell are normally about 1 to 2 mm in diam and therefore, in general, would be larger than the oil drops. Although the relative size of the three phases does not alter the basic adhesion processes between oil drops, mineral particles, and air bubbles, which depend on the physical and chemical properties of the interfaces involved rather than on the extent of these interfaces, it does alter the degree of deformation of the oil drops and air bubbles which will occur on adhesion. For mechanisms 1 and 2 to take place, the oil-water and mineral-water interfaces must be partially replaced by a mineral-oil interface while in mechanism 2 there is the additional requirement that the oil-water and air-water interfaces must be replaced by an oil-air interface. In view of the importance of the oil drop-mineral particle encounter and subsequent adhesion stages to both of the emulsion flotation mechanisms discussed, a study has been made of some physicochemical factors which control these processes for Nujol-cetytri-methylammonium bromide (CTAB)-quartz and Nujol-sodium dodecyl sulfate (SDS) -hematite systems. Experimental Electrokinetic Measurements.—The zeta potential of mineral particles was measured using a streaming potential technique similar to that described by Fuerste-nau.1 The streaming potential was measured using a multirange electrometer while the plug conductivity was measured using a 50 cycle sec1 bridge. Measurements were made on 28 x 65 mesh particles. Contact Angle Measurements.—A captive bubble technique was used to measure the contact angles for air bubbles and oil drops. The angles were measured on fracture faces of unmounted minerals which proved easier to clean than polished mounted specimens and should more closely represent a flotation system. Reagents: These have been described in a previous publication.0 Minerals: Rock crystal quartz from the New England district, N.S.W., was used for contact angle and streaming potential measurements. The quartz was hand

Jan 1, 1971

By James Gayley

The development of blast-furnace practice in America in the direction of large yields is mainly the history of our working since the year 1880, as the advancement that has been made in the last decade is greater than that in the third of a century previous. A new era in the manufactnre of pig-iron began in 1880 with the putting in blast of the Edgar Thomson furnaces. These furnaces at once leaped to the front as pig-iron producers, and have maintained that position—with but one brief interruption—ever since. I shall, therefore, confine myself mainly to a description of these works, showing the changes in design and practice by which these results have been achieved. In order to show more clearly the progress that has been made since 1880, I shall refer briefly to the best work that was done in the ten years previous to that time. The Struthers furnace, in Ohio, was one of the first to attract attention in the matter of large outputs. This furnace was 55 feet high, 16 feet in diameter of bosh, 9 feet in the hearth, and about 8 feet 6 inches at the stock-line. The fuel was raw coal. This furnace, in December, 1871, made 1602

Jan 1, 1891

By J. L. Dumanoir, Maurice Martin

The induction-electrical log is a combination of a SP curve, a short normal curve, and an induction log; all three logs being recorded simultaneously in a single run. The spacing of the short normal is 16 in. The induction log is designated as 5FF40, which means that the sonde involves five coils and a focusing system, and that the distance between the main coils is 40 in. Examples of induction-electrical logs are shown in Figs. 13 and 15. The right-hand track contains the induction conductivity curve. The scale of this curve is linear with the units of conductivity, i.e., mhos/m or millimhos/m (mmhos/m), increasing from right to left. The same curve can be read in the reverse direction as a resistivity log, with a hyperbolic scale. In the middle track, the solid curve represents the short normal. (An amplified short normal is also shown in Fig. 15). The dotted curve is the resistivity curve of the induction log, i.e., the reciprocal of the conductivity curve, recorded with the same linear scale as the short normal. The SP is in the left-hand track. In this combination, the SP curve and the 16-in. normal are the essential correlation curves, as in the conventional electrical log. The induction log provides a more accurate and detailed record of formation boundaries than the conventional log, especially in hard rock territories. Furthermore, the induction-electrical log makes possible the determination of fluid content, particularly in thin beds—at least qualitatively and very often quantitatively. In such thin beds, because of the adverse effect of the adjacent formations, the responses of the conventional devices are generally doubtful and/or incom-plete. Another advantage of the new combination is that the induction log is little affected by the presence of thin hard streaks interbedded within the permeable sections, whereas such occurrences are the cause of serious distortions of the long normal and lateral curves. The evaluation of saturation from any resistivity log implies the knowledge of the true resistivity R, of the bed and of the resistivity R.. of the flushed zone, or at least of the ratio Rxo/Rc. With the induction-electrical log run in fresh mud, the 16-in. nor-mal has a smaller radius of investigation than the induction log, so that the former reads closer to R.. and the latter closer to Rt. Thus, it has been observed that the ratio of the 16-in. normal to the induction log readings can be used as a basis for the interpretation in terms of saturation, with the help of appropriate charts. The purpose of the present paper is essentially to explain this procedure and to provide the corresponding charts. On the other hand, when a formation is deeply invaded, the response of any log (in particular the induction log) depends upon the radial distribution of formation resistivities behind the wall of the hole, which itself is a function of the arrangement of the fluids saturating the formation pore spaces. This paper, accordingly, will begin with a schematic description of the distribution of fluids and resistivities in the invaded zone. Next, some essential characteristics of the induction log will be reviewed. Finally, the determination of the interpretation charts and their application will be explained. The discussion will be confined to the case of fresh muds, i.e., muds whose resistivity is at least five times as great as that of the formation waters. With the present equipment the induction log is not well adapted for logging in salty mud. The Laterolog and guard electrode log are at their best under conditions of low resistivity mud. Accordingly, when these tools were introduced a few years ago, the use of salty mud was recommended. Now, with the introduction of induction logging, spe-

Jan 1, 1958

By M. W. Burkart, B. Lustman

Uranium-base alloys exposed to high temperature water fail either by uniform oxidation or by sudden cracking and disintegration of the metal. The disintegration results from the oxidation of a second phase which is precipitated during the corrosion process. The precipitate has been identified as a metastable hydride of uranium. URANIUM-BASE alloys consisting of the body-centered-cubic ? phase are susceptible to two different modes of corrosion failure when exposed to high temperature water. In the first process, a smooth oxide film is formed on the metal surface which continually flakes off during exposure and results in a uniform weight loss of the specimen. The oxide is present as a thin, adherent layer whose thickness remains approximately constant. As the metal oxidizes during corrosion, a nonadherent layer is built up on this film and continually sloughs off. Coincident with the uniform corrosion just mentioned, another process occurs which eventually leads to failure of the metal by cracking and general disintegration. The failure takes place during a relatively short time compared to the total exposure. To distinguish this type of failure from the uniform corrosion, the cracking or disintegration of the metal will be referred to as discontinuous failure. For the ? phase uranium alloys it is discontinuous failure rather than uniform corrosion that limits the useful corrosion life of the alloy. This paper will be concerned primarily with the mechanism of discontinuous failure. Physical Changes During Corrosion—The alloys used in this investigation were ? phase uranium alloys containing 7 to 12 wt pet Mo or Cb. The preparation of the alloys, the method of corrosion testing, and the actual corrosion results are presented in another paper.' The ? quenching treatment consists of annealing the alloy for 24 hr at 900°C in a sealed Vycor glass tube filled with helium and then water quenching to room temperature without breaking the tube. The corrosion behavior typical of a ? phase uranium alloy is shown in Fig. 1. This specimen was a U-12 wt pet Mo alloy tested in pressurized, degassed water at 650°F. The corrosion rate was practically constant at 0.28 mg per sq cm per hr or increased slightly until about 15 to 20 days of exposure, when the onset of discontinuous failure occurred in this particular sample, and the specimen soon began to crack and disintegrate. The simultaneous increase in the observed corrosion rate is a result of the increased area of exposure due to cracking of the specimen. The microstructure of a specimen that failed by cracking is shown in Fig. 2. The presence of a plate-like precipitate can readily be seen. Metallographic examination of corrosion specimens reveals that the onset of discontinuous failure is always preceded by the formation of a plate-like second phase in the ? uranium matrix. Hydrogen analyses of specimens periodically withdrawn from corrosion test reveal that the hydrogen content of the alloy increases on exposure to the high temperature water, as shown in Fig. 3. The hydrogen is available as a corrosion product resulting from the formation of UO2 by the reaction of the alloy with water. Specimens analyzed just prior to discontinuous failure contained as much as 1200 ppm H, whereas the plate-like phase appears to precipitate out at a hydrogen concentration of between 10 and 25 ppm. The observed increase in hydrogen content prior to and during the formation of the plate-like precipitate suggests that this constituent may be a hydride of uranium. Additional evidence linking the identity of this phase to a hydride is that it can be removed by vacuum annealing at temperatures of 100°C and above. Decomposition products of the ? phase would certainly not dissolve at such temperatures, nor could other likely products of corrosion, such as oxides, be dissipated at any of the test temperatures. The precipitation and growth of the second phase during corrosion is accompanied by an increase in hardness of the specimen. The hardness increase results from the dispersion of the harder precipitated

Jan 1, 1959

By E. J. Rapperport, E. D. Levine

The boundaries of the (a +ß) field in the Al-Li system were determined between 150°and 550°C utilizing quantitative metallography and lattice-parameter measurements. The solubility of lithium in aluminum decreases from 12.0at. pct Li at 550°C to 5.5 at. pct Li at 150°C. P Al-Li is saturated with aluminum at 45.8 at. pct Li and has this boundary value constant over the temperature range 150°to 550°C. THE solid solubility of lithium in aluminum has been determined by several investigators, 1-6 but, as shown in Fig. 1, there is little agreement among the various determinations. The earliest investiga-tions'-' are suspect because of the use of impure materials. Although high-purity materials were employed in more recent work,4'5 the experimental techniques may have led to contamination of the specimens. Probably the best work has been that of Costas and Marshall,6 who obtained close agreement between results obtained by two independent phase-boundary techniques: electrical resistivity and mi-crohardness. No detailed studies of the solubility of aluminum in the bcc ß phase, Al-Li, have been reported. Cursory investigations1,2,6 have indicated only that the (a+ß) -p boundary lies between 40 and 50 at. pct Li and is relatively independent of temperature. The present work was undertaken in order to provide an independent check on Costas and Marshall's determination of the solubility of lithium in aluminum, to extend knowledge of this solubility limit to temperatures below 225°C, and to make an accurate determination of the solubility of aluminum in Al-Li. EXPEFUMENTAL Alloy Preparation. In view of the difficulties encountered in previous investigations of the A1-Li system, close attention was paid to the use of methods of alloy preparation and treatment that would minimize contamination. Aluminum sheet (99.99 + pct Al) was vacuum-induction melted in a beryllia crucible to remove hydrogen. Lithium (99.9 pct Li) was charged with pre-melted aluminum into a beryllia crucible, in a helium-filled drybox. The crucible was sealed in a Vycor tube and transferred from the drybox to an induction furnace. Melting of alloys was performed by induction heating in a helium atmosphere. Solidification was accomplished by means of a suction apparatus, shown in Fig. 2, in which the alloy was forced by changes of pressure into a 3/16-in. inside diam closed-end beryllia tube. This technique produced rapid solidification of a small portion of the melt, resulting in alloys with a high degree of homogeneity. Typical lithium distributions are presented in Table I. Transverse sections 1/8 in. long were cut from the alloy rods, and each section was split in half longitudinally. One half of each section was analyzed for lithium, and the opposing halves were employed for phase-boundary determinations. Lithium contents were determined by flame photometry with an accuracy of 1 pct of the amount of lithium present. Thermal Treatments. Homogenization and equilibration heat treatments were performed in electrical-resistance furnaces with temperatures controlled to ± 2OC. Calibrated chromel-alumel thermocouples were employed to measure temperature. Homogenization was performed in helium-filled l?yrex tubes for 1 hr at 565°C. The encapsulated specimens were then transferred directly to furnaces maintained at lower temperatures for equilibration. Equilibration times were 2 hr at 550°C, 8 hr at 450°C, 27 hr at 350°c, 90 hr at 250°c, and 285 hr at 150"~. These times were chosen on the basis of conditions employed by previous investigators. Alloys were quenched from the equilibration temperatures by breaking the capsules into a silicone oil bath. By performing all possible operations either in sealed capsules or in a helium-filled drybox, the specimens were given minimum exposure to the atmosphere. Quantitative Metallography. Metallography of Al-Li alloys is difficult because of the atmospheric reactivity of the ß phase. It was found possible, however, to prepare surfaces of good metallographic quality by preventing contact with moisture during preparation. Grinding through 4/0 paper was performed in the drybox. The specimens were then transferred under kerosene to the polishing wheel. Three polishing stages were employed: 25-p alundum with kerosene lubricant on billiard cloth, 1-µ diamond paste on Microcloth, and 1/4-p diamond paste on Microcloth. Between stages the samples were cleaned by rinsing in trichloroethylene and buffing

Jan 1, 1963

By Seymour G. Epstein

Using a modified capillary-reservoir technique, electromigration of dilute solutions of silver in liquid bismuth has been measured with relatively good precision. The effects of experiment duration, temperature. current density, and silver concentration have been investigated. Chemical diffusion coefficients of silver in liquid bismuth were also measured at temperatures ranging from 300°to 600°C. The effective valence of silver in bismuth was calculated as a function of temperature from a comparison of electric mobilities and diffusion coefficients. In an alloy containing 1 wt pct Ag, the electric mobility of silver increased from 1.65 x X sq cm per v-sec at 300°C to 2.38 x 10-4at 600°C; the diffusion coefficient in-creased from 3.0 to 17.5 x 10-5 sq cm per sec over the same temperature range. Calculated values of effective valence decreased from 0.28 at 300°C to 0.10 at 600°c. ALTHOUGH there has been considerable progress in the theoretical treatment of electron-transport properties in liquid metals, the mechanisms of mass-transport phenomena in liquid metals are still not clearly understood. This is especially true for the case of electro migration, alternatively termed elec-trotransport or electrodiffusion, which is mass transport induced by an applied electric field. A thorough knowledge of the mechanisms governing electromigration will considerably aid in understanding the electronic state of an impurity atom in a liquid metal. Electromigration has been long observed and studied in liquid metals and alloys. However, no satisfactory theory to explain the observed effects has been developed. The disparity in the present theoretical treatments, summarized by Verhoeven,1 has been attributed to the difficulty in describing the momentum transfer between electrons and ions and to the lack of precise measurements in liquid metals, especially at elevated temperatures. Prior to the last decade most of the electromigration studies were qualitative, in that only the direction of migration of alloy constituents was determined with any degree of reliability. These results have been summarized by schwarz,2 who was able to measure the electric mobility of several elements in mercury. More recently electromigration in liquid metals has been measured by a variety of techniques, with a varying degree of success. Mangelsdorf3,4 made precise measurements on dilute amalgams at room temperature, using a technique relating changes in composition to changes in alloy resistivity, but was unable to make measurements at elevated temperatures. Using a modification of this technique, Verhoeven and Hucke5 measured electromigration and resistivities in liquid Bi-Sn alloys. However, the resistivity technique is not sensitive to small composition changes and is impractical for very dilute alloys. Verhoeven and Hucke6 also measured electromigration of several solutes in liquid bismuth by adapting the capillary-reservoir method for determining diffusion coefficients in liquids. The reported precision of these measurements was poor, however, primarily due to the large uncertainties in the chemical analyses to determine concentration changes. Belashchenko7 has summarized the recent Russian investigations of electromigration, many of which, however, are of questionable accuracy. The present study was initiated to develop an experimental technique which would be both versatile and sufficiently sensitive to yield precise measurements of electromigration of solutes in dilute metal alloys at elevated temperatures. Using this technique, a comprehensive study of silver in liquid bismuth was made to determine the effects of experimental variables on the apparent electric mobilities. Chemical diffusion coefficients of silver in liquid bismuth were also measured over the same temperature range for comparison with the electromigration data. EXPERIMENTAL TECHNIQUE Electromigration Measurements. Electromigration of silver in liquid bismuth was measured by the capillary-reservoir technique, similar to that used by Verhoeven and Hucke,6 but modified to yield more

Jan 1, 1967

By O. Hoover, M. Herman, V. V. Damiano

The Jetter and borie' teclznique of determining textures using a spherical specimen has been applied to tlze study of compression-rolled beryllium sheet. Snzall spheres the order of 1 mm in diam cut from the beryllium sheet were autotnatically rotated about tz41o axes using the G.E. single-crystal goniometer. Quantitative pole figures were obtained without tke need to apply absorption corrections. Compression-rolled beryllium exhibited peak intensities ,for (0002) planes of positions tilted 10 deg to the rolling plane and a near random distribution of (1010) planes about the nornal to the rolling plane. TECHNIQUES for determining textures of rolled sheet material are amply described in the literature. The techniques are found to be variations of two basic methods. One due to Decker, Asp, and arker, referred to as the transmission method, utilizes a thin-sheet specimen in which the X-ray beam enters the specimen from one side and the intensity of the beam which emerges from the opposite side is measured. The second method due to chulz,3 referred to as the reflection method, utilizes a thick specimen and the intensity of the beam emerging from the same side is measured. The two rotations of the specimen in the beam are designated a and 8. In order to completely determine the texture of sheet material, it is generally necessary to use a combination of the two methods. The calculations involved in correcting the raw X-ray data for absorption effects and the combining of the data obtained by the two methods are very laborious and time consuming. To avoid the intensity corrections which arise as a result of the changing diffraction volume and path length within the sample other methods have been proposed. The Norton method utilizes a cylindrically shaped specimen cut from the sheet material. Since the rods have rotational symmetry, the absorption correction is constant for rotations about the sheet texture. Jetter and Borie' employed a spherical specimen to analyze the fiber texture of extruded aluminum rods. The spheres were rotated rapidly about the fiber axis to include a large number of grains in the X-ray beam and changes in intensity with respect to tilts of the fiber axis were measured. The absorption correction was constant for all angles and was neglected. The Jetter and Borie' technique finds excellent ap- plication to very fine-grained low-absorbing metals in which the entire sphere volume can contribute to the diffraction volume. In the case of low-absorbing metals, however, serious limitations on specimen thickness occur as demonstrated by Braggs due to de-focussing effects. Peak shifts may occur which negate the assumption that integrated intensities are proportional to peak intensities. These limitations in sphere size to the order of 0.5 to 1 mm for beryllium require that the grain size be sufficiently small to include a large enough statistical sample. The present paper describes the application of spherical specimens less than 1 mm in diam to the quantitative determination of pole figures for compression-rolled beryllium sheet having a grain size the order of 10 p. EXPERIMENTAL 1) Specimen Preparation. Two techniques for spark-machining beryllium spheres were tried. One involved the use of a hollow cylinder as a cutting tool. The tool was fed into the rotating cylindrical specimen as shown in Fig. l(a). The hollow cylinder was carefully aligned such that the axis of the cylinder and the axis of the specimen lay in the same plane and were 90 deg to each other. As the hollow cylinder was fed into the rotating cylindrical specimen, a spherical shape was formed as shown in Fig. 1. Alignment was very critical. Slight misalignment resulted in the formation of a barrel-shaped specimen instead of a sphere. A second technique involved the use of a cutting wheel shaped as shown in Fig. 2 with a groove of the desired radius. A section of the sheet specimen was first turned into a cylinder on the left part of the cutting wheel. It was then shifted to the right and a spherical specimen was turned as shown in Fig. 2. The axis of the cylinder lay in the plane of the sheet. Flats corresponding to the rolling plane of the sheet were used to grip the specimen during the machining operation and these served to identify the rolling plane of the sphere. 2) Rotation of Spec=. The spherical specimen is shown mounted on the G.E. single-crystal goniometer in Fig. 3. The knob A of the goniometer shown in Fig. 3 rotates the specimen about the pedestal axis. These angles have been designated as @ angles. The knob B rotates the specimen about an axis perpendicular to the pedestal axis. These angles have been designated as p angles. A device was made to automatically drive the single-crystal goniometer by means of two flexible shafts connected to the A and B knobs as shown in Fig. 3. The motor system was designed to rotate the knob A, thus rotating the specimen through angles of $I while the B knob remained stationary. After one complete

Jan 1, 1967

By W. R. Shimer

IN his valuable report on Finishing Temperatures and Properties of Rails, I Dr. G. K. Burgess, Chief of the Division of Metallurgy, U. S. Bureau of Standards, has begun a line of investigation which should be continued by those interested in the subject, and who have proper facilities for carrying put the work. For the past year or more the Bethlehem Steel Co. has been conducting experiments to learn the effect of rail finishing temperatures on their physical properties and microstructure and the results are here given for the consideration of those interested in the rail situation. . Considerable differences of opinion have been expressed by various authorities, in the past, as to the effect of large or small grain size and high or low finishing temperatures of steel rails on their physical properties and wearing qualities. Low finishing temperatures and, therefore, low shrinkage, have been advocated on the theory that the wearing qualities would be improved. Others have recommended high finishing temperatures. The generally accepted cause for rail failures, due to the development ,of transverse fissures, is excessive wheel pressure on hard rails. One of the causes advanced for hard rails has been that they contain too high per centages of carbon and manganese; another that the rails were finished at too low a temperature, i.e., at or near the critical point. In the experiments herein described the rails were rolled from reheated blooms. All the rail blooms were charged hot in a reheating furnace and brought up to about the original ingot-rolling temperature before rolling into rails. These rails gave better results in deflection, withstood a greater number of drops before breaking, and showed greater ductility, than. rails of identically the same composition and section which were rolled, direct from the ingot. Rails rolled from reheated blooms, finished at somewhat higher temperatures than when rolled direct from the ingot, have a different microstructure, which the writer does not believe is due so much to the difference in finishing temperatures, as to the difference in

Jan 3, 1915

By P. K. Koh

With identical annealing heal treatment the development of major annealed texture component seems to depend primarily upon the degree of cold reduction. Cube texture was evident on annealing- 1/2-, 1,/4- , and 1/8-mil tapes at 760°C, but it dissap-)eared on 927°C annealing of 1/8-mil tape cold reduced 96.9 pct. Some cube texturee remained as tile strongest 927 °C annealed texture component in 1/4- and 1/2-mil tapes cold reduced 93.8 and 87.5 pet, respectively. The switching coefficient increases and the squareness ratio of the hysteresis loop decreases proportionally with increasing cube pole concentration. PREVIOUS studies 1,2 on the 1/8-mil ultra-thin molybdenum permalloy tape established cold rolled and annealed textures and their magnetic performance for switch-core and coincident-current memory applications, The major cold-rolled texture was found to be of {110}<335> which is quite similar to the cold-rolled texture of silver and 70-30 cartridge brass. The major annealed texture components were found to be of {120)-- <001> and {113)<785>. Although the direction for easy magnetization for this type of alloy by the single-crystal technique is not avaliable, knowledge from related studies indicated [Ill] as the easy magnetization direction, similar to that of nickel.&apos; Therefore, a cube orientation, if present in the tape core, would be most detrimental to its magnetic performance.3 In its cold-rolled state the tape had < 111 > directions in the rolling plane 14.5 deg from the rolling direction.&apos; But the coercive force of the tape in such condition will be excessive due to large amounts of internal stresses, and therefore makes its use impossible for memory applications due to long switching time. In lower nickel alloys, suchas 50-50 nickel-iron and 65 pct Ni-Fe sheets, previous investigators4"7 found the presence of cube texture on annealing at 900° to 1000°C. Although no cube texture was found in annealed 1/8-mil tape,"&apos; its presence in some annealed 1,/4-mil tape cores was firmly established a year ago as verified by significant differences in magnetic properties. The present investigation is devoted to the orientation study and related magnetic measurements on three thicknesses of the ultra-thin tape, namely, 1/8 mil, 1/4 mil, and 1/2 mil, cold rolled directly from annealed 4-mil stock in the cold-rolled state as well as after they were annealed at 760°C (1400° F) and 927°C (1700°F). The results obtained might serve to elucidate the development of annealed texture as well as to establish clearly the importance of preferred orientation on the magnetic performance of such memory tape core despite its well-known low magnetic anisotropy exchange energy. EXPERIMENTAL PROCEDURE Samples were taken from one production heat (0.010 wt pct C, 0.004 P. 0.016 S, 0.80 Mn. 0.29 Si. 79.69 Ni. 4.42 Mo. 0.054 Co, 0.002 Ti, 0.12 Al, 0.04 Mg, 14.56 Fe). Annealed 4-mil sheets were cold re-

Jan 1, 1962

By R. M. N. Pelloux

This study of aluminum-copper alloys had two aims: 1) To determine the effect of the amount and distribution of a second phase, CuAl2, on the creep-rupture strength, ductility, and fracture characteristics of the alloys. The work of Gemmell and grant&apos; on single-phase aluminum-copper alloys provided a basis for the present study. 2) To attempt to provide a relation between the microstructure and strength of two-phase alloys deformed at comparatively high temperatures (greater than 0.45 T,). The creep behavior of the two-phase magnesium alloys Mg;Ce and Mg-A1, has been treated by Roberts. 9 In work reported by Sully and Hardy4 and by Underwood, Marsh, and Manning~ on A1-Cu two-phase alloys, and also in a portion of the work of Gemmell and grant,&apos; aging took place during the creep tests. &apos;In the present work, overaged aluminum-copper alloys were subjected to creep deformation at two temperatures, 500 and 700OF. The overaging treatments to produce the precipitate dispersions were performed prior to the test, at temperatures which were the same as the ultimate respective test temperatures. Hence, the present study is concerned with the creep behavior of stable (in contrast to "underaged") two-phase A1-Cu alloys, i.e., alloys in which no depletion of the solid-solution matrix occurred during: creep. MATERIALS AND PROCEDURE A 2 and a 3 pct Cu alloy, supplied by Alcoa, were studied; Table I shows the compositions. The grain size of the specimens, 0.9 to 1.0 mm, was achieved by annealing the machined test bars for 2 hr at 1000°F, followed by furnace-cooling to 900°F, and homogenizing for 4 hr. Both compositions are in the single-phase condition at 900°F. Two types of overaged dispersions, termed "over-aged I" and "overaged 11" were prepared after the grain size and the homogenization anneals. The overaged I alloys were prepared by quenching to room temperature after homogenization, aging at either 500&apos; or 700°F for 72 hr, and air-cooling to room temperature. The overaged I1 alloys were prepared by furnace-cooling after homogenization, to either 500&apos; or 700°F, and holding at the necessary temperature for 72 hr. The times for furnace-cooling from 900°F to 700° and 500°F were, respectively, about 2 and 3.5 hr. The structures of the A1-2 pct Cu alloys are shown in Fig. 1 (overaged I) and in Fig. 2 (overaged 11). A comparison of Figs. 1 and 2 shows that in the overaged I alloys the precipitate particles along the grain boundaries are much more closely spaced and the grain boundaries are straighter than they are in the overaged I1 alloys. Further, the particle size and spacing in the grains are smaller than in the overaged I1 alloys. Microstructures of the A1-3 pct Cu alloys have not been shown; the structures of these alloys differed from those of the A1-2 pct Cu alloys only in that the distribution density of the particles was greater. The creep specimens had a gage section 1 in. long with a diameter of 0.155 to 0.195 in. Before testing, specimens were electropolished in a solution of 100 cc glacial acetic acid, and 30 cc of 60 pct perchloric acid, at 40&apos; to 50°F, at 24 v. The specimens were kept refrigerated prior to testing to avoid precipitation at room temperature. Constant stress creep tests were conducted; the load was applied 75 min after heating of the specimens to test temperature had begun. EXPERIMENTAL RESULTS Creep-Rupture—Fig. 3 shows the log stress-log rupture life plotfor the overaged alloys studied, and also for the underaged A1-2 pct Cu alloy.&apos; At 700°F, the stress-rupture life relationship is nearly independent of both the amount of precipitate (i.e., composition) and of the type of overaging treatment (i.e., precipitate dispersion). At 500°F it is apparent that the increase in rupture life that was ex-

Jan 1, 1960

By P. J. Burkhardt, L. V. Gregor

The oxidation kinetics of single-crystal silicon has been investigated using extremely dry oxygen as the oxidant. Two techniques were used. The first involved a flow system with which incremental thickness measurements were made. This sytem provided an oxygen ambient at atmospheric pressure which had a moisture content of less than 0.1 ppm of water. The second technique involved measuring the change in volume of oxygen with time in a closed system. A temperature range of 900O to 1200 "C and a pressure range of 20 to 760 Tory were covered. Both techniques showed that a simple parabolic rate law holds only at the higher temperatures. At lower temperatures, the data up to 5000Å can be fitted well to a linear-parabolic equation. The two constants in this rate equation are examined in terms of a physical model. The parabolic portion of the low-temperature oxidatLon fits along the high-temperature curve of an Arrhenius plot. The parabolic rate constant for the flow-system technique can be expressed by k = 2 x 10-9 exp (L 31 kcalRT) sq cm per sec. The manostatic technique gave k = 1 x 10-exp (- 23 kcalRT) sq cm per sec. By extending the thickness range to over 104. a rate law of X = At seems to fit all of the data better than the linear-Pavabolic law. Here the exponent n increases from 0.518 at 1150 V to 0.637 at 900°C. PASSIVATION of silicon planar devices through thermal oxidation is of such great importance that considerable effort has been devoted to the study of the process.17 Much of this work involves hydrothermal oxidation, in which H2O is the oxidant: whereby H2 is produced. It has been proposed that the reaction proceeds by the formation of Si-OH groups and hydroxyl diffusion through the film to react with the silicon surface. Thus, the silicon oxide layer probably contains residual hydrogen in some form after oxidation in H2O and it has already been established that hydrogen has a marked effect on the electronic properties of oxide-passivated silicon surfaces. Silicon is oxidized by oxygen at elevated temperatures; but the rate of oxide formation is considerably lower than that for 0." By using dry O2 as the sole oxidant, the presence of residual hydrogen is presumably avoided. At present, the mechanism of thermal oxidation by dry O2 is a matter for conjecture, and the presence of small amounts of H2O was reported to have a marked effect on the rate of oxide formation10 (perhaps on the electronic properties of the surface, as well). Hence, this study of the kinetics of silicon oxide growth in 0, was undertaken: 1) to determine the oxidation rate at atmospheric pressure in a system designed to exclude rigorously all traces of H2O in the ambient 0,; 2) to obtain oxidation-rate data in situ in dry O2 by means of a continuous monitoring of the amount of 0, consumed during oxide growth. These objectives are complementary—the first assesses what effects (if any) are obtained by excluding H2O from the reaction, and the second expands this information while at the same time avoiding the uncertainty inherent in relying upon incremental measurements of oxide growth to furnish kinetic data. EXPERIMENTAL PROCEDURE The conventional silica open tube in a resistance-heated oxidation furnace is subject to sources of trace H2O, even after the input O2 is thoroughly dried and the outlet gas stream is passed through a trap to prevent

Jan 1, 1967

By J. M. Hassler

Nowhere can there be found a more misleading statement than the old one that "Iron can be manufactured cheaper in the South." During the past decade ironmakers and users of iron have heard varied and sundry stories of the wonderful resources of the Birmingham district, including abundant ore and coal fields, cheap labor, a wonderful climate and similar industrial Utopian statements. Birmingham represents the major portion of the iron business in the South, and as Birmingham fares so goes the iron business of the South. The intent of this paper is to shed some light on the actual conditions surrounding ironmaking in the South, especially in the Birmingham, or North Alabama, district. By a presentation of facts it is desired to point out that the "cheap iron" of the industrial South is a thing of the past, primarily because of increased labor cost and because labor is radically different in performance to what it was years ago. Also, because most of the raw materials needed in ironmaking that would be classed better than inferior are gone. Important Factors The several important factors that have been responsible for this change are : 1. Shrinkage of the iron business in the South. 2. Increased labor cost. 3. The development of the South, with an industrial trend, without a substantial increase of its own iron-consuming market. 4. Increased freight rates, which has narrowed the market that might be reached from this district. 5. Depletion of the better grades of raw materials, both ore and coal. Shrinkage of Iron Business in South.—Table 1 was prepared in early 1936 and revised in 1937, of blast-furnace units in the North Alabama district, considering the year 1936 compared with a maximum number of furnace units of previous years, the peak point being very near the year

Jan 1, 1937

By Norman Carmichael

This paper describes the evolution of transportation at an important mining property, beginning at a time when the railhead was 400 mi. distant, and tracing the steps leading to the development of what is probably the heaviest ore train ever operated in underground mine service over narrow-gage tracks, a 300-ton ore train on a 20-in. track, at working costs closely approximating those obtained on systems involving much greater capital expenditure. Useful where geological and financial considerations render inadvisable the excavation and maintenance of large tunnels and heavier rolling stock. THE problem of transportation in the Clifton-Morenci district of Arizona has been one of peculiar difficulty and consequently has been an important factor in the cost of mining and treating the ores produced. From the crude beginning made over 50 years ago, many changes have been necessary to keep pace with the increased output of copper. A heavy-duty haulage system has developed on the original 20-in. track gage to meet the existent metal-mine conditions.

Jan 3, 1924

By N. Tiner

THE mechanical properties of magnesium-alloy castings are greatly improved by grain refinement, and at present considerable attention is being paid to methods of obtaining fine-grained castings. One method of achieving this end is the use of proper melting and superheating techniques. These have been employed commercially to a great extent, but no comprehensive study of the subject appears to have been published at present. Numerous investigations found in the literature include some reference to superheating techniques, 1-4 and Achenbach, Nipper and Piwowarsky,5 based principally on thermal analysis, ascribe the grain-refining action of superheating to the influence of solid foreign particles or dissolved gases present in the melt upon the course of crystallization. The primary purpose of this paper is to present the principal facts concerning the effect of superheating on grain size of magnesium alloys. Attempts are also made to explain the experimental results in terms of a general hypothesis. The investigations are limited chiefly to common commercial casting alloys. In order to carry on this work, it was necessary to determine the factors influencing grain size and to develop a proper technique for the preparation of samples. The preliminary tests made by the author indicated that the grain size of magnesium alloys resulting from the solidification of a melt is determined by alloy composition, presence of impurities, rate of cooling during solidification, thermal history of the melt and to some extent the structure of the charge used. The rate of cooling is in turn dependent upon the mass of the melt, pouring temperature, and dimensions, properties and temperature of the mold into which the melt is poured. The final grain size of the alloys is still further modified by heat-treatment subsequent to casting. It is not within the scope of the present paper to discuss all of these factors, and it would suffice to note here that when equal amounts of magnesium alloys are prepared from the same alloying materials, melted in graphite crucibles under the same thermal conditions, then cast into graphite molds at a constant temperature, the .resultant solids have the same grain size. By maintaining all other factors constant, it is thus possible to vary thermal conditions of a melt and to examine the grain size of resultant castings. PREPARATION OF SAMPLES AND GRAIN-SIZE TESTING The alloys investigated in this paper were taken from ingots made by Permanente Metals Corporation or prepared by the author with pure carbothermic magnesium and necessary alloying elements. Melting was carried out under a flux in a graphite crucible heated uniformly by an

Jan 1, 1945