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By D. A. Thomas, E. S. Meieran

Tungsten wires were examined by transmission electron microscopy after drawing and after high-temperature annealing. Drawn wire consists of highly elongated grains called fibers, whose long axis is parallel to [110]. Each fiber is ribbon-shaped, with the wide dimension of the ribbon parallel to (001) and the narrow dimension parallel to (110). Furthermore, most fibers are bent about [I10] and twisted along their length. The fibers are divided into cells, which in some cases contain a platelet substructure lying on (110) planes. The misorien-tations of these platelets accumulate to allow the macroscopic twist of the fibers. During annealing, several competing reactions occur, starting at different temperatures and progressing at different rates. Among these processes are fiber-boz~ndary migration, polygonization, dislocation rearrangement, and possibly impurity segregation. The fiber-boundary migration accompanied by the formation of transverse boundaries during polygonization leads to an equiaxed grain structure although recrystal-lization does not occur. There is a relationship between the flow stress of the wires and their average subgrain width in the form sy = s0 + kyd-1/2 . Also, there appears to be a relatio'nship between wire ductility and the formation of transverse boundaries during annealing at about 800°C. THERE have been many investigations of the structures and properties of tungsten wires1-4 due to their commercial importance for use as lamp filaments. The structural studies have so far been limited to optical microscope and replica electron-microscope studies. due to the difficulty of .-me- paring from wires thin foils which can be examined by transmission electron microscopy. However, this difficulty has been recently overcome,5 and it is now possible to examine tungsten wires by transmission electron microscopy as well as by other techniques. In this paper, the structure of drawn tungsten wire is described, as are the changes in the structure during high-temperature annealing. Some discussion of the relationship between structures and properties is also given. EXPERIMENTAL MATERIALS AND PROCEDURES Commercial 0.030-in.-diam doped tungsten wires drawn at progressively decreasing temperatures between about 1400° and about 800°C were examined. The composition, mechanical properties, and optical microstructures are described in detail elsewhere.' All experimental materials were vacuum-annealed for 10 ot 30 min at temperatures at 100°C intervals between 700° and 2000°C. Specimens were thinned for examination in the Siemens Elmiskop I electron microscope by the method of Meieran and Thomas.5 STRUCTURE OF AS-DRAWN WIRE The optical microstructure of as-drawn tungsten wire has been described by Peck and Thomas.7 They observed that wire in longitudinal section consists of highly elongated grains called fibers whose width varies between 1 and 10 µ, while in transverse section the fibers appear to be elliptical in cross section and bent about their common [110] wire axis. They explained this unusual appearance as being due to the drawing of a bcc material with a [110] texture, and predicted that the wide and narrow planes of the fiber cross section would be parallel to (001) and (110), respectively. The fibers apparently bend about the [110] axis during drawing to maintain grain boundary continuity during drawing. Transmission electron microscopy offers a way of checking these predictions as well as providing a more detailed picture of the wire structure. Figs. 1, 2, and 3 are typical electron micrographs of

Jan 1, 1965

not weaken. I saw him shortly before he was killed; his conduct under fire was splendid and an inspiration to his men. His loss is felt deeply by all ranks. Thanks to him and to others, who like him, paid the full measure of devotion to their country, our line was held until the critical situation in that vicinity was at an end. He died the true death of a soldier, with his face to the enemy. As we now look back, it is easy to believe that this holding of the line of defense intact by General Carey and his men was a determining factor in the outcome of the war. To have played so important and noble a part in this vital effort as that taken by Perry is assuredly the privilege of few. Our lives, it seems, are like capital entrusted to us to be expended as wisely and effectively as we may. With them we purchase whatever of accomplishment the stuff that is in us permits. It is impossible to escape profound regret that a career so full of the highest promise, and a personality so overflowing with all that is fine and lovable, should have been cut short at the age of thirty-one. Yet who can doubt that in a few months Perry bought with his life the fullest achievement of a life-time—a glorious part in the salvation of Liberty and Justice and Decency, indeed of Civilization itself! L. C. Graton.

Jan 1, 1920

By Joseph Hodgson

Introduction SINCE about 70 per cent. of the total cost of mining is due to underground work which is out of sight, it is essential that expenditures should be made here to the best advantage. A great many mistakes have been made which were expensive, but perhaps these have not even been detected by mine owners. In the future these may be minimized to some extent, especially if there is cooperative effort on the part of each employee. I have been interested in this subject for some years and have tried to deduce principles and methods. These have proved highly advantageous and may also be of help to others. Some corporations, like the United States Steel, and the Cleveland-Cliffs Iron Co., have done a great deal in this field by having stated meetings of their organizations, with the view to interchanging ideas among their men and educating them along the lines of concerted effort. Since no man knows all about the various branches of mining, it is advisable that frequent meetings of the operating department be held for the interchange of ideas and that all members of the organization have an opportunity to express themselves on the various subjects. It has often been found that in discussions between heads of departments, foremen and bosses, many valuable suggestions may be obtained which promote the best interests of the company. The method regarded as the most conducive to cooperative effort, and pursued by the organization, is to analyze and develope the different phases of various mining subjects at regular meetings.

Jan 5, 1916

not weaken. I saw him shortly before he was killed; his conduct under fire was splendid and an inspiration to his men. His loss is felt deeply by all ranks. Thanks to him and to others, who like him, paid the full measure of devotion to their country, our line was held until the critical situation in that vicinity was at an end. He died the true death of a soldier, with his face to the enemy. As we now look back, it is easy to believe that this holding of the line of defense intact by General Carey and his men was a determining factor in the outcome of the war. To have played so important and noble a part in this vital effort as that taken by Perry is assuredly the privilege of few. Our lives, it seems, are like capital entrusted to us to be expended as wisely and effectively as we may. With them we purchase whatever of accomplishment the stuff that is in us permits. It is impossible to escape profound regret that a career so full of the highest promise, and a personality so overflowing with all that is fine and lovable, should have been cut short at the age of thirty-one. Yet who can doubt that in a few months Perry bought with his life the fullest achievement of a life-time—a glorious part in the salvation of Liberty and Justice and Decency, indeed of Civilization itself! L. C. Graton.

Jan 1, 1920

By F. A. Forward, J. Halpern

A new process is described for extracting uranium from ores containing sulphidic minerals, which comprises treating an aqueous pulp of the ore with air or oxygen at elevated temperatures and pressures. The acid required to dissolve the uranium is generated during the leach through oxidation of the sulphides. The chemistry of the process is discussed and laboratory results are presented to illustrate the operation of the method and the variables which control it. With most ores, leaching at a temperature of 130°C and an oxygen partial pressure of 10 psi provides uranium extractions of 90 to 95 pct in 4 to 6 hr. The acidity and level of dissolved impurities in the leach liquor can be kept fairly low. The method is characterized by a number of advantageous features including low reagent cost, short retention times, and high recoveries. RECENTLY there have been developed several processes for extracting metal values from ores by pressure leaching techniques;' -' an example is the carbonate leaching process for uranium ores which has been studied in this laboratory.' Leaching is carried out under oxygen pressure to ensure oxidation of the uranium to hexavalent compounds which are soluble in carbonate solutions. During the course of investigations relating to this process, it was observed that sulphide minerals, such as pyrite, usually were oxidized under the conditions of the leach treatment resulting in the formation of iron hydroxides and sodium sulphate, i.e. 2 FeS= + 7Vz O2 + 8 Na,CO3 + 7 H,,O -* 2 Fe(OH)3 + 4 Na2SO4 + 8 NaHCO.,. [1]

Jan 1, 1956

By W. G. Lidman, H. J. Hamjian

' I HE fabrication of many materials from powders involves a sintering process. A mass of powder will sinter because of the excess free energy over the same mass in the densified state caused by the higher total surface area of the powder. An understanding of the kinetics and mechanism of sintering should assist in improving the properties of such materials. The present investigation conducted at the NACA Lewis laboratory deals with the sintering of chromium carbide. Dry sintering (sintering at a temperature below the melting point) was divided into two stages by Shaler:' the first stage, during which the particles preserve much of their original shape and the voids are interconnected, and the second stage, during which densification occurs and the pores are isolated. The mechanism of forming interfaces between particles, or welding together of particles, has been investigated by Kuczynski2 and may be described by any one or a combination of the following mechanisms: viscous flow, evaporation and condensation, volume diffusion, or surface diffusion. The mechanism by which pores are closed or eliminated (densification) during sintering, is of interest. Grain growth observed during sintering may be attributed to the variation in the surface energies of individual grains, causing some grains to grow at the expense of others. Grain boundary migration occurs presumably by a diffusion process, therefore the rate of grain growth would be expected to increase exponentially with increasing time and temperature. Thus, for practical sintering times of less than 1 hr, a certain minimum temperature may exist at which major structural and property changes will occur. Densification and kinetics of grain growth during sintering under pressure of chromium carbide were investigated to provide additional information which will aid in describing more accurately the sintering process and the mechanisms involved. This material was selected for this study because of the current interest in high strength, oxidation resistant refractory materials, such as carbides, which are sintered to produce solid, dense materials from powders. Sintering under pressure is a process where the heat and pressure are applied to the compact simultaneously, specimens for this work were prepared by sintering under pressure at different temperatures and for various time periods. Experimental Procedure Preparation of Specimens: Chemical analysis of the commercial chromium carbide used in this investigation was as follows: Cr 86.19 pct, C 12.14 pct, and Fe 0.2 pct. X-ray diffraction powder patterns gave characteristic diffraction lines of Cr3C2 crystal structure. Powder particle size was determined microscopically and the average initial particle size was 6 microns with 85 pct between 2 and 10 microns. Specimens sintered under pressure were formed in graphite dies3 heated by induction. Sintering temperatures were measured with an optical pyrometer by sighting into a 3/8-in. hole drilled 1 in. deep at the midsection of the graphite die. A load of approximately 1 ton per sq in. was applied to the powder. The die assembly was heated in 20 min to the highest temperature (2500°F') at which no increase in grain size could be observed, and less than 2.5 min were required to heat from this temperature to the maximum temperature (3000°F). Sintering temperatures and times for the specimens of this investigation are indicated in Table I. Analysis of Specimens: Specimens polished with diamond abrasives were etched to reveal the grain boundaries with a 1:1 mixture of 20 pct potassium hydroxide and 20 pct potassium ferricyanide heated to 160°F. Representative areas of each sample were photographed at 1000 diameters. The largest diameters of all well-defined grains were measured, but only the measurements of 15 of the largest grains were averaged in order to determine an index of grain size on the assumption that they were among the first to begin growth. Densities were determined from differential weighing of the samples in air and water. The reported density values are considered correct within ±0.01 g per milliliter. Results and Discussion Metal compacts have exhibited grain growth when sintered at temperatures about two-thirds of the absolute temperature of their melting point.' Grain growth also occurs during the sintering of chromium carbide and is illustrated by the micrographs shown in Fig. 1. These micrographs were prepared from specimens sintered for 90 min at temperatures ranging from 1371°C (2500°F) to 1648°C (3000°F). Average grain size and density measurements of specimens investigated are presented in Table I. The relationship between grain size and sintering tem-

Jan 1, 1954

By R. W. Stormont, F. Wald

The phase diagram of the Pseudobinary section PbTe-Fe was determined. It was found to contain a monotectic and a eutectic reaction, the latter one taking place at 14 at. pct Fe and 875° * 5°C. The solid solubility of iron in PbTe was found to be 0.3 at. pct by electronmicroProbe analysis. No solubility of PbTe was detected in iron. Slight deviations from true pseudobinary behavior were found to occur in the range of - 5 to 10 at. pct Fe. In the course of a general investigation of reactions of various metals with lead and tin telluride,' the lead telluride-iron system was reinvestigated. It had been established much earlier than iron does not chemically react with lead telluride but forms a eutectic with a melting point of 879" The eutectic composition or other related information has never been reported, but for a number of years iron has been in general use for contacting of lead telluride and lead telluride alloys for thermoelectric applications. It seems therefore desirable to clarify the exact constitution of the system to furnish a base for the long-term evaluation of bonds made between lead telluride and iron either by pressure contacting or by brazing methods. I) EXPERIMENTAL METHODS Lead telluride-iron alloys were prepared in 10-g charges, using premelted lead telluride. This material was prepared from high-purity, semiconductor-grade lead and tellurium obtained from the American Smelting and Refining Co. and described as 99.999 pct pure. The iron used was "Armco" iron; the major impurities found here were 0.02 pct C, 0.018 pct Si, and 0.015 pct Cr. All remaining impurities were less than 0.01, the total of all impurities not exceeding 0.15 pct. Charges were prepared in closed quartz arnpoules which were evacuated and in some cases backfilled with high-purity argon to retard excessive lead telluride evaporation and deposition in slightly cooler parts of the ampoule. For high iron concentrations, this can lead to total separation of the constituents, since the vapor pressure and the sublimation rate of PbTe are quite high.4 Nevertheless, since the ampoules are closed, no change in overall composition was expected and the nominal composition of all alloys was assumed to be retained. X-ray diffraction analysis, thermal analysis, and microsections were used in the evaluation of the alloys. The nature of the system was such that X-ray diffraction was not particularly helpful. It merely served to establish that at all concentrations PbTe and a! iron were in equilibrium at room temperature. Thermal analysis was carried out by taking direct temperature vs time curves on a Sargent recorder where a width of 10 in. was kept as 1 or 0.5 mv by use of an automatic bucking voltage network. Quartz ampoules with minimized dead space, coated with boron nitride and fitted with a thermocouple reentrant, were used as containers for the charge. At high temperatures and over long periods of time, boron nitride reacts with iron. For the thermal analysis runs, however, this was not significant. More significant was the fact that the vapor pressure of PbTe at some of the meas -uring temperatures apparently exceeded I atrn quite considerably. This, in some cases, caused the slightly softened quartz tubes to blow out if great care was not taken to contain them and minimize time and temperatures used. As containers pure nickel tubes were used which also served to avoid temperature gradients in the quartz ampoule. Nevertheless, the experimental difficulties at high temperatures were severe and the monotectic temperature could therefore not be determined accurately. In general, the accuracy reached by the thermal analysis setup in this case is *4"C as determined with gold, silver, and tin, under the conditions of analysis here. Inherently, the apparatus is capable of reaching accuracies better than i 1°C. Also, difficulties were encountered in microsection-ing. They were related to polishing, since it is rather difficult to avoid pulling the iron out of the weak and brittle lead telluride matrix. It proved best to follow a procedure where, after grinding to 600 grit on carborundum paper, a polish with 6 p diamond was used on nylon cloth. Finally, #3 "Buehler" alumina and an automatic polisher were used for -5 min only, to avoid relief. The best etching results were achieved with

Jan 1, 1969

By G. Baralis, P. Gondi, I. Tangerini, G. Scandola

The precipitation behavior of Zn-0.5 pct A1 alloy single crystals was studied by means of electrical resistivity measurements and by optical and electron microscopy. The single crystals for the resistivity measurements were prepared by an original method in - 100-p -thick sheets. The order of the precipitation kinetics ranged between 1 and 1.5. The dislocations play a relevant role in the first-order kinetics. Precipitation always occurs both on dispersed particles and on dislocations. Statistical examinations have shown that the first-order kinetics can have two different activation energies; i.e., the precipitation can have dz;fferent mechanisnrs which could not be identified, however, in the course of the research. During the tnetallographic exanzination of the precipitation structures a specific process of dislocation decoration was obsereed. The main purpose of this work was to study the contribution of dislocations to the precipitation. A number of authors have observed precipitation on dislocations and reference might be made to several monographs on the ubject.'' The possibility that dislocations also accelerate precipitation has been considered by Turn-bull3 and Fischer et al.4 The studies described in the present paper were carried out on zinc, chosen as a base metal owing to the ease with which dislocations can be introduced into it and because of the absence of excess vacancies after quenching in conditions where phenomena of accelerated precipitation still occur. Aluminum was preferred as alloying element because of the accelerated precipitation phenomena that resulted in a preliminary reearch. EXPERIMENTAL METHODS The observations refer to a Zn-0.5 pct A1 alloy. The zinc was 99.995 pct pure; a typical spectroscopical analysis is given in Table I. As a rule the alloy was subjected to homogenization, quenching, or slow cooling and annealing. Homogenization was carried out by heating at 390" to 410°C for 24 hr. From the homogenization temperature, some specimens were quenched and some slowly cooled at a rate of 2°C per sec. At this rate no precipitate was detectable under the optical microscope just after cooling. Quenching was carried out simply by dropping the specimens into water, aqueous ethylene glycol solution at -30" c, or liquid-nitrogen baths placed close to the homogenization oven. Vaseline oil baths were used with a thermal stabilization of 10-20 for both the aging treatments and the measurements; aging was generally carried out at 90" or 130°C. To avoid oxidation phenomena during heating, the vaseline oil baths had to be frequently renewed. The precipitation kinetics were studied by means of electrical resistivity measurements, using ans potentiometric method (reproducibility ± 5 x 10 5 v, that is 0.5 pct of the total voltage decreases on the specimens during precipitation). First, various types of specimens were tested, i.e., polycrystals, single crystals grown in capillary quartz tubes, and thin single-crystal sheets prepared by means of an original method requiring no container except for the natural oxide. Even if fully annealed, the polycrystals and the capillary grown single crystals showed resistivity in -creases, most probably due to dislocations introduced in the course of the measurements. Similar resistivity increases in pure zinc were noticed by another author. Only the single-crystal sheets showed no resistivity change; thus they were chosen for the subsequent tests. As already mentioned, these single crystals were obtained by using, as a container, the natural oxide on the zinc surface; the oxide strength is sufficient to maintain the original shape during melting with sheets up to 500 p thick. An initial zone melting and subsequent zone leveling, which led also to formation of the single crystals, were thus carried out on rolled sheets of the required thicknesses (- 100 p) and shape, lying on a flat silica surface. The resistivities were first evaluated by measurements at the liquid-nitrogen temperature. This method gave poor reproducibility, however, and this was attributed to the thermal cycles which had to be operated. To avoid cycles and handling, it was therefore decided to make measurements directly in the annealing oil baths; this required thermal stabilization at ilo-' "C. In this way only the resistance changes were measured. Specimens of pure zinc and of completely annealed alloy were always examined as controls together with those under consideration; only those measurement runs were taken into account where the reference samples showed no resistance increases. Again, the main inconvenience was due to oxidation and this was avoided by renewing the oil baths; even so data reproducibility was poor and the observations were therefore carried out on a large number (many hundreds) of specimens so as to provide indications of statistical value. For the transmission observations under the elec-

Jan 1, 1969

Meeting, Apr. 25, 1913.-President Rand recommended the appointment of the Nominating Committee (see p. i), and a Committee on the Use of Electricity in Mines (see p. xliv), which committees were duly approved and appointed. President Rand recommended the establishment of. a Committee on Mining Methods, and requested authority for the President to appoint the members of this Committee, both of which recommendations were approved. The name of the Committee on Economic Geology was, at its own request, changed to the Committee on Mining Geology. The request of the Iron and Steel Committee, that a meeting of the Institute, under the auspices of this Committee, be held in the latter part of October, the place of meeting to be decided later, was granted.

Jan 5, 1913

By W. H. Bassett, J. C. Bradley

In considering the effects of reducing gases on hot solid copper the following conclusions have been reached. (I) Depth of deoxidation of copper heated in reducing gas is grealer the smaller the amount of cuprous oxide originally present in the copper, the range studied being from 0.015 to 0.136 per cent. oxygen. It is suggested that the reason for this diflerence in depth of deoxidation is thai, when the copper is low in cuprous oxide, the reducing gas is diluted less by the gas that is formed in the reaction than when the copper is high in cuprous oxide; and the greater the concentration of the reducing gas the deeper the deoxidation. (2) The rate of deoxidation is much more rapid at the beginning of exposure than at the end, a condition especially noticeable at temperatures around 900" C.; that is, deoxidaion is retarded as the depth penetrated by the reducing gas increases. (3) Within the accuracy of the experiments arsenic in copper up to 0.5 per cent. has no tendency to increase or decrease the action of a reducing gas on the cuprous oxide presenx in the copper. In 1912 pieces of 0.365-in. hard copper rod 1/2 in. long were heated in a porcelain tube in an electric furnace, while illuminating gas was passed through. An approximate analysis of this gas is: Hydrogen 38 per cent., carbon monoxide 30 per cent., illuminants 13 per cent., methane 10 per cent., ethane 3 per cent., carbon dioxide 3 per cent., nitrogen 2 per cent., oxygen 0.4 per cent. After heating for various lengths of time at various temperatures, samples were quenched

Jan 1, 1926

By A. D. Rich

The term "bleaching clay" or "bleaching earth," as used in the oil industries, refers to clays that in their natural state, or after chemical or physical activation, have the capacity for adsorbing coloring matter from oil. There are three common types of bleaching clays: fuller's earth, activated clays, and activated bauxite. Fuller's earth, or naturally active clay, is prepared from bentonites (see Chap. 5) that possess natural activity. It is not activated commercially; in fact, earths of this type ordinarily do not respond satisfactorily to acid activation. Fuller's earth is prepared in pulverized as well as granular form for use in the contacting and percolation processes, respectively. Acid-activated clays also are of bentonitic origin. The basic raw clay, however, is of a type that has a very low natural activity but is highly activable by treatment with mineral acid. Commercial acid-activated clays generally possess several times the decolorizing power (bleaching efficiency) of the best quality of fuller's earth. The former are prepared commercially only in the pulverized grade because of the difficulties in obtaining a satisfactory granular product, and hence are used only in the contact process. Activated bauxite is made by heat-treating bauxite ore, which in its natural state has very little natural activity. The commercial product is prepared in granular form for use in the percolation process on petroleum oils. For the most part, bleaching clay is used commercially in the decolorization of animal, vegetable and petroleum oils, fats and waxes. It is applied in two ways: (1) by the percolation method and (2) by the contacting method. Percolation refers to the passage of oil through a bed of granular clay whereas contacting refers to direct agitation of oil and pulverized clay followed by removal of the clay from the oil by filtration. In either case, the decolorizing effect is obtained by intimate contact between the liquid oil and the solid adsorbent. Petroleum oils are treated commercially by either the percolation or the contact process. Animal and vegetable oils are treated by the contact process only. Composition The raw clays from which both fuller's earth and acid-activated clays are prepared are composed of hydrous aluminum silicates containing varying quantities of magnesium, iron, calcium and other elements. These raw materials are usually nonswelling bentonites derived from volcanic ash or lava by weathering and hydrothermal chemical reactions. The bentonites have as their chief mineral constituent montmorillonite, which has the formula [(OH)4Si6A14O20•nH2O], according to Grim. (See Chap. 5, ref. 6, p. 91.) The underlying reasons are not fully known for the natural activity of the fuller's earth type of clay and its usual failure to further activate with mineral acid in contrast to the natural inactivity of the activatable type of clay. However, it may be said that the bentonites that are responsive to the acid-activation treatment generally have not undergone any drastic metamorphism. The chemical composition is not a reliable means of discrimination between a nonactive, a naturally active, and a nonactive but activable clay, therefore it is not possible to forecast the ultimate quality of a clay on the basis of the raw-clay analysis alone. Table 1 gives typical analyses of representative clays of the foregoing classifications.

Jan 1, 1960

By AIME AIME

THE Hazleton district of the Pennsylvania Anthracite Region will be the scene Oct. 14 and 15 of the fall meeting of the Coal Division and the Pennsylvania Anthracite Section. Here, coal mining has been active for more than 100 years and hereabouts industrial necessity inspired the numerous inventions of the Pardees, Eckley B. Coxe, a former A.I.M.E. president, and the Marltles, who contributed much to the success of the Institute in its early days, as well as to the upbuilding of modern methods in the anthracite and bituminous industries. Headquarters will be the Altamont Hotel, Hazleton, Pa. There will be two technical sessions Friday, registration preceding the first which is scheduled for 11 a.m. to 1 p. m. The second will be called at 2:30 p.m. Saturday is reserved for mine and plant visits, with golf and tennis after luncheon for those so inclined. The ladies are cordially invited to the meeting and arrangements have been made for their participation in much of the program. The chairmen of the committees preparing for the meeting are: Donald Markle, president, Jeddo-Highland Coal Co., General Committee; R. E. Hobart, mechanical superintendent, Lehigh Navigation Coal. Co., Committee on Visits and Inspections; H. D. Kynor, general manager, Northumberland Mining Co., Committee on Programs and Papers; B. H. Stockett, general manager, Weston; Dodson, Inc., Reception Committee.

Jan 1, 1932

By Carl H. Samans

THE INFORMATION AVAILABLE on the rolling characteristics of the precious metals-gold, silver, the platinum metals and their alloys-is incomplete and mostly from scattered sources. In the present paper an effort has been made to assemble and correlate it and to fill in some of the gaps that exist. GENERAL ROLLING CHARACTERISTICS SOME EFFECTS OF IMPURITIES Gold and its alloys are generally considered to be hot short and hence are usually rolled cold. Cold rolling of the yellow, green, and pink gold alloys. Which customarily contain gold, silver, copper and zinc and frequently some nickel as well, introduces no new problems since reasonable reductions are quite feasible and the alloys show little tendency to fire crack in subsequent annealing. The white gold alloys. which usually contain little or no silver and 10 pct or more nickel, are very susceptible to fire cracking1 and hence wrist he given relatively heavy reductions, i. e., 8-10 pct or more per pass with a total reduction of about 50 pct between anneals, to minimize this tendency. In addition, it is preferable to keep the bar as flat as possible during rolling. Although no comprehensive study appears to have been made of the effects of impurities on the cold rolling characteristics of gold alloys, the observations of Nowack2 on the effects of small

Jan 1, 1948

In the late 19th century Fremont Pass was only a gateway to Leadville, Colo., 12 miles to the north. Some of the silver, lead, and zinc won from this famous camp crossed the Continental Divide at Climax, passing by the huge outcrop of molybdenum on Bartlett Mountain. This element, relatively un- known in the world of commerce, was then nothing more than a joke to play on greenhorn prospectors. Even 30 or 40 years later, after the demand for metals created by World War I had forced temporary use of molybdenum as an alternate for tungsten in tool steels, the Bartlett Mountain outcrop once again became merely a curiosity. With the persistent efforts of Brainerd Phillipson, for years the president of Climax and almost the only employe, use of molybdenum gradually began to grow, first in tool steel and later in the alloy steels required by the growing automotive industry. Mr. Phillipson was first an engineer and second a salesman. The combination of these two qualities is the key to the story, not only of Climax sales but also of the growth of molybdenum from an object of idle curiosity to the point where it is today, along with chromium and nickel, one of the most versatile alloying elements in the iron and steel industries and increasingly important in chemistry.

Aug 1, 1955

By J. E. Coyne, L. E. Tanner, J. E. Boyd

In recent investigations of the isothermal transformations of the retained 0 phase in a titanium alloy having 13 pct V, 11 pct Cr, and 3 to 4 pct Al, there have been indications that the w transition phase is the initial decomposition product at temperatures below about 950°C (510 c).' This metastable phase, found in a number of titanium-base alloys rich in stabilizing elements and known to have an adverse effect on their ductility and toughness, is not easily observed by the usual experimental techniques. Since wis coherent with the /3 matrix,495 distinct interphase boundaries are not revealed metallographically. However, in some cases, an etching effect (i-e., a "mottled" /3 surface) poorly resolved by light microscopy has been found to correspond with the presence of w.6 X-ray diffraction examination has generally been the most suc- cessful means for identifying this phase and crys-tallographic determinations have been made.4'5 Dynamic elastic modulus7 and electrical resistivity measurementse have also aided in the identification of w. In the current study, the electron microscope was utilized to examine microstructures in aged Ti-13V-11Cr-3A1 that were unresolvable by light microscopy techniques. Using negative parlodion replicas (shadowed with chromium at 27 1/2 deg) examination was made of various transformation

Jan 1, 1962

By AIME

BORN in 1899, in Bridgeport, Conn., E. A. Anderson grew up in a center of the nonferrous metal industry. Perhaps that had something to do with his selection of mining as a career while an undergraduate in Yale. After securing his Ph.B. in mining he worked for a year at Handy & Harman. By this time physical metallurgy had supplanted his interest in mining and he entered the Yale graduate school where he secured his M.S. degree in metallography under C. H. Mathewson. After completing his graduate work he entered the employ of The New Jersey Zinc Co. in their research division where he has remained ever since. The transition from graduate study to industry involved no disruption of technical interests. Academic research relating to the zinc-aluminum alloys, then coming into use for die-casting, was followed by extensive and productive industrial research in the perfection and commercialization of these alloys. Research on rolled zinc and rolled zinc alloys, corrosion and stress corrosion, dry cells, electroplating on zinc, and electrodeposition of zinc followed in overlapping succession as time passed.

Jan 1, 1947

By P. E. Arnold, G. S. Ansell

RELAXATION in metals has been studied in detail by many workers in recent years.1-5 These studies have shown that there is an energy-loss peak observed in a metal placed in mechanical resonance at low frequencies which may be correlated with various metallurgical processes. These experiments have been largely used to study single-phase materials. In order to study the effect of a finely dispersed second phase in a metal matrix upon this phenomenon, the relaxation behavior of an aluminum-aluminum oxide SAP-Type alloy in both the fine-grained as-extruded and coarse-grained recrystallized conditions was investigated by the use of internal-friction measurements. The alloys studied, designated MD 2100, consist of a matrix of commercial-purity aluminum containing a finely dispersed second phase of aluminum oxide. The aluminum oxide is present in this alloy in the form of fine platelets approximately 130A units thick and several microns on edge. The mean free path betwen dispersed platelets is approximately 0.5 p. The grain size of this alloy is extremely stable at temperatures as high as the melting temperature of the aluminum matrix. In the as-extruded condition the grain diameter is several microns, while in the recrystallized condition it is several millimeters in diameter. The damping characteristics of the alloy samples were determined using a torsional-pendulum device. The internal-friction constant was determined for this alloy in both the fine-grained as-extruded and coarse-grained recrystallized conditions over the temperature range from 343" to 923°K at frequencies of 0.9, 1.3, and 1.8 cycles per sec. An internal-friction peak was observed in testing the fine-grained alloys which was not observed for the coarse-grained alloys. This peak, which might be associated with a type of grain-boundary relaxation, was observed at each of the three different test frequencies for the fine-grained sample. The temperature at which the relaxation peak occurred for each of the three different frequencies is shown in Table I. From these data an activation energy of relaxation for each pair of frequencies was determined by comparing the temperature shift of the relaxation peak with frequency between each of the test frequencies, assuming that an Arrhenius-type rate equation is applicable. The activation energy of relaxation determined from these data is also shown in Table I. The mean value of the activation energy was about 6 kcal per mole. The activation energy for the relaxation process determined in this investigation indicates that the relaxation associated with the grain boundaries in this aluminum-aluminum oxide SAP-Type alloy is quite a different process than grain boundary relaxation in single-phase aluminum alloys. In these latter alloys, the activation energy for relaxation has been found to be the activation energy for self-diffusion, approximately 36 kcal per mole1,2 Where the activation energy is the same as the activation energy for self diffusion, it has been proposed that the relaxation phenomena is dependent upon vacancy formation and motion. It is apparent therefore, that, in this aluminum-aluminum oxide SAP-Type alloy, the relaxation must be due to another type of atom transport. It has been shown previously in studies of the high-temperature, low-stress, steady-state creep behavior of as-extruded aluminum SAP-Type alloys, that the activation energy for steady-state creep is one that may be characterized by the nucleation of dislocations from the grain boundaries. It is proposed that the relaxation behavior observed here is due to a similar effect. In this case, the internal-friction peak is a resonance behavior due to the time-dependent nucleation of dislocations from grain boundaries in the sample. A process of this type would have an activation energy which is undoubtedly stress-dependent and of the form Q = Q, + (dQ/du)u

Jan 1, 1962

By W. R. Toeplitz

Probably a more descriptive title would be "Much Ado About Nothing." By "nothing," of course, I refer to the porosity which is the main feature of this type of bearing. Porosity has a decided effect on the manufacturing techniques, the structure and physical properties, the oil content, and on the installation and service of oil-retaining porous bronze bearings. A simple curve can be drawn by plotting specific gravity along the abscissa and percentage of porosity by volume on the ordinate. A bronze composition, analyzing 89 Per cent copper, 9.75 Per cent tin, and 1.25 per cent graphite, has an absolute solid specific gravity of 8.5. At this specific gravity, of course, occurs the point of zero porosity. Conversely, at loo per cent porosity, the specific gravity is zero. A similar curve can be drawn for bearings impregnated with oil; the only change being that the specific gravity at loo per cent oil will be 0.89 if we assume that that is the specific gravity of the lubricant. The curve is useful in determining the oil content by volume for any specific gravity. The normal range of oil content for porous bronze bearings of this composition is from 35 to 16 per cent, which is in the specific gravity range of from 5.8 to 7.3. In addition to the amount of porosity, the type of porosity is important. The first consideration here is that the porosity must be intercommunicating. This can be determined by a number of simple tests. The first method, which is very accurate, is to extract the oil in the bearing by cycling

Jan 1, 1945

By John Chipman

THE equilibrium between titanium in liquid iron and titanium oxides has been studied by Hadley and Derge.' They have shown that a minimum occurs in the oxygen content of the metal between 0.1 and 1.0 pct Ti, but its exact level was not fixed. The oxide phase in this minimum range was principally TiO, containing some iron oxide. On the other hand, for concentrations above 5 pct Ti the oxide phase was TiO and the oxygen content of the metal increased rapidly with increasing titanium content. From their observations and the free energy of Ti0 and TiOz reported by Kelley and ah,' it is possible to derive approximate values for the activity coefficients of titanium and oxygen in liquid iron-titanium alloys and the conditions for equilibrium in steel deoxidation. Neglecting possible departures from the stoichio-metric composition, the condition of equilibrium with Ti0 may be expressed as follows: TiO= Ti_ + C) log K = log NTl + log [% O] + log yTi + log fQ Here as a matter of convenience the titanium concentration is expressed in mol fraction while that of oxygen is in weight percent. The activity coefficients are yTi and fo. The value of log fo approaches zero as the concentration of titanium approaches zero, while that of log yTi approaches a limiting value of In Fig. 1 the sum of log NTi + log [% 0] is plotted for mol fractions of titanium between 0.05 and 0.50. The smooth extrapolation gives a value of —4.15 which corresponds to log K — log y:i . We therefore have the equation: According to the data of Kelley and Mah,' the free energy of formation of Ti0 at 1900°K is -82,400 cal. The free energy of solution of half a mol of oxygen in iron, taking 1 pct 0 as the standard state, is -29,300 cal. From these we write: From these equations the activity coefficient of titanium at infinite dilution in iron is found to have a value of 0.011 or log y°. = -1.96. This is only an approximate value but is certainly better than the estimated 0.05 in Basic Open Hearth Steelmaking To obtain approximate values for the activity coefficient at intermediate concentrations, it is as- sumed that log yTi(l is constant and equal to -1.96. This corresponds to a value of E;: = 3 In yTi/aNTi = 9.0 which is not unreasonable We now have the value for the activity of titanium and the percentage of oxygen in equilibrium with TiO. It is therefore a simple matter to calculate the activity coefficient of oxygen which is shown in Fig. 2. The effect of titanium is rather large, being comparable to that of vanadium, but not so large as has been reported for aluminum. The slope of the line at low concentrations corresponds to E: = aln yo/ aNTi=-0.37. At concentrations below 1 pct Ti the deoxidation constant and oxygen content for equilibrium with TiO, can be calculated from the foregoing data and the free energy of formation of TiO,, which according to Kelley and Mah is -144,600 cal at 1900°K. The free energy of solution of oxygen has been given; that of Ti to form a dilute solution with 1 pct Ti as the standard state is RT ln (0.5585 y:i/47.9) = -34,800 cal. From these data we find (for concentrations in wt pct): TiO, = Ti + 2 -0; hFTgO0= + 51,200 cal log if =-5.89 The interaction coefficients, concentrations being expressed as wt pct, are e;: = alogfTi/a[% Ti] = +0.048 and e:' = a logfo,/a[ojTi] = -0.187. The calculation gives the following results which, in view of the impurity of the oxide phase, must be regarded as approximate:

Jan 1, 1961

EUGENE COSTE, ? Calgary, Alta.-Evidently in Argentine they have a petroliferous province just east of the Andes where very much the same conditions exist as are found on the east side of the Rocky Mountains and in the plains adjacent. It strikes me, though, that the same mistake is being made in Argentine in the exploration for oil as was made in Alberta, Canada; viz., drilling the wells too .near the seepages in the belt in the eastern part of the petroliferous province, too near the mountains. This same mistake was made in Alberta, with disastrous results; viz., only fissure production was found. The strata so near the mountains are tilted at a very strong angle, such as is described in this paper, and the dislocations are intense. On the other hand, we have found that when we get 100 or 200 mi. away from the mountains we get into oil and gas belts which are very prolific. So far our fields in Alberta have been gas, but in Wyoming, as you know, they get many thousands of barrels a day. I have no doubt that conditions in Argentine are exactly similar but that they have so far kept too near the mountains and that they want to explore the belts farther east to obtain better results.

Jan 4, 1919