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

The temperature dependence of the rate of grain boundary migration was measured in bicrystals of zone-refined lead containing from 20 to less than 1 ppm by wezght of tin. The apparent activation energy in the temperature range from 320" to 200oC is markedly dependent upon the solute tin concentration and upon the orientation relationship of the grains adjacent to the grain boundavy. The quantitative experimental observat~ons are compared with the predictions of various theories of grain boundary migration. In previous work.&apos;?&apos; the mobility of individual grain boundaries was studied as a function of impurity concentration and type of boundary. Grain boundary migration occurred at the expense of dislocation arrays which were introduced into the specimen during solidification. Boundary mobility in zone-refined lead at 300°C was markedly decreased by small additions of tin. 0.004 wt pct being sufficient to decrease the rate of grain boundary migration by a factor of 1000. The mobility of grain boundaries having polar orientation relationships near 38 and 22 deg about <Ill>, and 28 deg about <100>, was much less sensitive to tin concentration in the range studied. As a result, these boundaries have relatively high mobilities. The present paper is a continuation of the above study. Data are now presented on the temperature dependence of the motion of individual grain boundaries in zone-refined lead as a function of solute tin concentration and orientation relationship of adjacent grains at the grain boundary. The experimental observations are compared with the predictions of a number of theories of grain boundary migration3-8 which, prior to the present experimental investigation, could not be critically evaluated. EXPERIMENTAL PROCEDURE The striation or lineage structure of melt-grown single crystals of zone-refined lead, containing various additions of tin, was utilized to provide a driving force for grain boundary migration, as previously described.1,2 Each grain boundary under study separated the striated single crystal from another grain which was introduced by localized plastic deformation and recrystallization of a small region of the sample. The speed of migration of grain boundaries in dilute alloys of tin in zone-refined lead was investigated as a function of 1) tin concentration from < 0.0001 to 0.002 wt pct, 2) temperature in the range of 200" to 320°C, and 3) orientation relationship of the adjacent grains at the grain boundary. The substructure driving energy available for grain boundary migration was estimated to be about 4000 ergs per cu cm, within a factor of two, from specimen to specimen.&apos; The specimen dimensions, and growth and alloying procedures for the preparation of striated single crystals of lead of known tin composition, were as described previously.&apos; Each bicrystal was carefully wrapped in aluminum foil, and annealed in a well-stirred salt bath consisting of 50 pct NaNO2 and 50 pct KNO3, for known periods of time at a series of constant temperatures (*2°C). The grain boundary positions, before and after each anneal, were determined by etching lightly in a solution of 5 pct nitric acid in methyl alcohol, in order to follow the motion of the boundary and determine its rate of migration. Thus, the rate of motion of the grain boundary in a single specimen was measured at various temperatures. The above procedure was carried out for each grain boundary in seventeen different bicrystal specimens.

Jan 1, 1960

By R. L., Fullman

During the past year there have been a number of significant investigations that have furnished evidence on the driving forces governing grain growth and on the role played by boundary impurities. Thus Burke has shown that in high purity alpha brass the rate of grain growth in the earliest stages is approximately inversely proportional to the existing grain size. This relation agrees with one derived by Zener assuming that surface energy was the driving force in grain growth. Also in confirmation of the surface energy hypothesis, Burke found that growth virtually stopped when the grain boundaries or even only the grain corners were melted.

Jan 1, 1949

By C. E. Sims, G. A. Lillieqvist

The following presentation is more a summation of observations made and conclusions drawn over a period of three to four years than a report of experiments made with a definite objective. Tests were made, of course, to verify hypotheses, but the large mass of data was collected incidental to other work. Lack of space forbids the presentation of more than a few of those data. On the other hand, it is unfortunate that some of the most illustrative examples are not available. The work is admittedly incomplete but is presented in the hope that it will stimulate further work along a similar line. The answers to many of the questions left unanswered by this paper will be found only after long and painstaking study, such as is scarcely possible in a commercial laboratory where problems of immediate importance consume most of the time. It is also hoped that this study will in some measure throw light on some of the dark spots of steelmaking, and help to clarify some of the annoyingly vague references to "good practice." Only cast steel was studied and the conclusions apply to cast steel, but it is the authors&apos; opinion that the quality of rolled or forged steel is largely dependent on the quality of the ingot, which is a casting. Although this discussion deals almost entirely with inclusions, it is important that the reader understand that only those natural inclusions which owe their origin to the solubility of certain materials in steel and to the chemical reactions of steelmaking are considered. Accidental inclusions, such as entrapped particles of slag, nozzle, runner, or mold arc outside its province and are not considered. Such accidental inclusions are always dangerous and should be carefully avoided. Relation between Ductility and Nonmetallic Inclusions In September, 1928, an acid electric furnace was put into operation at the Indiana Harbor plant of the American Steel Foundries. Following the usual practice, aluminum additions were made in order to obtain sound castings. Immediately the problem of low ductility arose. Previous to that time, only open-hearth steel was produced, and, aluminum being used rarely in that steel, there had been practically no trouble with low ductility in the lower carbon range.

Jan 1, 1932

By C. O. Fairchild

ONE of the fundamental principles of efficiency is the use of adequate and permanent records. The rapid increase in the manufacture and use of recording pryometers is a proof of the appreciation of efficiency principles on the part of the manufacturers engaged in the various technical industries. Where recording pyrometers are not employed in an industry in which temperature measurements are necessary, one will generally find that a printed form is used upon which is written, periodically, the temperatures measured by an indicating instrument. It is no serious condemnation of the workman to state that such records are often "doctored," but it is rather a reflection upon the executive who puts such temptation in the way of a workman. One of the well-known "tricks of the trade" is to "force." a furnace so that it will be at the proper temperature during the periodic trips of the foreman or other official. Indicating instruments and recorders may be used together to great advantage. The recorder furnishes .a printed record and a check upon the operator of the furnace, and a record of value in correlating properties of the finished product with the heat treatment. The indicator should be of assistance to the operator in controlling the furnace or oven. Modern practice requires a temperature-recording instrument that is as simple as possible, rugged, reliable, and sufficiently accurate. Of these qualifications reliability is paramount, particularly in cases where the recorder is used for controlling the temperature automatically. By a reliable instrument is meant one that will run continuously with little attention and with a consistent degree of accuracy. That is, if it is in error by 5 per cent. one day, it must be in error by a like amount on any other clay, and not by 2 per cent. or 10 per cent. The earlier forms of recorders were complex and delicate, or mechanically unsatisfactory and inaccurate, and required considerable attention to keep them in operation. Within the past few years, however, the development in the manufacture of temperature recording devices has been highly satisfactory and many excellent instruments are now available. .

Jan 9, 1919

By D. J. Weintritt, R. G. Hughes

Statistics show arz increase in the average depth of wells drilled in recent years. As a corollary to this trend, drilling fluids have been improved in an effort to meet the problems inherent at temperatures approaching 500°F. Of importance are (1) deterioration of mud components and (2) the effect of solids on filtration and rheological properties. High-temperature, stable water-base and oil-bare muds are discussed. Those areas in which differences exist are pointed out. Results are based on data taken from the Fann consistotneter, rheometer and shear-strength measurements, static and dynamic filtration tests, methy-lene blue test for bentonite solids and specific heat measLrrenlents of muds. INTRODUCTION Higher well temperatures go along with the fact that the average depth of wells continues to increase. Recent data by Gardner&apos; lists 137 completions deeper than 15,000 ft for the first half of 1964 with a record second-half total of 167 wells drilling or proposed. In addition, there has been an increase in drilling for steam for power production or mineral recovery. In this application the depths are modest, but the mud may approach the critical pressure and temperature of water. Scearce and Magnon&apos; report drilling mud used at temperatures of about 700°F in the Salton Sea area of California. Most deep wells have been drilled with water-base muds. In recent years, however, there has been a substantial increase in the use of oil-base muds because of technological advances in effective additives. The significance of this development was dealt with in considerable detail by Simpson and his co-workers.3 Additiona1 field data have now been obtained to indicate that oil muds are competitive in control, performance and cost with the best types of water muds for use at high temperaturc. This parallel offer of two very different fluid systems, each offering a similar variability in performance, cost and convenience, has created the need to evaluate the merits of these fluids under specified conditions so that the advantages and disadvantages of each can be weighed in relation to the over-all drilling program. This paper is not intended as a review of all the factors. Rather, it attempts to emphasize: (1) important condltions and facts peculiar to high-temperature drilling muds, (2) that more than one imposed test condition or testing method is necessary to describe the quality of a mud at high temperature and (3) that elaborate experimental precautions are necessary whenever laboratory data are used in selection of a mud for field use. WHAT IS A HIGH-TEMPERATURE DRILLING FLUID? For the purpose of this discussion, a high-temperature drilling fluid is any system so formulated or treated to economically minimize the effects of temperature on the properties of the fluid. Our experience in drilling fluids suggests that these effects become obvious for many mud materials at temperatures of 300F or higher. It is understood that hydrolysis of starches, depoly-merization of certain organic thinners, or irreversible chemical reactions (such as that of clay and lime) can affect filtration, viscosity and shear strength at less than 300F. However, the temperature level is not a serious point and in no way affects the precautions and techniques used in this study. An up-to-date review of the literature on high-temperature drilling fluids and the many variations was treated by Rogers&apos;in 1963. EXPERIMENTAL REQUIREMENTS TESTING EQUIPMENT AND PROCEDURES With the advent of deeper drilling and increased demand for temperature-stable drilling fluids, new testing equipment and laboratory techniques were devised for the evaluation of drilling fluids subjected to elevated temperature and pressure. While the equipment has not been standardized, it is in widespread use. Milligan et al. Qescribe a filtration cell for determining the filtration properties of drilling fluids at temperatures in excess of 300F. They showed the effect of variations in temperature and pressure on oil and water muds filtered in the 300 to 400F range. The dynamic filtration apparatus described by Simpson6 permits the study of the filtration properties to temperatures of 350F for drilling fluids circulated over sandstone cores. Watkins et al.&apos; describe the use of pressure bombs for studying the effect of prolonged periods of elevated temperature upon the gelation or solidification of drilling fluids. Chisholm et a1.&apos; describe the use of a modified cement consistometer adapted for use in drilling fluid evaluations. A similar consistometer is used in this study, although the application and data-recording method have been changed. The consistency of a mud sample is measured by timing the movement of a soft iron bob which is magnetically moved up and down in the sample container.* Changer in the time of travel and the temperature of the mud at that moment are plotted with a two-point Brown Elec-tronik Recorder. A 10-in. chart with a speed of 4-in./hr is used. Fia.- 1 is a generalized internretation of the data ob-

Jan 1, 1966

By C. K. Leith

IN telling the story of Canada&apos;s minerals many interesting and spectacular details will be passed over to permit pointing out some of the significant inter- national aspects. No country now has enough of all minerals for its own use. The problems of satisfaction of both national and world demands under these conditions have become international in scope, and history supplies no obvious solutions. The minerals of Canada are coming to play a prominent part in such problems. Production and Reserves In the last decade Canada has rapidly advanced in mineral production. In 1928 the total value of mineral products from Canadian sources reached 273 millions of dollars. Canada ranks first in production of nickel, first in asbestos, second in cobalt, third in gold and silver, fourth in lead and copper, and sixth in zinc.

Jan 1, 1929

By AIME AIME

BY the end of 1943, the United States will be able to produce aluminum at a rate of 1,150,000 tons a year. How much aluminum is 1,150,000 tons? It is sufficient to replace every railroad passenger car in this country three times a year. Or, it would put a thirty-piece aluminum cooking utensil set in every one of America&apos;s 34,000,000 homes with enough metal left over to make 5,000,000 miles of aluminum transmission cable, such as was used in the electrification of much of rural America. Expansion of aluminum production capacity for the war program has occurred in three steps: (1) expansion by private industry; (2) the letting of contracts by the Defense Plant Corp. for the construction of additional aluminum plants which may remain after the war to compete with existing facilities; and (3) the more recently announced D.P.C. program for the building of emergency plants to make aluminum, using stand-by power available in large metropolitan centers power of relatively higher cost, making it questionable whether such plants, now gravely needed, will be able to compete in a peacetime economy.

Jan 1, 1943

Jan 1, 1957

THE developments in construction and operation of the basic open-hearth furnace that have taken place in recent years have placed new emphasis on the vital influence played by regulation and control of the combustion system in both furnace production and furnace life. The several factors influencing flame development, such as regulation of fuel supply, air supply, air preheat, furnace draft, and furnace reversal, must be controlled closely if successful furnace performance is to be accomplished. Rugged instrumentation of distinctive design is required to sup- ply dependable information concerning operating conditions, which is requisite to proper regulation of combustion. This chapter attempts to give a practical discussion of the various features of open-hearth practice and instrumentation related to the efficient heating of the furnace, control of temperature, and protection of the furnace structure from accidental overheating. The appended references will be helpful to readers wanting a more detailed treatment of individual topics. OPEN-HEARTH FUELS The most important open-hearth fuels are listed in Table 4-1 together with their compositions and other data useful for combustion calculations. A detailed discussion of open-hearth fuels is not attempted here, but certain factors peculiar to their application to this type of process are briefly indicated on the following pages. Very often an open-hearth shop is forced by economic factors to use a fuel to which its furnaces are not very well adapted, because the general fuel-allocation scheme for the works as a whole seems to demand it. Often a variable marginal supply of coke-oven gas or tar must be consumed by the open hearth, together with another fuel such as producer gas, natural gas, or oil, to fill out total requirements. Most furnaces employ more than one kind of fuel during their useful life; however, the partial redesign

Jan 1, 1964

By E. S. Bumps, W. F. Craig, M. Baeyertz

Metallurgists have looked at fractures macroscopically for many years and have evolved a vocabulary in which such words as "cleavage," "brittle," "shear," "ductile," "granular," "fibrous," and "silky" are used to describe the appearance of the fractured surface; but the meaning of these words in terms of metal structure is not well established. Observations of the structural meaning of "brittle" and "ductile" fractures in plate steels have been made, notably, by Kramer and coworkers1 and by Tipper.2 Grossman3 has studied the fracture of tempered martensite and combinations of ferrite and martensite. Notwithstanding these and other less concerted attacks on the problem, present understanding of fracture rests more on assumptions and logic than on experiment. It is the purpose of this paper to add a little to the growing fund of experimental observations of the nature of fractures in steel. The particular fractures to be described were obtained in conventional impact testing of an ordinary structural steel shape. In impact tests of the Charpy type, the specimens fail in a characteristic manner that depends on the steel and the temperature of testing. With ordinary structural and many other steel products, an appropriate range of testing temperature will cause a considerable change in the energy absorbed before fracture. This change is known as the energy transition and is accompanied, more or less closely, by alteration in the appearance of the fracture. At testing temperatures below the transition, the terms "brittle," "cleavage," or "granular" are used to describe the fracture; above it, "ductile" or "shear" are often used. Within the transition, the fracture changes from "brittle" to "ductile" by a progression in appearance, wherein the "brittle" portion of the fracture becomes restricted to a smaller and smaller central area of the fracture, as the testing temperature is raised and the "ductile" type of fracture is approached. All this is well known to metallurgists. The specimens under consideration are of the conventional V-notch Charpy type. They were taken from a structural steel shape of the following analysis: C Mn P S Si 0.17 0.46 0.009 0.029 0.03 Both longitudinal and transverse specimens were tested and examined. Fig 1 shows the energy values plotted against testing temperatures in the usual way. The curves for both longitudinal and transverse specimens show an energy transition, although the maximum energy absorbed at testing temperatures above the transition is greater in the case of the longitudinal specimens. Fig 2 illustrates the changes in the macroscopic appearance of the fractures that are associated with the energy transitions shown in Fig 1. Macrographs of the fractured surfaces of the specimens have been identified with the fracture ratings at intervals on each fracture curve. The numerical fracture rating on the ordinate of Fig 2 indicates the percentage of the area of each fracture that was considered to be "brittle" on macroscopic observation. Such rating of the fracture type in impact tests is now customary in many laboratories. Hereafter the specimens will be identified by reference to Fig 2 as 90 pct "brittle," 80 pct "brittle," and so on, in accordance with this macroscopic evaluation of the appearance of the fractured surface. The discussion of the fractures is divided into three parts. The first two are concerned with the mode of fracture and its relation to general structural features. As the same metal-lographic features occur in both longi-

Jan 1, 1950

By Gerald F. G. Sherman

The ore deposits of the Warren district, in which the mines of the Copper Queen Consolidated Mining Co. are situated, have been described in a number of technical publications, and will not be discussed here in detail. Certain of their characteristics, however, control methods of underground transportation and hoisting of ore. In the Copper Queen mine, the majority of the ore has occurred in a zone encircling the west boundary of the porphyry intrusion of Sacramento Hill. It has a width varying from 800 to 1,200 ft., and a thickness of about 400 ft. It reaches the surface in the older part of the mine to the northwest, but dips to the southeast, where it is reached at 1,400 ft. below the Czar collar, in its farthest extension at present developed on Copper Queen ground. There is one major extension from the northwest end of the zone toward the west along the Czar fault, and others of minor importance. Individual orebodies are scattercd through the zone in an eccentric manner, only matched by their own irregularities of form and size. Their most gencral characteristics are the softness of the ore and their grcat horizontal rather than vertical extent. It has been estimated that the average vertical thickness of ore in the Czar and Lowell divisions is between 30 and 35 ft. It is calculated by assuming it to be uniformly distributed over its horizontally projected area. In this zone, and for some distance above it, the ground has been subjected to intense alteration and intense but irregular oxidation. It has resulted in an enormous quantity of earthy or clayey material, which may be either ore or waste, which when wet is both heavy and tenacious. Below alteration, the ground is fairly hard, and the limestones contain primary ores differing from those heretofore considered typical of the camp, and which have not yet been thoroughly exploited. The mine production has been drawn from many orebodies spread over a great area.l A diagram map (Fig. I), of haulage drifts and loading stations, illustrates the situation in 1914.

Jan 1, 1916

By John J. Gilman

BECAUSE of their layerlike structure, zinc crystals exhibit strong anisotropies for almost all physical and chemical properties. This should, and indeed does, greatly influence the plasticity of zinc for various crystal orientations. At low temperatures, the investigator of this plastic anisotropy is plagued by the great variety of deformation modes that operate. However, at high temperatures (250° to 419°C) only two deformation modes predominate: basal (0001) and prismatic (1010) glide. Furthermore, since strain hardening is virtually absent at high temperatures, the plasticity for these two modes of deformation can be very simply described by means of two equations of state. It is the purpose of this paper to describe the experimental behavior of basal and prismatic glide in zinc crystals, and to interpret this behavior in terms of other physical properties (in particular, the thermal expansion coefficients and the elastic constants) using the theory of dislocations. Fig. 1 defines the two planes of the zinc structure that will be discussed. Glide occurs very readily on the basal planes at all temperatures, and there is a very large literature on this subject. Much of the literature has been reviewed by Schmid and Boas;&apos; it will not be reviewed here. Kolesnikovl was the first to show that if basal glide is circumvented by stressing a zinc crystal parallel to the basal planes (giving zero shear-stress on the basal planes) then, at temperatures above about 320°C, glide on the first-order prism planes occurs. His results have recently been confirmed by Cahn, Bear, and Bell." These previous workers have established the existence and crystallographic elements of prismatic glide; the present paper is concerned with the stress, strain rate, and temperature relations of prismatic glide as contrasted with basal glide. Experimental Methods The crystals were square ones, 6x6 mm, that had been grown in precision Pyrex tubes by a method that is described in detail elsewhere.&apos; Most of the crystals were 99.999+ pct Zn (New Jersey Zinc Co. CP grade). Some were alloyed with 0.1 -+-0.005 atomic pct Cd, and chemical analysis showed that almost all of the added cadmium persisted through the crystal-growing process. For measurements of nonbasal glide, crystals were oriented with their basal planes parallel to both the rod axis and one of the flat faces of the square cross section. However, the orientation of the close-packed directions [1210] with respect to the rod-axis was variable. For basal glide measurements, the angle between the basal plane and the specimen axis was 35". The orientations were measured by the Gren-inger back-reflection X-ray method. The problem of finding a suitable method of gripping the crystals was the most serious experimental obstacle that arose. Because of the large plastic anisotropy of zinc, the usual gripping methods were unsatisfactory. Some methods that were tried were: high melting-point solder, making heads on the ends by locally melting a crystal, and electroplating nickel on the ends to form enlarged portions. For all these methods, the regions of the grips were weaker than the crystals themselves. Finally, two methods were decided upon: bend tests and direct machining of tensile specimens. In the bend tests, specimens were loaded as simple beams so that gripping was not a problem. The beams were 1 in. long and the axis of bending was parallel to the hexagonal axis of the crystals. For the crystals that were machined into tensile specimens, brass bars with slots in them were used to support the crystals, and thereby minimize the distortions due to machining. The crystals were glued into the brass bars with plastic cement which was later dissolved away with acetone. See Fig. 2, left. No clamps were used near the crystals and the machining was done using a milling machine with a fly-cutter. The tool bit was very sharply pointed to minimize burnishing. The feed was less than 1 mil per cut. The depth of cut was 2 mil for roughing cuts, and % mil for the finishing cuts. This machining method produced surface layers of tiny recrys-tallized grains only 2 to 3 mil deep, and the bodies of the crystals were not measurably disturbed. After the crystals had been machined and removed from the brass holders, they were chemically polished until about 5 mil had been removed from all their surfaces. The polishing reagent consisted of equal parts of concentrated HNO,, 30 pct H3O and ethyl alcohol; it is described in detail elsewhere." A typical crystal is shown in Fig. 2, right. The I-shaped faces are normal to the hexagonal axis of the crystal; otherwise the projections at the ends would simply shear off when the crystal was loaded. The cross section in the 2?-in. gage length is 0.215x0.115 in. It was found that the polished

Jan 1, 1957

By H. D. Wilde

GREAT emphasis is being placed today on petroleum as a source of chemicals. Such prominence is well merited, for rapid strides have been made in developing processes for the conversion of petroleum into synthetic chemical products, which are now being made on a huge scale. These marvelous accomplishments have resulted in some highly optimistic predictions as to what can be expected in the future. Many of these forecasts are well justified, but some writers, especially those contributing to the Sunday supplements and the popular-cience type of publications, have let their imagination run wild and present a rather distorted picture of the possibilities in this field in the postwar period. Commercial manufacture of synthetic organic chemicals had its beginning in England with the establishment of a plant by Sir William Perkin in 1857 for the manufacture of "Aniline Purple" or "Mauve." The preceding year he had discovered in the laboratory how this dyestuff could be made from aniline, one of the many derivatives of coal tar, and he soon made commercial application of his discovery. Influenced largely by his success, organic chemists began research on production of a vast array of synthetic dyestuffs, medicinals, flavors, scents, and explosives. Rapid progress was made and by the turn of the century hundreds of these products were being manufactured. Most of these synthetic chemicals were derived from materials obtained as by-products in the conversion of coal into coke. These by-products are generally referred to as "aromatics" and are obtained by processing coal tar recovered in the coking process, so they are popularly known as "coal-tar chemicals." During the early years of this century, coal-tar chemistry was the wonder of the age, and rightfully so, since the products so made seemed limitless.

Jan 1, 1944

By E. J. Ripling

TUBES may be produced by a large number of forming processes, the most common of which will be discussed analytically in this paper. In no case will the stress analysis for any given tube producing process be derived formally for where such analyses are available, they may be referred to readily. Rather, emphasis will be placed on the interpretation of the theory of the different processes, few of which are developed to a state that will allow rigorous mathematical analyses, in an attempt to give a rational description of the effects of the different variables involved in each method. Tube producing methods can be divided into two groups: Those used to form shells, and those used to further work these shells into a shape more suitable for their final use. Among the first group are included roll piercing, extrusion and cupping for seamless shells, and bending with welding for welded tubes. The re-forming processes include sinking, drawing with a plug, and drawing with a rod. Only the plastic forming operations will be discussed here; other forming processes such as casting shells will not be considered. PRODUCTION OF SHELLS Shells for Seamless Tubing Piercing: The extremely important process of forming an axial hole in a billet by oblique rolling never has been analyzed satisfactorily, although a certain amount of experimental work relating to this process has been conducted. There are a number of factors that make piercing difficult to analyze; one of these is the fact that piercing is not a problem in plasticity, but one in fracturing, and the laws of fracturing are even less well understood than those of plasticity. If, however, it is assumed that fracturing occurs on a surface as a result of tensile stresses acting normal to this surface, piercing can be analyzed qualitatively by examining the stresses established in the oblique rolling process. To determine the origin of the tensile stresses that are thought to effect piercing, it will be necessary to know the angular relationships between the maximum stresses that are established in piercing. These angles quite frequently can be determined in a plastic deformation process by an examination of the deformed product. For example, consider the stresses established when a tensile test is conducted on a rectangular cross-sectional specimen of pearlitic steel. When stretched, this material first flows plastically, exhibiting the well-known yield jog on a stress-strain curve. The formation of the slip areas that give rise to the yield jog can be detected during the straining, since these flowed areas cause depressions on the specimen surfaces which can be seen if the surfaces are polished highly. The plastically strained areas also can be found after the specimen has been stretched to a strain not exceeding the yield jog, by sectioning the test piece and. etching these sections with Fry&apos;s etch. With this etchant, it is possible to dis-

Jan 1, 1951

By W. P. Sykes

THIS investigation was undertaken primarily to establish the relations existing between temperature and mechanical properties in molybdenum, nickel, and an aluminum-copper alloy. Molybdenum (m.p. 2500° C.) was chosen because it is partly similar to tungsten and partly similar to the common ductile metals. Also it is known to furnish, by proper treatment, a desirable material to use in studying relation of grain size and physical properties. The molybdenum used was of the quality that is drawn into wire 0.003 in. in diameter for use as filament supports in incandescent lamps; chemical analysis shows less than 0.1 per cent. of impurities. Nickel belongs to the same class as iron. Its melting point is 1450° C. and an allotropic change at about 370° C. results in a loss of magnetism above that temperature. This feature made nickel doubly valuable for the purposes of these tests. The nickel used was obtained from the Driver-Harris Co. as 0.090 in. (2.3-mm.) wire, annealed; analysis showed 99.8 per cent. nickel and 0.150 per cent. iron. Aluminum is one of the low melting-point metals. Some tensile tests at elevated temperatures have been reported by Bengough but the possibility of learning more with the low temperature and sensitive apparatus available recommended this metal. The samples marked Al are an aluminum-copper alloy; they contained 3 per cent. copper, 0.42 per cent. iron, and 0.21 per cent. silicon. The presence of the copper somewhat complicates the analysis of the results; but the action of copper in aluminum has been studied so that its influence might have been foretold, in part at least. The material and analyses were furnished by the Aluminum Castings Co. The nickel wire, which was deformed at 400° C., was drawn under a bath of molten lead and through a die, which also was immersed in the bath. A thermocouple was suspended in the molten metal to indicate

Jan 1, 1921

By Harry C. Gatos, Frank J. Bachner

It was shown through high-pressure experiments that tin loss by volatilizatim is necessary for the degrada-tion of the superconducting transition temperature of Nb,Sn associated with high-temperature annealing. Crystallochemical analysis of the degraded Nb3Sn showed that it constitutes a new phase with ordered niobium-site vacancies, created by the migration of niobium atoms to vaccnt tin sites. This new phase was found to form when 4 pct Nb-site vacancies were present. It has a transition temperature of 6&apos;K and a lattice parameter of 5.283A. A similar degradation effect was observed in Nb,Al. Its superconducting transition temperature dropped from 16.5" to 8" K following a high-temperature annealing. The superconducting temperature degradation in these 0-tungsten structure compounds is attributed to the disruption of the interchain d bonding by the periodic interruption of the niobium atom chains. By annealing the degraded Nb, Sn at 1000 C in nitrogen its normal superconducting behavior is restored most likely due to the incorporation of nitrogen atoms causing the elimination of the ordered vacancies. HANAK et al.&apos; have observed low superconducting transition-temperature values (T, - 9"K) in some NbsSn samples deposited from the vapor phase. They attributed such low T, values to disorder in the 0-tung-sten structure. Much lower T values (down to 5.6"K) were reported by Reed et al.zC for NbsSn samples annealed at high temperatures. These authors also attributed this degradation effect to disorder (random occupation of the A and B sites by niobium and tin) but pointed out that such disorder could be brought about (by high-temperature treatment) only in samples containing niobium in excess of the stoichiometric composition NbsSn. Both groups reported that the normal superconductivity behavior could be rever-sibly restored by appropriate heat treatment. Courtney et al., also found that degradation in NbsSn requires excess niobium brought about by the loss of tin during the treatment. However, these investigators proposed that the degradation is due to niobium-site vacancies resulting from the migration of the niobium atoms to the vacated tin atom sites. They did not consider the reversibility of the effect. The present study attempts to establish the nature of the above degradation phenomenon. EXPERIMENTAL PROCEDURES All compounds prepared for this investigation were made from the powders or filings of the elements which were intimately mixed, cold-pressed into a cylindrical pellet at approximately 50,000 lb per sq in., and then submitted to the desired heat treatment. The samples annealed under high pressure were placed in a MgO sample container which was mounted in a pyrophyllite tetrahedron designed for a tetra-hedral-anvil press. Details of the experimental arrangement are given elsewhere. This setup allowed heating at 1800°C or above under pressures in excess of 30kbars for 3 hr. The samples annealed in a vacuum were prepared in a high-temperature vacuum furnace which could reach temperatures up to 2400°C under a pressure of 2 x lo-&apos; Torr. For annealing in a reactive atmosphere, a quartz tube was placed in a clamshell furnace and the desired gas ambient passed through the tube. Lattice parameters were determined using a Debye-Scherer 114.6-mm camera. Cohen&apos;s method, programmed for the IBM 7094 computer, was used to calculate the lattice parameter from the measured d spacings. X-ray integrated intensity measurements were made on several samples. These samples were ground to -400 mesh and the powder mixed with a solution of collodion in amyl acetate. The mixture was poured into a depression milled in a bakelite disc. When the mixture dried, the surface of the disc was ground flat leaving a diffraction surface defined by the face of the disc. The disc was mounted in a Philips rotating specimen holder which allowed the rotation of the sample in the plane of the diffraction surface and the integrated intensity measured using a scintillation counter and a pulse-height analysis sys-tem. The superconducting transition temperatures were determined by means of self-inductance techniques.&apos; EXPERIMENTAL RESULTS AND DISCUSSION The Role of Tin Loss in the Degradation of Super-conductivity. The loss of tin during high-temperature annealing can be effectively suppressed by annealing under high hydrostatic pressures. Accordingly, a series of experiments were performed under pressures of approximately 30kbars. This pressure was the minimum under which high-temperature experiments could be safely performed in the particular pressure apparatus employed. Experiments were also designed to test high-pressure effects on the superconductivity behavior of NbJSn. The results of the high-pressure annealing experi-ments are summarized in Table I. All samples were prepared as described earlier. They were reacted and homogenized at 1000°C for 24 hr under argon at-

Jan 1, 1967

By A. U. Seybolt, J. L. Walter

The effects of the addition of 0.5 pct ThO2 (by volume) on the grain structure and texture of heavily rolled tungsten sheet were studied. Powder metallurgy ingots were rolled to sheet, 0.001 in. thick, and samples were annealed at temperatures from 1200" to 2500°C. The heating rate to the anneal temperature was varied from 3°C per min to 6500°C per min. The orientations of the largest grains were determined by X-ray diffraction. The disposition and loss of the ThO2 particles were determined by electron transmission microscopy and the activation energy for remozlal of the thorium was measured by mass spec-troscopy. Heating rates below about 800 C per min produced large, highly elongated grains. Higher heating rates produced much smaller, less elongated grains. The grain structure and texture of the slowly heated samples were identical to the structures and textures of heavily rolled tungsten foil conventionally doped with aluminum, silicon, and potassium but the recrystallization temperature was about 200°C lower. There was stringer-like dispersion of larger ThO2, particles superimposed on a uniform dispersion of fine particles. The particles increased in size and decreased in number with time at temperature. The loss of particles was accompanied by formation of grain boundary voids and surface pits. The activation energy for removal of the ThO2 was about 40 kcal per mole. THE addition of small amounts of aluminum, silicon, and potassium to tungsten has a profound effect on the grain structure of heavily rolled sheet1 or drawn wire."4 Thus, "doped" tungsten sheet, rolled to 0.001 in. and recrystallized, develops a structure consisting of large, highly elongated grains of a specific preferred orientation.&apos; It has been shown that the elongated grain structure was caused by a dispersion of particles, identified as mullite (Al6si2O13),1,4 in strings parallel to the rolling direction in sheet or to the wire axis. Identical results were obtained for iron which was doped with glass and rolled to 99 pct reduction of thickness and recrystallized.5 Again, the glass particles were disposed in strings parallel to the rolling direction. The strings retarded boundary migration in the lateral direction but grain growth was able to proceed relatively unhindered along the direction parallel to the strings.1,5 In both the doped tungsten and the glass-doped iron, the particles were highly plastic during the high-temperature deformation. Since mullite melts at about 1800°C and the glass employed melts at about 810ºC, the particles were probably molten during the recrystallization anneals (above 1800°C for the doped tungsten and 850°C for the glass-doped iron). There are indications in the literature that particles not plastic at hot-working temperatures (up to about 1550°C for tungsten) may also impart elongated grain structures by primary recrystallization of worked alloys. Examples are dispersions of tantalum carbide in chromium,6 and ThO2 in nickel where elongation ratios of recrystallization grains of up to 20:l were obtained.7 Strings of ThO2 particles in W-ThO2 wire have been seen by Rieck.8 In view of the available evidence, it was of interest to extend the previous studies of doped tungsten and glass-doped iron to include W-ThO2 sheet materials. Of specific interest was the grain structure, preferred orientation, recrystallization temperature, and disposition of the thoria particles. EXPERIMENTAL PROCEDURE A) Material Preparation. About 380 g of blue tungsten oxide (approximate composition WO3) was wet with a sufficient amount of aqueous solution of Th(N03)4 to provide 0.5 vol pct ThO2. The wet mixture was stirred to distribute the doping material uniformly throughout the powder. Stirring was continued while the mixture was heated until it was completely dry. The dried, doped mixture was then reduced to tungsten powder by heating at 850°C for 2 hr in a stream of dry hydrogen. The doped tungsten powder was hydropressed in a rubber sack at pressures of 50,000 psi to produce an ingot approximately 2 cm diam by about 5 cm long. Next, the pressed cylinder was heated in hydrogen for 2 hr at 1350°C to render it strong enough for machining. The cylinder was machined to a square cross section of 1.6 by 1.6 cm with rounded corners. Finally, the bar was heated for 2 hr at 2150°C in hydrogen to provide a sufficiently dense mate rial to withstand the hot-rolling operation. Prior to rolling, the ingot was reduced in thickness by about 20 pct by forging at 1550°C. This served to increase the density of the material and to widen it slightly for better rolling characteristics. The forged ingot was then rolled at 1550°C to a reduction of 45 pct of thickness, following which the rolling temperature was reduced to 1300°C and the slab rolled, with several reheats, to 0.050 in. Further reduction was accomplished at 800°C in tungsten sheet packs to a total reduction of about 99.85 pct. B) Annealing Treatment and Observation of Structure. Small samples of the rolled foil were annealed in one of two ways. Some of the samples were suspended in a covered tungsten can and annealed at temperatures from 1200" to 2200°C for various times in vacuum of l0-7 to 10-6 mm Hg. The can was heated by induction and temperatures were determined by optical pyrometry

Jan 1, 1970

By M. L. Samuels

DURING the period from 1910 to 1920, there was a lively interest in the subject of grain growth and many papers were published, followed by interesting discussions. Questions dealing with the fundamentals of grain growth-why and how it occurs-were treated in papers by Howe,1 Jeffries,2 Sauveur,3 Chappell,4 Beilby,5 Mathewson and Phillips,6 McAdam,7 Carpenter and Elam,8 Stead and Carpenter,9 Ruder,10 as well as others. Since that decade, much indeed has been done regarding the practical control of grain size, and it is now possible to order material having a size specified in the American Society for Testing Materials classification. Also, one hears the term "spliced boundaries" used in connection with certain tungsten lamp filaments" wherein it is important to prevent "sagging" between consecutive turns of the helix." This practical use of a certain knowledge as to the things that influence or even control grain growth should not be taken as an indication that the subject has been thoroughly explored and that nothing more can be learned from fundamental studies. It is with this thought in mind that a report of some observations and experiments on abnormal grain growth is believed justified. Abnormal grain growth is met with in heat-treating high-carbon steels in the austenitic range,13 in the hardening treatments of high-speed steels, 14.11 and in the low-temperature annealing of strained low-carbon steels as in sheet and wire material. Entirely aside from these instances of exaggerated grain growth, which some might consider as freakish, it is thought that abnormal growth is simply a case where the growth forces and the forces tending to prevent growth are almost, but not quite, evenly balanced. Information relative to grain-growth characteristics in general may be obtained from a study of abnormal growth conditions, which may be looked upon as vantage points. Reflection will show at once that if growth forces are great in comparison to inertia or resistance to growth, many crystals start to grow and, for that reason, none becomes very large, whereas if inertia is predominant no growth at all takes place. Under conditions in which

Jan 1, 1938

By C. W. Mac Gregor

THE observation of the flow layers, or Lüders&apos; lines, produced in mild steel when it is stressed into the plastic range often provides considerable useful information for the study of the fundamental mechanism of the plastic flow of metals. It is a commonly observed fact that as soon as the upper yield point in a mild-steel tensile-test bar is passed, an unstable condition develops in the equilibrium, the load on the testing machine drops and if the surface of the bar contains a thin mill scale, the latter begins to flake off rapidly along certain "lines." These "lines" are in reality traces of wedge-shaped flow layers and are formed by the inter-section of the surface of slip and the surface of the bar. The average plane of the flow layer itself has been found by various experimenters to be inclined at an angle of approximately 45° to the axis of the test bar. In a body of more complicated shape stressed in possibly a different man-ner, the tangent planes to the flow layers at each point seem in many cases to be inclined at an angle of about 45° to the principal stress direc-tions at the point. As examples of the latter may be mentioned the logarithmic spirals obtained when a rivet hole is punched in a thin plate, or when a tube is subjected to internal pressure only, etc. Hence if the flow layers are observed from an experiment, the shear-stress trajectories -the curves indicating the directions of the maximum shearing stresses in the body-may then be approximately determined. Since the latter curves form an orthogonal family inclined at 45° to the principal stress directions, the family of principal stress trajectories, or the curves indicating the directions of the principal stresses, may be thus obtained. Although the discontinuous type of stress-strain curve at the yield point is commonly observed with test bars of mild steel, more recent experiments have shown that this is by no means the only material exhibiting this interesting phenomenon. A similar effect has been observed in zinc and cadmium crystals, by Becker and Orowan;1 in duralumin and other aluminum alloys, by Dawidenkow, 2 Elm,3 Fell, and others; in copper and copper-alloy crystals, by Elam;5 in brass by Elam;5 in brass wires by deForest;6 in higher carbon steels, tungsten steel, and

Jan 1, 1939

By Stewart, J. B.

THE property at which this work was done consists of a large deposit of potash salts occurring in massive beds of rock salt, overlain by 600 ft. of salt-impregnated shales and marls. It is in the Province of Cataluiia, Spain, about 45 miles from the railway station of Mauresa and about a mile south of Suria. In addition to sinking the shaft, the program of construction work laid out by the European owners (not Spaniards) included a single-track narrow-gage railroad from Mauresa to the mine; one large office building and several large shop buildings, all of brick and concrete with steel truss roofs; two extensive benches for the future recovery plant; and a large village of stone dwellings for employees. The pay-roll showed approximately 1200 to 1500 men employed. After two years&apos; operation, ending early in the autumn of 1920, the shaft had been sunk 325 ft. and still had an equal distance to go to reach the potash; all tunnels for the railroad were done and the road-bed $0 per cent completed; only a little more than the foundations were completed for all the large buildings, and the excavations of the benches were about 75 per cent done-while only a fair start had been made upon the employees&apos; village. This was the state of affairs when the European owners decided to offer this property under a one-year option to an American syndicate, providing that they agreed to carry on the entire building program and to sink the shaft as fast as was consistent with the quality of work which they demanded, for they wished the shaft to endure at least 200 years.

Jan 1, 1926