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By John Nunes, Frank R. Larson

Temperature-dependent functions of various ten-sile flour stress and fracture parameters were investigated on iron and low composition alloys of Fe-C, Fe-Cr, Fe-Mn, and Fe-Ni. Data were obtained over a range of test temperatures from 200" to -196"C at an initial strain rate of 0.01 min". It was found that the strain-hardening exponent, n, for the Fe-Ni alloys increased significantly at very low testing temperatures with increased alloy addition. Also, the stress and strain at fracture followed a predictable transitional type of behavior. The flour stress-temperature dependence was evaluated employing the relation: M where it is shown that composition can strongly influence the constant M. An empirical formula describing this effect is as follows: M = MI (equivalent at. pct Ni)-'" Some preliminay, tests were run on several commercial steels to test the generality of this relationship. One of the phenomenological explanations of the ductile-to-brittle transition encountered in bcc metals is based upon the difference in the temperature dependence of the flow and fracture stresses.' It states simply that the fracture stress is relatively insensitive to temperature and that the yield or flow stress rises rapidly with decreasing temperature so that, when the flow stress reaches the fracture stress, brittle fracture occurs without appreciable plastic deformation. This behavior is illustrated schematically in Fig. 1 where the ductile-to-brittle transition is shown to occur at two possible temperatures. The lowest temperature, TB, represents essentially completely brittle behavior while the higher temperature, TN, represents "notch" brittle behavior. Support for this theory is obtained when it is observed that fcc metals, which do not commonly have a ductile-to-brittle transition, also do not commonly exhibit any strong temperature de- pendence of the yield stress. This relationship of yield or flow stress behavior with the ductile-to-brittle transition has been generally observed for most metals representative of these two crystallo-graphic structures. One exception to this generalization appears in the case of tantalum where no apparent ductile-to-brittle transition has been observed. However, this may simply be an indication that this type of behavior is not directly related to the flow stress and that some other mechanism such as twinning must also be operative. A comparison of the typical temperature dependence of the yield stress of some representative metals is shown in Fig. 2. In the study of the temperature dependence of the strength of metallic materials, considerable ef-

Jan 1, 1963

By Sherwin F. Kelly

One of the most succinct and illuminating perspectives of the field of geophysical exploration to appear in recent years is an article by E. A. Eckhardt, in the magazine Geophysics for October 1949. Although his review covers the year 1948, many of the data presented are apropos to a review of 1949, and form a pertinent background for a consideration of current progress. He presents charts of the world-wide distribution of gravimeter and seismograph activity in oil exploration, which show that surveys in the United States accounted for practically 68%; of all gravity work and 80%; of all seismic activity. Canada ranked second, with a proportion of roughly 6%, in each case; South America accounted for about the same percentage of seismic work, and double that amount for gravity surveys. Within the United States, Texas and Louisiana were the scenes of the greatest activity, both claiming about 60% of all surveys by each method.

Jan 1, 1950

[Executive J. V. W. REYNDERS, Chairman WILLIAM H. BASSETT E. DEGOLYER I-I. C. BELLINGER RICHARD PETERS, JR. Finance GEORGE OTIS SMITH, Chairman H. A. GUESS F. JULIUS FOHS Admissions GEORGE D. BARRON, Chairman DAVID LEVINGER P. A. MOSMAN H. K. MASTERS J. A, SINGMASTER Alternates F. G. BREYER C. W. HAMILTON F. E. PIERCE]

Jan 1, 1928

By B. E. Warren

Jan 1, 1965

By Joklik, G. F.

Most publicity about the copper industry nowadays is focused on the adequacy of ore reserves and on excessive mining capacity. These concerns, stemming from public awareness of actual and potential shortages and oversupplies, relate to production rather than consumption. Perhaps the reason for this one-sided view is that copper is thought of as a commodity which is conspicuously traded in world markets, rather than as one of many industrial materials that serve today's rapidly changing technology. Copper differs from other widely traded commodities in that its real cost of production has progressively increased since World War 11. The reasons for the increase are identifiable by analyzing operations in one of the world's large producing centres, the copper province of Arizona. Another respect in which copper differs from some other commodities is that increases in demand occur less automatically in the case of copper than they tend to in commodities whose consumption is more directly related to population growth. The copper industry's current inability to generate and attract needed investment capital is attributable to these differences between copper and other commodities; it suggests that the concept of copper purely as a commodity is outdated. The key to the problem is better integration between the activities of copper producers and users. Depending on circumstances, integration takes various forms- for example, investment tied to long-term sales con- tracts between producers in developing countries and consumers overseas; common ownership of producing and manufacturing facilities in industrialized nations like the U.S.; and consumer-oriented research and marketing by the copper producers.

Jan 1, 1978

By Ralph H. Sweetser

N Greenup and Carter counties, in the northeastern part of Kentucky, are the remains of many old charcoal furnaces built and operated during the period from 1818 to 1892. They were all included in what was called the Hanging Rock district. In the summer of 1930 I visited ten of these old blast furnaces, as follows:

Jan 1, 1931

By Francis T. Freeland

In the West many precious-metal mines are worked in patches by lessees, under conditions which closely resemble those of what is called " tribute-work" in Cornwall.* The company has its own foreman or inspector, and usually employs the engineman, blacksmith, pumpman, and perhaps other general workmen. As an inducement to work on a new piece of ground, where no ore is in sight, the company may advance a " footage"

Jan 1, 1896

By F. T. Havard

(Canal Zone meeting, November, 1910.) I. INTRODUCTION. THE present truce in litigation between Western smelting and ranching interests gives opportunity for a summary of the results achieved by metallurgists in condensing fume and de-acidifying furnace-gases. In the absence of complete records of past experiments, there has been a good deal of unnecessary duplication of attempts and' failures. Yet, especially under the recent policy of our large corporations, looking to the economic recovery of the values of by- and waste products, original and, in some cases, effective measures have been developed by American metallurgists. In the case of Bliss vs. the Anaconda Copper Mining Co., the Montana Supreme Court, recognizing the progressive efforts made to render the flue-gases innocuous, and the value to the community of the smelting company's operations, refused to hamper its work, and returned a verdict in favor of the defendant. In the trial, the experimental firms of the company in the so-called "affected region" were proved to be thriving perfectly, showing that immunity was guaranteed to vegetation and stock by the wide distribution of the sulphurous acid gas in the dry air of Montana. Indeed, L. S. Austin has proved that by the time the fume is 4,000 ft.. distant from the stack, the percentage of sulphurous acid has been diminished from 2.28 to 0.00045; and Angus Smith has shown that rain must contain 40 parts per million of free acid before vegetation is affected. The arsenic in the stack-gases is but a very small part of the original content of the ore, of which 80 per cent. and over is rejected in the concentrator and furnace waste-products or recovered in the flues. Nevertheless, neither the peace in Montana nor the armistice

Aug 1, 1910

By L. W. Pommier, F. B. Brien, A. K. Bhasin

In the field of mineral processing, although many operations are applied to suspensions of ore particles in fluids, there is a lack of fundamental knowledge relative to the flow resistance encountered by immersed bodies moving through solid-liquid suspensions. Previously proposed equations, based on the Ostwald-de Waele (power-law) model for non-Newtonian fluids, are exam ined in the turbulent flow region relative to a number of pertinent variables and their effects on the movement of immersed bodies. As more knowledge is acquired in regard to the effects of suspension variables on the rheological properties, useful relationships may be proposed to allow predictions of conditions to achieve optimum results for engineering purposes. In the field of minerals processing, many operations are applied to suspensions of ore particles in fluids. The differential movement of solids of various sizes and densities in suspensions is of utmost importance to gravity concentration, wet classification, flotation, hydrometallurgy, and pipeline transport of solids. The subject is also of importance to other branches of engineering; for example, those involved with soil mechanics, ceramic slips, and oil-well drilling fluids. There is a lack of fundamental knowledge relative to the flow resistance encountered by immersed bodies moving through solid-liquid suspensions. The problems encountered in the direct application of the well-known Stokes and Newton's Laws to non-Newtonian systems have been examined in a previous paper.' Equations were proposed based on the Ostwald-de Waele (power-law) model for non-Newtonian fluids. This present paper examines these equations in the turbulent flow region relative to a number of pertinent variables and their effects on the movement of immersed bodies. It is thought that, as more knowledge is acquired as to the effects of suspension variables on the rheological properties, useful relationships may be proposed to allow prediction of conditions to achieve optimum results for engineering purposes. The purpose of this paper is to make an initial assessment of the nature and magnitude of pertinent suspension variables. In order to avoid too voluminous a document, the examination of kinetics and mechanisms will be omitted at this time. THEORY A Newtonian fluid is defined as a fluid in which the stress is proportional to the rate of strain, 2 i.e.: H = viscosity; see Table I. for list of symbols The following equations are conventionally used to assess the motion of spherical particles moving under laminar and turbulent flow conditions through Newtonian fluids: When these relationships are applied in practice to suspensions, the liquid density is substituted by a composite suspension density, and viscosity is usually taken as that of the suspending liquid or an approximated "apparent viscosity." However, suspensions are non-Newtonian in character3 and thus, more than one viscosity parameter is required to describe their behavior. A number of models have been proposed for non-Newtonian fluids;2,4 among these the simplest is the Ostwaldde Waele or power-law model for incompressible fluids which for one dimensional flow may be reduced to:

Jan 1, 1970

By J. R. Lucas, R. L. Frantz

Mine sealing programs for the alleviation of acid mine drainage were begun by the Federal Government in the '30's. As part of an acid mine research project to The Ohio State University, a field test was undertaken to determine the effectiveness of mine seals for reducing mine acid. Details of the tests made at the McDaniels mine show the feasibility of air-sealing and flooding an acid-producing drift coal mine. Work by the University continues. The Federal Government undertook in the early thirties an extensive mine sealing program for the alleviation of acid mine drainage. In the states of West Virginia, Ohio, and Pennsylvania many general summaries have been made on this program but no critical evaluation with supporting data has been found on the effectiveness of mine seals for reducing mine acid. Because of this it was decided to undertake a field testing program as part of an acid mine research project of the Engineering Experiment Station, The Ohio State University. The objective of this phase of the project was to develop and install a field research laboratory for acid mine drainage studies. Specifications for such a mine laboratory were developed and resulted from the following considerations: 1) Size and preservation—the test mine shou1d be of limited size to permit frequent and detailed examinations; it should be in a reasonably sound condition to permit safe entry. 2) Isolation—the mine should be physically separated from all other mines. 3) Openings—a minimum number would be desirable to reduce the sealing problem. 4) Structure—the mine especially near the openings should be structurally sound. 5) Acid production—the mine should be producing significant quantities of acid. After considerable searching, the McDaniels mine was selected in the Hocking coal field in Vinton County just above Lake Hope State Park in southeastern Ohio. The small drift mine in the middle Kittaning coal consisted of two small rooms with one mine opening about 6 ft above a seasonal stream bed. Before it was finally decided to seal the mine, a short study was made of the acid drainage over several months. Fig. 1 shows a plot of acidity (milligrams per liter), flow (gallons per minute), and acid production (pounds per day) vs time over the sampling period. Because the coal was overlain with a porous sandstone, the mine drainage was consistent the year around even though the mine was

Jan 1, 1961

By V. N. Cox, C. H. Grant

Both the underwater method and the rock cratering method contribute useful information in evaluating and comparing new explosive compositions. Results indicate that metallized explosive systems which contain no high explosives can be formulated to offer more energy and to do potentially more work than other slurry explosive systems. Commercial field trials are presently being conducted with a metallized explosive that does not contain any high explosive. Although there have been only a few commercial blasts to date, the results are encouraging. The Dow Chemical Co. has been engaged in explosives research since 1953. The incentive for this research was based on the desire to find additional markets and uses for magnesium metal of which DOW is a heavy producer. The thermodynamic calculations for explosives incorporating light metals indicate energies approximately twice that of nonmetallized explosives currently being used. Early in 1960, additional patent rights were acquired from independent inventors and a development station at Virginia, Minn., was set up to conduct a commercial testing and market evaluation program with this new product. The actual manufacturing of the explosive was to take place in the boreholes. Due to the complexities involved in controlling the manufacture of the explosive in the borehole, performance was sometimes in doubt. Furthermore, experience indicated that the metallized explosive systems could not be evaluated by the standard laboratory methods then being used, and it was necessary for us to look for more suitable research methods. Tests were conducted on several known methods for explosive evaluation. The most promising were the Navy underwater method for energy evaluation and a modified Livingston crater method intended to compare explosive performance in rock. After shooting over 2000 charges of 8 to 60 lb under water and in taconites and granites with many types of explosives, a metallized explosive was developed which is now being manufactured at a pilot plant in Virginia, Minn. and is being evaluated commercially. UNDERWATER METHOD An underwater method of evaluating explosives has a number of advantages. A permanent site can be established and operated indefinitely. A large number of charges may be fired in a short length of time. The medium in which the explosive is shot is exactly the same for successive shots. Data are recorded electronically minimizing human judgment. A disadvantage of the underwater method is the lack of confinement provided by the water medium. Many explosive compositions require a greater degree of confinement to develop good energy release. Although the relative significance of the two components of energy release that are usually measured, the shock energy and the bubble energy, and their relationship to breaking rock are not clearly understood, the underwater method is a valuable research tool for screening explosive compositions and gaining an insight into the manner in which explosives release their energy. Fig. 1 shows schematically the underwater apparatus. The piezoelectric gages are calibrated tourmaline crystals which convert the shock wave to an electrical impulse which is transmitted to an oscilloscope and recorded on Polaroid film. The shock traces are picked up by scopes 1 and 2. Scope 1 is timed to pick up the full trace whereas scope 2 is timed to cover the first increment of the shock trace expanded, and therefore allows full inspection of the propagation and peak pressures. Scope 3 records the bubble trace. When the explosion occurs, a bubble of gaseous detonation products is formed. The outward momentum of the water keeps expanding the bubble even after

Jan 1, 1963

By F. W. Bowdish

A theoretical and experimental laboratory study has shown that the rate of breaking of oversized particles in a ball mill is proportional to 1) the concentration of such particles, and 2) the area of the balls, provided that the balls are larger than a certain size relative to the particles. If all undersized material were removed as formed, the rate of breaking would be almost independent of the quantity in the mill. Rate equations are given which are similar to those for zero, first, and second order reactions. Deviations of small balls from the equation for a second order phenomena are quantified by a factor called "nipping efficiency." Some data are correlated by a dimension-less equation, which is used to estimate nipping efficiencies from data not in the correlation. The investigation described here was undertaken after a literature survey revealed that little was known concerning the mechanism of breaking of particles within a ball mill and the effect of this mechanism upon grinding rates. One paper, by Roberts1 , offered a theory concerning the mechanism of breaking, and a rate equation for the breaking of particles larger than some size to particles smaller than that size. That paper provided the starting point for a theoretical and experimental investigation of grinding under carefully controlled conditions. THEORETICAL CONSIDERATIONS In his paper on the probability theory of ball mill grinding, Roberts theorized that "... a given expenditure of power leads either to a certain number of point to point blows per bp-hr or to a certain distance of line contact per hp-hr ..." He assumed that the balls touch each other during each blow or during moving contact. Then he said that a volume of pulp, dependent upon the size being considered, would be covered per minute within which all oversized particles would be crushed to particles smaller than that size. Naturally, the higher the concentration of oversized particles in the pulp, the higher the rate of which they would be broken. From this reasoning Roberts obtained the differential equation -dC/dt = k hp/ton C (1) where k is a constant for any size of particle, density of particle, and moisture content of pulp. C is the percentage of oversize in the material to be ground, t is the time, and hp/ton is the power input per ton of material in the mill. He then integrated the equation to log Co/Ct = k/2.3 hp/ton t , where Co and Ct are the percentage of oversize at time zero and t respectively. By always using the same quantity of material in a mill and assuming that it required constant power to run the mill, he was able to combine the horsepower per ton factor with the other constants to give an equation for a first order rate.

Jan 1, 1961

By A. Alonso, J. Daubenspeck

In the nickel extraction process at Nicaro, Cuba, dried and ground nickel bearing laterites are reduced at 1300-1400F in multiple-hearth furnaces. Nickel is leached from the reduced ore by aeration in an aqueous solution of ammonium carbonate. Nickel carbonate is precipitated from the liquor and calcined to yield nickel oxide. The following are the more important modifications of the Nicaro process since plant rehabilitation and expansion. Ten percent increase in tonnage was achieved without decreasing the fineness of the ore by minor mechanical modifications of the grinding plant. Another five percent increase in tonnage was attained by intentionally overloading the ore prepration and leaching circuits in an effort to control cobalt extraction. Modifications at the sintering plant allowed it to handle the entire output of the expanded plant. A fifty percent increase in leach liquor cooling facilities alone provided an increase in nickel production of five percent. Stronger fresh leach liquor for increased nickel washing efficiency was obtained through improved distribution of water to the ammonia absorption towers. Advantage was taken of the reduced calcine's capability to precipitate cobalt, and modifications in the leach liquor circulation provided controlled cobalt solubility with minimum harm to nickel extraction. Several process changes at the drying plant brought about a ten percent reduction in the fuel oil consumption at this pint. Controlled air addition to the reduction furnaces' upper hearths burned formerly wasted combustibles thereby reducing oil consumption by twenty percent. The nickel extraction process successfully emplayed on the extensive but lowgrade lateritic ores of Eastern Cuba at the U. S. Government owned Nicaro plant, has been previously described in various publications. The large mine and plant operated by the Nickel Processing Corporation, located on the northeastern shore of Oriente Province, have been recently expanded to a yearly capacity of about 50 million pounds of nickel. Essentially, the operation involves open pit mining of a limonite-serpentine ore mixture containing 1.3 to 1.4 percent nickel and 34 to 38 percent iron. The comparatively lumpy, wet (25 to 30 percent moisture) ore is first dried and ground prior to chemical treatment, to which the entire 7,000 tons per day feed must be subjected. In the initial chemical action the dried and ground ore is reduced with carbon manoxide and hydrogen at 1300-1400° in multiple-hearth furnaces. The resulting metallic nickel is selectively leached from the reduced calcine by aeration in an

Jan 1, 1961

By AIME AIME

MANY interesting papers, opportunity of seeing o1d friends, and an exposition showing all that is latest in equipment, all were factors in bringing a large crowd to Detroit during "Metal Week," October 2-6. The Institute's Iron and Steel and Institute of Metals Divisions held technical sessions at the Statler Hotel on October 4 and 5, and that hotel was also headquarters for the American Society for Steel Treating and the American Society of Mechanical Engineers, both of which also had technical sessions. The American Welding Society and the Wire Association met at the Book-Cadillac Hotel, and the exposition was staged at Convention Hall, out Woodward Avenue. All in all it was a big week for men interested in metal working. One of them stated to your reporter on the train en route to Detroit that this was the one convention that he never missed, and doubtless others felt the same way about it.

Jan 1, 1933

By F. H. Buchella, J. F. Buchanan

The San Manuel copper deposit is located about 45 miles northeast of Tucson. The concentrator, smelter, administration building, and other plant facilities are located about seven miles southeast of the ,nine area at the new town of Sari Manuel as shown on Figure 1 (Sketch).

Jan 1, 1961

By H. Kazemi, G. W. Thomas, M. S. Seth

The double-porosity model of Warren and Root7 for examining pressure drawdown and buildup phenomena in naturally fractured reservoirs has been extended to intetpret interference test results. Both analytical and numerical solutions are presented. The practicality of some of the assumptions in the Warren-Root model was also investigated. The standard procedure for interpreting interference tests in naturally fractured reservoirs beretofore employed an equivalent homogeneous reservoir model. A comparison of our results with the equivalent homogeneous model indicates the latter is inadequate for early time responses. For late time responses, however, the simpler equivalent homogeneous model yields favorable results. Finally, the effects of well spacing and the magnitude of the interporosity flow parameter are briefly cited. INTRODUCTION Interference tests can be used to provide reservoir information not obtainable from conventional pressure drawdown and buildup tests. The technique involves measuring the response in one or more wells arising from a pressure perturbation introduced into another well. It has been. successfully applied to single-layer, homogeneous, unfractured, isotropic and anisotropic formations to arrive at values of well storage capacity and a measure of directional permeability.l The techniques of interference testing usually can be extended to heterogeneous systems, provided the permeability contrast between any existing rock layers is not excessive.9 In such cases, the practical interference effects in an observation well of an interconnecting heterogeneous reservoir can be predicted using an equivalent homogeneous model. The calculated properties are then average values. Russell and Prats2 have demonstrated the utility of this approach for a single-phase, two-layer system. For naturally fractured reservoirs, some different approaches usually are necessary. The major departure from homogeneous or nearly homogeneous reservoir treatment is to characterize the fractured system as an entity having "double-porosity"; namely, we suppose the existence of both primary and secondary porosity, where the former is contained within a systematic array of identical rectangular matrix blocks and the latter is contained within an orthogonal system of continuous, uniform fractures (see Fig. 1). It is sufficient to assume that the permeability of the rock matrix is so small that movement of reservoir fluids to the producing wells is entirely through the fracture network. This assumption has been validated by Barenblatt3 and .employed by others?-7 Warren and Root7 used the double-porosity model to develop an interpretation of pressure drawdown and pressure buildup tests in naturally fractured

Jan 1, 1970

By J. E. Warren, J. H. Hartsock

An asymptotic solution to the equation that describes the flow of a slightly compressible fluid in an infinite porous medium has been used to estimate the interaction between two adjacent wells producing from a common reservoir. A direct method for approximating the interference time defined by Stevens and Thodosl has been suggested. An alternative definition for the time of interference, based on the minimum pressure change in the interference region, has been proposed; also, a direct method of determination has been prescribed. Examples have been employed to illustrate the use of both methods.

By Frank E. Woolley, Robert D. Pehlke

Jan 1, 1965

By C. F. Lucks, W. D. Wood, H. W. Deem

Electrical ad thermal-conductivity measurements have been made on titanium and 6 titanium alloys. The following expression was derived for calculating thermal conductivity from electrical conductivity: K = 0.626 s T x 10-8 + 0.00497 where K = thermal conductivity, cal sec-1 cm-2 cm0C-1 s = electrical conductivity, ohm-]cm-1 T = temperature, deg Kelvin This expression gives calculated thermal conductivities that are not in error by more than 10 pct from the experimental values for A-55 titanium and the 6 alloys measured; namely, A-110AT, C-110M, C-130AM, Ti-6A1-4V, Ti-140A, and Ti-155A, which are representative of the presently available commercial a and a-ß titanium alloys. THERMAL conduction in a gas, liquid, or amorphous solid is accomplished by energy diffusion from molecule to molecule, a relatively slow process. For this reason, such materials have a low thermal conductivity. When a material is crystalline, there is in addition a heat transfer by a vibratory motion of the crystal lattice. It is the contribution of this lattice conduction that makes a crystal a much better conductor than a gas, liquid, or amorphous solid. Lattice conduction, however, does not account for the relatively enormous thermal conductivity of a metal. This is explained by the freedom of movement of valence electrons. These valence electrons drift in a metal in a direction toward a drop in electrical potential and, to a lesser degree, in the direction of a temperature drop in the metal. Since both the electrical and thermal conductivities of a metal depend upon the presence of free electrons, there should be some relatively simple relation between the two. Wiedemann and Franz in 1653 first discovered an approximate empirical relation between the electrical and thermal conductivities of metals at the same temperature. This ratio varies appreciably with temperature, and Lorenz later showed that by adding a temperature factor to the Wiedemann-Franz ratio the value of K/(s T) is constant, where K is the thermal conductivity, a the electrical conductivity, and T the absolute temperature. This Lorenz constant shows a greater variation for alloys than it does for pure metals, the ratio increasing slightly as the proportion of alloying elements increases. It has been found that a closer correlation between electrical conductivity and thermal conductivity can be obtained by means of an equation of the form K - A s T + B [1] where A and B are constants. In this equation the term AsT is the contribution of electronic conduction and B is the contribution of lattice conduction to the total thermal conductivity. EXPERIMENTAL MEASUREMENTS Electrical-resistivity and thermal-conductivity measurements on titanium and 6 titanium alloys serve as the basis for determining an equation of the K = AsT + B type for titanium alloys. Specimens—Table I shows nominal compositions of the 7 metals on which electrical and thermal conductivities were measured. The electrical and thermal-conductivity specimens for each alloy were taken from stock of the same heat and usually from adjacent sections of the same bar. All of the metals measured were in a mill-annealed condition. Methods—Electrical-resistivity measurements

Jan 1, 1959

By R. G. Vardiman, M. R. Achter

Observations of dislocation structure in niobium are presented using two techniques. Triangular pits developed by electroetching are confined to orientations in the stereographic triangle between the (111) pole and planes of the (1ll) zone and require the presence of carbon. Some unusual electroetching phenomena at other orientations are noted. A chemical etch of dislocations decorated by the addition of carbon to 50 ppm reveals the complete dislocation line structure in a surface layer up to 30 p deep, with a resolution of less than 1 p. This effect is independent of surface orientation. The structure of subboundary nets may be resolved for misorientations up to about 1'. Dislocation structures found in strain anneal grown crystals, such as helices, prismatic loops, and high-density areas, are observed. The measurement of dislocation density is discussed and values obtained in different ways are compared. IN the course of some work on the response of refractory metals to thermal-mechanical treatments, it was desired to examine the defect structure of relatively low dislocation density crystals of niobium in bulk form. Surface and bulk methods for the observation of dislocations have been reviewed by ~melinckx,' and include etch pitting, decoration, and various X-ray techniques. The dislocation line structure has been developed by decoration in a few metals, although observations were limited to certain orientations, or by the coarseness and nonselectivity of the precipitate. The most commonly used technique is etch pitting. In niobium, etch pits have been developed chemically'0," in material of high impurity content and electrolyti-cally'' in relatively pure material. In this paper, etch pits developed electrolytically, and the dislocation line structure of a surface layer developed by decoration and chemical etching, are examined, and observations are presented from both techniques. EXPERIMENTAL METHODS Our starting material was electron-beam-melted niobium, swaged to 4 or -in.-diam rod. Chemical analysis is given in Table I. Single crystals were grown by a strain anneal technique using 1 to 2.5 pct of strain and growth temperatures of 1700" to 2300"~.'~ Some crystals grown by zone melting were also examined. The desired surface orientation was exposed either by spark machining or by sectioning with a cut-off wheel and prepared for etching by electro-polishing.

Jan 1, 1969