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By M. Cohen

THERE seems to be a natural urge for the human mind to wonder about the beginning of things. When an explosion occurs, we immediately inquire "what set it off?" If a person contracts a disease, we are likely to ask "how did it happen?" On a much loftier plane, when we reflect about the universe, there is the inevitable question "what, or rather Who, started it all?" In principle, these varied queries have at least one attribute in common: they are attempts, whether earnest or casual, to search out the origin of events in nature. Accordingly, they involve not only scientific, but philosophical and even re1igious matters of deep concern. It is evident that, in a broad sense, the phenomenon of nucleation is enmeshed in this enticing concept of "the beginning", but we must extract the scientific component of the problem for our present purposes. Nucleation, as in the case of phase transformations, is best regarded from the standpoint of kinetics. There are then two main steps, which may come in either order: (a) Experimentally, one attempts to measure the frequency with which transformation centers spring into existence; and (b) theoretically, one seeks a model that will account for this observed birth-rate. Temperature, composition, strain, and prior history are some of the important variables that must be considered both experimentally and theoretically when dealing with nucleation in the solid state. Such interaction of theory and observation is an integral part of science in general, but it is particularly significant in the nucleation problem because the very beginning of a phenomenon invariably occurs on too localized a scale in both space and time to be detected with available techniques. Thus, there is little hope of making direct measurements on the nucleus during its birth or to ascertain the exact nature of the process; one can only infer the details of nucleation from the model whose predicted behavior seems to harmonize best with the measured rate of nucleation and its dependence on known parameters. In the field of solid-state nucleation, both theory and experiment call for much ingenuity, but somehow the conceptual schemes have spawned faster than they can be tested by observation. This is not to say that there are many basically new ideas in modern nucleation theory; rather, as we shall see, it is because the required fine-scale measurements are of immense technical difficulty. Quite likely, some of the nucleation models existent today have survived only because of the latitude permitted by meager data. There is great need to bring theory and experiment into better balance in this important area of physical metallurgy. Although one can

Jan 1, 1959

By Charles S. Barrett

This paper is a progress report covering metallographic applications of the electron microscope that have been made during the past year at Carnegie Institute of Technology. An account is presented of the techniques that have been most satisfactory, the difficulties encountered, the resolution obtained, and the peculiarities that have been noted in the microstruc-tures. About 1200 exposures have been made during the year on the instrument, which is an RCA type B2 transmission microscope,' and a number of these have been selected to illustrate the results obtained. prints are also included showing the common types of falsities—to borrow a term from the biological field, the "artifacts." ln brief, the paper is a record of our attempt to determine the value of the electron microscope in the study of the structure of metals and alloys. In addition to comments on techniques and the quality of photomicrographs obtainable with them, the paper discusses the nature of the etch attack on a few metals, and the possible relation between the fine structure revealed by etching and the mosaic block structure of the grains, since numerous papers and reviews are available on the subject of imperfection in crystals, the comments here may be very brief; in fact, are restricted almost entirely to points having to do with recent theories relating the strength of metals to imperfections and to spacings of slip lines. Specimen Preparation and Photographs Mechanical polishing by hand was used throughout this work. Precautions that must be taken in microscopy at high magnification, which have been well explained by Vilella in his book on Metallographic Technique for Steel, are likewise important with the electron microscope. This applies particularly to the need for these polishing and etching (each successive polish becoming less severe and each etch lighter), since the fina1 etch should in general be no heavier than is used for oil-immersion optical microscopy and in many instances should be much lighter (compare Figs. 6a and 7a, 6d and 7b). An extremely light etch, of course, is incapable of cutting through a flowed layer of appreciable thickness. Unquestionably it would be very advantageous in each instance to compare the structures obtained by electrolytic polishing with those obtained by mechanical polishing, but difficulties with the electrolytic method have prevented this in the following collection of prints. The choice of etchant is important, of course; for example, picral proved superior to nital for tempered martensite. With the exception of Figs. Ib and 16, the replicas used were of silica, deposited upon polystyrene and floated from the polystyrene in ethyl bromide according to the method of Heidenreich and Peck.2 The samples were mounted in Bakelite, polished and etched, then the polished Bakelite

Jan 1, 1944

By Charles S. Barrett

This paper is a progress report covering metallographic applications of the electron microscope that have been made during the past year at Carnegie Institute of Technology. An account is presented of the techniques that have been most satisfactory, the difficulties encountered, the resolution obtained, and the peculiarities that have been noted in the microstruc-tures. About 1200 exposures have been made during the year on the instrument, which is an RCA type B2 transmission microscope,' and a number of these have been selected to illustrate the results obtained. prints are also included showing the common types of falsities—to borrow a term from the biological field, the "artifacts." ln brief, the paper is a record of our attempt to determine the value of the electron microscope in the study of the structure of metals and alloys. In addition to comments on techniques and the quality of photomicrographs obtainable with them, the paper discusses the nature of the etch attack on a few metals, and the possible relation between the fine structure revealed by etching and the mosaic block structure of the grains, since numerous papers and reviews are available on the subject of imperfection in crystals, the comments here may be very brief; in fact, are restricted almost entirely to points having to do with recent theories relating the strength of metals to imperfections and to spacings of slip lines. Specimen Preparation and Photographs Mechanical polishing by hand was used throughout this work. Precautions that must be taken in microscopy at high magnification, which have been well explained by Vilella in his book on Metallographic Technique for Steel, are likewise important with the electron microscope. This applies particularly to the need for these polishing and etching (each successive polish becoming less severe and each etch lighter), since the fina1 etch should in general be no heavier than is used for oil-immersion optical microscopy and in many instances should be much lighter (compare Figs. 6a and 7a, 6d and 7b). An extremely light etch, of course, is incapable of cutting through a flowed layer of appreciable thickness. Unquestionably it would be very advantageous in each instance to compare the structures obtained by electrolytic polishing with those obtained by mechanical polishing, but difficulties with the electrolytic method have prevented this in the following collection of prints. The choice of etchant is important, of course; for example, picral proved superior to nital for tempered martensite. With the exception of Figs. Ib and 16, the replicas used were of silica, deposited upon polystyrene and floated from the polystyrene in ethyl bromide according to the method of Heidenreich and Peck.2 The samples were mounted in Bakelite, polished and etched, then the polished Bakelite

Jan 1, 1944

By R. P. Alger, C. A. Doh, M. P. Tixier

The principle, the equipment and field operation of sonic logging are described. The tfio-receiver system produces logs independent of hole size and mud. Field experience is given and forms the basis for the interpretation of the log. The derivaiion of porosity values from measured velocities is discussed, according to the type of formations (hard formations, compacted sands, and unconsolidated formations). The time-average equation proposed by M. R. J. Wyllie, A. R. Gregory and L. W. Gardner is uscd as a basis for the computation of porosity in limestones, cemented sandstones and compacted sands. Variations in the lithologic character of limestones do not seem to change the porosity calibration markedly. The compaction of sands is related to the compaction of shale adjacent to them; and, thus, the shale velocity is used for the establishtnent of empirical relations for the computation of porosity in un-consolidated formations. Various forrnu.las are tentatively presented to account for shale and fluid content. Field experience demonstrates that considerable attenuation of sonic energy takes place in unconsolidated formations, particularly when gas bearing, and in fractrured formations. Unusually large attenuation produces skipped cycles, a feature easily recognized. The application of sonic logging to structura1 studies is featured, showing its possible integration with the dipmeter. Correlation and its application to the irrterpretation of seisrmic surveys are reviewed. The paper is illustrated with field examples. Sonic logging is the recording of the time required for a sound wave to traverse a definite length of formation. Sonic travel-times are inversely proportional to the speed of sound in the various formations. The speed of sound in subsurface formations depends upon the elastic properties of the rock matrix, the porosity of the formations and their fluid content and pressure. Below the "weathered" or low-velocity layer extending from 50 to 100 ft or so below the surface, sound velocities may range from about 6,000 ft/sec in shallow shales to as much as 34,000 ft/sec in dolomites. In hard formations (well cemented and/or compacted), the sonic log reflects the amount of fluid in the formations; hence, it correlates well with their porosity. In unconsolidated formations, which are usually of fairly high porosity, the sonic log gives an approach to porosity determination, when its readings are corrected for lack of compaction, shaliness, and fluid content. In such formations the sonic log may also indicate the presence of gas and may distinguish between oil- and water-bearing beds. Field experience with the sonic log in soft formations is more limited than that in hard formations. As a result, interpretation in soft formations is not as well developed at the present time. In all types of formations the sonic log is of considerable value for correlation and for the more detailed and accurate interpretation of seismic data. EQUIPMENT AND PRINCIPLE FIELD OPERATION The basic features of the sonic log" are a two-receiver system and two available short spacings. The log is recorded on film using a standard field unit. An SP curve is run along with the sonic curve to give a more interpretable log and to establish absclute depth control for comparison with other logs run in the same well. If desired, a gamma-ray curve may be recorded simultaneously with the sonic curve. Fig. 1 shows the sonic-gamma ray combination sonde. The sonic portion consists of a sound transmitter and three receivers mounted 3, 4 and 6 ft from the transmitter. When the first and second receivers are used, a sonic log of I -ft spacing (distance between receivers) is obtainea. Use of the first and third receivers provides a 3-ft spacing. The transmitter emits pulses at the rate of l0/sec. After the transmission of a pulse the first arrival of sound energy at each receiver triggers its response system. The differ-

By Evans B. Mayo

This study examines the structural framework of the Southwest for evidence of the four principal trends of lineament tectonics. It attempts to classify their intersections and compares the positions of those trends that appear most favorable with the positions of the presently known mining districts. This is a controversial topic. The author, in presenting his analysis, is aware that the study of lineament tectonics and relation of ore districts to regional structure is complicated by insufficient data and, unavoidably, by personal bias. The development of lineament tectonics has been summarized by Umbgrove.' Early attempts to fit ore districts into the Cordilleran framework were made by Billingsley and Locke, who do not refer to lineament tectonics, although their appoach is similar; they observe that heat and fluids, including the ore-depositing fluids, are most likely to rise at or near intersections of major structures where the crust is fractured, or weakened, to great depth. As a result of studies distributed over the earth-including ocean basins as well as continents— some tectonists recognize four dominant structural trends: 1) northwest; 2) northeast; 3) nearly east-west, or equatorial; and 4) nearly north-south, or meridional. Baker' proposed a theory to account for these trends and Sonder" called their world-wide arrangement the regmatic shear pattern. Moody and Hill proposed a much more complicated shear network which, although fascinating and perhaps ultimately useful, will not be followed here. In a recent review of deformation within the Cordillera, Wisser mentioned the four fundamental directions. The fact that many geologists deny the existence of the regmatic shear pattern implies that the fundamental structures are far from obvious. It may mean, also, that some geologists are not accustomed to examine regional and world maps analytically. The maps require much study, and certain features should be isolated on overlays. Even so, with the present limited knowledge, uncertainties remain. The following analysis is a qualitative experiment, subject to change as information accumulates, and should be supplemented by the western sheet of the Tectonic Map of the United States.' Many have probably gained the impression that the Cordillera of the West is oriented northwest-southeast and from this, unless experience rules otherwise, it is natural to assume that the structure likewise trends northwest-southeast. To an important extent this is true, yet anyone tracing off the western sheet of the Tectonic Map all the recorded north west-southeast structures may be surprised to see what a small part of the entire area they occupy. In southwestern U. S. (Fig. 1) the northwest-southeast structures are mostly restricted to the eastern, southern, and western parts. The eastern margin of the Cordillera from northern Colorado to the International Boundary near El Paso, Tex., is obviously determined by some structure other than northwesterly ones. In eastern Nevada and far southward toward the Gulf of California many mountain ranges, valleys, and faults are meridional. In the Rocky Mts. of Colorado, and at many places in southern Arizona, the crystalline Pre-Cambrian is foliated northeast-southwest. The Uinta Mts. of Utah trend approximately east-west, in much the same way as a broad belt of transverse, west-northwest structures—the Texas lineament of Hill",' and Ransome10 in southern Arizona, southwestern New Mexico, and southern California. It seems, then that there are four regmatic shear directions in the Southwest, but at many places they are discontinuous, and their projections must be inferred. To clarify these trends the four sets have been isolated into two systems: 1) northwest-northeast and 2) east-west-north-south (Figs. 2 and 3). Northwest-Northeast System: A number of prominent northwest-trending zones of structure are easily recognized. They are designated by circled Roman numerals, the northeast-trending structures by circled capital letters. Perhaps no two geologists would agree completely on the positions of all these belts. Names given below are for convenience only, and may be discarded where other names have priority. (I) The Sierra Nevada-Lower California belt contains the Jurassic-Cretaceous granitic massifs of the Sierra Nevada and Lower California. These

Jan 1, 1959

By H. Doi, Y. Fujiwara, K. Miyake

In order to throw light on the mechanism of plastic deformation of WC-Co alloys, compressive tests of WC-(7 to 43) vol pct Co alloys have been carried out at room temperature, and stress-micro strain relation has been investigated in detail. The analysis of the factors affecting the yield stresses reveals that the yield stresses can be predicted by modified Oro-wan's theory if one properly estimates the planar in-terfiarticle spacings. Conzpressive straining of some of the alloys by 0.066 to 0.17pct increases the decrements by a factor of as much as 3.4 to 14, whereas the corresponding increase in the electrical resistivities is less than 10 pct. The analysis of the decrement data in terms of -Gramto and Lücke theory shows that the marked increase is attributed to increased dislocation darnping itt the binder (cobalt) phase. By cornbilling the decrement data and the conzjwession duta, one obtains the relation between flow stress in shear (?t) and increase in dislocation density (p): At = const . v6 . This is interHeted to mean that the mechanism of strain hardening of CirC-Co alloys is essentially sarne as the one for dispersion strengthened alloys. The possible effect of bridge formations between the carbide particles has also been examined. OWING to the combination of hardness, strength, and other physical and chemical properties, WC-Co alloys have opened the way for unique fields of applications, the recent ones being, for instance, anvils for super-high-pressure generation apparatuses. In such applications, the alloys are frequently subjected to very high compressive stresses: these stresses may cause the alloys to deform plastically and eventually to fail. However, much remains obscure regarding the nature of the plasticity of the alloys. Evidently, the alloys owe their high strength to the hard carbide particles which frequently occupy as much as 80 to 90 pct in volume fraction, whereas the ductility required for practical applications is provided by the small amount of the binder phase between the carbide particles. When the volume fraction of the carbide phase is not very large, deformation behavior of the alloys may be described by some of the current dispersion strengthening theories. However, greatly increasing the carbide phase is thought to lead to some carbide skeleton structure or bridge formations owing to the increased chances for direct contacts between the carbide particles;1,2 this may appreciably affect the plasticity of the alloys. Regarding the effect of formation of the carbide skeleton structure, it is interesting to note the work by Ivensen et al.3 on compression tests of the alloys containing somewhat large carbide particles; they observe extensive generation of slip bands in the carbide particles after application of some preliminary compressive stresses. They interpret the results in terms of plastic deformatiot: of the carbide particles which are supposed to have formed a skeleton structure; the binder phase plays only a passive role, at least in the early stages of the deformation. That carbide crystals exhibit microplasticity at room temperature is apparent from the work of Takahashi and Freise4 and French and Thomas5 on indentation of WC single crystals. On the other hand, Dawihl and coworkers6-10 maintain that even when volume fraction of the carbide phase is very large (for instance, more than 90 pet), a very thin binder layer generally exists between the carbide particles. They interpret the results of the extensive mechanical tests in terms of the plasticity of such a layer. Gurland and Bardzil11 point out that decrease in ductility of the alloys with increase in the carbide phase is caused by the effect of plastic constraint exerted by the dispersed carbide particles. Drucker12 further develops this concept from a continuum-mechanics approach on an assumption that a continuous thin binder layer separates the carbide particles. A common feature of the studies reported so far on the plasticity of the alloys is that the information deduced is invariably qualitative in nature. Thus, very few systematic experiments for obtaining reliable and sufficiently detailed stress-strain curves of the alloys varying widely in the microstructural features have been carried out. In particular, it may be of special interest to investigate in detail the early stages of the plastic deformation of the alloys in order to shed light on the strengthening mechanism. However, such work appears to be extremely rare. Doi et al.13 recently reported a first brief account of the results of some quantitative analysis of the plasticity of the alloys in terms of dislocation theory. Their experiment was rather limited in the composition range covered (volume fraction occupied by the carbide phase: 79 to 83 pct), and thus they could not necessarily elucidate the controlling mechanism of plastic deformation of the alloys of a more general composition range. Consequently, in the present investigation, deformation behavior and some other physical properties of the alloys were investigated and discussed in more detail over a much wider composition range. SPECIMEN PREPARATION WC-Co alloys used in this experiment were prepared in cylindrical or rectangular form by sintering in vacuo compressed mixtures of tungsten carbide and cobalt

Jan 1, 1970

By Frederic P. Dewey

This old and well-known method of determining silver is, in bullion work, so far superior to the furnace-assay that it is looked upon with reverential awe by many, if not by most, users, and its ease of execution, with proper equipment, commends it highly where much commercial bullion work on silver is required. The method is so thoroughly well known that a description of it here may seem to be unnecessary, but many thousands of determinations are annually made by it in the U. S. Mint Service and its practice is there reduced to an art. This is necessary both for the sake of economy of time, and because high-grade work with it requires constant practice. It is useless for a person who uses it only occasionally to expect to attain high accuracy with it, without spending more time upon a detemination than is warranted in a busy commercial laboratory. It is always employed in the Mint service whenever possible, but its chief field is in the determination of silver in standard silver (ingots and coin), which is 900 fine in silver and 100 fine in copper, and I shall first briefly outline its use on this metal and then take up various points in detail, especially as related to the accuracy of the results obtained. For this determination 1,115 mg. of standard metal are weighed and transferred to a glass-stoppered bottle, the metal is dissolved in nitric acid, and 100 cc. of a standard solution of NaCl run in. The bottle is then vigorously shaken and a measured portion of a decimal salt solution added, and again shaken, if necessary. These operations are repeated until the silver is precipitated. Standard metal being 900 fine, 1,115 mg. should carry 1,003.5 mg. of silver, which is a convenient figure to work with.

Jan 1, 1914

By Lyle L. Marsh, David L. Douglas

CORRELATION was made between the heat treatment and hardness of three U-Ti alloys ranging in composition from 8.5 to 50 atomic pct Ti. The following important observations were made: 1) A direct quench of y U-Ti solid solution resulted in the formation of a hard martensitic phase in low-titanium alloys. 2) Subsequent tempering initially increased the hardness by the precipitation of a fine dispersion of U2Ti; further precipitation of U2Ti with tempering time eventually resulted in softening. 3) High-hardness levels were obtained also by isothermal transformation of an 8.5 atomic pct Ti alloy at 400º and 500°C. 4) The crystal structure of the phases present at the solution-treating temperature (one region in the phase diagram excepted) and the temperature within a given phase region affected the hardness of both quenched and isothermally transformed alloys. Introduction It has been known since 1887 that the mechanical properties of metals were dependent upon their microstructure. Sorby pointed out in that year that annealed gray iron castings were softer than chilled iron castings by virtue of the graphite which had replaced hard cementite in the microstructure. Over the years, interest has increased in the effect of microstructure on the mechanical properties of metals, and now high-strength levels may be achieved by bringing about the dispersion of a second phase or by other microstructural adjustments. The nature of a second phase in an alloy strongly influences the properties. For example, the size, shape, amount, and distribution of a second phase plays a very important role in the ultimate properties of an alloy. Microstructural control is achieved by heat treatments. Hence, any alloy system of potential use should be understood in terms of its response to heat treatment and the resultant effects upon the properties.

Jan 1, 1958

By Roy Lindgren

SINCE the year 1643, when the first blast furnace in America for treating iron ore was built at Saugus, Mass., out of mica schist quarried in the neighboring district, the procurement of a suitable refractory for furnace lining has been a problem of concern to the operators of furnaces. The stacks built of mica schist continued to smelt iron ore until about 1836, when, according to F. H. Norton, the first firebrick were produced1, at Queens Run, Pa. Other writers speak of brick having been molded and burned in Massachusetts about the year 1834. In 1841, Andrew Russell began to produce medium refractory plastic clay brick near East Liverpool, Ohio, that were used for lining blast furnaces1. The well-known Kentucky clay-producing district was not opened up until the year 1871, but since then it has produced a large percentage of the linings for iron blast furnaces. While some strides have been made by the refractories industry during the 100 years that have passed since the first firebrick were produced, it has been only during the last two decades that any real progress has been made towards bettering the product, even though the method of production had improved. Perhaps the fault lies with the user of the brick rather than with the producer, for not sooner demanding a supe-rior product. During the past 15 years the tonnage produced per lining has increased from 500,000 gross tons to 1,000,000 gross tons, and now some furnaces are producing 1,600,000 gross tons and better on a single lining. It is true that enlarged capacity of furnaces and improved practice have accounted for some of this increase in tonnage, nevertheless better quality in firebrick must be given credit for its share. However, we are not yet ready to say that we have reached a maximum life of furnace lining. We believe that a better product can be produced and that the refractories industries of America will, through their extensive research depart-

Jan 1, 1937

By W. P. Sykes

IN CONNECTION with a study of tungsten steels, Honda and Murakami1 reported an investigation of the system iron-tungsten. This report included a tentative equilibrium diagram, photomicrographs of various alloys in the series, and qualitative measurements of hardness and magnetic properties. The present investigation originally had as its object the study of the hardness and tensile properties of a series of carbon-free iron-tungsten alloys. But, as the work progressed it became evident that the system possessed other features of interest, so the scope of the investigation was enlarged. MATERIALS The iron powder used in preparing the alloys was obtained as follows: Iron oxalate was precipitated from a ferrous-sulfate solution by the addition of a solution of oxalic acid. This oxalate, after thorough washing, was ignited to iron oxide, which after reduction in hydrogen at about 1000° C. yielded iron powder containing but about 0.2 per cent. iron oxide and about 0.005 percent. carbon. Tungsten metal in the form of powder, such as is used in the manufacture of filaments for incandescent lamps, was the other constituent. This material analyzed 99.8 per cent. tungsten and contained no carbon, The metal powders, in the desired proportions, were mixed by tumbling and formed, under pressure of 20 tons per sq. in., into rods 3/8 by 3/8 by 10 in. To form the alloys without contamination, sections of the pressed rods were placed on alundum slabs and heated in an alundum tube wound with a tungsten resistor and packed in heat-insulating material. While the resistor was heated, a stream of hydrogen was continually passed through both the tube and the case containing it. The tungsten winding on the tube, as well as the material heated within the tube, was thus protected from oxidation. Such a furnace will operate constantly

Jan 2, 1926

By I. R. Kramer

The apparent activation energy, U, JOY plastic deformation of aluminium, copper, and gold single crystals and polycrystalline aluminum was found to he dependent upon surface condition. At low strains, the value for U for aluminum single crystals was 4200 cal per mole ; however, this value decreased to 920 cal per mole when the specimens were polished during the test at a rate of 50 X 10-5 win-1 The activated volume also was found to increase with the rate of metal removal. That the surface plays an important role in plastic-deformation processes has been adequately demonstrated.1-4 Of particular interest at this time are the observations4 that the creep rate of single crystals of fee metals is increased markedly when specimens are polished during the deformation process. These observations were interpreted in terms of a dislocation debris layer at the surface regions of the crystal. This layer, which appears to be a region containing a high concentration of dislocations or segments of dislocations, not only will impede the egress of dislocations on the primary slip system, but will also provide a barrier against which dislocations may pile up. By this means, a stress which opposes the motion of dislocations will be generated. It is considered that this stress must be taken into account in any theory which describes the plastic-deformation process. Although a detailed dislocation model cannot be given at this time, it may be stated that the stresses opposing the motion of dislocations arise from the dislocations in the debris layer, Ts, and ti due to the resistance to motion imposed by internal obstacles such as Lomer-Cottrell barriers, subgrain and grain boundaries, forest dislocations, and so forth, as well as the resistance due to the presence of jogs on dislocations and the interaction of the stress fields of dislocations, and so forth. In essence, we have added an additional term, ts, to the usual form of the equation T = Ta- Tb, where Tb is the back stress due to the various types of obstacles which impede the motion of dislocation. Accordingly, the net stress, t, acting on a dislocation may be written as where Ta is the applied shear stress. For deformation which occurs by a thermally activated process5,8 ?=Ae-u/kT = A e(u,-VT)/kT [2] and U = Uo- Vt PI where U = activation energy for plastic flow, y = shear strain rate, Uo = activated energy for plastic deformation in the absence of stress and depends upon the particular deformation process, V = activated volume, k = Boltzmann constant, T = temperature, OK, and A = frequency factor. From Eqs. [I] and [3], U = Uo- V(Ta - Ti - TS) [4] and it is seen that if Ts decreases, the activation energy, U, must decrease if V remains constant. However, as will be shown, V is a function of the surface conditions. In their work on aluminum, Lytton and coworkers7 reported that at low strains the activation energy was 3400 cal per mole and at high strains it was 28,000 cal per mole. The lower value was interpreted in terms of the energy necessary to overcome the Peierls force, while the higher value was associated with the energy necessary for dislocations to move by a cross-slip process. It will be shown that the lower activation energy is associated with the surface debris layer rather than with the Peierls force. EXPERIMENTAL PROCEDURE Single crystals having a nominal cross section of 1/8 in. and a 3-in. gage length were prepared by a modified Bridgman technique using a multiple-cavity graphite mold. The initial purity of the metals was 99.997, 99.999, and 99.999 pet for aluminum, copper, and gold, respectively. The orientation of the specimens is given in Fig. 1. The measurement of the activation energy as a

Jan 1, 1964

By J. Burns Read

IT IS the purpose of this paper to summarize, as far as possible, the metallurgical information and experience gained by the Ordnance Department, during the War, in the manufacture of artillery cartridge cases, to describe the tests to which artillery cartridge cases were put, and to summarize the knowledge and experience gained in this testing. The authors wish to acknowledge the aid given by manufacturers, army officers, and civilian employees of the Ordnance Department in obtaining these data. Artillery cartridge cases are cold drawn from circular disks punched from strips of rolled brass. The manufacture involves from 25 to 30 main operations, which are done almost entirely on a punch press. Descriptions of the operations have appeared in various periodicals and, therefore, will not be given here. After each cupping, or drawing, operation, except the last, the cases are annealed at from 540° to 650° C. (1000° to 1200°F.), to remove all the hardening stresses set up in the metal and to allow complete recrystallization. After each annealing, the cases are pickled in niter cake or sulfuric-acid solution and then washed in water to remove all traces of acid. In some instances, the cases are then immersed in a cyanide-salt solution, and afterwards rinsed in water, to remove the thin layer of copper that forms on the surface of the cases during the acid pickle. The last cold-drawing operation is followed, by the heading operation which, by flattening the head of the case on the outside, causes the metal to flow on the inside to approximately the proper finished dimensions. The mouth, or open end, is then annealed at 430° to 480° C. (800° to 900° F.) by immersion in a salt bath or by gas flames. After being washed, the cases are tapered, when they are ready for machining, inspection, and testing.

Jan 4, 1922

By H. O. Hofman

WHEN dry chlorine gas is made to act in the cold upon finely¬divided gold,' it converts the latter with evolution of heat into auro-auric chloride, Au2CI4, a hard, dark-red, hygroscopic salt. Moisture splits this salt into aurous and aerie chloride, Au2C14 = AuCI + AuCI3; treatment with water converts it into auric chloride and gold, 3 Au2CI4 = 4 AuC13 + Au,. Aurous chloride, when stirred with water, undergoes a similar decomposition, 3 AuCI = AuCI3 + Au,. These decompositions of auro-auric chloride and of aurous chloride furnish the explanation for the practice of moistening an ore before it is treated by the Plattner chlorination-process; practical experience having shown that gaseous chlorine gave an unsatisfactory extraction with dry ore. According to Rose,' fine gold is acted upon more slowly by chlorine than gold containing some base metal, e.g., copper. He also states that small quantities of silver increase the rate of solution, but adds that the coating of silver chloride formed checks, and finally stops, further action, if the percentage of silver be increased beyond a certain undetermined amount. Bromine' acts upon finely-divided gold in a manner similar to chlorine; the auro-auric bromide, Au2Br4, however, is not hygroscopic. Upon treatment with water it is decomposed as is the corresponding chlorine salt. It is generally believed that bromine does not act as energetically upon gold as does chlorine. This seems to be borne out by the results in the leach-

Mar 1, 1905

By T. G. Digges, C. L. Vold, M. R. Achter

A study was made of the effect of the growth conditions on the perfection of single crystals of niobium (columbium). Dislocation densities, determined by means of double-crystal diffractometer measurements , were not greatly affected by the method of crystal preparation but could be reduced by annealing treatments. However, the size, sharpness, and tilt angles of the substructures, observed with X-ray reflection macrograph, were sensitive to variations in growth procedures as well as to subsequent thermal treatments. Although the dislocation density was the same in both types, there were more low-angle bound-aries in crystals grown by zone melting than in those prepared by strain anneal. Mechanisms to account for these observations are discussed in terms of dislocation movements. A planned study of the structure-sensitive properties of refractory metals required the use of single crystals of a high degree of structural perfection and, for ease of handling, of large cross section. It appeared that the strain-anneal technique could satisfy both of these requirements. First, crystals grown in the solid state have been reported to be more perfect than those obtained from the melt.' Second, the diameters of rods which may be produced by zone melting should have a theoretical limit determined by specific gravity, thermal conductivity, and surface tension, while the diameter of strain-annealed rods is limited only by practical considerations. Previously it was shown that niobium (columbium) single crystals of 1 in. diam2 may be grown by strain anneal, compared to the 0.5 in. maximum diameter achieved by zone melting, as reported for molybdenum by Belk.3 The current research was undertaken to investigate and optimize the effect of various process variables on the perfection of 1/4 and 1/2-in.-diam niobium single crystals grown by strain annealing and to compare their perfection to those grown by zone melting. Characterization of these crystals was more conveniently accomplished by means of X-ray than by metallo-graphic techniques. EXPERIMENTAL PROCEDURE Specimen Preparation. Zone-melted crystals of 1/4 in. diam were produced by the standard electron-beam zone-melting technique. The swaged and cleaned rods were outgassed, in the solid state at a temperature near its melting point, at a rate of 12 in. per hr, and single crystals were grown by making two molten passes at 2 in. per hr. By maintaining a zone length of 4 to % in., very uniform single crystals several inches long were obtained. For the strain-annealed crystals, an induction heater was used, in preference to other types of heating, to take advantage of the good penetration of large sections. A five-turn coil, 1 in. long, operating at 10 kc and powered by a motor generator, was contained in a vacuum chamber. The rod, suspended from the upper end, was raised through the coil for both recrystallization and crystal growth. In preliminary work single crystals of the same material were also grown with single and multiturn coils powered by a 450-kc generator. A vacuum of 2 X 10-6 Torr was maintained at temperatures up to 2400°C. Starting with electron-beam-melted ingots of 21/2 in. diam, the analysis for which is given in Table I, the material was cold-swaged to the desired cross section of 1/4 and 1/2 in. diam and then recrystallized. The rods were then strained in a tensile machine and converted to single crystals by passing through the induction coil. As with zone melting, control of orientation is possible by the use of special procedures. Other investigators, see for example Williamson and smallman,4 have reported that orientation control may be achieved by a bending technique. In the present work the strained rod is partially lowered through the coil to start the growth of the crystal. Then it is removed and bent at a point in the poly crystalline portion. Finally, it is returned to the chamber and growth is continued "around the corner". This procedure has certain limitations. If the bending operation exceeds the critical strain, recrystallization may take place. Also, the amount of bending which can be imparted to the rod is limited by coil geometry, and up to now has been 10 deg. However, by repeating the bending and growing operations it should be possible to attain any desired orientation. In preparation for X-ray examination, single crystals were sectioned and planed by means of the spark-erosion technique. To obtain the maximum reflected intensity, the (110) plane was exposed for examination. They were then etched 3 to 5 min in a mixture of con-

Jan 1, 1967

By Will Coghill

As the title indicates, this paper treats of the degree of liberation of minerals after grinding. To obtain the supporting data a "tool" not commonly used by metallurgists has been employed. It is the "heavy solution." The advantages gained through its use are shown. Actual ores were employed in order to make the study concrete. The selection was somewhat incidental and happened to embrace the red iron ores of Alabama. So, any reader interested in these ores will find some of their properties described. The red ores constituted the material examined and a somewhat new adaptation of heavy solutions was the tool of examination. If either the ores or the tool interest the reader these notes may be of some value. The writer's chief interest was in the rate of liberation of locked grains. Ores are generally ground preparatory to concentration and as long as the concentrators make suitable products the effectiveness of the grinding is likely to be unquestioned. But when suitable products are difficult to make, an investigation becomes imperative. In such a case a dissection of the ore might be made to find the cause of the trouble. Such a condition of unsuitable products exists in the low-grade red iron ores of Alabama. They are difficult to concentrate. To be sure it might be said that the concentration of iron ores is a new thing and that the ore-dressing methods are undeveloped, but a glance at the industry reveals an abundance of methods and devices for almost all imaginable conditions. Concentrating machinery has not taken a part in this investigation; the use of it would have been only machinery testing, and should never precede the ore testing which consists of such methods as herein outlined. When the properties of the ores have been gleaned the machinery may be used more effectively.

Jan 12, 1926

By Archer Wheeler

The Boston & Montana Reduction Works at Great Falls, Mont., was formerly the reduction works of the Boston & Montana Consolidated Copper & Silver Mining Co., and continued as the reduction plant for the independent company until .June 1., 1910, when the consolidation of a large number of the operating companies of Butte was effected. It then became merged in the Anaconda Copper Mining Co. as the Boston Montana Reduction Department of the Anaconda Copper Mining Co. The history of copper converting at this plant, while not covering the entire period of the commercial use of the process in this country, does cover by far the larger part of it, and as the operations and appliances of the process have undergone many changes during the time, it may, perhaps, be of some interest to put the record of these changes into permanent form. The plan followed in the preparation of this paper has been to give first a brief chronological record of the principal events and changes and then, even at the risk of some repetitions, to give more detailed account, of some of these changes under separate headings. The headings for the complete paper are as follows: 1. General Chronological Review. 10. Development of Different Classes 2. Mechanical Manipulation of Converters After Class I. 3. Casting of Finished Copper. 11. Basic Lining. 4. Tamping of Linings. 12. Number and Size of Tuyeres. 5. Early Acid Linings. 13. Cast Copper Tuyeres. 6. Acid Linings With the Use of Ore. 14. Efficiency of Air. 7. Introduction of Flux Through the 15. Size of Converter Mouth. Tuyeres 16. Height of Converter. 8. Bottom Blast. 17. Summary. 9. Disposal of Converter Slag.

Jan 8, 1913

By Cloyd M. Smith

B. F. TiLLson*— The manifold difficulties of accurate anemometry in irregular sections of mine passageways, the irregular distributions of velocities in cross sections of the same, and the disturbing influence of the observer upon the air flow, all indicate an undesirable inaccuracy of results obtainable by any standardized method of traversing the section by an anemometer. It seems obvious that another, and simpler, method should be used to determine the volume of air flow in mine passages, namely: 1. At appropriate locations cement or calked framework rings should be installed permanently to equalize the irregularities of sectional contour and provide a place and means of attachment for a temporary cloth brattice which bears a rigid orifice. 2. The measurement of the velocity of air flow through the orifice may then be by anemometer or, preferably, by Pitot tube measurements of the differential pressures on both sides of the orifice in accordance with the standard practices available in engineering 1iterature. † The constants may be determined for various measuring positions in relation to the resulting "vena contracta." 3. The position of the person who makes the measurements is behind the brattice out of the air stream. The Pitot tube does not offer as disturbing an obstruction as the anemometer. A recording gauge may be employed to integrate fluctuations in air flow through that portion of the mine. No traverses are required because the reading may be at a single central point. An anemometer can be used with an orifice flow. The orifice will increase the air velocity at the measuring point, with correspondingly more accurate measurements where the normal air velocity through the passageway is low. Portable brattices might be devised with the cushioning rims which would seal against irregular rock surfaces where permanent rings were not available or feasible. The development by the Ventilation Committee of standard procedures and devices for the orifice measurement of the flow of mine ventilating air might be a desirable project for this coming year. C. M. Smith (author's reply)—Thank you for your discussion of my paper on underground anemometry. Your suggested method of measuring underground air flow is a novel one which might be applicable in some situations. It should be tested along with other suggested methods in any investigation of this subject. G. E. McElroy*—In spite of the adverse publicity that vane-anemometer methods of air measurement have had in the past and that contributed by the present paper, I endorse Mr. Erickovic's statement that anemometer traversing "has proved to be widely applicable, expeditious and simple" and add that available methods are accurate enough for the purposes for which they may be used. The fact that the great majority of minor mine officials assess relative changes in rates of air flow by comparison of crude vane-anemometer measurements, known to average 20 to 30 pct high, has no important bearing on this subject, because state inspection standards were based originally on such methods of air measurement. Federal inspection standards are based on actual rates of flow as determined by traversing, and interest in traversing methods is rapidly increasing. In considering traversing methods, three aspects are of major importance: (1) the absolute accuracy of calibrations; (2) the degree of interference with normal flow conditions introduced by traversing methods designed for accurate measurement by shaft-mounted instruments; and (3) the proper "method" factor to use for approximate measurements by hand-held instruments. With respect to absolute accuracy of calibrations, we have always placed reliance on calibrations made by the National Bureau of Standards, with which manufacturers' calibrations have usually agreed very closely. It is therefore particularly disturbing to find7 that calibrations made previous to June 1947 are presumably about 5 pct in error because of excessive registry caused by the thin flat plates on which anemometers were mounted for calibration. Velocities corrected for calibration have therefore averaged about 5 pct low in all probability. In this connection, it is interesting to note that an anemometer calibrated against Pitot-tube measurement by a single-point method in the Bureau of Mines experimental coal nine in 1923 indicated this same difference of about 5 pct and that the same instrument calibrated by a traversing method in a metal mine some months later indicated a difference in the same direction of about 4 pct. These results are reported by the Bureau of Mines.8 Regarding the degree of interference, or changes in velocity distribution, caused by the position of the observer's body in traversing operations, misconceptions seem to be especially prevalent, resulting in increasing advocacy of methods, such as the "clear section" method outlined in this paper, that cause just the type of interferences that they are designed to avoid. The degree of interference for any method may be gauged easily by a few experiments with a velocity-pressure gauge connected to a Pitot tube or with an indicating velocity meter such as the Velometer. In an experiment cited by McElroy and Richardson,# a decrease of 5 pct was noted at ten widths upstream from a 6-in. plank, whereas an observer's body at about the maximum practical distance of 6 ft downstream from the instrument is only about four widths away. In the Bureau of Standards paper previously mentioned, it is recommended that supports used in calibrations be at least 16 widths downstream. In practice, therefore, a downstream position of the observer is ruled out as far as accurate measurement is concerned. Operation of the anemometer by rigid shaft support from a point outside the section is seldom practicable; however, accurate results can be obtained, with the anemometer rigidly attached to a short shaft and held at arm's length, by an observer advancing across the traversed section while he faces the opposite wall and stands sideways to the current, provided that he keeps the instrument at least 3 ft away from his body at all times and traverses the entire section with it. If the traverse can be started with the observer in a side recess, the entire section can be covered in one operation. Normally, it would be covered in two half-sections. The presence of the observer's body does not, as is commonly supposed, increase the average velocity throughout the remaining part of the section. Rather, the velocities 1 to 2 ft on either side of his body are increased, but the distribution of velocities throughout the rest of the cross section remains normal, and a traverse made as stated gives a true average velocity for normal-flow conditions. Regarding the proper "method" factor for accounting for interference in the approximate methods of traversing with hand-held instruments, here again confusion prevails, for which the writer must assume some of the blame. Comparison of consecutive traverses made by shaft-held and hand-held 4-in. anemometers in field work after the tests reported by McElroy and Richardson' gave method factors

Jan 1, 1950

By B. C. Johnson, K. L. Sublette, F. L. Prestridge

A problem common to the petroleum and mining industries is the resolution into its component phases of mixtures composed of a polar liquid dispersed in an immiscible, continuous nonpolar liquid. In the petroleum industry the polar liquid is water or brine and the nonpolar liquid is crude oil. The source of the entrained aqueous phase is connate water and/or condensed steam used in secondary and tertiary recovery methods. In the mining industry dispersions of polar liquids in immiscible, nonpolar liquids are created in solvent extraction (SX) systems. In these systems the polar, dispersed liquid is leachate or stripping solution while the nonpolar, continuous liquid is the extraction solvent.

Jan 1, 1984

By Billy L. Crowder, John M. Fairfield

The implantation of B+ , P+, and As&apos; into silicon has been studied with the purpose of making shallow p-n junctions. The influence of such parameters as 1) ion energy, 2) target orientation and temperature, 3) total dose, and 4) annealing schedule was investigated. An energy range of 70 to 300 kev was used for boron and phosphorus implants and up to 500 kev for arsenic. It is found that the experimental projected range agrees well with theory and that shallow junction depths can be made reproducibly. ION implantation has received much attention recently as a technique for doping semiconductors. Specifically, it has the potential of supplementing or replacing the diffusion process as a method for making p-n junctions. In a few specific cases it has been used successfully to make semiconductor junction devices. Potential advantages of ion implantation doping over diffusion techniques are: 1) It affords greater control of shallow junction depths (< 0.2 µ) while maintaining high peak concentrations. This is particularly important for high-speed switching devices, since lower junction capacitances and resistances can be achieved. 2) More precise registration of small planar structures can be realized if proper masking procedures are employed. This advantage is especially useful in the design of high-density integrated circuits. It has been used to advantage in FET fabrication since the edge of the source or drain can be aligned precisely at the edge of the gate electrode.&apos; 3) Ion implanatation permits lower temperatures than diffusion techniques. This factor alleviates the problem of compatibility of diffusivities often encountered when designing multiple-junction structures. Also, the lower temperatures create fewer thermal defects and dislocations, which may account for the high efficiency of some ion-implanted solar cells.2 4) Impurity profiles can be more easily tailored to resemble ideal distributions. Successful exploitation of the potential advantages of ion implantation techniques will depend on increased knowledge and understanding of the subject. The factors likely to be influential in determining impurity distribution profiles in ion-implanted single-crystal targets have been reviewed by J. F. Gibbons.3 In addition to the mass and energy of the implanted ion, the total dose, target orientation, and target temperature are important parameters. The annealing temperature required for removing lattice damage and incorporating the implanted species on an electrically active site is very important. This paper describes an investigation of some of these factors. Implants of boron, phosphorus, and arsenic into silicon have been studied. Energy ranges of 50 to 300 kev were used for boron and phosphorus and up to 500 kev for arsenic. In addition to the implantation energy, the effects of total dose, target temperature, and post implant anneal have been investigated. EXPERIMENTAL PROCEDURE The implantation targets were silicon wafers cut from Czochralski-grown crystals, lapped, and chemically polished. The orientations were (111), (110). and (100) with misorientations of up to 7 deg from the principal axis. For this study, accurate target alignment (i.e., within 0.1 deg) was not available and quoted misorientation values should be regarded as approximate . The implantation equipment consisted of an ion source, a 300-kev linear accelerator tube, an electromagnetic separator, and the associated target supporting and beam focusing assemblies. The ion source was a simple oscillating electron type source,4 which has been described elsewhere.5 The gaseous compounds BF3, PF5, and AsH3 were used as ion sources for B+, P+, As+, and AS+&apos;. Analyzed current levels of up to 20 pamp could be obtained; however, for this investigation target current levels of 1-3 µ amp were usually employed. The analyzed ion beam was collimated through a double slit (1.4 x 0.4 cm) and swept perpendicularly to the long axis of the slit such that an area of about 2 sq cm on each target was covered. Dosages of around 1015 cm-2 were normally employed, but smaller amounts were also used for comparison. A uniform flux density over the bombarded area was assured by the continuous use of profile monitors similar to those described by Wegner and Feigenbaum.6 Post-implant annealing was accomplished in an argon atmosphere in a temperature range of 600" to 950°C. It was not part of the purpose of this investigation to study the annealing kinetics; however, some isochronal and isothermal anneal experiments were conducted to determine the time and temperature necessary to render a reasonably high portion of the implanted ions electrically active (i.e., higher than 50 pct). Post-implant anneal temperatures of around 900° and 600°C were required for boron, and arsenic and phosphorus implants, respectively. Arsenic and phosphorus implants increased in conductivity rather abruptly at the proper anneal temperature of the isochronal curve, but boron increased more gradually over a wider range. Isothermal anneal curves were reasonably flat after 10 min, so an anneal time of 1/2 hr was used for the experimental results described below. The profiling techniques were: 1) neutron activation analysis, 2) differential sheet resistance,7 and 3) junction staining.8 The differential sheet resistance technique is commonly employed in this type of study. Its principal disadvantage is the uncertainty of the ef-

Jan 1, 1970

By I. R. Kramer, L. J. Demer

Aluminum single crystals were pulled in an electrolytic cell allowing surface removal during the deformation. The extent of Stages I and 11 of the stress-st-aitz curve was increased and the slope decreased as the rate of metal removed from the surface was increased. An increase of the strain rate caused a decrease in the effectiveness of the metal removal. The data indicate that the work-hardening coefficient in Stage I is determined primarily by the conditions which exist on the surface of the crystal. In Stages 11 and 111, both surface effects and internal barriers are important. ALTHOUGH numerous investigations have been conducted on the plastic flow characteristics of metals in an attempt to explain the mechanism of work-hardening, relatively few studies have taken into account the influence of the surface. In all current theories of work-hardening it is assumed that the impediments to the movement of dislocations are within the crystal. The barriers due to the surface and the existence of solid and liquid films have been neglected even though it has been demonstrated that the surface exerts a large effect. A number of investigators1-l8 have shown that solid films on the surface of single crystals markedly affect their mechanical behavior. In general, the presence of a solid film tends to increase the yield stress and increase the work-hardening rate. Often, on single crystals, Stage I and, at times, Stage II regions are completely suppressed. Various mechanisms have been offered for the effects of oxide and metal films as well as the influence of electrolytes. Of these, concepts concerned with the locking of surface dislocation sources and the blocking of dislocations at the surface resulting in pileups appear to be actively considered at present. Barrett,11 Takamura,6 Gilman,19 Lipsett and King,20 Shapiro and Read,10 and Weiner and Gensamer21 are among those who have interpreted their results in terms of piled-up dislocations at the surface, while Adams.22 and Chalmers and Davis23 have explained their experimental observations in terms of locking of surface dislocation sources. In general, the change in plastic flow properties due to electrolytes has been explained in terms of the unblocking or unlocking of dislocations by the removal of the oxide films. In considering the two proposed mechanisms, it appears that the locking of sources of surface dislocations by a solid film should exert a primary influence only on the critical resolved shear stress for flow and not on the slopes of Stages I and 11. However, the blocking at the surface of dislocations from internal sources may also affect the critical resolved stress and furthermore exert an influence throughout the whole plastic range. In certain cases it does not seem feasible to explain the results of experimental observations in terms of locking of surface dislocation sources. The abnormal aftereffects found by Barrettll,12 by removing the oxide by an acid treatment are excellent evidence of the blocking of dislocations at the surface. Additional evidence in favor of a blocking due to a pileup of dislocations at the surface may be found from the observations that the critical resolved shear strength continues to increase with the thickness of the oxide layer until very heavy oxide layers are formed. If the locking of surface dislocations sources were the dominant factor, the critical resolved shear stress would not be expected to increase after all of the surface sources were locked by the formation of the oxide. This may be expected to happen after a few atomic layers of the oxide are formed. In spite of the above evidence on the strong influence of the surface on the plastic flow characteristic, this has been ignored in current theories of work-hardening. Seeger24,25 suggested that most of the dislocations may slip out of the crystal only when the specimen axis is within certain areas of the orientation triangle. In other areas the resolved shear stress in other glide systems is large enough to generate dislocations which can form Lomer-Cottrell locks, thereby decreasing the average slip distance in some directions and causing a larger hardening rate. Friede126 assumed that at the beginning of Stage 11, a large number of Lomer-Cottrell dislocations are formed by a catastrophic process which used up all the Frank-Read sources on the secondary slip-planes. In this manner a fixed number of Lomer-Cottrell locks is formed which act as barriers against which the dislocations can pile up. In Stage 111, Seeger24 and Diehl, Mader, and Seeger25 proposed that Lomer-Cottrell barriers are circumvented by the cross slip of extended screw dislocations. Cottrell and Stokes,27 Friedel,26 Cottrell,26 and stroh29 suggest that the Lomer-Cottrell dislocations collapse under the stress field of the dislocation pileup. It is the purpose of this paper to report the changes in Stages I, II,and III of the deformation process in

Jan 1, 1962