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By A. H. Geisler, F. Keller

Some of the important changes that take lace in the structure of aluminum alloys are largely submicroscopic in character. This is especially true of the changes that accompany age-hardening and recrys-tallization. Although improved metal-lographic practices have been helpful in indicating some of these changes indirectly, results are limited by the resolving power of optical microscope lenses. The electron microscope, however, provides a new and important means for investigating the fine structure of metals in a range not possible heretofore. It is anticipated that this microscope will yield new and useful information to metallurgists when suitable techniques are developed to utilize its very high resolving power. Several unique methods have been devised to permit the examination of the structure of opaque samples by the electron microscope. These are all based 011 the principle of producing a very thin film that represents the prepared surface of the opaque metal sample, which can be examined in the transmission microscope; however, the available methods fall into three categories, depending on the manner in which the film is obtained. With the oxide-film method developed by Mah13-l7 a very thin surface layer of the metallographic sample is converted into oxide by a thermal, chcmical or anodic treatment. .After removal from the metal sample by one of the special techniques described by Evans,l9 this oxide film is examined in the electron microscope, and is found to portray the structure of the original metal surface. Films formed on aluminum,8,l7 nicke1,7 iron3,8,9 and a nickel-beryllium alloyl1 by heating; films formed on iron8,9 by chemical action; and films formed on aluminum3-'" by anodic oxidation, have been examined. The other two are more recent methods developed principally in this country; they consist in making the thin film in the form of a mold or replica of the surface contour of an etched sample. With the negative replica method the thin film is made directly on the sample; with the positive replica method it is made on a negative reproduction of the sample. With both methods, variations in the contour of the metal sample, caused mainly by etching, produce variations in the thickness of the surface replica. Because of the direct dependence of the amount of scattering of the illuminating electrons upon the thickness of the film penetrated, only the variations in thickness of the replica are responsible for tones in the electron image. Negative replicas are made by forming a thin film of some suitable material directly on the polished and etched metal sample, and derive their name from the fact that after removal from the sample they have the high and low points in the sample reversed, as shown in Fig. I. Nega-

Jan 1, 1944

By F. Keller, A. H. Geisler

Some of the important changes that take lace in the structure of aluminum alloys are largely submicroscopic in character. This is especially true of the changes that accompany age-hardening and recrys-tallization. Although improved metal-lographic practices have been helpful in indicating some of these changes indirectly, results are limited by the resolving power of optical microscope lenses. The electron microscope, however, provides a new and important means for investigating the fine structure of metals in a range not possible heretofore. It is anticipated that this microscope will yield new and useful information to metallurgists when suitable techniques are developed to utilize its very high resolving power. Several unique methods have been devised to permit the examination of the structure of opaque samples by the electron microscope. These are all based 011 the principle of producing a very thin film that represents the prepared surface of the opaque metal sample, which can be examined in the transmission microscope; however, the available methods fall into three categories, depending on the manner in which the film is obtained. With the oxide-film method developed by Mah13-l7 a very thin surface layer of the metallographic sample is converted into oxide by a thermal, chcmical or anodic treatment. .After removal from the metal sample by one of the special techniques described by Evans,l9 this oxide film is examined in the electron microscope, and is found to portray the structure of the original metal surface. Films formed on aluminum,8,l7 nicke1,7 iron3,8,9 and a nickel-beryllium alloyl1 by heating; films formed on iron8,9 by chemical action; and films formed on aluminum3-'" by anodic oxidation, have been examined. The other two are more recent methods developed principally in this country; they consist in making the thin film in the form of a mold or replica of the surface contour of an etched sample. With the negative replica method the thin film is made directly on the sample; with the positive replica method it is made on a negative reproduction of the sample. With both methods, variations in the contour of the metal sample, caused mainly by etching, produce variations in the thickness of the surface replica. Because of the direct dependence of the amount of scattering of the illuminating electrons upon the thickness of the film penetrated, only the variations in thickness of the replica are responsible for tones in the electron image. Negative replicas are made by forming a thin film of some suitable material directly on the polished and etched metal sample, and derive their name from the fact that after removal from the sample they have the high and low points in the sample reversed, as shown in Fig. I. Nega-

Jan 1, 1944

By W. C. Krumbein

GEOLOGICAL problems are approached from a geometrical (space relations) viewpoint, a kinematical (time sequence) viewpoint, or a dynamical viewpoint. The first two require sound training in conventional geology and in field methods. The third approach requires a solid foundation of chemistry, physics, and mathematics. Modern training for geologists should include close integration of basic sciences with geological principles. INTRODUCTION Our knowledge of the earth has increased tremendously during the last half century. We know more about its surface configuration, the distribution of its natural resources, the procession of living forms that inhabited it in the past, the chemical composition of its oceans, the areal distribution of its surface rocks, the movements of its atmosphere, and so on. Not only do we know more facts about the earth, but we have a better understanding of the processes that take place on and within it, such as the nature of earthquakes, the thermodynamics of the atmosphere, the chemical equilibria involved in the formation of igneous rocks, the mechanics of stream flow, the dynamics of the earth's origin, and so on. Many sciences contributed to the sum total of this knowledge, including such established disciplines as geology, geography, physics, chemistry, astronomy, biology. Out of this accumulation of new knowledge grew also a group of new sciences, such as seismology, oceanography, meteorology, volcanology, hydrology. Collectively these latter are known as the geophysical and geochemical sciences, and to a large extent they began as branches of geology. Until the turn of the century, for example, the study of earthquakes (seismology) was a part of geology, although as early as 1846 Mallet, a physicist, had suggested that the subject could be investigated by elastic-wave theory. Comparatively little progress was made along these lines until the seismograph was developed near the turn of the century; since then, additional earthquake data have accumulated rapidly, but more important, the interpretation of these data essentially has kept pace with their accumulation. In similar fashion, meteorology was generally considered a branch of geology as recently as one or two decades ago. Considerable progress had been made in such aspects as weather forecasting, but the science dates its recent rapid rise from the year 1911, when Bjerknes first applied the principles of dynamics to the analysis of air masses. The rapid development of such disciplines as oceanography, volcanology and hydrology was due in part to the application of principles of chemical equilibrium, of dynamics, and of thermodynamics to earth problems, by men who were essentially physicists or chemists by training. The last half century, therefore, and particularly the last two decades, saw the influx of numerous chemists and physicists into the realm of the earth sciences. In the meantime the main body of geology itself showed a marked growth, and

Jan 1, 1941

By W. C. Krumbein

GEOLOGICAL problems are approached from a geometrical (space relations) viewpoint, a kinematical (time sequence) viewpoint, or a dynamical viewpoint. The first two require sound training in conventional geology and in field methods. The third approach requires a solid foundation of chemistry, physics, and mathematics. Modern training for geologists should include close integration of basic sciences with geological principles. INTRODUCTION Our knowledge of the earth has increased tremendously during the last half century. We know more about its surface configuration, the distribution of its natural resources, the procession of living forms that inhabited it in the past, the chemical composition of its oceans, the areal distribution of its surface rocks, the movements of its atmosphere, and so on. Not only do we know more facts about the earth, but we have a better understanding of the processes that take place on and within it, such as the nature of earthquakes, the thermodynamics of the atmosphere, the chemical equilibria involved in the formation of igneous rocks, the mechanics of stream flow, the dynamics of the earth's origin, and so on. Many sciences contributed to the sum total of this knowledge, including such established disciplines as geology, geography, physics, chemistry, astronomy, biology. Out of this accumulation of new knowledge grew also a group of new sciences, such as seismology, oceanography, meteorology, volcanology, hydrology. Collectively these latter are known as the geophysical and geochemical sciences, and to a large extent they began as branches of geology. Until the turn of the century, for example, the study of earthquakes (seismology) was a part of geology, although as early as 1846 Mallet, a physicist, had suggested that the subject could be investigated by elastic-wave theory. Comparatively little progress was made along these lines until the seismograph was developed near the turn of the century; since then, additional earthquake data have accumulated rapidly, but more important, the interpretation of these data essentially has kept pace with their accumulation. In similar fashion, meteorology was generally considered a branch of geology as recently as one or two decades ago. Considerable progress had been made in such aspects as weather forecasting, but the science dates its recent rapid rise from the year 1911, when Bjerknes first applied the principles of dynamics to the analysis of air masses. The rapid development of such disciplines as oceanography, volcanology and hydrology was due in part to the application of principles of chemical equilibrium, of dynamics, and of thermodynamics to earth problems, by men who were essentially physicists or chemists by training. The last half century, therefore, and particularly the last two decades, saw the influx of numerous chemists and physicists into the realm of the earth sciences. In the meantime the main body of geology itself showed a marked growth, and

Jan 1, 1941

By W. C. Krumbein

Geological problems are approached from a geometrical (space relations) viewpoint, a kinematical (time sequence) viewpoint, or a dynamical viewpoint. The first two require sound training in conventional geology and in field methods. The third approach requires a solid foundation of chemistry, physics, and mathematics. Modern training for geologists should include close integrltion of basic sciences with geological principles. Introduction Our knowledge of the earth has increased tremendously during the last half century. We know more about its surface configuration, the distribution of its natural resources, the proccssion of living forms that inhabited it in the past, the chemical composition of its oceans, the areal distribution of its surface rocks, the movements of its atmosphere, and so on. Not only do we know more facts about the earth, but we have a better understanding of the processes that take place on and within it, such as the nature of earthquakes, the thermodynamics of the atmosphere, the chemical equilibria involved in the formation of igneous rocks, the mechanics of stream flow, the dynamics of the earth's origin, and so on. Many sciences contributed to the sum total of this knowledge, including such established disciplines as geology, geography, physics, chemistry, astronomy, biology. Out of this accumulation of new knowledge grew also a group of new sciences, such as seismology, oceanography, meteorology, volcanology, hydrology. Collectively these latter are known as the geophysical and geochemical sciences, and to a large extent they began as branches of geology. Until the turn of the century, for example, the study of earthquakes (seismology) was a part of geology, although as early as 1846 Mallet, a physicist, had suggested that the subject could be investigated by elastic-wave theory. Comparatively little progress was made along these lines until the seismograph was developed near the turn of the century; since then, additional earthquake data have accurnul~ted rapidly, but more important, the interpretation of these data essentially has kept pace with their accumulation. In similar fashion, meteorology was generally considered a branch of geology as recently as one or two decades ago. Considerable progress had been made in such aspects as weather forecasting, but the science dates its recent rapid rise from the year 1911, when Bjerknes first applied the principles of dynamics to the analysis of air masses. The rapid development of such disciplines as oceanography, volcanology and hydrology was due in part to the application of principles of chemical equilibrium, of dynamics, and of thermodynamics to earth problems, by men who were essentially physicists or chemists by training. The last half century, therefore, and particularly the last two decades, saw the influx of numerous chemists and physicists into the realm of the earth sciences. In the meantime the main body of geology itself showed a marked growth, and

Jan 1, 1946

By W. C. Krumbein

Geological problems are approached from a geometrical (space relations) viewpoint, a kinematical (time sequence) viewpoint, or a dynamical viewpoint. The first two require sound training in conventional geology and in field methods. The third approach requires a solid foundation of chemistry, physics, and mathematics. Modern training for geologists should include close integrltion of basic sciences with geological principles. Introduction Our knowledge of the earth has increased tremendously during the last half century. We know more about its surface configuration, the distribution of its natural resources, the proccssion of living forms that inhabited it in the past, the chemical composition of its oceans, the areal distribution of its surface rocks, the movements of its atmosphere, and so on. Not only do we know more facts about the earth, but we have a better understanding of the processes that take place on and within it, such as the nature of earthquakes, the thermodynamics of the atmosphere, the chemical equilibria involved in the formation of igneous rocks, the mechanics of stream flow, the dynamics of the earth's origin, and so on. Many sciences contributed to the sum total of this knowledge, including such established disciplines as geology, geography, physics, chemistry, astronomy, biology. Out of this accumulation of new knowledge grew also a group of new sciences, such as seismology, oceanography, meteorology, volcanology, hydrology. Collectively these latter are known as the geophysical and geochemical sciences, and to a large extent they began as branches of geology. Until the turn of the century, for example, the study of earthquakes (seismology) was a part of geology, although as early as 1846 Mallet, a physicist, had suggested that the subject could be investigated by elastic-wave theory. Comparatively little progress was made along these lines until the seismograph was developed near the turn of the century; since then, additional earthquake data have accurnul~ted rapidly, but more important, the interpretation of these data essentially has kept pace with their accumulation. In similar fashion, meteorology was generally considered a branch of geology as recently as one or two decades ago. Considerable progress had been made in such aspects as weather forecasting, but the science dates its recent rapid rise from the year 1911, when Bjerknes first applied the principles of dynamics to the analysis of air masses. The rapid development of such disciplines as oceanography, volcanology and hydrology was due in part to the application of principles of chemical equilibrium, of dynamics, and of thermodynamics to earth problems, by men who were essentially physicists or chemists by training. The last half century, therefore, and particularly the last two decades, saw the influx of numerous chemists and physicists into the realm of the earth sciences. In the meantime the main body of geology itself showed a marked growth, and

Jan 1, 1946

By W. C. Krumbein

GEOLOGICAL problems are approached from a geometrical (space relations) viewpoint, a kinematical (time sequence) viewpoint, or a dynamical viewpoint. The first two require sound training in conventional geology and in field methods. The third approach requires a solid foundation of chemistry, physics, and mathematics. Modern training for geologists should include close integration of basic sciences with geological principles. INTRODUCTION Our knowledge of the earth has increased tremendously during the last half century. We know more about its surface configuration, the distribution of its natural resources, the procession of living forms that inhabited it in the past, the chemical composition of its oceans, the areal distribution of its surface rocks, the movements of its atmosphere, and so on. Not only do we know more facts about the earth, but we have a better understanding of the processes that take place on and within it, such as the nature of earthquakes, the thermodynamics of the atmosphere, the chemical equilibria involved in the formation of igneous rocks, the mechanics of stream flow, the dynamics of the earth's origin, and so on. Many sciences contributed to the sum total of this knowledge, including such established disciplines as geology, geography, physics, chemistry, astronomy, biology. Out of this accumulation of new knowledge grew also a group of new sciences, such as seismology, oceanography, meteorology, volcanology, hydrology. Collectively these latter are known as the geophysical and geochemical sciences, and to a large extent they began as branches of geology. Until the turn of the century, for example, the study of earthquakes (seismology) was a part of geology, although as early as 1846 Mallet, a physicist, had suggested that the subject could be investigated by elastic-wave theory. Comparatively little progress was made along these lines until the seismograph was developed near the turn of the century; since then, additional earthquake data have accumulated rapidly, but more important, the interpretation of these data essentially has kept pace with their accumulation. In similar fashion, meteorology, was generally considered a branch of geology as recently as one or two decades ago. Considerable progress had been made in such aspects as weather forecasting, but the science dates its recent rapid rise from the year 1911, when Bjerknes first applied the principles of dynamics to the analysis of air masses. The rapid development of such disciplines as oceanography, volcanology and hydrology was due in part to the application of principles of chemical equilibrium, of dynamics, and of thermodynamics to earth problems, by men who were essentially physicists or chemists by training. The last half century, therefore, and particularly the last two decades, saw the influx of numerous chemists and physicists into the realm of the earth sciences. In the meantime the main body of geology itself showed a marked growth, and

Jan 1, 1941

By J. T. Shimmin

THE past twenty-five years has been a period of unparalleled improvement in all lines of mining and metallurgical equipment, but probably none has undergone greater refinement and development than the vacuum filter. Beginning a quarter of a century ago, there has been steady advancement in the art of vacu-um filtration until today its use has become virtually standard practice for dewatering throughout the entire metallurgical industry as well as in important parts of the chemical and industrial processing fields. The credit for the first successful application of vacuum filtration 'at the Consolidated Mercury mines in Utah in 1902 undoubtedly belongs to George Moore. There, it is said, his filter reduced the loss of gold in the slime and sand from $1.25 to 40c. per ton. Successful applications were subsequently made by Mr. Moore at the Liberty Bell mines, Telluride, Colo., the Lundberg, Dorr &Wilson mill at Terry, S. D., and elsewhere. E. L. Oliver is generally credited with, having done the most to work out the necessary continuity of op-eration exemplified in the well-known continuous vacu-um filter which bears his name. Others made improve-ments also, but in my opinion all the new ideas advanced in recent years are modifications of the fundamental principles originated by the two pioneers, Moore and Oliver. Considerable interest has been shown recently in the new type of continuous internal-type vacuum filter which is associated with my own name1. In response to frequent inquiries regarding it and the steps which led up to its invention, I am giving herewith a brief account of the early history of this development and some of the more important installations which have been made during the last year or so. A. M. Nicholas (now deceased), an Australian engi-neer, conceived the idea, several years ago, of manu-facturing a continuous vacuum filter with the filter medium applied upon the inside of the drum, as con-trasted with existing drum filters in which the medium is applied externally. Nicholas recognized that a ma-chine of this type would be simpler than one with a tank and would overcome some of the difficulties en-countered with tank filters on certain classes of pulps, and he appreciated the value of having filtration take place in the same direction as the gravitational settle-ment of the solid particles in the pulp, the pulp being retained within the drum instead of being held against the outside surface. The ease of starting up after a shut down was likewise realized by Nicholas. It was tried in the United States, but was not entirely success-ful primarily due to mechanical defects.

Jan 5, 1928

By W. C. Krumbein

GEOLOGICAL problems are approached from a geometrical (space relations) viewpoint, a kinematical (time sequence) viewpoint, or a dynamical viewpoint. The first two require sound training in conventional geology and in field methods. The third approach requires a solid foundation of chemistry, physics, and mathematics. Modern training for geologists should include close integration of basic sciences with geological principles. INTRODUCTION Our knowledge of the earth has increased tremendously during the last half century. We know more about its surface configuration, the distribution of its natural resources, the procession of living forms that inhabited it in the past, the chemical composition of its oceans, the areal distribution of its surface rocks, the movements of its atmosphere, and so on. Not only do we know more facts about the earth, but we have a better understanding of the processes that take place on and within it, such as the nature of earthquakes, the thermodynamics of the atmosphere, the chemical equilibria involved in the formation of igneous rocks, the mechanics of stream flow, the dynamics of the earth's origin, and so on. Many sciences contributed to the sum total of this knowledge, including such established disciplines as geology, geography, physics, chemistry, astronomy, biology. Out of this accumulation of new knowledge grew also a group of new sciences, such as seismology, oceanography, meteorology, volcanology, hydrology. Collectively these latter are known as the geophysical and geochemical sciences, and to a large extent they began as branches of geology. Until the turn of the century, for example, the study of earthquakes (seismology) was a part of geology, although as early as 1846 Mallet, a physicist, had suggested that the subject could be investigated by elastic-wave theory. Comparatively little progress was made along these lines until the seismograph was developed near the turn of the century; since then, additional earthquake data have accumulated rapidly, but more important, the interpretation of these data essentially has kept pace with their accumulation. In similar fashion, meteorology, was generally considered a branch of geology as recently as one or two decades ago. Considerable progress had been made in such aspects as weather forecasting, but the science dates its recent rapid rise from the year 1911, when Bjerknes first applied the principles of dynamics to the analysis of air masses. The rapid development of such disciplines as oceanography, volcanology and hydrology was due in part to the application of principles of chemical equilibrium, of dynamics, and of thermodynamics to earth problems, by men who were essentially physicists or chemists by training. The last half century, therefore, and particularly the last two decades, saw the influx of numerous chemists and physicists into the realm of the earth sciences. In the meantime the main body of geology itself showed a marked growth, and

Jan 1, 1941

By J. W. Leonard

This expanded and more detailed supplement to earlier published work1 is offered as a means to demonstrate the high empirical correlation which exists between the readily measured coal bench scale test parameters of volatile matter (d & a.f.), Hard-grove grindability index (HGI), Koppers cone bulk density (BD) and pulverization level (% passing a 1/8-in. screen) to the less readily measured full scale coke stability index. Thus, Fig. 1, 2 and 3 represent the correlated test data contained in Tables I, II and III respectively. Ninety-six coals are correlated so that 97% of the resultant cokes fall within two points and 100% fall within three points of the actual tested coke stability indices. The main generalizations which can be drawn from the correlation of these coals are as follows: 1) The coke stability indices for higher bulk density coals (46.0 BD to 50.6 BD) appear to be largely influenced by differing combinations of factors for coals above and below a pivotal point of approximately 36% to 37% volatile matter. Below this pivotal volatile matter coke stability index appears to be influenced largely as a result of changes to the coal volatile matter and pulverization level. While above this pivotal volatile matter coke stability indices appear to be dependent on the coal hardness, as measured by the HGI, and to some extent upon coal volatile matter. Pulverization appears to have little influence on the coke stabilities of the harder coals (52 HGI to 58 HGI) of greater than 36% to 37% volatile matter. 2) The coke stability indices for lower bulk density coals (41 BD to 45.9 BD) appears to be largely influenced by changes to coal volatile matter and pulverization level for softer coals above approximately 58 HGI. 3) The main empirical observation to be drawn from these results is that for coals above approximately 36% to 37% volatile matter the quantities of hard and soft constituents as measured by the HGI are important when defining coal rank for correlation to the coke stability index.

Jan 1, 1965

By J. H. Frye, D. L. McElroy, E. E. Stansbury

The rates of growth of pearlite in high-purity Fe-C alloys have been measured as a function of the transformation temperature. These and other data have been correlated in terms of a derived rate equation. Activation energies for the growth were found to be 24,200 cal per mol of austenite for the 0.78 pct C alloy and 27,600 cal per mol for the 0.93 pct C alloy. Theoretical implications are discussed. AN excellent review of the the theoretical and experimental studies on the mechanism and kinetics of the eutectoid reaction has been presented recently by Mehl and Dube.' They have pointed out that these investigations have followed two lines of approach: 1—experimental studies and derivations of expressions for the overall transformation characteristics, and 2—derivation of expressions for the nucleation and growth rates in terms of fundamental processes. Investigations of the latter type have been concerned for the most part with the nature of the growth at the austenite-pearlite interface in plain carbon and alloy eutectoid steels. They discuss two theories of the rate of growth of pearlite from aus-tenite—those of Brandt and of Zener. Both derive rate equations which are based on the assumption that carbon diffusion is the controlling mechanism. Mehl and Dube,' Zener,2 and Brandts. " have attempted to calculate growth rates by use of these equations together with thermodynamic and diffusion data. The results are encouraging, but agreement is not so good as to constitute verification of the theories. Furthermore, it Is not clear how these equations are to be used to study the effect of alloying elements which apparently exert little influence on carbon diffusion, but markedly decrease growth rates. It is not clear whether or not the addition to iron of an alloying element which does not diffuse during transformation can alter the rate of growth of body-centered from face-centered cubic iron. That it can greatly decrease the overall transformation rate has

Jan 1, 1954

By J. J. Reed

The mines of southeast Missouri's Lead Belt have been in operation since 1864, almost 100 years. During this period about 10 pct of the total ore available has been left in place as pillars, and this now represents the best ore reserve left to the older mines. St. Joseph Lead Co. has been investigating various plans of pillar recovery for several years. The example to be described is only one possible approach under a specific set of conditions. Conditions vary greatly in the different areas within the Lead Belt, and the same approach would be entirely inadequate in certain other areas, but there are important sections where this system is clearly applicable. Horizon mining is practiced in the Lead Belt, and stopes may vary from 10 ft to well over 100 ft high. Fig. 1 is a plan view of 6100 stope, the area to be discussed. For these mines this is a small stope, only 10 to 12 ft high. Before any plans were drawn up for pillar recovery, three independent estimates of the pillar grades were made by the mine superintendent, the mine captain, and the mine geologist. After these results were averaged, pillars indicated to be of economic grade were marked for removal as shown. At this stage several alternatives were considered: 1) retreat with caving, 2) concrete replacement pillars, and 3) systematic bolting and retreat. A retreating system with caving was not chosen because the roof was known to be too bad even to permit loading a blasted pillar before caving would begin. Concrete replacement pillars would have been too costly and would have required a large crew, bulky materials, and unwieldy equipment. Systematic bolting was chosen as being most acceptable for the following reasons: 1) Limited area and spans were involved. 2) Only minor modifications to the jumbo would be required for bolting. 3) Only a two-man bolting crew would be needed. 4) Only compact bolting materials would be required. 5) The bolting plan could be modified to allow

Jan 1, 1960

By B. H. Kear, B. J. Piearcey

The orientation and temperature dependence of the tensile and creep propevties oj Mav-M200 crystals halle been determined. Crystals oriented for single slip exhibit ,maximum ductility, minimum work hardening, and least creep resistance, whereas crystals in multiple slip orientations show nzinimu~n ductility, strongest work hardening, and greatest creep resistance. At 1400" and 1600°F there is a marked improzlenzent in creep strength for orientations approaching [001] and [111], indicating that interactions between dislocations gliding in intersecting octahedral slip systems play an important role in creep resistance. At 1800°F the creep strength is much less dependent on orientation, which is rationalized in terms of slip in cube planes as well as octahedral A frequent mode of failure in high-strength cast nickel-base superalloys is by intergranular fracture, particularly along those grain boundaries oriented transverse to the major stress axis. VerSnyder and ~uard' demonstrated that this problem could be overcome by eliminating transverse grain boundaries through unidirectional solidification. Piearcey and versnyder2 made use of this principle in the development of unidirectionally solidified gas turbine blades and vanes, where the growth direction of the columnar grain structure coincides with the axis of principal stress under operating conditions. The present investigation was undertaken to determine if further improvement in properties may be obtained by eliminating grain boundaries altogether, so as to take advantage of the well-known dependence of mechanical properties of single crystals upon the orientation. 1) EXPERIMENTAL PROCEDURE Single crystals of Mar-M200* were grown from the melt under vacuum by a modified Bridgman method. The melt was poured into a preheated alumina mold, and crystal growth was promoted from one end by appropriate gradient cooling. Tensile and creep specimens (2 in. diam by $ in. gage length) were prepared by a series of operations involving electrical discharge machining, precision grinding, and electropolishing. The orientations of the specimens were determined by the Laue X-ray back-reflection method. Tensile tests were carried out in aWiedemann machine with furnace attachment, using a strain rate planes. In all orientations imzpvouement in the strength charactevistics of the material can be induced by heat treatment. Creep ad stress rupture data for (001) oriented crystals are compared with similar data obtailted previously joy random polycvystalline material, and also columnar grained material having a prejevved (001) orientation. The single-crystal )material exhibits both longer rupture life and lower minimum creep rate at all temperatuves, and the rupture elongation is comparable with that in the columnar grained material. From these results it is concluded that single crystals should and useful application in gas-turbine blades and tanes. The optimum orientation for a blade is considered to be with its axis of principal stvess parallel to (001) ou (111). of 0.0001 sec-'. Load and extension were recorded directly on an X-Y recorder. The strain measuring device consisted of extension arms attached to the grips at one end and leading out of the furnace to an LVDT (linear variable differential transformer) at the other. Creep tests were performed using a standard constant load creep frame. 2) DISCUSSION OF RESULTS 2.1) Structure of Alloy. The structure and segregation in as-cast and heat-treated Mar-M200 has been described in detail else where.~ The main features are as follows: the as-cast material is heavily cored, due to pronounced dendritic segregation during solidification; the dendrites are rich in tungsten and cobalt whereas the interdendritic regions are rich in chromium, titanium, nickel, and carbon. The structure consists of -60 vol pct coherent precipitate of y', basically Ni3(A1,Ti), in a matrix of y (nickel-base solid solution), interspersed in the interdendritic regions with minor MC carbides and -y' eutectic. The y' particles, and y-y' eutectic, contain more titanium, aluminum, and nickel, and less tungsten, cobalt, and chromium than the y matrix. Heat treatment partially removes segregation, eliminates the eutectic, refines the y' dispersion in y, and gives additional partially coherent M23Cs carbide. An as-cast crystal, therefore, is composed primarily of two oriented phases (y + y'), whereas the normally heat-treated crystal consists of three oriented phases (y + y' + MZ3Cs). Typical electron transmission micrographs of the y + y' structure are shown in Fig. 1. Crystals grown in the (100) orientation develop a simple unidirectional dendritic structure, Fig. 2, since (100) happens to be the preferred direction of growth for dendrites in this material. Crystals grown in the {110) and (111) orientations, however, tend to promote equal growth, generally in separate colonies, in the two and three geometrically favored (100) growth directions, respectively. In other orientations of growth, a single (100) dendrite direction generally pre-

Jan 1, 1968

By R. E. Ogilvie, A. R. Kaufmann, S. H. Gelles

The solid-solubility limits of iron in beryllium were determined between 850o and 1200oC by analysis of differential type multiphase diffusion couples, using an X-ray absorption technique. The maximum value of the solubility limit was found to be 0.92 ± 0.02 at. pct (5.46 wt pet) at the eutectic temperature 1225°C. The solubilities of nickel and beryllium were determined between 900°and 1200°C by the same technique and the maximum solubility was found to be 4.93 + 0.01 at. pct (25.2 wt pet) at the eutectoid temperature, 1065°C. A previously unreported high-temperature phase which decomposes eutectoidally at 1065 °C was found to exist in the beryllium-nickel system at a composition of approximately 8 at. pct Ni (36 wt pet) by diffision-couple analysis. The presence of this phase was confirmed by thermal analysis and metallo-graphic analysis of the structure resulting from the eutectoid decomposition. G. V. Raynor1 has treated the solid solubilities of some of the elements in beryllium on the basis of the "Hume-Rothery" rules2 which have been modified to include ionic size and ionic distortion effects. It was predicted that the solubility of iron and nickel in beryllium should be slightly less than that of copper. The lowering of the solubility, according to Raynor, is due to a more unfavorable relative valency effect and an ionic size effect. Kaufmann and corzine3 have compiled data on the solubilities of elements in beryllium and have discussed them in the light of the Raynor paper. These authors feel that, because the elements having the greatest solubility in beryllium systematically fall in the Group VIII and IB Columns of the periodic table, the electronic structure greatly influences the maximum solid solubility of elements in beryllium. The solubility of iron in beryllium was determined by Teitel and cohen4 as part of the study of the beryllium-iron phase diagram. The determination was carried out by X-ray and thermal analysis and according to the phase diagram presented, the maximum solubility of iron in beryllium is 0.41 at. pct (2.5 wt pct) at 1225oC. However, it is estimated that the uncertainty in the position of the a-beryllium primary solid-solution boundary is about 0.5 at. pct (3wtpct). Losana and Goria3 in studying the beryllium-nickel phase diagram, determined the solid solubility of nickel in beryllium by thermal analysis. They found the maximum solubility to be between 1.65 and 2.65 at. pct (10 to 15 wt pct) at 1240°C. This value decreased rapidly with decreasing temperature. In determining approximate ranges of solubilities for different elements in beryllium, Kaufmann, et al,8 reported a value of between 1.3 and 1.7 at. pct (7.9 to 10.1 wt pct) for the solubility of nickel in beryllium. The value was obtained by metallographic examination of quenched alloys and lattice-parameter measurements. However, the authors also noted a single-phase structure for a 1.7 at. pct Ni alloy (10 wt pct) on cooling from the liquid. This would indicate a higher solubility range than was reported. ~isch,' in his X-ray studies of beryllium-copper, beryllium-nickel, and beryllium-iron intermetallic compounds, reports the disappearance of a second phase (Ni,Be2) in the beryllium primary solid solution at approximately 4 at. pct (20 wt pct). THEORY The analysis of concentration gradients in diffusion couples has proven to be a useful tool in determining phase equilibria.8-14 In this particular study the diffusion couples were chosen to straddle the expected composition range of the phase boundary, then heat treated at a given temperature and the concentration gradient evaluated. The composition of the phase boundary for a given temperature appears at a point of discontinuity of the composition gradient. Examples of typical phase diagrams and the concentration gradients which should be found in such systems are shown in Fig. 1. In the present work, gradients of the form of Fig. l(c) were obtained in diffusion couples made of pure beryllium and two-phase alloys of beryllium with either iron or nickel. The composition at the point where the gradient becomes discontinuous, Cs, corresponds to the solubility limit of either iron or nickel in beryllium. The analysis of the concentration gradients was carried out by an X-ra absorption method developed and applied by Ogilvie and later used by Moll13 and Hilliard.l4 It depends on the fact that the absorption of X-rays by matter is determined by the concentration and type of the various atomic species present. The relationship for the intensity, I, of a monochro-

Jan 1, 1960

By H. R. Ogden, E. S. Bartlett, A. G. Imgram

Unmodified disilicide coatirigs were applied to sheet-tensile specimens ofCb-Dg3 and Mo-TZM veJractovy- metal alloys. Coating thickness, degree of coating-substrate interdiffusion, and specimen geonzetry (notched and plain were included in the variables studied. Tensile tests were made to determine the ductile-lo-brittle transition temperature. The disilicide coating modestly increased the transition temperatlre of TZM, but had no effect on 043. Neither material condition (recrystallized or stress-velieved) nor specimen geometry (notched or unnotched) significantly altered the effects of coatings on the transilion temperatures of. the alloys. Cracks in the brittle coatings did not propagate into the substrate, and fracture modes appeared to be the same for both un-coated and coated specimens. MOST potential structural applications for refractory metals and alloys involve exposures to oxidizing environments at elevated temperatures. The general lack of oxidation resistance of these metals will require protective coatings to allow fulfillment of their potential. Currently preferred coatings for the oxidation protection of refractory metals are brittle intermetallic aluminides or silicides. These are typically formed on the surface of the refractory-metal substrate by a diffusion reaction between the substrate and a gaseous or liquid medium that is rich in aluminum or silicon. Because of the brittleness of these coatings, they will sustain no plastic deformation at low temperatures. They are frequently cracked by cooling from the coating temperature because of the thermal-expansion mismatch with the substrate alloy. Even if they survive cooling intact, they crack rather than sustain deformation under load at low temperatures. Thus, when a coated refractory metal is strained beyond the elastic limit of the coating at low temperatures, the mechanical environment of the substrate would include both static and dynamic cracks. These might be expected to influence the flow and fracture behavior of the substrate. This could be manifested in an altered fracture mode and/or an increase in the normal ductile-to-brittle transition temperature of the refractory-metal substrate. This paper presents the results of a research program that was conducted to determine the influence of the presence of a brittle surface coating on the low-strain-rate tensile behavior of typical refractory metals at low temperatures. EXPERIMENTAL PROCEDURES Material Preparation. Thirty-mil-thick sheets of molybdenum TZM alloy (Mo-0.5Ti-O.1Zr) and colum-bium D43 alloy (Cb-IOW-1Zr-O.1C) were obtained commercially. These alloys were selected as substrate materials representing two classes of materials important in current refractory-metal technology. The TZM was in the stress-relieved condition, and exhibited a heavily fibered grain structure. The D43 had been processed by the duPont "optimum" fabrication schedule,' and exhibited slightly elongated grains typical of this process. Tensile specimens of two geometries were prepared from these materials: 1) plain specimens with 0.2-in.-wide 1.0-in.-long gage sections; 2) specimens similar to above, but with a 0.06-in.-diam hole drilled in the center of the gage section, providing a stress concentration factor, Kt, of 2.5. The "notch" geometry was selected to represent a typical condition of a rivet hole or other geometric discontinuities as might be encountered in various applications. Machined specimens were degreased, with a final rinse in acetone, prior to the application of coatings. Specimens of each substrate and configuration were pack-siliconizedin a particulate mixture of 80 pct A1203, 17 pct Si, and 3 pct NaF. Specimens were embedded in this mix (contained in graphite retorts) and coated in an electrically heated argon-atmosphere furnace under time-temperature conditions to effect nominal 1- and 3-mil-thick silicide coatings: Coating Thickness, mils Thermal Treatment 0.6 to 1.4 24 hr at 982°C 2.4 to 3.2 48 hr at 1093°C Coating kinetics were similar for both the TZM and D43 substrates. These treatments had little or no visible effect on the substrate microstructure as determined by optical metallography. The coatings on TZM were essentially single-phase unmodified disilicides, while those on D43 showed substantial evidence of modification by proportionate reaction with the respective substrate elements or phases, as shown in Fig. 1. It was recognized that these coatings might not be particularly desirable regarding protective capability. However, it was desired to circumvent possible inter -ferring chemical interaction with the substrate by pack additives such as chromium, titanium, boron, aluminum, and other elements that typify the better protective coatings for these materials.' Thus, the results presented apply specifically to the simple silicide coatings investigated. They may not be rep-

Jan 1, 1967

By G. L. Chierici

Starting from Muskat's theory of water and gas coning, maximum permissible oil production rates without water and/or free-gas production have been determined, in a broad range of reservoir and well parameters, using the potentiometric model technique. The main assumptions made are as follows: (1) the reservoir rock is homogeneeous (either isotropic or anisotropic); (2) the volume of the aquifer underlying the oil zone is very small, so that it does not contribute to reservoir energy; and (3) the gas cap expands at a very low rate, so that it can be assumed to be in quasi-static conditions. The results obtained are presented in the form of diagrams which can be used for solving two types of problems: (1) given the reservoir and fluids characteristics, as well as the position and length of the perforated interval, determine the maximum oil production rate without water and/or free-gas production; and (2) given the reservoir and fluids characteristics only, determine the position and length of the perforated interval which optimize the maximum permissible oil production rate, without water and/or free-gas production. INTRODUCTION In oil reservoirs where the oil-bearing formation is underlain by an aquifer which does not participate in the production mechanism, water-coning is a limiting factor to the flow rates of producing wells. Production rates are usually kept to a value that will prevent the water from entering the wells. The entry of water into a well lowers its productivity by increasing the weigbt of the fluid column; moreover, the separation of water from the effluent, at the surface, may constitute a very difficult problem in cases of heavy viscous oils. A similar situation is encountered in oil reservoirs with a gas cap overlying the oil-saturated zone; here a downward gas cone is induced by the flow of oil towards the producing wells. Production rates must be low enough to prevent the gas from being produced; producing gas from the gas cap would be a waste of energy. Of course, water-coning and gas-coning phenomena can occur at the same time in the same reservoir if the oil-producing formation is both overlain by a gas zone and underlain by a water zone. Due to its relevant practical importance, the mechanism of coning was studied by many people.2,3,5-8 Defining the conditions for getting the maximum water-free and/or gas-free oil production rate is a difficult problem, often encountered under one of the following aspects: 1. Predict the maximum flow rate that can be assigned to a completed well without the simultaneous production of water and/or free-gas. 2. Define the optimum length and position of the interval to be perforated in a well, in order to obtain the maximum water and gas-free production rate. A systematic study of these problems was made by means of the electrical analog technique. The results of this study are presented here, under the form of a set of curves providing solutions for the above stated problems. These curves are valid only for homogeneous forrnations, either isotropic or anisotropic. Should the formation be non-homogeneous (by horizontal or vertical variation of permeability, shale diaphragms, fractures, etc.), a specific potentiometric study would be required for each specific case. Especially when shale diaphragms of some radial extension are present, the critical rates observed are much larger than would be expected from the diagrams. STATEMENT OF THE PROBLEM In the present study the aquifer is supposed to be of such limited volume that it does not contribute to the energy of the reservoir. Moreover, the gas cap is supposed to expand at such a low rate that the potential gradient in the gas cap is negligible. Under static conditions water-oil and gas-oil interfaces (T1 and T2) are both horizontal. When the reservoir production starts, below each well these interfaces take a cone-like shape (Fig. 1) having as an axis the axis of the well. This shape results from the equilibrium between potential gradients in the oil zone and gravitational forces due to density differences between oil and water and between oil and gas. Assuming the oil-bearing formation to be homogeneous and the oil to be incompressible, the analysis of the problem (see Appendix) shows that the oil-water and gas-oil interfaces are stable only if the oil production rate of the well is not higher than the following values.

Jan 1, 1965

By Fred C. Bond

COMPRESSION TESTS THE standard method of determining the crushing resistance of rocks consists of crushing prepared shapes under slow compression, and expressing the ultimate crushing resistance at the load causing failure in pounds per square inch of crossectional area perpendicular to the crushing force, with the height approximately equal to the diameter. One-inch cubes or cylindrical drill cores are commonly used. Cubes and drill cores are cut by a high-speed steel disk with diamond dust embedded in the edges, and running under a water spray. Such a saw will cut one square inch or more of hard stone per minute. An oiled, spherical, swivel compression block of small diameter should be used to equalize the pressure. Each sample is crushed between sheets of cardboard or blotting paper extending about one-half inch beyond the edges of the stone. A cloth is wrapped around it to prevent dangerous explosive shattering. It is probably preferable to place the swivel block below the specimen, with either a rigid head or another swivel block above. Whatever the arrangement, the conditions should be selected that will develop the maximum crushing strength of the specimen, even though its top and bottom planes may not be precisely parallel. The cardboard pads may be dispensed with if the ends of the specimens are polished smooth. The use of lead pads was discontinued because of the observed tendency to split the material. The samples are weighed and measured before breaking, and the density is calculated. Cubes that contain bedding planes or veinlets are usually placed with these vertical and parallel to the crushing force, in order to develop the maximum resistance possible. A number of compression tests were made on Canadian ores, by Forrest Nagler, of the Allis-Chalmers Manufacturing Co., and are listed alphabetically in Table 1. These tests were made on one inch cubes or on diamond-drill cores approximately one inch in diameter and one inch long. The drill cores represent virgin rock, while the cubes may have been previously weakened by explosives. Compression tests have been made in the Allis-Chalmers Milwaukee Laboratory on a number of ores and other materials. These are listed alphabetically in Table 2. In test No. 1339, on limestone from the Hanna Coal Co., comparison was made between 2 by 2-in. diamond-drill core segments and one-inch cubes cut from the cores in the same strata. Results for the cylinders are tabulated directly below those for the cubes. The bedding planes were normal to the compressive force in breaking the cylinders and parallel in breaking the cubes, which accounts for the lower strength obtained from the cylinders. The percentage of net linear compression at the ultimate pressure was measured in test No. 1055 for Fontana TVA quartzite as 0.30 for cube A, and 0.37 for cube D.

Jan 1, 1946

By James M. Stapleton

IT has long been recognized by blast- furnace men that correct top distribution of materials is very important in efficient and economical furnace operation. Thousands of experiments on top design, filling, sizing, and other operations have been carried out to improving furnace performance by securing uniform distribution. Many of these experiments have worked out satisfactorily and have been passed along to the industry. Many of them have been discarded and forgotten. It has been the custom to judge the results of such experimentation by the results shown in improved or lowered furnace efficiency. While the effect on furnace practice will have to continue to be the final criterion of experimental changes, it has always been a desire of blast-furnace men to ascertain the reason for failure or success. Efficiency in the blast furnace approaching the maximum can be measured in several ways: (I) by actual operating results as revealed in the coke rate and tonnage figures, and (2), in the degree to which the top gas approaches the limiting ratio of CO/C02 for the reduction of iron oxide by CO gas. This ratio is shown in the equilibrium curve in Fig. I for the system Fe-O-C and CO2-CO-C. The closer the top gases approach this limiting ratio (set at 1.08 by Martin1 because of the effect of limestone calcination) the more efficiently we may expect a furnace to operate. The fact that low CO/C02 ratios parallel eficient operating performance caused us to investigate the cause of good or poor distribution and the effect of filling and other changes on furnace operation. Heretofore it has been possible to take a sample of furnace gas (usually from the dust catcher) and from it determine how closely the reducing gases were to the ideal or limiting value as set by the equilibrium diagram. However, to find just where in the top area the distribution was distorted and the top-gas CO/CO2 ratios were distant from equilibrium values has been a difficult and expensive investigational procedure. In an effort to overcome this difficulty, apparatus was designed to take gas samples and temperatures across the top radius of the furnace. It was hoped that with the aid of this apparatus traverse sampling of the ascending gases could be simplified, and the cost of sampling substantially lowered. Routine experimenting could then be maintained and results checked with furnace operation. It must be emphasized that a traverse sampling is necessary for a true picture, as single samples at any one point are unreliable. This statement can be verified by an examination of Tables 3 to 6, showing results obtained at our furnaces in a large number of tests. APPARATUS The design of the equipment for taking the samples was governed by the need for providing a simple, routine test that could be performed fairly quickly without adversely affecting normal furnace operation.

Jan 1, 1943

By Orville R. Lyons, A. C. Richardson

During the past few years there has been a growing demand by coal operators for detailed information about the performance characteristics of the various dryers now being manufactured, preferably in such a form that the information could be used to determine the type of dryer best suited to a particular drying problem. A few operators have been desirous of going even further, because they are of the opinion that present-day dryers are not properly designed and that fundamental studies of dryer design should be undertaken. This growing demand for a method of dryer evaluation and the indicated need for fundamental research resulted in the sponsorship by Bituminous Coal Research, Inc. of a project at Battelle Memorial Institute to investigate the thermal drying of coal. In investigating this problem, the most feasible method of attack appeared to be a survey of active operations to determine the present status of the thermal drying of coal. Data were obtained, usually by actual plant tests with the cooperation of the various preparation engineers and their staffs, for 9 screen-type dryers, 8 rotary-type dryers, 3 continuous-pallet-type dryers, 2 flash-type dryers, I tray-type dryer, and I cascade-type dryer. The testing program provided: (I) data for 24 coal-drying operations, (2) information about the inherent characteristics of the coals dried, (3) information about the previous treatment that the coal had received, and (4) information about operating costs. The data obtained through the dryer survey and relationships determined from the data make it evident that all of the types of dryers included in the survey can be operated with the same degree of effectiveness if each type of dryer is used to dry the sizes of coal for which it is best suited. It should be noted that it is usually undesirable and often impossible to dry different sizes of coal in one type of dryer. By use of the data in the report, any prospective dryer user, having determined the surface moisture percentage and screen-size analysis of the coal to be dried, the tons of water to be removed per hour, and the final surface moisture percentage desired, should be able to determine with a fair degree of accuracy: (I) the difficulty of the drying problem, (2) the approximate cost of drying, (3) the required dryer inlet gas temperature and volume and exhaust gas temperature and volume, (4) the type of dryer to use, and (5) the size of dryer required. The method of testing the dryers and determining the difficulty of drying can be used by operators already having dryers to check the performance of their particular dryer and determine whether they are operating effectively. Considerably more information was obtained from the survey of thermal drying than was anticipated when the survey was first considered. However, a great deal of work still remains to be done in the field

Jan 1, 1949

By W. J. Kroll

W. J. Kroll (Belgium)—Those who are acquainted with the metallurgy of our forefathers may have occasionally a good time when glancing at recent publications in which aged discoveries are unconsciously reported as novelties. We know very well, that oxygen blowing of iron has been described by old Bessemer. The author of the present article is, however, not aware of the fact that the process he describes, the fused salts scrubbing, was already used in the middle of the last century by St. Claire Deville in his attempts at making higher-purity aluminum from raw AlCl3 by sodium reduction. The same fact escaped the three investigators to whom the author refers. The technical grade AlC13 produced by St. Claire Deville from impure oxide, chlorine, and carbon (Oersted process) was contaminated with Sic4 and FeC13, which he removed on an industrial scale by various methods.' He sublimed, for instance, his chloride in contact with iron nails, or aluminum chips, or in hydrogen, which reduced the FeC13 to the less volatile FeCl2. He used also alkali-alkaline earth chlorides as a solvent for A1C13 and FeC13 in presence of iron as a reducing agent, and sublimed his purified AlC13 from solvent salts. The successors of Deville used also zinc or lead as a reducing agent. These methods were later used currently for the purification of BeCl2 and for collecting this compound in a salt bath, suitable for fusion electrolysis. More recently, the same Deville process has been described as applied to the purification of ZrCL4, as part of a method of extraction of ZrCL4 from silico zirconium, which later was reacted with FeC12 in a separate part of the equipment. According to the patent referred to3 the ZrCL4 is dissolved as a gas in a carrier salt such as alkali-alkaline earth chloride, from which it can be reclaimed in a purified form by distillation. A bath of NaCl/KCl is recommended in the specifications. The FeC12-FeC13 go in the salt solution in which raw ZrCl4 is introduced by bubbling, while Sic4 and Tic4 pass through the bath and escape in the atmosphere. purification by this salt-solvent method is thus well described. It may be worth while insisting on some minor details about which the author did not bother too much. One of these concerns the material of construction for the container. If iron is used, and if no other reducing agent is added, then it is the iron of the pot that acts as a reagent in the breakdown of FeC13 to FeCl2, and corrosion can be expected. This shows the importance of using extraneous large surface-reducing agents, of which there is a choice. Zir-

Jan 1, 1963