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By R. M. Waterstrat, E. C. van Reuth

BINARY- alloy phases having the A15-type crystal structure have been described as occurring at a simple and more or less invariant stoichiometric composition (A3B) which corresponds to the relative number of atoms occupying each of the two crystallographi lattice sites in this structure.1,2 It is frequently assumed, therefore, that each crystallographic site is occupied exclusively by one kind of atom. In most cases, however, there have been insufficient experimental data to establish whether atomic ordering is, in fact, complete. Recent studies have shown that binary A15-type phases are sometimes stable over an appreciable composition range3''* and, occasionally, the composition range of stability does not even include the "ideal" A3B stoichiometric composition.5-7 We have observed the existence of nonstoichiometric A15-type phases in the binary systems Cr-Pt and Cr-Os. This has not been reported in previous work on these alloy systems.1,8-11 A series of alloys, each weighing approximately 30 g, was prepared by are-melting in an Ar-He atmosphere using 99.999 pct Cr, 99.999 pct Os, and 99.99 pct Pt as starting materials. Each alloy was melted four times with a total weight loss of less than 1 pct. The stoichiometric (A3B) alloys were sealed in evacuated quartz tubes and annealed at 1200°C for periods of time ranging from 3 days to 2 months. Examination of the alloy microstructures revealed that little change had occurred over this time interval and it was therefore assumed that the microstructures were fairly representative of equilibrium conditions. No evidence of contamination was observed although there was apparently some loss of chromium which was confined to a thin layer at the surface of the specimens. The quartz tubes were quenched from the annealing temperature into cold water. X-ray diffraction and metallographic examination of the stoichiometric alloys revealed an estimated 10 to 30 pct of second phases which were tentatively identified as phases previously reported in these binary-alloy systems.8-11 A second series of alloys was prepared by mixing -325 mesh metal powders having a nominal purity of 99.9 pct and compressing these mixed powders in a cylindrical die at a pressure of 43,000 psi. These alloys, each weighing 15 g, and some of the arc-melted alloys were annealed in a high-temperature vacuum furnace heated by tantalum strips at a pressure of 10-8 Torr and were rapidly cooled by turning off the furnace power. X-ray and metallographic examination of both series of alloys served to establish the composition ranges of the A15-type phases. Although some chromium losses occurred during the vacuum annealing, they were largely confined to a thin layer on the outer surfaces of the samples. It was established that the A15 phases occur in the Cr-Pt system at 21 ± 1 at. pct Pt after 1 week at 1200°C and in the Cr-Os system at 28 ± 1 at. pctOs after 1 day at 1400°C (see Table I). We also observed that an arc-melted stoichiometric (A3B) alloy in the Cr-Ir system was single-phase (A15-type) in the "as-cast" condition in agreement with previous work.8,13 In addition we obtained a sample of the Cr-Os A15-type phase from Argonne National Laboratory. This alloy contained less than 1 pct second phase12 and was submitted to a density measurement. The density measurement yielded a value of 11.14 g per cu cm in comparison to a theoretical value of 11.25 g per cu cm calculated using the observed lattice constant (4.6806Å) of this alloy. The uncertainty in measurement was 0.1 pct but the sample may have contained some cracks or minor imperfections which could account for the low experimental value. We have also studied the atomic ordering in these phases by means of integrated line intensity measurements using thick, flat, rotating powder samples and CuK a radiation in an X-ray diffractometer. We have obtained order parameters of 0.90 for the Cr-Pt phase, 0.89 for the Cr-Ir phase, and 0.64 for the Cr-Os phase using the formula: where s is the usual Bragg and Williams order parameter, ra is the fraction of chromium atoms in A sites, and FA is the fraction of chromium atoms in the alloy. The values obtained are estimated to be accurate within ±4 pct. If the unusually small value for the order parameter of the Cr-Os A15 phase were due to the existence of lattice vacancies on the "B-atom" sites, then a density of 10.04 g per cu cm would be expected in contrast to the observed value of 11.14 g per cu cm. We, therefore. conclude that the fraction of lattice vacan-

Jan 1, 1967

By Nicholas J. Grant, Oliver Preston

PUBLICATION of data by Irmann' indicating outstanding thermal stability and elevated-temperature strength properties in a sintered aluminum powder product (SAP) stimulated interest in the strengthening of metals by means of a highly dispersed oxide phase. This material was produced by compacting, sintering and extruding a fine flake aluminum powder, resulting in a dense product containing 10 to 16 volume pct alumina, which arises from the thin oxide film on the starting powder, highly dispersed in a matrix of pure aluminum. The method of producing SAP, and the stable high-temperature properties obtained from it, introduced the possibility of developing superior materials for high-temperature service by powder metallurgy methods. The composition of the materials of this type which are presently under consideration is predominantly metallic, containing from less than 1 pct up to about 20 volume pct of the oxide. As a result, other properties of these materials, such as electrical and thermal conductivity, thermal shock resistance, and to a certain extent ductility, notch sensitivity, machinability and hot working properties, are also predominantly metallic. These alloys do not constitute, therefore, a completely new class of materials as do the cermets, but rather present a new means of modifying the properties of a metallic matrix. In this sense, SAP type alloys are more closely analogous to the alloy aging systems. While the strength properties realized in the oxide-pure metal systems at the lower temperatures are substantially less than the best attainable in the aging systems, the thermal instabilities in the latter make them of less value for use at temperature much above their optimum aging temperatures, as indicated in Fig. 1. While the means of obtaining an oxide dispersion are more difficult and costly than conventional aging processes, in the light of the as yet limited understanding of such systems there is considerable promise of improved high temperature properties arising from the thermal stability of these structures. Since the development of SAP in 1946, its properties and the properties of a series of similarAl,O,-A1 products containing from about 1 to 20 pct aluminum oxide have been fairly extensively studied and reported.'- "articular attention has been given to

Jan 1, 1958

By L. D. Ricketts

' In recent years the metallurgical field of the copper industry has expanded greatly, the copper ores have become lean add diverse in charactcr, and we are obliged to treat such ores on a very large scale. On the commercial side, the operating and consulting staffs of the great mining companies have been enlarged and organized, and no great capital expenditure is decided upon until it has been investigated and recommended by a highly organized force of specialists as a committee. I believe that in the scientific field and in the most valuable proceedings of our -various societies the old idea of one-man point of view and one-man treatment of principle and detail together has been splendidly developed and should continue, but for the advancement of our art we should deliberately discuss subjects among ourselves in order to do away with the idiosyncrasies of the individual and to gain a composite view reprcscnting the best thoughts of many men. In the development of new ideas leading to the introduction of new methods, the societies could enlarge their present great field of usefulness if such discussion be had, and in my opinion further great good could be done if a number of men of different qualifications and experience would join in preparing a joint book, each dealing with his particular problem, but consulting the other men. In this way individualism would be preserved and various processes would be described, and if properly reviewed the paper would be palpably capable of analysis, and the student would have at his command the associated efforts of a group of qualified engineers. I have neither the time nor the qualifications to make an investigation and study in detail of hydro-metallurgical processes, but for some years I have foreseen the development of such processes, and I have a deep interest in the subject and have given some of its phases careful consideration from a long-distance viewpoint. I have assisted in directing many experiments and in reviewing the merits of many processes, and am glad to make some introductory remarks with the understanding that other gentlemen present will freely and candidly enter into the discussion and help to fill out the few bare bones that I can uncover.

Jan 1, 1916

By V. Koump, T. F. Perzak, R. G. Olsson

The rate of dissolution of recrystallized alumina in molten iron oxide in equilibrium with iron at 1450°C was studied by rotating alumina disks in the melt. The samples were rotated from 1 to 12 min at speeds from 54 to 3270 rpm. It is concluded from the experimental results that the process is limited by diffusion in the liquid boundary layer. The interdiffusion coefficient for the dissolution of alumina disks in pure molten iron oxide was estimated to be about 3 xl0-5= sq cm per sec. THE erosion of refractory materials is of considerable importance in iron- and steelmaking processes. Since many refractories contain alumina, this investigation was undertaken to develop a further understanding of the erosion mechanism. Shurygin et al.1-3 have investigated the rate of dissolution of alumina in molten silicates and molten fluorides by rotating alumina disks in various melts. The rates were reported to be limited by diffusion in the liquid boundary layer. In the present investigation the rate of dissolution of alumina in molten iron oxide in equilibrium with iron was studied in a similar manner; alumina disks were rotated at different speeds in molten iron oxide at 1450°C. The relationship between the rate of dissolution of the flat surface of the disk and the speed of rotation was used to determine whether the process is limited by diffusion in the liquid boundary layer or by some chemical reaction mechanism. APPARATUS AND EXPERIMENTAL PROCEDURE A schematic diagram of the experimental apparatus is shown in Fig. 1. The iron oxide melts were contained in 2-in.-diam high-purity iron crucibles that were centered in a cylindrical graphite susceptor. Prior to each sequence of experiments, sufficient reagent-grade ferric oxide was added to a crucible to form approximately 350 g of molten iron oxide; the depth of the melt was about 11/2 in. To prevent excessive erosion of the crucible, about 70 pct of the required iron was added to the crucible in the form of iron powder. The mixture was melted in an atmosphere of purified argon by induction heating with a 250-kc generator. After the oxide was molten, a Pt/Pt-10 pct Rh thermocouple at the exterior of the crucible was calibrated against an iron-sheathed thermocouple immersed in the melt and was thereafter used to regulate the melt temperature. All experiments were conducted at 1450°C with a probable error of 10°C. The alumina disks were constructed from pure re-crystallized alumina having a density of 3.7 g per cu cm (porosity approximately 6 pct). For each disk sample a 1-cm-diam alumina cylinder of known length (0.9 to 1.0 cm) was cemented into a ground seat at the end of a 1.27-cm-OD centerless ground alumina tube. The ends of the tube and cylinder were flush and served as the disk surface. When mounted in the apparatus the alumina tube was guided by tungsten carbide bearings and rotated by a variable-speed motor. The bearing and drive assembly could be raised and lowered in order to allow the sample to be quickly moved in and out of the melt. At the start of an experiment, a sample was preheated for several minutes directly above the melt, and then immersed in the middle of the melt to a depth of a in. and rotated for 1 to 12 min at speeds of 64 to 3270 rpm. The speed of rotation was measured by a hand tachometer. At the start and completion of each experiment, a melt sample was withdrawn with a cold copper rod and the alumina content was determined by chemical analysis. During individual experiments the alumina concentration of the melt changed by the order of 0.25 wt pct. Average melt compositions for individual experiments were used in the subsequent computations and were in the range between 0.12 and 4.3 wt pct alumina. The extent of dissolution was determined by sectioning the end of the sample and measuring the final length of the alumina cylinder with a microscope. Since the exposed end of the cylinder, i.e., the disk surface, was etched in a manner characteristic of this geometry, a number of measurements were made on

Jan 1, 1969

By J. H. Wernick, J. E. Kunzler

HIGHLY pure metals are needed for low-temperature electron transport studies in progress. Recent improvements in purification techniques, such as zone refining, have made it possible to obtain metals with improved purity. For some metals, the improvement has been to the extent that ordinary analytical techniques are inadequate and special methods are needed.1 For other metals purification is more difficult, so that simple but rapid analytical methods are desirable as an aid in evaluating the effectiveness of purification procedures. Furthermore, it is desirable to be able to determine the impurity level of the sample or ingot with the minimum of physical disturbance of the material. In order to aid in the preparation of purer metals, techniques involving the measurement of electrical resistance at liquid-helium temperatures have been devised for studying impurity distributions in zone-refined ingots and other bulk samples without destroying the ingot or its geometry. The method yields information on the variations in purity along the length of the ingot or sample and provides a measure of the overall purity of the material. Compared with ordinary analytical methods, the resistivity method is rapid, sensitive, and does not require significant physical disturbance of samples with reasonable shapes. It has the disadvantage that resistance measurements are not specific, i.e., they do not identify the impurity. However, this disadvantage is offset by the advantage of being able to establish a measure of the overall purity so far as electrically active" impurities are concerned. METHOD AND ITS BASIS The method is based on the well-known fact that the resistivity, at Liquid helium temperatures, of a reasonably pure metal containing no regions with additional phases decreases with increasing chemical purity or a decrease in the number of physical defects. It is convenient to separate the total resistivity into three parts: where is the resistivity due to the scattering of the conduction electrons by the lattice vibrations or phonons, p is the contribution due to physical defects, and originates from the effect of chemical impurities in the metal. Insofar as Matthiessen's rule is obeyed,2 pphys and pchem are independent of temperature. Except possiblyin the very purest metals, ptherm is negligible at liquid helium temperatures and For zone-refined metals, which normally are well annealed and consist of large grains, at the chemical purity levels thus far attained the available data indicate that pphys is negligibly small or at least constant throughout the ingot. Assuming that the effect of physical defects is negligible for isotropic metals, This assumption appears consistent with most of

Jan 1, 1959

By G. Meyrick, H. W. Paxton

Observations on the tensile deformation of single crystals of austenitic stainless steels as a function of composition, orientation, and temperature are described and compared with relevant data for other alloys. Crystals free from second phases show sharp yield points followed by Lüders' extensions of up to 20 pct. The critical resolved shear stress is strongly temperature-dependent increasing fourfold between 423O and 77°K. A temperature-independent low rate of hardening follows the Luders' extension and is frequently associated with overshoot. Unlike pure metals where Proficse cross slip usually occurs at the end of linear hardening, this stage is terminated either by cross slip or by slip on the conjugate system, the particular node apparently depending upon initial orientation and composition. The presence of 6 ferrite or martensite has a profound effect upon the magnitude of the yield stress and the shape of the stress-strain curve. In experiments on transgranular-stress corrosion cracking of austenitic stainless steels in boiling magnesium chloride, several workers1'2 have shown that increasing amounts of nickel tend to reduce the probability of specimen failure. Reed and paxton3 have observed in single crystals that the macroscopic crack plane changes as the nickel content is increased. For 18 pct Cr-8 pct Ni, the crack plane is sensibly perpendicular to the applied tensile stress; for 20 pct Cr-20 pct Ni the crack plane is (100). The average crack-propagation speed is much lower in the 20 pct Ni crystals. Furthermore, the possible importance of stack-ing-fault energy in nucleation and growth of cracks has been suggested by a number of workers. While the general effect of variations in stack ing-fault energy appears to be quite well-correlated with observed variations in cracking characteristics, each of the theories assigns rather different detailed reasons for these effects. Because the stack ing-fault energy of austenitic steels is believed to be increased with increasing nickel content, and because some theories of trans-granular cracking postulate a mechanical stage in the crack propagation (rather than relying entirely on electrochemical solution), it appeared to be of some interest to investigate the mechanical properties of a series of different compositions of aus-tenite single crystals. These experiments were considered of intrinsic value in view of the relative scarcity of such data on fcc alloys. This paper gives the results of some experiments carried out with this aim in mind, and suggests various 'other experiments which may be helpful in future studies. The experiments are also of interest in view of the recent interest in obtaining higher-strength steels by control of the imperfection content of austenite; although the compositions are not directly comparable, the results are still probably valuable. Comparisons with experiments on other fcc alloy crystals are made where possible to see how well the general pattern of behavior is understood. EXPERIMENTAL PROCEDURE The alloys used in this investigation were vacuum-melted heats of nominally 20 pet Cr-20 pet Ni-60 pet Fe, 20pctCr-16 pct Ni-64 pct Fe, and 20 pctCr-12 pet Ni-68 pet Fe.* Analyses of the material are

Jan 1, 1964

By Charles W. Chesterman

Perlite is a glassy volcanic rock which will, upon rapid controlled heating, expand or "pop" into a frothy material of low bulk density, valued as a lightweight aggregate. The term perlite also is applied to the expanded product. The chemical composition of perlite ranges from that of rhyolite to that of andesite; the water content ranges from 2 to 5%. Most perlite is pale gray, but some is black, brown, or even green. Inclusions in perlite are common and include phenocrysts of quartz, feldspar, biotite, and hornblende, and miscellaneous rock fragments. Occurrences of perlite are restricted to areas of Tertiary and Quaternary volcanic rocks. Perlite occurs as flows associated with thick accumulations of pyroclastic debris and other flow rocks, as dikes, sills, domes, and as selvages of intrusive bodies of volcanic rock. Individual flows of perlite range in thickness from a few feet to as much as 100 ft and commonly cover several square miles. Dikes and sills of perlite generally are small, but domes generally are substantial in size and may be as much as several miles in diameter. Most perlite deposits are large enough and topographically situated so as to lend themselves to low-cost open pit mining methods. Conventional equipment is employed in the mining of perlite. Although milling procedures may appear to be simple, care is exercised in order to produce a carefully sized product and to minimize the production of excessive quantities of fine materials, which have limited use and are considered as waste. Perlite is processed, or "popped," in one of two basic types of furnaces: horizontal rotary or vertical stationary. Both types of furnaces include product collection and dust control systems. Many commercial deposits of perlite are known to occur throughout the world, and although no exact estimate of reserves is available, there appears to be an adequate supply to meet current and future worldwide requirements. End Uses The uses of expanded perlite are many and varied and are based primarily upon its physical and chemical properties. Because of its (1) low bulk density, which generally ranges between 2 and 20 lb per cu ft; (2) low thermal conductivity "K" factor (Btu per hr per sq ft per OF per in, of thickness), which ranges between 0.267 for loosely packed perlite (bulk density of 4.48 lb per cu ft) to 1.25 for perlite gypsum plaster; (3) high resistance to fire; and (4) low sound transmission, expanded perlite is used to a great advantage as aggregate and insulating material in the construction industry. Early uses of perlite were related exclusively to the construction industry, which now consumes about 60% of the domestic production. The primary use of perlite now is as aggregate in insulation boards. Other uses of perlite in 1971 were as aggregate for plaster, horticultural aggregate, low-temperature insulation (cryogenics), and concrete. Because of its low thermal conductivity ("K" factor), high adsorption of sound, low bulk density, and fire resistance, perlite aggregate plasters hold many advantages over conventional plaster. Perlite aggregate plaster lends itself to machine applications, dries quickly, and has relatively high elasticity which reduces cracking after drying. These same features make perlite useful as aggregate in portland cement concrete and asphalt concrete for construction wherever weight reduction, insulation, and acoustics are of prime importance. Perlite-portland cement concrete offers up to 20 times more thermal insulation than conventional concrete, and because of this it finds wide application in roof decks and floor fill in multistory buildings, in

Jan 1, 1975

By Blamey Stevens

In this paper, which is a logical extension of my paper, The Laws of Intrusion,1 the various pressures of emanation and their mechanical causes and effects on the large scale of nature are determined, and a classification of emanations is deduced therefrom. • The Subterranean. Sea. The subterranean sea is here defined as the intercommnnicating water contained in the trains of pores and fissures of the rocks down to great depths. Whether the actual amount of water constituting this subterranean sea be large or small, does not enter into the present argument, since the static pressure of this water at any particular depth is not a function of the quantity : it involves only the depth and the density of the water. Densities. The total pressure at depths down to 10 or 15 miles is made up of the rock-stresses investigated in my previous papers, and the pressure of the subterranean sea. The latter component must evidently be equal to the weight of a solid column of the overlying water of unit sectional area. As mater expands with heat, it should really be necessary to sum the density at every level. A knowledge of the densities of mater under a variety of conditions is therefore needed, but does not seem ever to have been ascertained for such combined pressures and temperatures as we have to consider. The specific gravity of water at 28' C. for various pressures up to 400 atmospheres, has been determined by Barus, 2 who

Jan 1, 1913

Henry D. Hibbard, High Bridge, N. J. (Communication to the Secretary): There is one chemical factor which has not been considered in the author's tabulation of tests, but which is none the . less important because it cannot be practically estimated, and that is the element oxygen. This element has been, and probably will continue for some time to be, one of the great causes of the continual discrepancies between the chemical and physical properties of steel. Probably oxygen occurs, in important proportions, only in soft steel, such as that which we are now considering. In this steel its physical effect is to diminish tensile strength and elongation. The percentage of oxygen in the steel, under working-conditions that are as uniform as possible, is likely to vary inversely as that of the manganese, or perhaps, and more probably, it may bear even an inverse geometrical ratio to the manganese-content. At all events, to follow the author's plan, the line representing the loss of strength due to oxygen is probably a curve. Plotted by itself, the line would probably be straight; that is, the decrease in strength would be proportional to the increase in oxygen, but if the results were superposed on the percentages of manganese, they would give a curve, because the percentages of oxygen increase faster than those of manganese decrease. Were the oxygen-line to be developed and added to the diagram, it would seem that the manganese-line should then be straight. Due allowance for the effect of oxygen, therefore, would modify two features of the paper. It would increase the figure for the strength of pure iron from 38,000 to about 45;000 pounds per square inch, and it would straighten out the manganese-curve. The manganese-line in the paper is curved between 0.50 and 0.20 per cent. Above 0.50 per cent. it is straight, which may be ascribed

Jan 1, 1893

By J. E. Hove

The high temperature physical properties of graphite are reviewed and interpreted in the light of present day knowledge of the mechanisms affecting these properties. The thermal and mechanical behaviors only are discussed and, whenever possible, comparisons are made with other refractory materials. Possible further studies are indicated, including some carbide work. AS long as the term high temperature implied only temperatures up to about 1000°C, the materials problems which arose could usually be handled by fairly conventional metal alloy types, such as the Co-Cr-Ni superalloys, for which there exists a great deal of technology. Perhaps this temperature can still be considered an upper limit for normal applications, but it is certainly true that the number of abnormal applications is increasing rapidly. The advent, in recent years, of ram-jet and rocket missiles and of high power nuclear reactor heat sources has raised a host of questions concerning the basic problem of what material to use in the temperature range up to 2000°C and higher. While there are, of course, many metals, in the second and third transition series, which melt at considerably higher temperatures than this, these metals are, at present, pretty well excluded from practical use by other considerations, such as re-crystallization, chemical activity, or excessive plastic deformation. The behavior of metals, from the standpoint of dislocation theory, is just beginning to be understood and thus there is some hope for the future development of very high temperature metals, but the immediate problems would most logically appear to have solutions involving the nonmetals, such as the refractory ceramics and graphite. For this reason, there is presently a great deal of engineering and experimental research being performed on the latter materials, much of this research being exploratory in the sense of gathering new property data. The situation, so far as graphite is concerned, is somewhat more fortunate than with the other refractory solids in the sense that a great deal is already known about its basic properties. This stems both from the fact that the carbon-carbon bond has been of interest to chemists for a long time (and graphite can be considered as a very large aromatic molecule, if desired) and the fact that its properties, both as a function of temperature and of radiation damage, are of critical importance to nuclear reactor designers. It is still true, of course, that such fundamental questions as why graphite remains solid to such a high temperature and why it has such a high thermal conductivity cannot entirely be answered at the present time. It is, nonetheless, meaningful and instructive to consider such problems in the light of existing knowledge. This is what the present paper will attempt to do. Before going on, it may be appropriate to classify graphite and justify its discussion before readers primarily interested in metals. Graphite is comparatively unique among materials in that there is always a property or group of properties which precludes calling it either a metal, a semiconductor, or a ceramic. It has the high electrical and thermal conductivities of a metal, but the artificial, poly-crystalline types show a negative thermal coefficient of electrical resistivity, generally characteristic of semiconductors. On the other hand, semiconductors, by definition, show an ever increasing resistivity as the temperature is lowered, whereas graphite approaches a finite, and, indeed, a rather low resistivity in the region of 10°K and, furthermore, a good single crystal of graphite has a positive temperature coefficient, as for a metal.' On still another hand, its porosity and brittleness at lower temperatures would put graphite in the ceramic class although, unlike most ceramics, it is readily machinable and has a high resistance to thermal shock. All things considered, it is probably more nearly appropriate to call graphite a metal than anything else. Although certainly outstanding in some ways, graphite has its peculiarities and, especially if the reader is unfamiliar with the data, it is probably valuable to review some representative property variations at high temperature. This review is meant to be mainly illustrative and no attempt has been made to be exhaustive. Review of High Temperature Properties At ordinary pressures, graphite does not melt, but sublimes directly into the gaseous phase at about 3700°C. Although the phase equilibrium diagram is still in some doubt, graphite will melt, at a slightly higher temperature, at pressures in excess of about 100 atm. The chief difficulty of using graphite in an oxidizing atmosphere is that the reaction rate becomes quite high at fairly low temperatures. If a threshold oxidation temperature2 is defined as the temperature at which graphite loses 1 pet of its weight in 24 hr, the value in air is 450°, the value in steam is 700°, and the value in carbon dioxide is 900°C. Efforts are presently being made to raise this threshold temperature either by impregnation with a retardant of some type (sodium tung-state and phosphoric acid, for example) or by a suitable metal or oxide coating. It is probably fair to say that, to date, these attempts have not shown any outstanding success in all respects. Most commercial graphites are fabricated by impregnating a carbon flour (say of coke or lampblack particles) with some type of hydrocarbon

Jan 1, 1959

By Charles A. Mitke

Discussion of the paper by CHARLES A. MITKE, presented at the San Francisco meeting, September, 1915, and printed in Bulletin No. 105, September, 1915, pp. 1941 to 1958. GERALD SHERMAN, Bisbee, Ariz.-Mr. Mitke justly might have made much stronger his claim for increase in efficiency of labor due to the introduction of forced ventilation. The product per man shift in stoping in the Gardner division has practically doubled. While it is true that improved methods have been responsible for a great part of this gain, and what is due to better ventilation cannot be definitely known, yet it is also true that the results could not have been obtained in that division as it was in 1912. . The paper discusses the two systems of ventilation in use, exhaust and pressure. In both the object is the same, to take foul air or gas out of the mine by the most direct course and replace it by fresh. In coal mines, the exhaust system is in almost universal use, and since the most advanced work in ventilation has been in that class of mines, it was naturally the first one to be considered. It has the advantage of leaving all adits, shafts, or other openings free for use. Doors are only needed to direct the course of the air, and not to confine it. Its disadvantages appear in case of fire, or if the ground over the mine is much broken by subsidence. The fan must work in gas in the case of a -fire, and may be. damaged or destroyed either by heat or by corrosive gas. At the time of the fire in the Lowell division of the Copper Queen, a small exhaust fan was placed over a ventilating raise, but the vanes and housing were destroyed by sulphurous gases within a few weeks. If the ground above the mined area is much broken, as is frequently the case when the ore deposit is thick vertically, a good deal of air is likely to pass through it, particularly if it is near the surface. Leakage from this source is a loss to the exhaust system by short circuiting, which is exaggerated by a contraction or block in the air course. It serves as an added outlet in the pressure system. This is strikingly shown at the United Verde, where many jets of steam may be seen coming up through the ground above the stoped country on a cold day.

Jan 12, 1915

By O. N. Carlson, S. A. Bradford

Discontinuous yielding in tensile tests was observed in V-O alloys in the temperature ranges of 150° to 175°C and also 350° to 400°C. The magnitude and intensity of the serrations were found to vary considerably with oxygen content. Maxima were observed in tensile and yield strengths and in the strain-hardening coefficient at the higher temperature only. The strain rate sensitivity was observed to be negative between 150° and 400°C. THIS investigation was undertaken to study the effect of oxygen on the tensile properties of iodide vanadium in the temperature range of 25o to 450°C. Brown1 observed an increase in strength between room temperature and 400°C in vanadium metal, and found that oxygen and nitrogen had a rather pronounced effect on the strength and ductility. A maximum in the tensile strength was observed by Rostoker et al.2 near 300oC and by Pugh3 around 450°C for calcium-reduced vanadium. Pugh also found a maximum in the yield strength and in the strain-hardening exponent, and minima in the elongation and strain rate sensitivity at the same temperature. Eustice and Carlson4 reported the appearance of serrations in the stress-strain curves between 140° and 180°C in iodide vanadium containing 600 ppm O. These anomalies in the mechanical properties indicate that strain aging occurs in vanadium, but the impurity or impurities responsible for the above-mentioned effects have not been identified. The phenomenon of strain aging is usually characterized by the return of the yield point after interruption of a strength test. In the temperature range where strain aging occurs, the yield and tensile strengths attain maximum values, elongation and strain rate sensitivity exhibit minima, and discontinuous yielding is generally observed in the stress-strain curve. Cottrell5, 6 has postulated that strain aging is due to the migration of solute atoms to dislocation sites to produce locking after the dislocations have broken free from their impurity atmospheres during the initial yielding. At the strain-aging temperature the process is a dynamic one in which the solute impurity atoms diffuse to the vicinity of the moving disloca- tion producing "locking" which gives rise to maxima in the tensile strength and serrations in the elongation curves. Cottrel17 has noted that discontinuous yielding in iron occurs when the diffusion coefficient of nitrogen, D, and the strain rate, i, are related by D = 10-9 €. EXPERTMENTAL PROCEDURE The vanadium metal employed in this study was prepared by the iodide refining process as described by Carlson and owen.8 A representative analysis of the vanadium used in this investigation was: 150 ppm O, <5 ppm N, <1 ppm H, 150 ppm C, 150 ppm Fe, 70 ppm Cr, <50 ppm Si, 30ppm Cu, 20 ppm Ni, <20 ppm Ca, <20 ppm Mg and <20 ppm Ti. Alloys containing from 200 to 1800 ppm O, all of which lie in the solid solution range of the V-O system, were prepared by arc melting vanadium together with portions of a high-oxygen master alloy. The master alloy was prepared by tamping pure V2O5 into holes drilled in a vanadium ingot and arc melting this five or six times in an inert gas atmosphere, inverting the button between each melting step. The oxygen content of the master alloy was then determined by vacuum fusion analysis. Vanadium containing less than 150 ppm O was prepared in the following manner. A bar of iodide vanadium was deoxidized by sealing it in a tantalum crucible with a few grams of high-purity calcium. This was held at 1100°C for 4 days to allow time for the oxygen to diffuse to the surface and to react with the calcium vapors. The calcium oxide product was later dissolved from the surface of the bar with dilute acetic acid. In this way vanadium containing from 20 to 50 ppm O was prepared. Sample Preparation. The are-melted ingots were cold swaged into 3/16-in. diam rods and these were machined into cylindrical tensile specimens with a reduced section of 1.00-in. length and 0.120-in. diam. The test specimens were annealed for 4 hr at 900°C in a dynamic vacuum of mm of Hg to remove hydrogen from the metal. This recrystal-lization treatment produced a uniformly fine-grained structure with a mean grain size of approximately 0.06-mm diam. The oxygen contents reported in this paper were determined by a vacuum fusion analysis of the tensile specimens after testing. Analyses for other interstitial or metallic impurities showed no significant changes from that of the original material. Tension Tests. Tension tests were performed on a screw-driven tensile machine at a constant cross-head speed of 0.01 in. per min. Tests at elevated temperatures were carried out by heating the

Jan 1, 1962

GEORGE F. COMSTOCK (author&apos;s reply to discussion*).-Mr. Thum&apos;s description of the effects of butt welding and spot welding on the micro-structure of steel are interesting and timely. The speed with which the changes noted by Mr. Thum must take place is indeed remarkable, but the writer has noted a similar very rapid diffusion of carbide in annealing a t a rather high temperature certain samples of soft sheet steel containing massive cementite segregated on a small scale. The massive cementite in such steel can be dissolved and distributed very quickly if the proper temperature is attained. Mr. Thum&apos;s explanation of the structure he found in the spot welds seems entirely reasonable, but the mystery of the decarburized material in the butt weld is one that might well be the subject of further research. The possibility of decarburization by air ,might perhaps be worthy of a little more consideration than he gives it, for the oxides formed would be gaseous on account of the presence of carbon, and hence not visible in the microscope, and the effect of the pressure might be to squeeze the carbon oxides, which would normally form blow-holes, out of the metal or possibly into such small volumes as not to be noticed The removal of carbon by liquation and squeezing into the fin would be an effect similar to the "bleeding" of a steel ingot that is rolled while the center is still liquid, giving a soft low-carbon interior in the finished section while the segregate was removed in cropping the pipe. This effect in Mr. Thum&apos;s butt welds could, however, only be obtained if the weld was heated to near the melting point of the steel, and if the carbon was considerably segregated in the bars at the start, for the first effect of the high temperature would be to promote diffusion rather than the contrary segregation and Equation. It is gratifying to learn from Dr. Ruder&apos;s remarks that his researches have resulted in no disagreement with the few points brought out by the writer&apos;s experiments. In addition to the three forms in which nitrogen may occur in iron that he mentions, it would seem that a fourth form is often found; This is apparently a eutectoid, like pearlite, and sometimes almost as coarse as the massive cementite seen in soft steel sheets that have been annealed for a long time. One of the things needed in the metallographic study of steel is an etching reagent that will distinguish definitely between nitride in this form and the more common pearlite or cementite.

Jan 6, 1919

D. EPPELSHEIMER, * Middletown, Ohio.-The housing of employees has so many and so varied aspects that in order to reach even an approximately correct solution it is necessary to have in mind a few fundamental principles; but it is not possible as yet to write these housing principles in the clear and correct form that is possible with many of our natural laws. Manifestly, the problem depends first on the kind of people it is necessary to house. What is suitable for the Southern unattached negro is not suitable for the married skilled American. The influx of colored labor has affected quite a number of what were satisfactorily housed communities. The second important factor is the relative proportion of the number of employees to the total employable population of the community in which the industry is located. The employer of a hundred men in. a large city has little responsibility in the matter of housing his employees. If he employs 75 per cent. of the employable population in a community of 27,000, as is the case of the company with which the writer is connected, it means a large responsibility. In the establishment of an entirely new plant in a more or less isolated place, the responsibility becomes greater. As engineers, we design and write the specifications for the machinery to accomplish a definite purpose, and proceed to house it, provide the necessary buildings with their accessories in the way of cranes, or heating systems, or sprinkling systems, as the case may be. There is no reason why the operating force should not be built up in very much the same way: design the organization, write its specifications so that the employment department can secure the proper men, and then house that organization with just as much thought and care as is given the plant. In the plant, the various machines will work along certain definite lines and accomplish certain results; but even if we start with the proper organization it takes considerable time to get that organization working together. One of the most important elements to this end is the proper housing of the organization. A man usually spends more time at home than at work. Proper surroundings and a comfortable, convenient house of good appearance exercise an influence that cannot be denied, and an employee situated in such surroundings is far more inclined to follow the policies of his employer and take an active part in furthering them

Jan 5, 1919

By Lawrence Veiller, D. Eppelsheimer

D. Eppelsheimer, * Middletown, Ohio.—The housing of employees has so many and so varied aspects that in order to reach even an approximately correct solution it is necessary to have in mind a few fundamental principles; but it is not possible as yet to write these housing principles in the clear and correct form that is possible with many of our natural laws. Manifestly, the problem depends first on the kind of people it is necessary to house. What is suitable for the Southern unattached negro is not suitable for the married skilled American. The influx of colored labor has affected quite a number of what were satisfactorily housed communities. The second important factor is the relative proportion of the number of employees to the total employable population of the community in which the industry is located. The employer of a hundred men in a large city has little responsibility in the matter of housing his employees. If he employs 75 per cent. of the employable population in a community of 27,000, as is the case of the company with which the writer is connected, it means a large responsibility. In the establishment of an entirely new plant in a more or less isolated place, the responsibility becomes greater. As engineers, we design and write the specifications for the machinery to accomplish a definite purpose, and proceed to house it, provide the necessary buildings with their accessories in the way of cranes, or heating systems, or sprinkling systems, as the case may be. There is no reason why the operating force should not be built up in very much the same way: design the organization, write its specifications so that the employment department can secure the proper men, and then house that organization with just as much thought and care as is given the plant. In the plant, the various machines will work along certain definite lines and accomplish certain results; but even if we start with the proper organization it takes considerable time to get that organization working together. One of the most important elements to this end is the proper housing of the organization. A man usually spends more time at home than at work. Proper surroundings and a comfortable, convenient house of good appearance exercise an influence that cannot be denied, and an employee situated in such surroundings is far more inclined to follow the policies of his employer and take an active part in furthering them than one dissatisfied with his home and surroundings, which feeling

Jan 1, 1919

By Charles S. Barrett, Robert F. Mehl, Dana W. Smith

The Widmanstatten figures found in the steels have been long recognized and in some aspects carefully studied,&apos; especially as they occur in cast hypoeutectoid alloys. Aside from the practical importance of the structures obtained in the steels by various heat treatments, a study of the characteristics of these figures is interesting because of the rich opportunity the system affords to obtain new data on the mechanism of segregation from solid solutions. This opportunity is twofold: first, by changing composition within the austenite range the proeutectoid precipitate may be changed from that of ferrite to that of cementite, thus offering the same opportunity for changing the type of precipitate while maintaining the same basic lattice as that afforded by the Cu-Zn alloys;2 and second, the eutectoid inversion leads upon drastic quenching to the formation of martensite, a Widman-statten figure of unique interest from the crystallographic viewpoint, particularly in comparison with those formed on slow cooling.3 We have, therefore, two types of structure to study: that formed on slow cooling of hypoeutectoid and hypereutectoid alloys, and that formed on quenching hypoeutectoid, eutectoid, and hypereutectoid alloys. For each of these types of structure we require the crystallographic plane in the mother austenite along which the precipitate forms (we shall see that the precipitates in these alloys are invariably platelike in form), and also the orientation of the precipitate upon this plane. Some of these

Jan 1, 1933

By J. H. Slater

THERE is nothing particularly new about the use of sinter in a blast-furnace burden. For many years flue dust has been sintered at the various blast-furnace plants to put it in a form that could be recharged to the furnace with some assurance that it would stay in the second time. This paper is not a compilation of scientific data but only an attempt to give our experience with sinter. There are some unexplained discrepancies in the tests given here, such as the flue dust produced and iron tonnages, but the results given are the results that were obtained. Sinter is not the cure-all for blast-furnace problems. A good coke is still the most important factor in good furnace operation. However, good sinter is a big help. As flue dust is produced under varying operating conditions and fluctuates greatly in carbon content, it is difficult to produce from flue dust alone a uniform sinter, which will give satisfactory blast-furnace results. Sinter made from flue dust alone will change in character with every carbon variation. Almost invariably flue dust con-tains carbon in excess of the amount necessary to make good sinter, and this excess must be burned out, This, of course, necessitates reduction of the speed of the sintering machine and thus a decrease in tonnage, An alternative is to dilute with a carbon-free material to use up the excess carbon. High-carbon material when sintered results in a very dense, undesirable prod-uct, since the excess heat melts the charge into a hard, nonporous mass, and tends to form refractory silicates.

Jan 1, 1940

By F. C. Newton

REFINERS of lead by the Parkes process have always been solicitous of recovering the zinc used in the desilverization, and justly so, as the loss in zinc constitutes one of the heavy costs in this method of refining. Part of this loss is due to the absorption of zinc by lead, and in the present state of knowledge is not recoverable as metallic zinc. The remainder of the zinc, which finds its way into the precious-metal-bearing crust, is recoverable and naturally engages the operators&apos; most exacting attention. Careful elimination of the impurities in base bullion has enabled the refiner to produce a zinc crust better adapted to retorting, which reflects favorably in the zinc recovery; and to produce a richer crust, thereby lowering the zincking cost, as the increased efficiency of the zinc results in less of it being in circulation. It is obvious that if the ratio of concentration be increased, a lessening of the amount of crust formed will ensue, throwing less work on the retorts and diminishing the amount of retort metal sent to the cupels, thus making an actual money saving in all these operations. In the effort to obtain a rich crust, the metallurgist has increased the heat to a considerable degree, upon the assumption that at the higher temperature the zinc-silver alloy could be squeezed free from the adhering lead. A further possibility for improvement suggested itself in the freezing-point curve of Prof. H. C. Carpenter, upon zinc and silver. Study of this curve disclosed the existence of a definite chemical compound, . Zn3Ag2, with a freezing point of 665° C., a promising compound for practical application.

Jan 2, 1915

This discussion of the paper of Chester W. Washburne should have been printed following the remarks of H. A. Wheeler, in Bulletin No. 100, April, 1915, pp. 835 and 836, but was inadvertently omitted. ROSWELL H. JOHNSON:-There is one reason why the hydrostatic interpretation of gas pressure is not wholly acceptable. As we go clown in the sands we seem to get excesses of gas. Particularly in this field it becomes excessive in quantity relative to the amount of water in the sand. If this holds in other fields as well it must mean that there has been an ascension of water, because these sedimentaries when laid down, were filled with connate water. If we do get an ascension of connate water, produced by some such phenomena as its expansion by heat or by the formation of new gas by pressure upon organic materials at great depth, we can hardly expect the pressure to be controlled merely hydrostatically. * In reply to Mr. Wheeler&apos;s inquiry as to gas wells with pressure higher than hydrostatic pressure, I would cite the original wells given by Orton on which he based the hydrostatic theory. He used in his calculation a head of 600 ft. above tide, assuming the outcrop of the Manitoulin Islands to be in Lake Superior, whereas the Trenton does not outcrop at Lake Superior. The Manitoulin Islands are in Lake Huron, the level of which is 580 ft. above tide. No allowance is made for the lower density of the fresher water near the outcrop, the weight taken for the whole column being the water of high density found at the wells.

Jan 5, 1915

By David L. Holt, Walter A. Backofen, Anwar-ul Karirn

ANNEALING the binary alloy, Mg-0.5 wt pct Zr in a hydrogen atmosphere results in extensive precipitation of zirconium hydride. The morphology of these precipitates has already been investigated.lm3 Squires, Weiner, and phillips4 found, following creep testing of the hydrided alloy at 450" and 500°C, that hydride denuded zones formed along grain boundaries that were aligned approximately normal to the tensile axis. Zone formation was attributed to diffusional creep by magnesium transport down the prevailing stress gradients.4&apos;5 Recently, electron microprobe analysis by Karim, Holt, and Backofen6 showed the zones indeed to be zirconium-free and furthermore it was shown that in compression, zones formed along boundaries approximately parallel to the stress axis. Thus it was confirmed that the zones are formed by diffusional creep. Typical zone-formation is shown in Fig. 1. Karim, Holt, and Backofen also measured the con- tribution to the total strain, from diffusional flow, slip creep, and grain boundary shear: results showed that diffusional strain tends to saturate with increasing imposed strain, while grain boundary shear eventually becomes the dominant deformation mode. It was suggested in explanation that the precipitate-denuded zones are soft and easily sheared, such deformation contributing to the grain boundary shear measurement. A point to be emphasized is that the Mg-0.5 Zr alloy was not superplastic for the index of strain rate sensitivity of flow stress, m = a log log 6 was only 0.25. It was recognized that diffusional creep in a poly crystalline aggregate must be accompanied by boundary shearing.&apos; The suggestion was that the non Newtonian-viscous character of diffusional creep in the Mg-0.5 wt pct Zr alloy is due to resistance to sliding of boundaries lying approximately parallel to the tensile axis.= The work described in the present note should be seen against the above background for it represents initial efforts to observe in a similar way diffusional creep in a superplastic alloy. Previous work with the ternary-alloy Mg-6 Zn-0.5 Zr, pellet extruded, showed it to be superplastic however it does not contain resolvable precipitates to act as internal markers for diffusional creep. Also the fine grain size of the alloy (0.5 p) made conventional metallography rather difficult. Solubility relationships in the Mg-Zn-Zr system are not well known, however making reasonable guesses about the probable phase diagram of the ternary, Mg-Zn-Zr, various heat treatments were attempted to produce hydride precipitation. Finally a 16-hr anneal at 495&apos; in hydrogen was found to pro-

Jan 1, 1970