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By Vsevolod Krivobok

THE re-crystallization of metals has been the subject of much scientific investigation, some of which has resulted in a better understanding of this extremely important and interesting phenomenon. Unfortunately, while many have propounded theories of re-crystallization, but a few have presented experimental evidence as to how it takes place. If this can be determined the question, why re-crystallization occurs, may be answered more definitely. Re-crystallization in single phase metals consists of a complete rearrangement and re-sizing of the grains, of which the structure is composed, while the type of structure remains the same. That is to say, if the structure before re-crystallization is composed of a number of polyhedral grains of different shape and size, a particular spot after re-crystallization will be seen to consist of grains in no way different from the original except in size and shape. The re-crystallized grains may be smaller or larger, depending on the treatment received; and, while the re-crystallization may be brought about by means of heat treatment only in passing through a critical range, yet it is common knowledge that single phase metals subjected to cold working are possessed of a tendency toward re-crystallization, even if the heating does not reach critical range. The study of re-crystallization would, of course, be much easier if we had single crystals of any metal as the original material with which to study the phenomenon of re-crystallization, since it would permit the observation of structural changes at what amounts to enormous magnification, by changing the scale of the specimen. In metals of more normal grain size the crystal boundaries introduce complications, but the process, it may be assumed, is essentially the same. Such an opportunity

Jan 2, 1926

By Craig R. Barreft, Oleg D. Sherby

The steady-state creep characteristics of pure polycrystalline copper were studied in the temperature range 400" to 950°C and in the stress range 400 to 7000 psi. Tests were conducted in dry deoxidized hydrogen and all specimens exhibited high ductility before fracture. Two activation energies for creep were established as a function of temperature. Above about T/T, = 0.65, the activation energy for creep was 48,000 cal per mole whereas between 0.5 and 0.65 T, it was 28,000 cal per mole. The observed temperature dependence of the activation energy for creep follows the same trend as exhibited by the self-diffusion coefficient of copper in copper single crystals and silver in silver single crystals. It is therefore believed that the rate-cmtrolling mechanism in creep of copper in the stress and temperature range studied is diffusion-dependent and is probably associated with a dislocation-climb process. The low activation-energy region is attributed to enhanced volume difFusion from the presence of dislocations which act as short-circuit paths for diffusion. THERE is extensive experimental evidence1,2 that the activation energy for creep, Q,, for pure poly-crystalline metals tested at temperatures above one half the absolute melting temperature (0.5 Tm) is a constant and equal to the activation energy for volume self-diffusion, Qsd This equality is generally interpreted as meaning that creep in this temperature range is controlled by a dislocation-climb process. The existence of high-temperature creep activation energies not equal to the respective self-diffusion values has been suggested both theoretically3"5 and experimentally.6-8 Two examples of apparent nonequality between Q, and Qsd have been reported for the cases of silver7 and copper,' where activation energies for creep much lower than those for self-diffusion persist to rela- tively high temperatures (up to 0.6 T,). These observations suggest that dislocation climb may not be the only important process in the high-temperature deformation of these metals. That dislocation climb does indeed occur relatively slowly in these two metals due to their low stacking-fault energy has been suggested by many investigators.9-10 Although the creep behavior of copper has been studied extensively at low temperatures, the high-temperature activation energy for creep is not well-defined. The data of Feltham and Meakin8 indicated that Q, is temperature-dependent above one half the melting temperature, equaling a value of -30,000 cal per mole at temperatures up to 550°C and increasing to a value of -49,000 cal per mole at 700°C. No data has been reported above 700°C. The value of 49,000 cal per mole is very near the value of Qsd for copper reported by Kuper et al." as 47,100 cal per mole. In view of the lack of high-temperature creep data and the apparent temperature dependence of Q, for copper the present investigation was undertaken to determine the value of Q, over the temperature range of 400" to 950°C. It was hoped that such a study would clearly document the temperature dependence of Q, and yield significant information as to the nature of the rate-controlling creep mechanisms. MATERIALS AND PROCEDURES The material used in this investigation was high-purity OFHC copper. After rolling and recrystal-lization treatments spectrographic and chemical analyses showed only 0.0008 pct Ag, 0.0002 pctCa, 0.0002 pct H2, and 0.002 pct O2 as trace impurities indicating a purity of greater then 99.995 pct. Specimens were machined from cold-rolled sheet and the gage sections polished with 2/0 emery paper prior to annealing treatments. Annealing was done in both vacuum and dry deoxidized hydrogen atmospheres. No variation in creep strength was found as a result of the different annealing atmospheres. The final annealing temperature was either 700°, 800°, or 1000°C depending on the temperature range to be studied. These treatments resulted in average grain diameters of 0.03, 0.4, and 1.0 mm, respectively. The precise mechanical-thermal history of these

Jan 1, 1964

By Nicholas J. Grant, A. W. Mullendore, Paul Predecki

The Duwez technique of splat cooling in which a molten droplet of metal is accelerated and made to impact on a cold, highly conducting substrate was investigated.- An apparatus for producing "splat" was constructed employing an explosive powder charge to accelerate the molten metal. Transport of the molten metal just prior to impact with the substrate was studied by means of high-speed photography. The molten particles are small spherical droplets from about 1 to 50 µ diameter. The average cooling rates for aluminum, silver, and a gold alloy splatted on nickel substrates at room temperature were determined experimentally and were found to vary from 18 to 5 x 10' C per sec. The heat-transfer coeficients for pure aluminum and pure silver splats cooled on nickel substrates at room temperature were found to be 2.7 to 6.8 and 13.6 to 54.2 cal per sec sq cm 'C (2 to 5 x 104 and 1 to 4 x 18 Btu per hr sq ft OF), respectively. Solidification rates in pure aluminum and silver splats were calculated. "SPLAT cooling" is a term describing a technique for extremely rapid freezing and cooling of molten metals and alloys to room temperature or below. The technique was developed by Duwez et al.' in 1960, and after refinement2 consisted in transferring a few tenths of a gram of molten metal to near sonic velocity to strike a suitably placed cold copper surface. Upon impact, the metal spread into a thin nonuniform film called a splat, about 10-4 cm thick. The splat particles produced in this manner were thin enough in some areas to be suitable for transmission electron microscopy, without further treatment, and, together with X-ray data, yielded a variety of structures which would be classified as follows: 1) supersaturated solid solutions (increase in solubility limit), 2) metastable crystalline stoichiometric and non-stoichiometric intermediate phases ( in Au-20.5 at. pct Si and in Au-14 at. pct Sb, respectively), 3) amorphous alloys, 4) retained high-temperature phases, 5) alloys having equilibrium phases present, but with unusual, markedly altered structures. The crystalline phases present in splats were usually extremely fine-grained and had low dislocation densities. Present interest in splat cooling centers around a study of the unusual structures produced by the technique, their contribution to alloy theory, and the possibility of the development of new or unusual properties. In addition, the technique is being examined for the production of bulk quantities of new high-strength alloys for low- and high-temperature use. Although a number of alloy systems have already been investigated by the technique, relatively little is known about the mechanism of splat formation and the physical conditions encountered by the metal during solidification and cooling. The purpose of this work was: 1) to determine the velocity, shape, and size of the molten metal droplets just prior to impact with the cold substrate; 2) to try to estimate or measure solidification rates, heat-transfer coefficients, and cooling rates in splats. EXPERIMENTAL TECHNIQUE Splatting Apparatus and Procedure. An apparatus similar to the type originated by Duwez et a1.,2 but employing an explosive charge to accelerate the molten metal, was used. A "Ramset" fastening tool (a gun normally used for driving studs into concrete, steel, and so forth) was mounted vertically above a resistance-heated graphite crucible as shown schematically in Fig. 1. A splat product was produced by melting a few tenths of a gram of metal at the position shown in Fig. 1, and then exploding a powder charge in the breach. The shock wave thus generated traveled down the barrel into the furnace, ejecting the molten metal through the 0.06-in.-diameter hole at the bottom of the crucible. The ejected metal was impacted on a high-conductivity metallic substrate where it formed a splat. High-Speed silhouette Photography. In order to investigate the size and shape of the ejected, molten metal just prior to impact with the cold substrate, high-speed silhouette photographs were taken, and are shown in Figs. 2 and 3. These photographs were obtained with the aid of an Edger-ton, Germeshausen, and Grier microflash unit and a submicrosecond flash drive equipped with a variable time delay. Two types of triggers were

Jan 1, 1965

By E. G. Leonardon, C. Schlumberger, M. Schlumberger

Last year the authors presented a paper that discussed the various electrical measurements they perform in drill holes, which they name "electrical coring."' The object of the present paper is to give a brief account of the points of scientific interest that have been elucidated by further field work and laboratory research, as well as the economic results that have been attained recently. The practical examples given in this paper are drawn, for the most part, from the field work performed in Russian oil fields during the years 1931 and 1932. This is due to the fact that, thanks to the comprehensive cooperation of the Russian geologists and scientists, the authors are allowed to make public a large amount of recant information. In other countries in which the authors are engaged in similar work, the competition between private companies makes it imperative, for a considerable lapse of time, to avoid publication of the results obtained. The following points will be discussed successively, under separate headings: 1. Electrochemical phenomena in drill holes. 2. Stratigraphic correlations and tectonic studies. 3. Relations' between the productivity of oil horizons and their electrical resistivity. 4. Location of coal seams. 5. Summary and conclusions. Electrochemical Phenomena in Drill Holes Technical Publication 462l described the author's discovery concerning the existence of important differences of potential spontaneously gener-

Jan 1, 1934

By R. E. Sabaski

Total grinding mill system life is dependent upon the original selections and specifications of its components: the mill, its drive, drive motor, motor control, and power system. This paper discusses the complex considerations involved and the critical decisions which must be made by the buyer, the mill manufacturer, and by the gear vendor during the proposal and ordering stages. Interrelations between the mill manufacturer and the gear vendor, application of ACMA standards, how drive standards and specifications are refined through steady-state and computer-simulated torsional analyses are included, along with correlational field testing, as demands for larger sizes challenge the current state of the art.

Jan 1, 1984

By R. M. Waterstrat

X-ray diffraction and metallographic examination of binary Mn-rich alloys with Ti revealed the presence of intermediate phases in this system. A binary R phase has been identified and also a phase having an a-Mn type structure. The X-ray pattern of the phase TiMn3 is presented and a tentative phase diagram for the Mn-rich portion of this binary system has been constndcted. MANGANESE-rich alloys with titanium have been subjected to thermal analysis at temperatures down to 1100°C by Hellawell and Hume-Rothery.1 Their results indicate the existence of an intermediate phase TiMn3 in this binary system. This phase appears to coexist with the Laves phase TiMn2, and with terminal solid solutions based on the allotropes of manganese, at least down to 1100°C. The above investigators did not attempt to determine the crystal structure of this phase, however. Since, by analogy to the binary systems Mn-V and Mn-Cr3 one might expect to find a phase in this region of the diagram, it seemed desirable to obtain X-ray diffraction patterns of alloys in the concentration range in question, in order to ascertain whether the sigma phase or related structures occur. EXPERIMENTAL PROCEDURES Alloys were prepared by arc-melting electrolytic manganese and iodide titanium in a water-cooled copper crucible under a helium atmosphere. Excess manganese was added to each melt in order to allow for losses incurred during melting. The alloys were then wrapped in molybdenum foil and sealed in evacuated quartz tubes for annealing at various temperatures, as shown in Table I, followed by quenching in cold water. Although the inside of the tubes showed evidence for some loss of manganese from the specimen during annealing, there was no evidence of any reaction between the specimen and either the molybdenum foil or the quartz tube at these temperatures. It was later found that the manganese loss was considerably reduced by annealing these alloys in sealed quartz tubes containing one atmosphere of purified argon. As an added precaution the surface of each specimen was ground off before crushing the alloys to -270 mesh powder, using a hardened steel mortar and pestle. X-ray powder patterns were obtained using either FeKa or CrKa radiation in an asymmetrical focusing camera, which gave excellent dispersion of the closely spaced lines. Pictures were also obtained using a Debye camera of 5-cm radius which provided data in the angular region not covered by the focusing camera. The alloy specimens were polished and examined metallographically, using an etchant consisting of 60 pct glycerine, 20 pct nitric acid, and 20 pct hydrofluoric acid. The 10-g buttons were in each case broken in half and found to be well-melted and free of any gross segregation. One half of certain alloy buttons was submitted to chemical analysis in the "as-cast" condition. No appreciable change in composition seemed to occur during annealing . RESULTS The X-ray pattern of alloy Ti1.17Mn0.83 was found to agree well with that of the ternary R phase which was first found in the Mo-Cr-Co system,' and re-

Jan 1, 1962

By Nichols J. Grant, Bill C. Geissen

In low temperature phase diagrams, liquidus curves below about 1500°C are relatively easily established, e.g., by thermal analysis or separation of coexisting solid and liquid phases, followed by chemical analysis. Experimental difficulties increase considerably at higher temperatures and in systems involving more reactive metals. Although there are now thermocouples available for use from 1600" to 2400°c, as summarized by Caldwell,' the need for frequent calibration, aging, and contamination problems, and unavailability of suitable protection tubes has sharply limited their use at higher temperatures. Many of the high melt- ing metals are found to react with refractory oxides. TO avoid such problems, a frequently used procedure is the diffusion and saturation method, as described by Spedding et a1.' for the system La-C. This technique involves the annealing of one metal or a suitable alloy in a crucible of the other element at a temperature above the melting point, followed by chemical analysis of the center of the melt, after equilibrium is established. Further, if an alloy system is to be investigated employing the electron microbeam probe, and calibration charts have been established, it may be possible to measure the alloy concentration at the center of a cored as-cast structure, and to conclude from this points on the liquidus curve in a manner similar to the one to be described. It is known that in phases with a broad homogeneity range the rapidly cooled, cored, as-cast structure of an alloy presents concentrations having different lattice constants; this spread of lattice constant values contributes to the broadened lines of a powder pattern for the as-cast condition. The region of the crystal which is first to solidify will then correspond to the edge of the lines if the change of the lattice parameters with concentration is monotonous. In the course of the determination of the Ta-Tr phase diagram,3 it became evident that such behavior made it possible to construct the

Jan 1, 1963

MINNEAPOLIS-HONEYWELL Regulator Co., and Trans-Weigh Co., have come up with a conveyor belt that thinks. The belt weighs material and then figures out the tons-per-hour that it carries. And you can't fool it by adding or subtracting material along the way. It makes allowances for any additional material as well as for any loss. The belt rides along a set of rollers. The force exerted on the rollers is transferred to a gage. The weight of the belt is subtracted electrically. Final measurements are fed into an electronic recorder which indicates the flow at the moment and the total amount which has been carried by the belt.

Jan 1, 1952

By W. F. Carew, F. A. Crossley

The stress for rupture in 500 hr at 1000° F has been reported to be about 13,000 psi higher for Widmanstitten than for equiaxed microstructures for the Ti-7A1-3Mo alloy.1,2 Also, limited data indicated Widmanstatten and equiaxed micro-structures to have approximately the same creep resistance at 1000°F.' Recently, data have been obtained which show Widmanstatten structures to be significantly more creep resistant than equiaxed structures at 1000°F, see Fig. 1. These data represent several ingots and several heat treatments of the solution treat and age type. The thermal history and tensile properties corresponding to the creep data are given in Table I. The creep data were taken from creep-rupture tests. The associ- ated rupture data are given in Table 11. It may be noted that total creep deformations are considerably greater for equiaxed structures. Previous evaluations of stability indicated that all of the structures tested are stable with respect to exposure to stress at elevated temperature.1,2 For a minimum creep rate of 10-4 in. per in. per hr the difference in stress levels is indicated to be about 17,000 psi. Holden,et found an irreversible contraction upon heating three a-ß titanium alloys in the equiaxed condition above their ß-transus temperatures. The alloys were: Ti-6Al-4V, Ti-155 A (5Al-1.3Cr-1.5Fe-1.2Mo), and C-130 AM (44-4Mn). The net contractions in length between the original equiaxed and the final Widmanstatten structures measured at room temperature were: 0.4, 0.4, and 0.7 pct, respectively. The greater creep and rupture resistance of the WidmanstStten structure of the Ti-7Al-3Mo alloy may be associated with the phenomenon

Jan 1, 1959

By W. Shockley

THIS lecture can best begin with a statement of the chief conclusion: The metallurgical industry will find profit in supporting fundamental research on dislocations. This support should be done both in their own laboratories and in universities. My lecture consists of an exposition of the basis for this conclusion. The experience on which I base it is drawn largely from two fields in solid state physics—one field is transistor electronics and the other is dislocation theory. At present the relationship of solid state physics to technology is different in these two fields. In electronics without question, the physics has led the technology. In metallurgy, on the other hand, the technology in the form of metallurgical art is far ahead of the fundamental science. In transistor electronics, physics has suggested and can still suggest previously unachieved combinations of matter that will have new and useful properties; that is, the physicist can make specific predictions. The physicist can also have some confidence that the predicted devices will actually come into existence in a matter of months or years and that they will live up to the predictions. In metallurgy, the physicist cannot to a comparable degree make predictions and have the same hope that they will lead to something new and valuable. There are a number of reasons for this difference. The first is simply historical. Transistor physics is young. It may be regarded as dating from the announcement of the transistor, in which case it is about four years old, or from the first real control of semiconductors as materials (this was accomplished largely by metallurgists, by the way) in which case it is about ten years old. Metallurgical art, on the other hand, is thousands of years old. There is no doubt that the advance of this art has been and will be hastened by a good fundamental understanding of the quantum theory of atomic phenomena. It, is too much to expect, however, that theory will soon catch up with the lead that practice has gained in a thousand years, and that theory will then point out specific pathways to better materials. It seems more probable that modern atomic theory will serve to interpret and organize information much as thermodynamics has done through phase diagrams. In this lecture, I shall emphasize an important feature common to both solid state electronics and to metallurgy. This common feature is the harmonizing principle that justifies discussing electronics and metallurgy as related topics in solid state physics. In both cases the important properties of the materials arise from imperfections. By imper- fections I mean deviations of the materials from perfect single crystals. The imperfections may be of many forms. From the point of view of utility they may be either good or bad, and a given type may be good or bad depending on circumstances. The technical material of my lecture will be divided into two parts. The first will be chiefly concerned with four types of imperfections in germanium crystals. The control of these imperfections makes possible the fabrication of useful electronic devices. A good example of such control is the junction transistor, which I shall discuss from this viewpoint later. The junction transistor, as some of you may have heard, can be used as an amplifier of electrical signals and in a number of respects surpasses what has hitherto been achieved with vacuum tubes. The second part of my technical material will be concerned with dislocations. For about fifteen years the theoretical physicist has had dislocations in mind as the most important kind of imperfection in metals. He has, however, until recently had experimental material of a highly speculative nature to back up his assertions. I am fortunate in the timing of this lecture to be able to describe some recent results that put dislocations on a far more definite basis than has been the case in the past. In fact there are now some experiments which reveal the characteristic properties of dislocations almost as clearly as experiments in transistor physics reveal the properties of holes and electrons, properties that I shall soon describe. It is this advance in the status of dislocations that emboldened me to make my initial assertion that the metallurgical industry will profit from supporting fundamental research on dislocations. Transistor Electronics In order to discuss imperfections in semiconductors, it is necessary to visualize a reference condition that may be regarded as perfect. In the cases of silicon and germanium, which find application in transistor electronics,' the perfect structure is the diamond structure shown in Fig. I. In this structure, each atom is surrounded by four neighbors with which it forms four covalent or electron-pair bonds. These bonds use all of the four valence electrons possessed by each of the silicon or germanium atoms. The electronic structure of the crystal is thus complete and perfect. A crystal of silicon or germanium with a perfect electron-pair bond structure would be an insulator, In order for electrical conduction to occur, it is necessary for imperfections to arise in the electronic structure. In this lecture, I shall discuss four possible imperfections whose symbols and relationships are indicated in Table I. We shall consider first, as an example, a crystal of silicon containing an arsenic atom as an impurity.

Jan 1, 1953

By M. Van Siclen

THE outstanding fact in connection with dust disease in the United States at present is the growing recognition of its seriousness by state officials and by the more progressive operators of mining, metallurgical and allied industrial plants. The same may perhaps be said of labor in some of its better organized centers, but the average independent non-union workman continues, as of yore, to suffer the toll of disability and even of death from dust inhalation without realization of the source of his ill-being. Progress in the betterment of the handling of sufferers from dust disease and of the conditions creating dust hazards in mining and allied industries is pursuing a course similar to that of the now widespread campaign against accidents, in which the risk is more obvious, more severe, and was naturally recognized. sooner. The coming on of dust disease is generally relatively slow and its immediate effects not infre-quently masked by or attributed to other diseases. Marked exceptions to this general rule have occurred in districts where the dust is particularly pernicious, such as the Rand and Joplin; yet such exceptions, unhappy in themselves, opened the eyes of medical men, and of those in other localities charged with the responsibility for the welfare of industry, to the much more widespread if less spectacular hazard existing from the inhalation of dust in all rock-excavating operations and all industrial operations creating inorganic dust, whether it be crushing and grinding, sand-blast-ing, granite-cutting, or what not. Advancement to date in the United States in prevention and treat-ment has been slow, yet the record shows that quantitative methods for determining the degree of hazard and means for decreasing it were being developed as far back as 25 years ago; and that more rapid progress may be looked for from now on. In 1908, in this country, F. L Hoffman?(1) discussed the mortality from consumption in dusty trades, especially brass foundries; and in 1913 E. R. Hayhurst(2) described the effects of inhalation

Jan 1, 1933

By M. Van Siclen

THE outstanding fact in connection with dust disease in the United States at present is the growing recognition of its seriousness by state officials and by the more progressive operators of mining, metallurgical and allied industrial plants. The same may perhaps be said of labor in some of its better organized centers, but the average independent non-union workman continues, as of yore, to suffer the toll of disability and even of death from dust inhalation without realization of the source of his ill-being. Progress in the betterment of the handling of sufferers from dust disease and of the conditions creating dust hazards in mining and allied industries is pursuing a course similar to that of the now widespread campaign against accidents, in which the risk is more obvious, more severe, and was naturally recognized sooner. The coming on of dust disease is generally relatively slow and its immediate effects not infre¬quently masked by or attributed to other diseases. Marked exceptions to this general rule have occurred in districts where the dust is particularly pernicious, such as the Rand and Joplin; yet such exceptions, unhappy in themselves, opened the eyes of medical men, and of those in other localities charged with the responsibility for the welfare of industry, to the much more widespread if less spectacular hazard. existing from the inhalation of dust in all rock-excavating operations and all industrial operations creating inorganic dust, whether it be crushing and grinding, sand-blasting, granite-cutting, or what not. Advancement to date in the United States in prevention and treatment has been slow, yet the record shows that quantitative methods for determining the degree of hazard and means for decreasing it were being developed as far back as 25 years ago; and that more rapid progress may be looked for from now on. In 1908, in this country; F. L Hoffman?(1) discussed the mortality from consumption in dusty trades, especially brass foundries; and in 1913 E. R. Hayhurst(2) described the effects of inhalation

Jan 1, 1933

By T. L. McCall

THE late Walter Herd1 in 1929 gave a full description of past and present conditions in No. 2 mine, Springhill, Nova Scotia, developed theories regarding the cause of these bumps and made certain suggestions regarding possible methods of future development. Recapitulating briefly from Mr. Herd's paper, the seam is bituminous coal, averages 9 ft. in thickness and has a well defined parting containing fusain about 14 in. from the roof. This roof coal is somewhat stronger than the rest of the seam and has a tendency to cling to the roof. The pitch of the seam where it is now being worked is about 20°. The first manifestations of bumps began when the room and pillar workings had reached a depth of cover of 1900 ft. and under continuously increasing depth of cover these bumps increased to such an extent, both in number and severity, that in the year 1924 it became apparent that some change in the system of extraction was necessary. After closely studying all the factors involved and benefiting largely by valuable out-side advice obtained by the Provincial Department of Mines of Nova Scotia,2 the system of working was changed from room and pillar to longwall retreating. Mr. Herd's paper described in detail three remarkable bumps in the year 1928 in April, July and October that affected the 5700-ft. and 5900-ft. East levels, the last bump being so severe both in intensity and in extent of damage done that this district was abandoned. The longwall workings to the west of the slope had been stopped in the year 1926 owing to an inbreak of water, coming from the flooded waste of No. 3 seam lying some 400 ft. vertically overhead. This inflow was not excessive, but a large quantity of water being impounded in the old workings it was considered advisable to take the prudent course and not incur the risk of possibly increasing the flow by further working. This district has remained idle ever since.

Jan 1, 1934

By G. Chesneau

Two great discoveries of this century have diminished the dangers of fiery coal-mines,—the sifety-lamp, conceived in 1815 by Sir Humphrey Davy and successively improved by many engineers, such as Clanny, Marsaut, Mueseler, Fumat, etc., and safety-explosives, the appearance of which is comparatively recent, hut which, thanks to the persevering labors of several technical commissions (especially the French commission on explosives), and of the manufacturers and experimental users of these powders, appear likely to play, in the protection of the miner, a part as important as that of the safetylamp itself. Brit while it is true that by the use of a safety-lamp of approved form, and the exclusive employment, with all prescribed precautions, of these new explosives, complete security should be assured, even in highly fiery atmospheres, experience has shown that the imprudence of workmen, or the bad condition of a lamp, may nullify these protective means, so that it ought to be the constant care of the engineers of fiery mines to dilute the fire-damp by good ventilation so far as to maintain always and in all parts of a mine a proportion of this gas below the lower limit of explosiveness belonging to a mixture of air and methane. Good ventilation still remains the best preventive of explosions from fire-damp, and since, even with a rational and well-controlled mine-ventilation, the volumes of air traversing galleries and rooms are liable to vary within wide limits by reason of open doors, falls of rock, or other accidental causes, it follows that but a few thousandths of fire-damp should be left in the normal atmosphere of the mine-workings, so that a considerable

Jan 1, 1894

By E. W. Engle

Fox several years the Fansteel Products Co. has been engaged in the production and development of various of the rarer metals. It is at present engaged in the commercial production of tantalum, tungsten, and molybdenum in a very high state of purity. The information contained in this paper is partly a general compilation from various sources and partly information obtained as a result of recent years of work in the laboratory of this company. Tantalum, tungsten, and molybdenum form a group peculiar to themselves among the commercially available metals. Their very high melting points (tantalum 2770° C., tungsten 3350° C., and molybdenum 2550° C.) set them apart so far as the metallurgical processes for their production are concerned. Further, when properly prepared and treated they will stand a somewhat unusual degree of cold work, that is work below the temperature at which marked crystal growth takes place. Such cold-worked metal may show a high tensile strength; tantalum to 130,000 lb. per sq. in., tungsten to 490,000 lb., and molybdenum to 260,000 lb., in the form of fine wire. In physical appearance, these metals are not unlike some steels; they may be better described by saying that polished tantalum some¬what resembles lead; polished tungsten, iron; and polished molybdenum, nickel. The polished surfaces of all three remain untarnished in ordinary air. Air containing corrosion-producing impurities will, in general, show molybdenum the least resistant to corrosion and tantalum the most resistant. Molybdenum has, however, a high degree of resistance to corrosion by hydrochloric acid, a property that should render it of commercial interest. On the other hand, it is markedly attacked by some of the weaker organic acids.

Jan 3, 1925

By J. C. Bartlett

The following discussion was suggested by an experiment of Mr. Krom, the Manufacturer of air-jigs, to illustrate the superiority of air over water as a medium of concentration. The paper is written in the interest of no system of concentration, but simply to test the experiment, and, perchance, to add something to the general fund of information on the subject. To speak of testing an experiment by a theoretical discussion, may seem a misuse of terms, but the theories concerning falling bodies and the resistance of fluids are pretty well crystallized into laws, which may properly be used to show where experiments which seem to refute them were improperly performed, and that instead of refuting they only corroborate. It is well known that a sphere of galena & inch in diameter, and a sphere of quartz 1/2 inch in diameter, are equal falling in water ; that is, these two spheres, being placed together in a column of water at rest or in motion, will practically remain together, filling or rising together, or remaining in suspension. Mr. Krom, to show that these

Jan 1, 1879

By R. C. Buehl, M. B. Royer

High manganese slags of low phosphorus and iron content are produced by air oxidation of high phosphorus spiegeleisen in a basic-lined converter. Control of phosphorus and iron within specification limits for ferromanganese ore feed is obtained by a unique cyclic operating procedure. Various types of slags, or synthetic manganese ore, can be made. AN affiliated paper' describes the production of high phosphorus spiegeleisen containing 14 to 23 pct Mn and up to 4 pct P in an experimental blast furnace from open-hearth slag or manganiferous iron ore. This phosphorus content is too high for use of the spiegel in normal steel-production operations. Consequently, a preferential separation must be effected whereby the manganese is concentrated in a product that is usable in industrial operations. The preferential separation methods being investigated for this phase of the work are confined to pyrometal-lurgical processes for ready incorporation into steel-plant operations. It is fortunate that manganese is more actively oxidizable than iron or phosphorus, and therein lies a preferential separation method for isolating manganese from these two elements. Silicon is more strongly oxidizable than manganese, and its oxidation precedes, or occurs simultaneously, with manganese. Therefore, manganese and silicon are separable into a high manganese oxide slag phase while the phosphorus and iron remain in the molten metallic state. Complete separation of these elements represents an ideal condition which is not generally attainable in actual operations. This pyro-metallurgical method for separating manganese from phosphorus and iron by preferential oxidation was investigated by blowing 500 lb of metal in a basic-lined vessel to obtain preliminary information on the effectiveness of the procedure. Certain conditions of attainment in the separation process are desirable in any method for removing manganese from high phosphorus spiegeleisen, such as: 1—High recovery of manganese in the oxidation product; 2—the product to be of equal or better quality than ferromanganese-grade ore—48 pct Mn minimum, less than 10 pct SiO2, and Mn-P ratio of 300:1; and 3—attainment of the enumerated objectives in a product amenable to industrial handling, such as a slag of high manganese content that will flow from the processing vessel and of sufficient fluidity for ready separation of metallic granules that may have become mixed with the manganese slag phase. Previous Work Recovery of manganese from low grade ores and industrial byproduct slags by smelting to spiegeleisen, with subsequent oxidation to synthetic ferro-manganese-feed ores, has been a subject for periodic investigation during the past four or five decades in the United States and Germany. Joseph' and associates of the Bureau of Mines North Central Experiment Station, Minneapolis, Minn., smelted manganiferous iron ores of the Cuyuna range, Minn., to spiegeleisen and subsequently tried air and ore oxidation procedures for concentrating the manganese into synthetic ferrograde manganese ore. Joseph's results on the operation of a side-blown basic-lined converter for air oxidation of manganese from molten spiegeleisen were so discouraging that the procedure was abandoned after 11 blowing tests. Much slag was thrown from the converter vessel; phosphorus content was four to five times the maximum allowable for ferro ore; and a manganese-iron ratio of only 2 or 3:1 was obtained in the slag instead of the required 8:1. Oxidation of manganese from spiegeleisen with about 0.5 pct P, by adding iron ore to molten spiegel in an experimental open-hearth furnace, proved moderately successful in Joseph's experiments. The main drawback to the operation was the necessity for over-oreing for effective oxidation of the manganese with consequent too high iron oxide residual in the slag. Furthermore, the phosphorus content was proportional to the iron concentration and therefore much too high, so that several hours of reduction by a carbonaceous material were required to adjust the iron and phosphorus to the desired content of high grade ferro feed. A troublesome feature of the slag product of the spiegel oxidation process was its lack of fluidity if the silica content was less than 10 pct, the concentration considered desirable for the synthetic ore. Approximately twice the desired concentration of silica was required to impart enough fluidity for transfer from the vessel by pouring. The acute shortage of manganese in Germany

Jan 1, 1953

By Martin Weinstein

A technique is described for preparing finegrained lead telluride by ultrasonic agitation of a solidifying melt. Material prepared by this technique is dense and chemically homogeneous. N-type PbTe, containing 0.03 mole pct PbIz, has been made and its thermoelecCric Properties have been measured as a function of temperature. For comparison, the properties of similarly doped PbTe made by cold pressing and sintering, and by extrusion, have also been measured. The ultrasonically prepared material compares favorably with the others in its thermoelectric-efficiency factor. Comparison of compressive-flow curves for the three kinds of PbTe show that the ulhasonically prepared material has much superior ductility. The cleavage strength of the ultrasonic material is related to the grain size, D, by the Petch relation:Extrapolation to infinite grain diameter yields a fracture strength of 5000 psi for single-crystal PbTe. WHEN metals and semiconductors solidify in a mold they normally assume one of three cast structures illustrated in Fig. 1.' Solidification in a casting starts at the mold walls where a large number of fine crystals of random orientation can be nucleated to form the chill zone. Because of the anisot-ropy of the growth rate, those crystals whose direction of maximum linear growth is parallel to that of the heat flow grow faster and crowd out the crystals of less favorable orientation. A second zone, having a preferred orientation, called the columnar zone, thus forms adjacent to the chill zone. The speed of growth of the columnar grains will depend, in the case of limited undercooling of the melt, on the rate at which heat can be abstracted. The columnar zone can extend to the center of the casting, Fig. l(a), but it is frequently followed, in solid-solution alloys, by another zone of equiaxed randomly oriented grains in the central portion of the casting, Fig. l(b). The equiaxed structure in Fig. l(c) represents the completely grain-refined case where the equiaxed grain size is small. The third type of structure is the most desirable because it imparts a somewhat higher strength for all except high-temperature applications, it reduces segregation of the doping constituent, and it reduces the possibility of hot tearing (the separation of grains due to the melting of a low-melting point constituent in the grain boundaries). In order to obtain fine-grained castings, the nu-cleation frequency must be increased and grain growth must be restricted. Various techniques have been employed for obtaining this end, namely: rapid cooling, vibration, and inoculation of the melt. The success of these techniques depends upon the characteristics of the metal species and on factors controlled by heat transfer through the crucible walls. Recent studies2" have shown that the application of ultrasonic energy to the solidifying ingot is an extremely powerful tool in the improvement of the crystalline structure of metallic castings. Both the mechanical properties and homogeneity of the ingots are improved. Ultrasonic oscillations may affect the crystallization process by 1) permitting subcritical nuclei to agglomerate and thus form nuclei of sufficient size to cause crystallization, 2) changing the state of surface adsorption of various catalysts found in the liquid melt, 3) breaking pieces of solid from the solidified surface near the supercooled region thereby increasing the number of possible nuclei, 4) causing temperature fluctuations to occur in certain parts of the melt thereby increasing the supercooling at specific points in the liquid, and 5) decreasing the critical nucleus size by increasing the pressure at specific points in the melt.' Various investigators have concluded that the effectiveness of the ultrasonic oscillations results from cavitation which disrupts the growing solid-liquid interface The present paper describes the application of ultrasonic oscillations to the crystallization of the semiconductor N-type PbTe. The purpose of this study is to prepare crystalline

Jan 1, 1964

By C. H. Mathewson, J. A. Collins

The process of plastic extension of face-centered cubic single crystalline rods is so well understood, since the notable studies of Taylor and Elam,1 that the change in orientation of any crystal by slip and rotation may be predicted from the measured elongation. It is customary to assume a very homogeneous deformation, wherein gliding lamellar arc free to rotate so that their slip direction continually approaches the axis of the rod, until a second slip system comes into operation; whereupon conjugate slip proceeds quantitatively to an end adjustment with the [121] direction in the axis of the rod. This process has been checked in malty face.-centered cubie materialsand and readily permits the preparation of specimens that have been subjtvted to various determinable amounts of shearing action. It is elearly of interest to study in such measurably strained speeimens the, development of a recrystallized structure on annealing and if possilble detect the source of nuclei from which the new crystals grow. Strain-:~nneali~ig experiments of this charactcr have been performed by others but not in detail sufficient to permit a study, for example, of the number of recrystallized grains vs. the amount of shear. In the experiments now reported, this was done with a wide variety of orientations covering nearly the entire range of slip on a single system and corresponding to amounts of shear (ratio of shearing distance to distance between lamellae at the conclusion of a test of from 0.08 to 0.57. A particular point wa-made of determining the crystallite rotation, or small angular range. assumed by the octahedral slip plane after these various amounts of shear. The, mechanism of reerystallization and the magnitude and effeet of recovery on the recrystallization process was investigated.

Jan 1, 1940

By J. A. Collins, C. H. Mathewson

The process of plastic extension of face-centered cubic single crystalline rods is so well understood, since the notable studies of Taylor and Elam,1 that the change in orientation of any crystal by slip and rotation may be predicted from the measured elongation. It is customary to assume a very homogeneous deformation, wherein gliding lamellar arc free to rotate so that their slip direction continually approaches the axis of the rod, until a second slip system comes into operation; whereupon conjugate slip proceeds quantitatively to an end adjustment with the [121] direction in the axis of the rod. This process has been checked in malty face.-centered cubie materialsand and readily permits the preparation of specimens that have been subjtvted to various determinable amounts of shearing action. It is elearly of interest to study in such measurably strained speeimens the, development of a recrystallized structure on annealing and if possilble detect the source of nuclei from which the new crystals grow. Strain-:~nneali~ig experiments of this charactcr have been performed by others but not in detail sufficient to permit a study, for example, of the number of recrystallized grains vs. the amount of shear. In the experiments now reported, this was done with a wide variety of orientations covering nearly the entire range of slip on a single system and corresponding to amounts of shear (ratio of shearing distance to distance between lamellae at the conclusion of a test of from 0.08 to 0.57. A particular point wa-made of determining the crystallite rotation, or small angular range. assumed by the octahedral slip plane after these various amounts of shear. The, mechanism of reerystallization and the magnitude and effeet of recovery on the recrystallization process was investigated.

Jan 1, 1940