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Jan 1, 1900

Jan 1, 1916

Jan 1, 1912

By B. M. Larsen, T. E. Brower

INTRODUCTION AND SUMMARY BY "thermochemical factors" we refer to those variables which affect the net heat which must be put into the bath in order to make a heat of steel from any given set of charge materials. This is admittedly only one phase of the production rate problem. The whole problem includes also consideration of rate of charging, flame radiation intensity, rate of optimum fuel input obtainable without undue damage to the furnace structure and any variations in conditions such as stirring, slag volume or viscosity which affect the rate at which heat can flow down and away from those exposed surfaces where the heat is first received from the flame. Because a given type of charge in a shop is often considered as being nearly constant in both physical and chemical characteristics from one heat to another, and because such a state of affairs may be thought of as resulting in a reasonably constant net heat requirement, this requirement is usually neglected as an invariable, inevitable matter, about which nothing can be done. With normally variable charge, and variable percentages of limestone and cold pig, however, the net heat requirement can be subject to very appreciable change; it may also be affected by such things as the currently popular procedure of blowing oxygen into the bath, To bring the general problem of production rate into better perspective, therefore, it seems worthwhile to try to evaluate the net bath heat requirement and the amount by which it may change through variation in different factors. Because our calculated values of net heat are admittedly uncertain, we have tried to check them in part by statistical data on actual production rates over rather large groups of commercial heats. The results of calculation of net heat requirements in a wide range of actual commercial practices may first be summarized briefly. We find a wide range between the extremes of different practices, as would be expected, with duplex practice (essentially blown metal plus hot metal) having essentially a zero net heat requirement, an all-cold charge practice somewhat over 1 million Btu per ton of steel and a high hot metal practice about 0.75 million Btu per ton. Over the commercial range of scrap plus hot metal practice, increasing the percentage of hot metal from 40 to 78 pct, with other factors nearly constant, decreased the net heat by only some 5-10 pct, The net heat is increased by about 1.2 pct for each I pct of the metallic charge present as cold pig. Calculated values of oxygen supplied by air varied from about 25 up to 60 lb per ton of steel, and in a 60 pct hot metal practice, an increase from 32 to 52 lb oxygen from air decreased the calculated net heat from 0.88 to 0.74 million Btu per ton. Use of pure cold oxygen to substitute for about one half of the total charge ore (about 28 lb oxygen replacing 145 lb ore per ton of steel) decreased the

Jan 1, 1948

By Oliver Bowles

ALTHOUGH Oliver Bowles retired as chief of the nonmetal economics division of the Bureau of Mines last year, that retirement has not lessened his active interest in the field of nonmetallic minerals, in writing, nor in his hobby, cultivation of African violets. Excellent co-ordination of the timing of a professional meeting and a flower show permitted him on at least one occasion to attend technical sessions and take in the African violet exhibition which happily arrived simultaneously in one city. Dr. Bowles celebrated his seventieth birthday on Jan. 10, 1947, and

Jan 1, 1948

By B. M. Larsen, T. E. Brower

Introduction and Summary By "thermochemical factors" we refer to those variables which affect the net heat which must be put into the bath in order to make a heat of steel from any given set of charge materials. This is admittedly only one phase of the production rate problem. The whole problem includes also consideration of rate of charging, flame radiation intensity, rate of optimum fuel input obtainable without undue damage to the furnace structure and any variations in conditions such as stirring, slag volume or viscosity which affect the rate at which heat can flow down and away from those exposed surfaces where the heat is first received from the flame. Because a given type of charge in a shop is often considered as being nearly constant in both physical and chemical characteristics from one heat to another, and because such a state of affairs may be thought of as resulting in a reasonably constant net heat requirement, this requirement is usually neglected as an invariable, inevitable matter, about which nothing can be done. With normally variable charge, and variable percentages of limestone and cold pig, however, the net heat requirement can be subject to very appreciable change; it may also be affected by such things as the currently popular procedure of blowing oxygen into the bath. To bring the general problem of production rate into better perspective, therefore, it seems worthwhile to try to evaluate the net bath heat requirement and the amount by which it may change through variation in different factors. Because our calculated values of net heat are admittedly uncertain, we have tried to check them in part by statistical data on actual production rates over rather large groups of commercial heats. The results of calculation of net heat requirements in a wide range of actual commercial practices may first be summarized briefly. We find a wide range between the extremes of different practices, as would be expected, with duplex practice (essentially blown metal plus hot metal) having essentially a zero net heat requirement, an all-cold charge practice somewhat over I million Btu per ton of steel and a high hot metal practice about 0.75 million Btu per ton. Over the commercial range of scrap plus hot metal practice, increasing the percentage of hot metal from 40 to 78 pct, with other factors nearly constant, decreased the net heat by only some 5-10 pct. The net heat is increased by about 1.2 pct for each I pct of the metallic charge present as cold pig. Calculated values of oxygen supplied by air varied from about 25 up to 60 lb per ton of steel, and in a 60 pct hot metal practice, an increase from 32 to 52 Ib oxygen from air decreased the calculated net heat from 0.88 to 0.74 million Btu per ton. Use of pure cold oxygen to substitute for about one half of the total charge ore (about 28 Ib oxygen replacing 145 Ib ore per ton of steel) decreased the

Jan 1, 1949

By B. M. Larsen, T. E. Brower

Introduction and Summary By "thermochemical factors" we refer to those variables which affect the net heat which must be put into the bath in order to make a heat of steel from any given set of charge materials. This is admittedly only one phase of the production rate problem. The whole problem includes also consideration of rate of charging, flame radiation intensity, rate of optimum fuel input obtainable without undue damage to the furnace structure and any variations in conditions such as stirring, slag volume or viscosity which affect the rate at which heat can flow down and away from those exposed surfaces where the heat is first received from the flame. Because a given type of charge in a shop is often considered as being nearly constant in both physical and chemical characteristics from one heat to another, and because such a state of affairs may be thought of as resulting in a reasonably constant net heat requirement, this requirement is usually neglected as an invariable, inevitable matter, about which nothing can be done. With normally variable charge, and variable percentages of limestone and cold pig, however, the net heat requirement can be subject to very appreciable change; it may also be affected by such things as the currently popular procedure of blowing oxygen into the bath. To bring the general problem of production rate into better perspective, therefore, it seems worthwhile to try to evaluate the net bath heat requirement and the amount by which it may change through variation in different factors. Because our calculated values of net heat are admittedly uncertain, we have tried to check them in part by statistical data on actual production rates over rather large groups of commercial heats. The results of calculation of net heat requirements in a wide range of actual commercial practices may first be summarized briefly. We find a wide range between the extremes of different practices, as would be expected, with duplex practice (essentially blown metal plus hot metal) having essentially a zero net heat requirement, an all-cold charge practice somewhat over I million Btu per ton of steel and a high hot metal practice about 0.75 million Btu per ton. Over the commercial range of scrap plus hot metal practice, increasing the percentage of hot metal from 40 to 78 pct, with other factors nearly constant, decreased the net heat by only some 5-10 pct. The net heat is increased by about 1.2 pct for each I pct of the metallic charge present as cold pig. Calculated values of oxygen supplied by air varied from about 25 up to 60 lb per ton of steel, and in a 60 pct hot metal practice, an increase from 32 to 52 Ib oxygen from air decreased the calculated net heat from 0.88 to 0.74 million Btu per ton. Use of pure cold oxygen to substitute for about one half of the total charge ore (about 28 Ib oxygen replacing 145 Ib ore per ton of steel) decreased the

Jan 1, 1949

By William P. Shinn

IT seems proper to present in the Transactions of the Institute, from time to time, formal record of the advances made in the arts and sciences to which our organization is devoted-milestones in the highway of progress-from which our successors may measure what they in their turn have gained. The admirable address of the Hon. Abram S. Hewitt, then president elect of the Institute, on "A Century of Mining and Metallurgy in the United States," read at the opening of the meeting held in this hall in June, 1876, forms a point of departure, and the conclusion of the eighth decade of the nineteenth century and the end of the first five years of our country's second century seem to offer a fitting time for again making up our record. The period since 1875 has been marked by a degree of activity in mining and metallurgical industry never before equalled in our history, while the progress made in the science and art has been, if possible, still more noticeable. Whether we consider the mining of iron, ore, and coal, or of the precious metals,-the advances made in smelting the former and in reducing the latter, the extraordinary increase in the production of Bessemer steel, or the science of Thomas and. Gilchrist, which makes the hitherto rejected phosphorus the corner-stone of success,-the past five years are alike memorable for the progress they have shown and to some of the most marked features of this progress I will now oriefly call your attention. It may be of interest in this connection to note the following figures, showing the growth of the population of the United-States during the last three decades :

Jan 1, 1881

By F. L. Bosqui

A. L. BlomFIeld, Denver, Col. (communication to the Secretary.*) — Mr. Caldecott says on p. 67: "The Dorr thickener shown, while a useful device when crushing with cyanide solution for removing surplus solution from slime pulp prior to air-lift agitation or vacuum filtration, is not adapted to effect as complete a separation of water from settled slime as the ordinary intermittent settlement and decantation." This statement might have passed muster in this country several years ago when. the Dorr thickener was a new device, but its use in hundreds of mills in the United States has demonstrated that as thick a product is being discharged from it as was obtained from the intermittent settling which it has supplanted. • It is interesting to note that recent investigation, especially the work of 11. 6. Coe and G. H. Cleveilger,' in the March Bulletin of the Institute, under the title: Laboratory Method for Determining the Capacities of Slime Settling Tanks, has developed the general theory of settlement and explains the results obtained in practice. Just as free settlement is a function of surface area, so thickening after the zone of free settlement is passed is a function of time. The time required is obtained by the capacity or volume provided in the settler for this thickening zone. Each pulp is a problem in itself, both in regard to free settlement and to time required to reach a commercially finished thickness. Some pulps require 48 hr. and more to reach a density of 40 per cent. solids; others no coarser to the screen test reach a density of 65 per cent.' solids in a fraction of that time. In thickening any pulp a point is reached where the increase in density is so slow as to be commercially unprofitable. When any part of the pulp has reached this point it should pass on for treatment—its place in the thickener should be occupied by pulp which has not yet reached the commercial limit. By doing this the whole volume of the settling tank is kept in active use. Thus the continuous thickener keeps the whole tank at work to its commercial limit, while the intermittent settler has much of its volume occupied at times by pulp which is either quite finished thickening or at least thickened past the commercial point. The mechanical efficiency of the continuous thickener can be the only argument for limiting this statement. In my own experience I have never

Jan 1, 1916

By R. J. Marcotte, C. T. Eddy, R. J. Smith

THE objectives of the investigation herein reported were to determine: (I) the S-curves for certain selected cast steels, (2) whether or not the published S-curves for wrought steels are satisfactory for use on cast steels of similar composition, and (3) to prepare hardenability curves of the selected cast steels. In order to make the final comparisons between cast and wrought steel more completely tangible, it was deemed advisable not only to determine S-curves for the steels submitted in the cast condition but also to roll some of the cast-steel test bars and determine comparison S-curves on such wrought material. This procedure eliminates the composition variable and makes it possible to reveal the differences resulting from plastic deformation of the cast structure in addition to providing the comparison with published data on wrought steels. CAST STEELS The cast steels selected for the preparation of S-curves, or time-temperature transformation curves, were similar to S.A.E. series 1030, 2330, 4130 and 4330. Of these the 1030 was supplied by The Crucible Steel Casting Co., Cleveland, Ohio, and the other three by The Sawbrook Steel Castings Co., Lockland, Ohio. The steels were furnished in the as-cast condition. The manufacturers supplied the chemical analyses and the properties that could be obtained in the heat-treated condition-all of which is summarized in Table I. [ ] PROCEDURE The metallographic and dilatometric procedures and equipment were in general standard. The specific technique employed was described in a report of the Steel

Jan 1, 1945

By C. A. Wright

Since the adoption by the U. S. Bureau of Standards several years ago of specifications for standard 100- and 200-mesh sieves, frequent requests have been received that this Bureau test and certify sieves of other sizes than these. With a view to the adoption of a series of standard testing sieves which might be of use to all industries making fineness tests, this Bureau for two years has been studying the question of such a standard screen scale. Various scales that have been proposed were considered, and information was sought of representative firms in the various industries interested as to their requirements. Manufacturers of sieves have also been consulted as to the desirability of different screen scales and the practicability of their manufacture. As a result of this study of the question, a conference was called at the Bureau of Standards, Apr. 20, 1916, of representatives of various committees of the American Society for Testing Materials, American Society of Civil Engineers, American Institute of Mining Engineers, American Foundrymen's Association, Mining and Metallurgical Society of America, American Water Works Association, American Institute of Metals and the American Spice Trade Association; also representatives of the Committee of Revision of the U. S. Pharmacopæia, the U. S. Geological Survey, the U. S. Bureau of Mines, the U. S. Office of Public Roads and Rural Engineering, the U. S. Office of Grain Standardization and the U. S. Bureau of Standards; also representatives of a number of private firms engaged in industries in which sieves are used, such as the glass, the drug milling, the abrasive, the asphalt, the mining, the spice, the chemical, and the graphite industries; also representatives of the firms in this country manufacturing wire cloth and sieves. This Conference, after considering the various screen scales either proposed or now in use, adopted as a Standard Screen Scale that given in Table 1, and recommends that it be adopted generally by scientific,

Jan 1, 1918

By Danforth R. Hale, R. E. Blair

Minerals for electronic and optical uses divide easily into two sections: (1) quartz and (2) minerals other than quartz. Quartz Quartz, having a great usefulness discovered by the radio communication enthusiasts about 1918, has become a subject of amazingly expanded interest in the US over the past decade as a man-made mineral and a multimillion dollar crystal-growing business. An economic summary of the commercial growing of quartz crystals has a place in a handbook directed to the mineral engineering industry when it is remembered that quartz crystals have long been an important commercial mineral, and that the raw material for "cultured quartz"-that is to say, quartz crystals grown through the ingenuity of man-is still natural quartz. Nearly all the natural crystals come from Brazil. The larger pieces which meet rigorous standards of quality are used for electronic and, to a lesser extent, optical components. Smaller pieces and fragments are used for vitreous silica. The need for high quality material in quantity led to US government-sponsored research programs in the 1940s that have resulted in the factory growing of beautiful crystals of prescribed shape, size, and quality. The development of the cultured quartz crystal is typical of man's success in adapting the product of the mine to increasingly sophisticated uses. A remarkable achievement perhaps, but foreshadowed by experiments in 1908 by Giorgio Spezia (1908), an Italian geologist studying the relative effects of temperature and alkaline environment on the solubility of quartz. Modern radio equipment is most often controlled as to frequency by the presence in the circuit of a separately added "crystal"-the 1918 discovery responsible for the existence and growth of the quartz industry. The "crystal" is quartz, but this component is a carefully oriented and prepared slice from a crystal, but not a crystal as recognized by a rock hound or seen in a museum. How quartz operates to control frequencies is not a proper subject for a handbook on industrial minerals, and references should be consulted (Cady, 1964; Mason, 1964). Quartz belongs to that class of materials called dielectrics: those that do not conduct an electric current but permit electric fields to exist and act across them. Quartz shows the "piezoelectric effect," which means that when a quartz plate is mechanically deformed against its natural stiffness, one of its surfaces becomes negatively charged, the other, positively charged. When the plate is released from the stress quickly, the charges disappear as the plate regains its original shape, but because of mechanical momentum the plate deforms in the opposite direction (to a lesser amount) and the surfaces correspondingly become charged in the opposite direction. By coating the two surfaces thinly with metal and attaching flexible wires, these charges may be brought into an electronic circuit. If the surfaces are suddenly electrically charged by movement of current through the wires, the "converse piezoelectric effect" occurs -the plate deforms. Carry the thought further and it is realized that an alternating current flowing through the wires responds to the mechanical oscillation of the plate and is keyed to this oscillation. By controlling the thickness of the plate its mechanical vibration frequency can be varied through a wide range. One type of quartz plate, called the AT-cut, having a precisely defined orientation with respect to the crystallographic axes of the crystal, vibrates on a microscopic scale much as a book would deform when placed flat on a table and the top cover moved parallel back and forth with the hand. There are at least 17 other orientations which have been studied, some of

Jan 1, 1983

By R. J. Marcotte, C. T. Eddy, R. J. Smith

The objectives of the investigation herein reported were to determine: (I) the S-curves for certain selected cast steels, (2) whether or not the published S-curves for wrought steels are satisfactory for use on cast steels of similar composition, and (3) to prepare hardenability curves of the selected cast steels. In order to make the final comparisons between cast and wrought steel more completely tangible, it was deemed advisable not only to determine S-curves for the steels submitted in the cast condition but also to roll some of the cast-steel test bars and determine comparison S-curves on such wrought material. This procedure eliminates the composition variable and makes it possible to reveal the differences resulting from plastic deformation of the cast structure in addition to providing the comparison with published data on wrought steels. Cast Steels The cast steels selected for the preparation of S-curves, or time-temperature transformation curves, were similar to S.A.E. series 1030, 2330, 4130 and 4330. Of these the 1030 was supplied by The Crucible Steel Casting Co., Cleveland, Ohio, and the other three by The Sawbrook Steel Castings Co., Lockland, Ohio. The steels were furnished in the as-cast condition. The manufacturers supplied the chemical analyses and the properties that could be obtained in the heat-treated condition—all of which is summarized in Table I. The metallographic and dilatometric procedures and equipment were in general standard. The specific technique employed was described in a report of the Steel

Jan 1, 1945

By W. P. Haynes

ESTIMATED United States crude-oil production during 1943 established a new annual peak of 1,500,000,000 barrels, a daily average of 4,118,000 barrels. This would be an increase of 315,000 barrels per day, or 8 per cent over 1942 and 7 per cent over 1941, the previous peak. During the first ten months of the year, production jumped from 3,782,000 barrels per day in January to 4,400,000 in October. Available data for the last two months of the year indicate a leveling off of this trend, with daily rates slightly above 4,400,000 barrels.

Jan 1, 1944

By R. A. Haney, S. J. Gigliotti

Over the past ten years, analysis of the acceptability of face ventilation systems has been based on numerical criteria rather than solely a study of air flow and methane patterns in the face area. This type of analysis has become possible primarily because of the instrumentation and mathematical models developed by the Ventilation Division, Pittsburgh Health Technology Center, Mine Safety and Health Administration (MSHA). To properly use these mathematical models, large amounts of methane and airflow data must be collected in the face area during mining activities. To supplement underground testing of face ventilation systems, a full scale model of a face area was built. This model includes a full scale model continuous miner, a face ventilation system, a gas release system, and a remote methane detection system. The remote methane detection system consists of an array of twelve methane sensors located throughout the face area. Data from the sensors are transmitted to strip chart recorders. Methane, air quantity, and other data collected during a test are entered into a computer for analysis. This paper presents the data entry system, the models used for data analysis, the test results, and the application of these results to a face ventilation system.

Jan 1, 1983

By T. H. Aldrich

(Chattanooga Meeting, October, 1908.) Tars paper is intended only to give a preliminary account of experiments made, and conclusions reached, concerning the treatment of certain refractory low-grade gold-ores, the profitable reduction of which may furnish a useful guide to the solution of similar mining and metallurgical problems, not only in the gold-bearing belt of the Southern United States, but perhaps in other regions also. It must be regarded as simply a ?report of progress," preceding a more elaborate and conclusive report of regular practice. The mines of the Hillabee Gold Mining Co. are located upon what is generally known locally as Hog Mountain, on the northern edge of Tallapoosa county, Ala., about 15 miles from Goodwater and 14 miles from Alexander City, stations on the Central of Georgia Railway. Gold has been known since 1839 to exist on this property, where it was discovered in that year by a man named Johnston. The property was worked for placer-gold by the old miners, and there are now the remains of four attempts to operate it by stamp-mill and plate-amalgamation. The present owners purchased it in 1896, and since that time they have experimented at frequent intervals, in order to devise a process that would satisfactorily recover the gold. In 1903 regular operations were begun. Geologically, the mountain consists of an intrusion of what has been pronounced true granite in altered sedimentary slates. The cooling of the granite produced shrinkage-cracks, which have become veins. There is considerable question as to the period of the slate formation; but it is undoubtedly, in my opinion, of Carboniferous age. The veins, about 50 in number, strike N. 60° to 80° E.; dip approximately 65° from the horizontal; vary from a few inches to 25 ft. (being in gen-

Nov 1, 1908

By G. E. Klinzing, S. H. Chiang, R. M. Kakwani

Filtration and dewatering results of -500 µm (-32 mesh) Pittsburgh seam coal are discussed with reference to the microscopic structure parameters, i.e., particle segregation in the cake and particle and pore size distributions at different layers. At low solid concentration of 0.33 kg coal/kg water, a non-uniform cake structure is observed where particle and pore sizes increase from the top to bottom layers in the filter cake. An increase in the solid concentration in slurry produces more uniform cake structure and higher filtration and dewatering rates. Air bubble entrapment in the coal filter cakes is also discussed.

Jan 1, 1985

The following is an incomplete list of members and guests who called at Institute headquarters during the period June 10, 1919, to July 10, 1919. Anvil A. Anderson, Rapid City, S. D. Roy N. McBride, U. S. Army. R. Hay Anderson, Mexico City, Mex. R. S. McIntyre, Berkeley, Calif. W. A. Barnes, San Francisco, Calif. H. R. Maier, Brooklyn, N. Y. Bennett R. Bates, Denver, Colo. Wm. D. Mainwaring, Philadelphia, Pa. Harlan H. Bradt, Duluth, Minn. Wm. E. Milligan, Chrome, N. J. H. Brings, San Francisco, Calif. Willard S. Morse, Tacoma, Wash. Robert S. Burg, Ocean Park, Calif. Arthur Notman, Bisbee, Ariz. D. W. Butner, Congo Belge, Africa. P. Nugue, Chalon Sr. Saone, France. George A. Camphuis, El Paso, Tex. George A. Packard, Boston, Mass. Fred Canan, Denver, Colo. C. L. Petzel, New York City. Walter H. Coleman, Prescott, Ariz. V. Porreaud, Paris, France. Fred Crabtree, Pittsburgh, Pa. Fred S. Porter, Seattle, Wash. Ross E. Douglas, Rancagua, Chile. R. W. Prouty, Morenci, Ariz. F. A. Downes, Golden, Colo. Charles E. Prior, Brooklyn, N. Y. W. G. Eberhardt, Tucson, Ariz. Louis Ravicz, Minneapolis, Minn. Charles H. Fulton, Cleveland, Ohio. Wm. Reed, El Oro, Mexico. Wm. R. Grunow, New York City. E. J. Ristedt, Globe, Ariz. Orr R. Hamilton, Lansing, Mich. A. M. Rodgers, Middletown, N. Y. T. N. Havlin, St. Louis, Mo. J. C. Scoles, Salt Lake City, Utah. G. M. Henderson, Weston, Mass. C. E. Siebenthal, Washington, D. C.

Jan 8, 1919

By JOHN BIRKNBINE

MR. NEILSON was born Aug. 12, 1842, at Philadelphia, Pa., where he died Dec. 30, 1906. His business career began with his graduation, in the class of 1862, from the Polytechnic College of the State of Pennsylvania. For a short time after graduation he was instructor in mathematics at the college, and then became associated with Messrs. Booth & Garrett, chemists, of his native city: In 1867 he was sent to the Adirondack mountains to care for mining interests of the late Jay Cooke, and spent about three years there, operating the forges at Elizabethtown, Essex county, N. Y. He also prepared an interesting monograph on Catalan forges and their operations. In 1868 he published a chart showing the material progress of the United States, and the cost of certain staple products during a series of years, which is believed to be the first of its kind issued in this country. In 1870 he made a trip to the Pacific Coast, prior to entering the service of the Pennsylvania Steel Company. In 1871, when the Logan Iron & Steel Co., of Burnham, Pa., failed, Mr. Neilson was appointed receiver, re-organized the company, became' its General Manager, and spent more than four years in this work. In the meantime, he became interested in the Freedom forge of the same place, and, with Mr. Wm. Burnham and Mr. Milton Brosius, laid the foundations for what is now the Standard Steel Works. From Jan. 1, 1877, to April 1, 1890, he was General Manager of these works, and closely associated with the Baldwin Locomotive Works. In 1878 he was in charge of the first consignment of Baldwin locomotives to Europe, which, with a picked crew of men from Baldwin's, he took to Eydtkennen, Russia, and placed in service. In 1890 he resigned from the Standard Steel Works and ac-

Jul 1, 1907

By K. A. Gschneidner, O. D. McMasters, T. J. O’Keefe

X-ray diffraction, differential thermal, ad rnetallo-graphic methods were used to establish the Dy-Pb Phase diagram. Lead additions lower the 1377°C transformation temperature of dysprosium to 1360°C leading to an inverted peritectic reaction. The 327°C melting point of lead is lowered by dysprosium additions to about 326°C yielding a eutectic reaction. A second eutectic reaction occurs at 13.3 at. pct Pb and 1200°C. The dysprosium-richest intermetallic compound DysPb3 melts congruently at 1695°C and crystallizes in the hexagonal Mn5Si3 (D8,) type structure. The peritectic decomposition temperatures for the remaining compounds are Dy5Pb, at 1555C, DyPb2 at 955C, and DyPb3 at 880°C. A fifth compound near the DyPb stoichiometry exists over a 310°C temperature range decomposing at 1130°C by means of an inverted peritectic reaction and melting incongruently at 1440°C. The crystal structures of the compounds are discussed. A systematic study of the rare earth-lead alloy systems is underway in an effort to supply information concerning the alloying behavior of the rare earth metals. The Dy-Pb phase diagram is the fourth system to be investigated in this study. The Yb-Pb,1 Y-Pb,2 and Eu-Pb 3 diagrams have been published recently. Utilization of the rare earth series of metals as a research tool in this manner should yield a better understanding of alloy formation. EXPERIMENTAL PROCEDURE Materials. The lead used in this investigation was obtained from Cominco Products, Inc., and was specified to be 99.99 pct pure. The dysprosium was prepared in this Laboratory by the calcium reduction of the fluoride followed by distillation of the dysprosium. The major impurities in the dysprosium in ppm are: A1 (<40), Ca (400), Er (<50), Gd (<200), Ho (<200), Mg (<50), Si (30), Ta (400), Tb (<100), Y (<50), 0 (651, H (15), N (not detected), F (430), C (35). Alloy Preparation. Most of the alloys were prepared by melting weighed amounts of dysprosium and lead in sealed tantalum crucibles. The tantalum crucibles were sealed by are-welding in a He-Ar atmosphere welding chamber. Thus the alloys are in contact with He-Ar at about 1 atm pressure. Homogenization was achieved by holding them in the liquid state for about 1 hr, cooling, inverting the crucibles, remelting, and repeating the process at least twice. Since these alloys were prepared in sealed tantalum crucibles, chemical analysis for final composition was thought to be unnecessary. No detectable reaction of these alloys with the tantalum crucible was observed by metallographic examination. Metallographic evidence was also used to confirm the homogeneity of some of the alloys prepared in this manner. The compositions of a few alloys, which were prepared by nonconsum-able are-melting, were corrected for the small weight losses involved by assuming that the weight loss is due to vaporization of lead. The specimens obtained from the alloy samples were prepared under a dry-argon atmosphere because they were rapidly attacked by air and moisture. Thermal Analysis. Differential thermal analysis methods were used to determine the liquidus curves and reaction horizontals of the system. Both Pt vs Pt + 13 pct Rh and W + 5 pct Re vs W + 26 pct Re thermocouples were used to measure the temperature. An X- Y recorder was used to record the specimen temperature and differential electromotive force between the specimen and molybdenum standard. The arrest temperatures were measured potentiometri-cally. The accuracy limits (* values) associated with the reaction temperatures obtained by this method were estimated on the basis of both the reproducibility of the particular temperature value and the accuracy of the thermocouple at a given temperature. Liquidus temperatures were obtained from cooling arrest data while both heating and cooling arrest data were used to establish the horizontals of the diagram. Heat treatments during the thermal analyses of the alloys between 40 and 70 at. pct Pb were necessary in order to approach equilibrium conditions. The samples were held at temperatures between the various peritectic horizontals for l to 2 hr before the thermal analyses were continued. The entire range of compositions was investigated at the expense of a minimum amount of materials by adding appropriate amounts of lead to master alloys. More than sixty alloys were analyzed by this differential thermal method and for each alloy the results given herein are taken from two or three heating and cooling cycles. X-Ray and Metallographic Methods. Slice specimens for metallography and powder specimens for X-ray diffraction were prepared from rod-shaped samples which had been melted in sealed 0.62 5-cm-diam tantalum crucibles. The specimens were heat-treated in sealed tantalum crucibles which were protected by sealing them in argon-filled quartz ampules. Quenching was accomplished by breaking the ampules in ice water after heat treatment. X-ray powder specimens were sealed in 0.3-mm-diam glass capillaries under a dry-argon atmosphere. Copper, iron, and chromium radiation were used to obtain the powder patterns for these alloys. More than 150 powder patterns were obtained for specimens of various compositions and heat treatments. Included in these were several patterns for specimens which had purposely been oxidized. Patterns from specimens which had been accidentally exposed

Jan 1, 1969