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By William B. Phillips

The concentration of natural magnetites has been carried on in this country for several years, and more or less information has been collected on the subject. Various inventors, availing themselves of the magnetism which is inherent in such ores, have devised machines for separating the impurities from the ore by means of the electric current; and a greater or less degree of success has rewarded their painstaking and persevering efforts. We are now fairly in position to judge of the value of the process as applied to such material. It is not my purpose to speak of this matter further than may be required by the emergencies of the case. I shall assume that most engineers and metallurgical chemists are already acquainted with what has been done at the Chateaugay mines, at Mineville, at the Benson mines, at the Weldon and Ogdensburgh mines, and at Cranberry; although, at this latter place, there has not been so much done as we could wish. I shall not now speak of the various types of separators. From the time of William Fullarton, to whom was granted an English patent, in 1792, for separating iron-ore by the application of magnetic attraction, down to the present time, a great. many devices have been suggested, and a great many patents taken out for this purpose; but it is not necessary now to enter upon a discussion of their merits. Perhaps, at some future meeting of the Institute, after we shall have experimented further with some of the machines on the market, there may be an opportunity to contribute something to the current knowledge of the efficiency and economy of separating-machines. In this paper I propose to give, as briefly as possible, the results already reached in converting a non-magnetic ore into magnetic ore, and then concentrating it over a magnetic separator of the alternate-polarity type. I am aware of the work

Jan 1, 1896

Jan 1, 1941

Jan 1, 1940

J. B. MCGRAW, New York, N. Y. (written discussion*).-In Mr. Burke Baker's description of the process of the American Briquet Co., he speaks only of the attractive features, but every process which uses a compound or emulsified binder has certain undesirable features which must be considered. In making an emulsion, the success of which depends upon the introduction of the various ingredients at certain fixed temperatures and the complete intermixing of a soluble solution with an oil which has absolutely no affinity for it, considerable difficulty is found in keeping the various factors in strict accordance with the formula. To serve its purpose properly or, in other words, to be right for easy mixing with the coal, it should be of a certain predetermined density. Among the controlling factors of this ate the proportion of moisture contained and the temperature of the oil when introduced. If the latter is higher than intended, a greater proportion of moisture will be evaporated than is proper, and if the oil is not sufficiently hot the process of emulsification is retarded. These various factors can be controlled with more or less certainty where working in a laboratory or in a small experimental way, but when it is attempted on a large commercial scale, certain obstacles not otherwise apparent are likely to be encountered.

Jan 5, 1918

By H. I. Aaronson, C. Wells

Configurations of ferrite crystals have been found in a plain carbon steel which appear to have resulted from the nucleation of new ferrite crystals at the interphase boundaries of previously formed crystals despite the high carbon concentrations which necessarily develop at these boundaries. This phenomenon has been termed sympathetic nucleation. An attempt has been made to reconcile the occurrence of sympathetic nu-cleation with current nucleation theory. THIS investigation is one of a series on the formation of proeutectoid ferrite from austenite. From the viewpoint of chemical composition, this reaction consists of the nucleation and diffusional growth of crystals of carbon-poor ferrite within a matrix of carbon-rich austenite. The austenite adjacent to the austenite-ferrite boundaries will be greatly enriched in carbon, approximately to the value of the y/(a + y) equilibrium curve or its metastable extrapolation at the temperature of transformation. Those areas of austenite appreciably farther removed from the growing ferrite, on the other hand, will be relatively unaltered in composition, especially at the earlier stages of transformation. Since rates of nucleation are considered to decrease exponentially with decreasing supersaturation,' the frequency with which ferrite nuclei appear at austenite-ferrite boundaries should be negligible in relation to that at which they form in other regions of the austenite. During this investigation, however, many groupings of ferrite crystals have been found which appear to have resulted from the nucleation of ferrite at austenite-ferrite boundaries. This phenomenon has been given the name of sympathetic 71.1tcleation. A number of micrographs of morphological configurations caused by sympathetic nucleation will be presented, after which an explanation for this reaction will be proposed in terms of current nucleation theory. Some of the structures to be considered are composed of bainite, an aggregate of ferrite and carbide, rather than of ferrite. Since ferrite and bainite differ only in that bainite forms under conditions which result in the nucleation of carbides behind the advancing austenite-ferrite boundaries,' it will usually be unnecessary, for the purpose of this paper, to distinguish between the two reaction products. All studies were performed on an electric furnace steel (obtained from the Vanadium Alloy Steel Co.) containing 0.29 pct C, 0.76 pct Mn, 0.25 pct Si, 0.005 pct P, and 0.007 pct S. The alloy was cast as a 150 Ib, 7x7 in. cross section ingot and forged into bars 2x2 in. in cross section. These bars were homogenized for 48 hr at 1250°C in an Endo-Gas atmosphere. The depth to which decarburization penetrated during this heat treatment was determined by chemical and microscopic analyses and the affected metal was removed by machining. Specimens for isothermal transformation studies were cut from the remaining material; most of these specimens were 1/2x1/4X1/16 in., though some with a thickness of 1/32 in. were prepared for use at the shorter reaction times and lower reaction temperatures. Specimens were austenitized for 30 min at 1300°C, isothermally reacted for various times at temperatures ranging from 775" to 475 "C, and then quenched in iced water. The austenite grain sizes within individual specimens ranged from ASTM Nos. 1 through —4. A commercial heat-treating salt which was continuously deoxidized by an immersed graphite crucible served to minimize the loss of carbon during austenitizing; thick covers of powdered graphite and immersed graphite rods effectively prevented decarburization in the lead pots employed for the isothermal reaction treatments. The heat-treated specimens were sectioned and mounted in Bakelite. Following the completion of standard grinding and mechanical polishing procedures, the specimens were electrolytically polished with a Buehler-Waisman apparatus and etched in 2 pct nital. Experimental Results Rules of Evidence for Sympathetic Nucleation—On the basis of observations made on a single plane of polish, one precipitate crystal may be considered to have been sympathetically nucleated at the inter-phase boundary of another precipitate crystal when the following conditions are fulfilled: 1) The sympathetically nucleated crystal is not in contact with a grain boundary or a subboundary in the matrix phase. 2) The shape, size, and location of the crystal at whose boundary sympathetic nucleation occurred (hereafter termed the base crystal) and the crystal formed by sympathetic nucleation substantially pre-clude the possibility that the plane of polish em-ployed may have concealed the fact that both crys-tals actually nucleated at a grain boundary or a sub-boundary in the matrix phase.

Jan 1, 1957

By Charles F. Hickey, Eric B. Kula

Thermomechanical treatments applied to the maraging steels include a) cold working in the austenitic condition at 650°F, followed by transformation to martensite and aging, b) cold working in the murtensitic condition and aging, and c) cold working in the aged condition with and without subsequent reaging. The strength increases in these steels are very small compared to the increases observed in conventional carbon and alloy steels. The changes that are observed are compatible with the strengthening mechanisms operative during thermomechanical treatment of conventional steels, however. Differences are caused by the absence of a carbide precipitate and the low work-hardening rate in both the solution-treated and the aged conditions. ThE 18 pct Ni maraging steels represent a class of steels which are finding great interest for high-strength applications.1~2 They are essentially carbon-free, and contain 7 to 9 pct Co, 3 to 5 pct Mo, and 0.2 to 0.8 pct Ti. Although austenitic at elevated temperatures, they can be air-cooled to room temperature to form a martensite, which because of the absence of carbon is relatively soft. On subsequent reheating age hardening occurs and strength levels of 250 to 300 ksi yield strength can be attained. These steels appear to be particularly suitable for studying the response to various thermome-chanical treatments for additional reasons other than the obvious one of attempting to improve their already attractive properties. Thermomechanical treatments can be defined as treatments whereby plastic deformation, generally below the recrystal-lization temperature, is introduced into the heat-treatment cycle of a steel in order to improve the properties. With an absence of intermediate transformation products on air cooling the maraging steels have good hardenability and hence can readily be cold-worked in the austenitic condition prior to transformation to martensite. Further, they can be worked in the martensitic condition prior to aging, and even can be deformed in the fully aged condition. Finally, it is of interest to compare their re- sponse to that of the more conventional alloy and carbon steels, where the role of carbides is important in the strength increase by thermomechani-cal treatments. The thermomechanical treatment of conventional steels has been the subject of a recent review.' I) MATERIALS AND PROCEDURE The steel used in this investigation was a commercially produced vacuum-melt heat, which had been rolled to 0.090 in. and mill-annealed. The composition of the alloy was as follows: 0.02 C, 0.08 Mn, 0.10 Si, 0.009 P, 0.009 S, 18.96 Ni, 7.34 Co, 5.04 Mo, 0.29 Ti, 0.05 Al, 0.004 B, 0.01 Zr, and 0.05 Ca. Unless otherwise stated the heat treatments used were the standai-d solution treatment at 1500°F for 1 hr, air cool, followed by a 900°F, 3 hr age. In this condition, the material exhibited 232 ksi yield strength and 239 ksi tensile strength. Mechanical properties were determined by Vicker's hardness measurement (20 kg) and by tensile tests on standard 1/2-in.-wide, 2-in.-gage-length sheet tensile specimens. Notch tensile tests were run using the 1-in.-wide NASA type, edge-notched specimen.4 Fracture-toughness determinations were made on 3-in.-wide, center-notched, fatigue-cracked specimens, following the recommendations of the ASTM Committee on Fracture-Toughness Testing.4 An electric-potential technique was used for measuring the crack size at the onset of rapid crack propagation5 which is necessary for calculations of Kc, the critical stress-intensity factor under plane-stress conditions. The critical stress-intensity factor under plane-strain conditions KI, was also calculated, using the stress at which the first observable crack growth occurred. 11) RESULTS A) Cold-Worked in the Austenitic Condition. The reported M, temperature for the 18 pct Ni maraging steel is about 310°F.1 Therefore, a temperature of 650°F was selected as suitable for rolling in the austenitic condition. Specimens were solution-treated at 1500°F for 1 hr, air-cooled to 650°F, and rolled varying percentages from 0 to 60 pct, at 20 pct reduction per pass. Tensile and hardness properties after aging at 900°F for 3 hr are shown in Fig. 1. The tensile strength increases from 253 to 271 ksi and the yield strength from 247 to 265 ksi as a result of a reduc-

Jan 1, 1964

By J. H. Brophy, S. J. Michalik

A constitution diagram for the system Mo-Ir has been determined. The maximum solubility of iridium in molybdenum is 16 at. pct at 2110ºC and decreases to less than 5 at. pct at 1500°C. The solubility of molybdenum in iridium is 22 at. pct. Three intermediate phases appear in the system: 8 MoJr, having the p-tungsten structure; a phase, a cornplex tetragonal structure; and the hcp ? phase. Metallography, melting point determinations, X-ray diffraction and fluorescence, and electron micro-probe unalyses were employed in establishing the diagram. PREVIOUS to the present investigation, the intermediate phases in the Mo-Ir system were identified, but no detailed account of the phase diagram has been reported in the literature. Raub1 investigated alloys of Mo-Ir over an extensive range of composition between the temperatures of 800º and 1600°C. The in-termetallic compound MosIr was found to exist with nearly pure molybdenum, as the solubility of iridium in molybdenum was not detectable parametrically in this temperature range. MO3Ir was found to be iso-morphic with a ß-tungsten type structure, having a parameter of 4.959Å. An intermediate hcp phase, designated as the ? phase, ranged in composition from 52 to 78.5 at. pct at 800ºC, and from 41 to 78.5 at. pct Ir at 1200°C. Parameters noted for the ? phase were as follows: at 42.7 at. pct Ir, a = 2.771i0, c = 4.4366, c/a = 1.601; at 78.5 at. pct Ir, a = 2.736A, c = 4.378A, c/a = 1.600. Molybdenum was found to be soluble in iridium up to 16.5 at. pct Mo (83.5 at. pct Irj, with the parameter of iridium increasing to 3.845A at the solubility limit. Knapton,2 who investigated alloys between 15 and 85 at. pct Ir, essentially agreed with Raub's data, but, in addition, found a a phase in as-melted alloys near 25 at. pcto Ir. The oaphase lattice parameters were a = 9.64Å, c = 4.96Å, c/a = 0.515. The a phase was replaced by the 8 -tungsten phase on annealing at 1600°C. Knapton concluded that the a was stable only at elevated temperatures, and placed the composition of the a phase at approximately 30 at. pct Ir. The intermetallic compound Mo3Ir, with a lattice parameter of 4.965A, was included among the 8-tungsten structures reported by ~eller.' Matthias and Corenzwit,4 and Bucke15 studied the superconducting nature of MosIr, and reported a superconducting transition temperature of 8.$K. The present investigation describes the phase relationships in the Mo-Ir alloy system determined by melting point measurements, X-ray diffraction and fluorescence, and metallography. EXPERIMENTAL PROCEDURES Alloys for the determination of the phase diagram were prepared from powders. Commercial 99.9 pct Mo from Fansteel Metallurgical Corp. and 99.9 pct Ir powder from J. Bishop and Co. Platinum Works were used. The powders were weighed to nominal compositions, mixed, and then pressed, without binder, into compacts weighing 4 to 6 g. These were presintered in uacuo between 1200' and 1400°C for 1 hr, to reduce the degree of spattering during subsequent arc-melting. The compacts were arc-melted in a nonconsumable tungsten electrode furnace six times on alternate sides on a water-cooled copper hearth in an atmosphere of zirconium-getter ed argon at 500 mm of mercury pressure. In almost all cases, this procedure yielded buttons of satisfactory homogeneity. The composition of all melted buttons were confirmed by X-ray fluorescent analysis using the experimentally determined ratio of the iridium La1 line intensity to that of the molybdenum Ka1 line as a function of composition. In this determination four alloys analyzed by wet chemical methods were used as standards. An uncertainty range of ±1 at. pct has been attributed to all indicated compositions. All heat treatments and solidus measurements were carried out in tantalum resistance heating elements in vacuum conditions of 10-4 to 10-5 mm of mercury. A detailed account of this procedure has been reported by Schwarzkopf and Brophy.8 In the heat treatment and solidus measurements of iridium-rich alloys (50 at. pct Ir or greater), a tungsten lining was inserted into the tantalum resistance heating element because of a eutectic reaction which occurs between iridium and tantalum at 1948ºc.7 Heat treatments and solidus measurements carried out at compositions less than 40 at. pct Ir both with and without tungsten linings within the resistance

Jan 1, 1963

By Raymond C. Boettner

The present work had for its purpose: 1) the identification of crack nucleation sites in AISI 4340, quenched to martensite and tempered over a range of 'temperatures; and 2) the comparison of fatigue processes in AISI 4340 with processes observed previously in pure metals From constant def1ection-bending fatigue tests, martensite boundaries were identified as the favored crack nucleation sites in quenched and tempered AISI 4340. It, also, was concluded that the fatigue processes operating- in this lous-alloy steel were similar to Processes observed in pure tnetals. ALTHOUGH much engineering data has been accumulated on the fatigue properties of quenched and tempered martensitic steels,' fatigue as a process is not as well understood in martensite as it is in pure metals.' Important features of the fatigue process, such as the identity of the nucleation sites, have not been determined in the commercially important high-strength low-alloy structural steels. The present work had for its purpose: 1) the identification of crack nucleation sites in a low-alloy steel, i.e., AISI 4340, which had been quenched to martensite and tempered over a range of temperatures; and 2) the comparison of fatigue processes in the AISI 4340 with processes observed previously in pure metals. This comparison of the fatigue processes in the different tempers was restricted to the high-strain low-cycle part of the S-N curve. Under these test conditions, previous work on a number of metals has shown that a large number of cracks are nucleated in less than 30 pct of the fatigue life.3 Furthermore, crack nucleation sites are not restricted to inclusions but are also associated with intrinsic structural characteristics of the metal. MATERIAL A 20-lb ingot of vacuum-melted AISI 4340 (for composition see Table I) was hot-rolled to 1-in.-diam rod and then cold-rolled to a 1-in.-wide strip, 0.08 in. thick. Fatigue specimens, see insert of Fig. 1, were machined from the strip with the long dimension parallel to the rolling direction. m this orientation, the stringers of 1 to 2 p inclusions present in the sheet lay parallel to the stress axis in the specimens. The specimens were austenitited at 2050°F in order to obtain a large prior austenite grain size, i.e., 2 mm, which facilitated the subsequent identification of the prior austenite boundaries. A helium atmosphere was used to minimize decarburization. After austenitiza-tion at 2050°F, the specimens were transferred to a 1450°F furnace so that specimen distortion was held to a minimum in the subsequent oil quench. Previous work4 indicated that refrigeration in liquid nitrogen prior to tempering reduced the percentage of retained austenite in the quenched specimens to less than 5 pct. Tempering was carried out in air over the temperature interval of 200°to 800°F to produce a range of mechanical properties, Table I. The preparation of the fatigue specimen was completed by grinding about 0.005 in. from each surface and electropolishing in a chrome trioxide-acetic acid solution for 30 min. Examination of etched cross sections of specimens prepared in this fashion showed the foregoing specimen preparation to be adequate for the removal of the decarburized layer present after the heat treatment. Transmission electron microscopy showed that the as-quenched microstructure of this alloy consisted of a mixture of martensite plates containing either a high density of dislocations or microtwins. Previous work5'6 indicated that in the course of oil quenching autotem-pering resulted in the formation of E carbide on the martensite and microtwin boundaries. Tempering for 2 hr at temperatures up to about 400°F resulted in further precipitation of the E carbide. Finally, at about 400°F, cementite began to replace the E carbide on the martensite and microtwin boundaries in addition to forming a Widmanstatten structure within the plate matrix. EXPERIMENTAL S-N curves were obtained using electropolished specimens cycled at 1800 cpm as cantilever beams in fully reversed bending at selected constant deflections. The deflections were translated into surface strains by means of a calibration curve obtained through the use of strain gages. An argon atmosphere was used to minimize environmental effects. To investigate the development of fatigue slip bands, the specimens of the different tempers were unidirec-tionally bent to a surface strain of 0.005 to 0.007, photographed to record the location and appearance of slip bands so introduced, and then cycled to failure

Jan 1, 1968

By H. I. Smith

WHEN Spain established colonies on the North American continent, some of her land grants, in what is now the United States, reserved to the Crown deposits of gold, silver, and mercury. Later mineral rights were reserved under some of the English Crown charters involving land in the eastern part of North America, with provisions for the payment of royalties thereon to the Crown. Reservation of mineral deposits to the United States Government was instituted by an ordinance of Congress on May 20, 1785, which applied to such deposits in the Northwest Territory, then north of the Ohio River and east of the Mississippi River, and provided that there should be reserved "one third of all gold, silver, lead, and copper mines, to be sold or otherwise disposed of as Congress shall hereafter direct." Little was known then of the mineral resources of the country; the Great Lakes copper region had just come into the possession of the United States by treaty and much of the western mineral land still belonged to France and Spain. The policy of leasing mineral deposits was enacted by Congress under the act of March 3, 1807, which provided that "the President of the United States shall be, and is hereby, authorized to lease any lead mine which has been or may hereafter be discovered in the Indiana Territory, for a term not exceeding five years," and in the same year the Government reserved 345,600 acres of land in northern Illinois, valuable for lead. In 1816 Congress provided that in all cases where a tract of public land containing a lead mine or salt spring was applied for by settlers on the public domain, no permission to work the mine or spring would be granted without the approbation of the President of the United States. By the act of March 1, 1847 (9 Stat. 146), the control of mineral lands was transferred, with all records, from the War Department to the Treasury Department, and by the act of March 3, 1849 (9 Stat. 395), supervisory powers over lead and other mines of the United States were transferred to the Secretary of the Interior. Following the discovery of gold in California in 1848, President Polk advocated the leasing of mineral lands acquired from Mexico under the treaty of 1848. However, owing to the lack of communication and transportation facilities and the consequent difficulty of checking on production and operations, leasing was found impracticable. Mining was permitted to be carried on in each district under rules made by the miners themselves and patterned after the Mexican mining system. To meet the situation, Congress enacted mining laws in 1866, 1870, and 1872, which provided for possession by location and for private ownership, after discovery, by patent of essentially all mineral deposits belonging to the United States, except coal. Many other acts were passed by Congress applying to specific regions and states, reserving salt, lead, or other minerals, some of which provided for the leasing of such deposits. However, very few if any leases were issued thereunder. Not until 1901 (31 Stat. 745) were the mining laws extended to include salt, and in 1910 they were revised to specify salines and associated products. At the turn of the century, it became more and more evident that the mining laws developed for metallic minerals were not practical for the development and conservation of oil and gas, coal, potash, phosphate, or oil shale. Following withdrawals by the Secretary of the Interior as authorized by the act of June 25, 1910, the Department of the Interior recommended leasing legislation; however, it was not until February 25, 1920, that the Mineral Leasing Act was passed by Congress. This act authorized leasing all public lands potentially valuable for oil, gas, coal, phosphate, sodium, or oil shale. The Organic Act, creating the Geological Survey in 1879, imposed upon its director the duty of classifying the public lands.' The early years of the Survey were devoted largely to the accumulation of fundamental data and, with only minor exceptions, land classification was not seriously undertaken until 1906. Since that year, it has been actively pursued with respect particularly to leasable minerals and water power values. On March 3, 1873 (17 Stat. 607) Congress authorized the sale of coal lands of limited acreage to individuals at $10 to $20 an acre, depending on the distance from a railroad, and in 1907 a new scale of prices was adopted by the Secretary of the Interior, based, more logically, on the quality and thickness of the coal deposits, their depth below the earth's surface, and their accessibility. At that time it was much cheaper and easier to obtain incidental title to coal rights under the homestead laws at $1.25 an acre. On March 3, 1909, the first separation act (35 Stat. 844) became a law. It authorized patents, with a reservation of the coal and mining rights involved to the United States, to persons who in good faith had entered public lands under the non-mineral land laws prior to withdrawal, classification, claim, or report that such lands were valuable for coal. It solved the problem only partially, and the practice thereupon adopted by the department of making coal withdrawals "from all forms of entry" instead of "from coal entry" expedited the more complete solution effected by later acts. By the act of June 22, 1910 (36.Stat. 583) withdrawn and classified coal lands were declared subject to entry under the homestead, desert land, and Carey acts, provided a waiver of the coal rights accompanied the application, and by the act of April 30, 1912 (37 Stat. 105) the same privilege was extended to State selections and isolated tracts. The act of August 24, 1912 (37 Stat. 496) extended the separation policy to lands withdrawn for oil and gas in Utah, and finally the act of July 17, 1914 (38 Stat. 509) extended it to all nonmineral filings on public lands theretofore or thereafter

Jan 1, 1955

By J. B. Newkirk, A. H. Geisler

The alloy Cu4Pd has a disordered face-centered-cubic structure when quenched from temperatures between 478ºC and the melting point (about 1100°C). Below 478ºC an ordered phase is stable. The results of a Debye-Scherrer X-ray analysis indicate that the ordered phase has a tetragonal unit cell described by the space group C24h — P42/mt with 2 Cu in 2a, 2 Cu in 2f, 4 Cu in 4j (x = 0.2, y = 0.6), 4Pd in 4j (x = 0.4, y = 0.2), and 8 Cu in 8k (x = 0.1, y = 0.3). The orientation relationship between the face-centered-cubic phase and the ordered tetragonal phase is given by: [100],,. // [130]al,. COO1Ia.d.//COO1I,,.. • The behavior of Cu,Pd is typical of ordering alloys except that the transformation is very sluggish. The increase in hardness and the microstructural and X-ray diffraction effects are interpreted in terms of coherency strains caused by the ordering. AN anomalous construction in the Cu-Pd phase diagram (Fig. 1) was reported in 1939 and has been allowed to stand without further published attention since that time. The odd figuration about the composition 10 to 27 atomic pct Pd is derived mostly from the work of Jones and Sykes.1 Evidently several features of this binary system require further study if the constitutional forms are to be well understood. The present paper includes a study of one of these features, that is, the crystal structure of a single ordered alloy containing nominally 20 atomic pct Pd. This choice of composition was suggested by the work of Harker and associates who determined the structure of Ni4Mo2 and Ni4W.3 The nature of the ordering process in Cu4Pd was studied also by observing the hardness, microstructure, and Debye-Scherrer patterns of specimens which had been aged at various temperatures after quenching from an initial disordering treatment. Experimental Methods A 20 gram ingot of Cu4Pd was made by melting spectrographically standardized copper from Johnson, Matthey, and Co., and commercially pure (99.5 + ) palladium in an argon-filled quartz tube. Chemical analysis showed that the ingot contained 80.0 atomic pct Cu. The ingot was rolled about 60 pct to a strip 0.060 in. thick and was homogenized for 16 hr at 950°C in low pressure argon. Rods cut from the rolled strip were worked into wire 0.015 in. in diameter, and specimens for hardness and microscopic examination were cut from the remaining strip. All specimens, with the exception of some of the wire, were given an initial disordering treatment by heating for 16 hr at 950°C, followed by water quenching. A 10 cm length of as-drawn wire was water quenched after being held in a temperature-gradient furnace4 for 89 days. Room-temperature Debye-Scherrer photograms were then made at points along the wire to determine the temperature below which the ordered phase was stable. Although the accuracy of temperature determination in the gradient was only about ±10 °C, the temperature gradient was sufficiently gradual that the sensitivity was much better and locations which had differed by as little as 1°C could be distinguished. An analysis of the crystal structure of the well ordered alloy was made by X-ray diffraction using a specimen cut from this wire. The change of Debye-Scherrer pattern as ordering progressed was studied by using isothermally aged samples of initially disordered wires. The wires were sealed under low-pressure argon in small quartz tubes for heat treatment. After the aging treatment, the tubes were quenched in water and photograms were made at room temperature in a 10 cm diam camera using filtered Cu kX. (A = 1.540511) Hardness was measured on a Vickers hardness tester using a 10 kg load and 2/3 in. objective lens. Reported values are the average of at least three impressions made on flat specimens 0.060 in. thick. After the hardness of a heat-treated sample had been measured, it was resealed in low-pressure argon and returned to the furnace for continued aging at the same temperature. In this way, two samples served for all aging times at each temperature. Hardness specimens which had been aged 500 hr or more were used for metallographic examination after the final aging treatment. A dilute potassium-dichromate etching solution was used.

Jan 1, 1955

By D. Mills, G. B. Craig

ZIRCONIUM has been float-zone-refined in an electron-beam furnace and the redistribution of oxygen, iron, and tungsten has been measured. The iodide zirconium used in the present experiments initially contained both oxygen and iron in the range 100 to 200 ppm by weight, and tungsten in amounts less than 10 ppm. Float-zone refining of zirconium, using induction heating, has previously been attempted by Kneip and Betterton1 and Langeron.2 Kneip and Betterton were primarily interested in the removal of iron and nickel. They achieved some purification, with respect to both these elements, in material given up to six passes at 150 mm per hr under an argon atmosphere. Langeron reported purification for a large number of elements after four completed passes in a static vacuum system operating at pressures less than 10-6 mm of Hg and with rates of zone travel between 30 and 40 mm per hr. He did not report oxygen concentrations, but stated that there was inverse segregation of this element. westlake5 has also used a minimum of four zone passes to remove iron from zirconium. No rates or conditions were given. Belk6 has shown that tungsten contamination can occur during electron-beam melting. He reported an increase from 0.01 to 0.05 pct by weight tungsten in molybdenum after four complete zone passes. The vacuum system for the electron-beam unit used in the present investigation consisted of a single-stage rotary pump backing a liquid-air-trapped oil-diffusion pump. A pressure of less than 10-8 mm of Hg was obtained with Dow-Corning 705 fluid in the diffusion pump. In order to avoid contamination of the zirconium by evaporation from the tungsten filament, a special focusing cage4 was employed. Three rates of zone travel, 114, 38, and 4 mm per hr, were investigated, with the liquid zone moving from the bottom to the top of the bar. The bars used were 3 mm diam and the total melted length was 130 mm. Oxygen was analyzed by neutron-activation analysis using a neutron flux of 10' neutrons per sq cm per sec to form the isotope N16 by the 016 (n,p) N16 reaction. The standard deviation is quoted for each oxygen determination. The iron and tungsten analyses were performed spectrographically, and the precision is estimated to be ±6 pct. Analyses for tungsten were all below the detectable limit of 10 ppm, confirming the protection given by the focusing cage. No significant redistribution of oxygen was found at the two higher rates of zone travel. The redistribution of oxygen and iron obtained after five passes at a rate of zone travel of 4 mm per hr (1.1 x 10-4 cm per sec) is recorded in Tables I and 11. Burris, Stockman, and Dillon3 have estimated the distribution of solutes during multipass zone refining. Using their curves for an effective distribution coefficient of Keff = 1.5 and 2 for oxygen and Keff = 0.3 for iron, the expected concentrations were estimated for the present material. These are shown in Tables I and 11, along with the experimentally measured values. The calculated concentrations are based on a molten-zone length of 10 pct of the total melted length, whereas in the present experiments the molten zone was approximately 5 pct of the total melted length. The effect of zone length on solute redistribution is most pronounced after a large number of zone passes. Comparison with Pfann's published data8 for solute redistribution for various Keff's and zone lengths indicates only small differences at low numbers of completed zone passes. It is evident that the expected distribution has not been realized in the case of iron. Scrapings of material deposited on the inner surfaces of the electron-focusing cage were found to be magnetic. It is, therefore, concluded that redistribution of iron is masked by evaporation. Deposition of iron inside the focusing cage was observed at all rates of zone travel. The results of the investigation may be summarized as follows: 1) Segregation of oxygen is typical for a solute with a distribution coefficient, Keff > 1. 2) No redistribution of oxygen takes place at high rates of zone travel. 3) The distribution coefficient for oxygen lies between 1.5 and 2.0. 4) Purification with respect to iron occurs mainly by evaporation. 5) The focusing cage is effective in preventing tungsten contamination.

Jan 1, 1967

By Eckhard Nembach

The phase diagram of the system Pb-In has been investigated between -27° and + 40°C, using nzainly X-ray dijfraction. In accordance with t her mo dynamic measurements by Heumann and Predel, a segregation occurs at low temperatures, though not in the form of a nziscibility gap. THE phase diagram of the system Pb-In has been the subject of extensive investigations,1&apos;1 but recently Heumann and prede13 concluded from their thermodynamic data that a new feature should occur below room temperature. These authors observed that the maximum values for the enthalpy and entropy of mixing, which occurred at a composition of 50 at. pct Pb, were +400 and —1.7 cal per g-atom deg, respectively. From this the authors estimated that a miscibility gap should occur below 30°C, centered at 50 at. pct Pb. Resistivity measurements seemed to support this view. These authors proposed the phase diagram outlined in Fig. 1. Three phases exist at 30°C: the tetragonal indium phase with c/a > 1, the tetragonal intermediate phase a, with c/a < 1, and the fcc lead phase. During an investigation of the superconducting properties of Pb-In alloys. it has been observed4 that aging a specimen with 50 at. pct Pb for 14 days at -18°C decreased the superconducting transition temperature about 0.13"K and tripled the transition width. In this paper, the results of an investigation of the Pb-In phase diagram in the temperature range from — 2T to +40°C are reported. Superconductivity and X-ray methods have been used. 1) SPECIMEN PREPARATION The materials were provided by the American Smelting and Refining Co. According to the manufacturer their purity was 99.999 pct. The weighed amounts of the constituents were sealed in quartz tubes under an atmosphere of 10 torr helium, mixed for 24 hr in a rocking furnace at 380°C, quenched in ice water, and homogenized at 20" to 30°C below the solidus line, established by Heumann and Predel. The annealing times were 144 hr for specimens containing Less than 30 at. pct Pb and 36 hr for the remainder. 2) SUPERCONDUCTIVITY EXPERIMENTS The specimens were quenched from the homogeniza-tion treatment into ice water and their superconducting transition temperatures T, measured. The procedure used has been described in Ref. 4. The transition was detected by the change of the mutual induc- tance of two coaxial coils containing the sample. T, was defined as the temperature at which 50 pct of the total change in inductance had occurred. The repro-ducibility with which T, could be measured was i0.002"K. Then the specimens with lead contents between 38 and 75 at. pct were aged for 7 days at temperatures between -30" and 40°C. If this treatment caused T, to change by more than 0.005"K or the width of the transition to increase by more than 0.002"K, it was concluded that the specimen had undergone a phase change and no longer consisted only of the fcc lead phase: as it did immediately after homogenizing. The result is shown in Fig. 2. From this one can estimate at what temperatures and concentrations phase changes occur. The X-ray measurements were based on these preliminary results. 3) X-RAY EXPERIMENTS Because of the softness of the material, relatively coarse powders. 75 p, had to be used, which were filed in a helium atmosphere from homogenized specimens. The powders were annealed at least 30 min at temperatures between 120" and 16OJC, depending on their concentration, and quenched in ice water. Then their X-ray patterns were taken at -178°C with a Picker diffractometer, model 3488K, and a cold stage. on which the specimen was in thermal contact with a liquid-nitrogen reservoir. In this way the following relation was established for the fcc lead phase: a = 4.697 + 0.00247C for 40 5 C 5 75 11 where n is the lattice constant (A) and C is the at. pct of lead. The coarseness of the powder made it impossible to use lines with 0 > 75 deg; therefore n was averaged from lines with 45 deg 5 0 5 75 deg. The results were reproducible to within i0.05 pct. Relation [I] is very similar to the one found by Heumann and Predel at room temperature. Following this, homogenized specimens with compositions between 15 and 56 at. pct Pb were aged for at least 10 days at temperatures between -27" and

Jan 1, 1970

By Arthur F. Taggart

MR. CHAIRMAN: Congratulations! Your four-ring milling show this year was a dandy. It cleared our minds, for a few hours at least, of what Hitler, Hirohito, the New Deal, and the tribe in the Treasury are trying to do to strangle American enterprise. We mustn&apos;t forget this, but it&apos;s a relief to get our thoughts away from it occasionally. GRINDING-There was a further contribution to the excellent work that the Allis-Chalmers laboratory staff has been doing for the grinding fraternity in compiling-and publishing-a carefully quantitative list of comparative resistances of ores and other materials to comminution (T.P. 1579, Bond-Maxson). A diagnostic accuracy of ± 10 per cent was claimed for estimates based on these figures. Are they really that good? How about some of you men in the field writing M&M about it?

Jan 1, 1943

Jan 1, 1941

Jan 1, 1941

By D. F. Kaufman, E. D. Levine, L. R. Aronin

The deformation of&apos; impure beryllium crystals by basal glide at room temperature invariably tevminates by basal cleavage after a few percent strain. It is generally accepted that .fracture of this type is caused by the splitting of low) -angle boundaries, or bend planes, by obstacles that restrict the motion of the bed planes in the deforming crystal. The details of such a process have been developed by Stroh, who showed that the high tensile stress norrnal to the basal plane in the region where the bend plane is split results in the propagation of a basal cleavage crack, provided there is no available dejorvrlatzon mode having a shear component normal to the basal plane It has been postulated that puvification of beryllium might lead to increased basal ductility by the vemoval of barviers to bend plane motion and possibly by the activation of nonbasal defor~rlation systems. Large increases in the amount of basal glide that can he sustained prior to fracture have been observed in crystals purified by zone refining. In each case, eventudal fracture was by sharp basal cleavage, suggesting that the split bend plane model still applies to tile fracture of beryllium of rensonably high purity. In the present work, calculations are made to show to what extent basal duetilits can be increased by purification while the split bend plane .fracture process remains applicable. Experimentally observed ductilities are generally somewhat lower than those predicted by calculation because of premature failure due to defects introd~cced during specimen preparation and testing. SEVERAL investigators1-4 have studied the deformation characteristics of beryllium single crystals of commercial purity, and have related the strong anisotropy of plastic deformation in single crystals to the problem of brittleness in polycrystalline beryllium. For most orientations, the principal deformation mode is basal slip, which, at temperatures between 300" and 900°K, begins at a critical resolved shear stress of approximately 1500 g per sq mm and terminates after 3 to 6 pet glide strain by cleavage on the basal plane in the neighborhood of (1120) bend planes that are formed during the deformation. This type of fracture, which is also observed in zinc at low temperatures, has been interpreted by stroh5 to be caused by the splitting of bend planes by obstacles to their motion. In the Stroh model, a (11.20) dislocation wall, or bend plane, moving along the slip direction under the action of the applied stress, encounters obstacles which cause part of the bend plane to be held up, the other part continuing to move. Stress concentrations are built up in the region where the bend plane is split, with a high tensile component normal to the basal plane, resulting in a microcrack at the end of the split wall. Because no deformation mode having a shear component at an angle to the basal plane is available to relieve the stress at the crack tip, the crack can propagate under a sufficiently high applied stress. The Stroh criterion for crack propagation is given by

Jan 1, 1964

By D. Harrington

WHEN the word gas is mentioned in connection with mining, almost invariably it is inferred that the explosive gas, methane, is in mind and that it must refer to coal mining. While it is true that methane occurs, or is likely to occur, in almost any or all coal mines, it is also a fact that the metal mines of the world have in them by far a greater variety of gases than have the coal mines. In many cases the gases in metal mines are as dangerous to individuals as the gases likely to be found in coal mines; in some instances the metal mine gases are even more deadly. The coal mine is more likely to have methane than the metal mine, in rare instances it may have high percentages of nitrogen or high carbon dioxide, or there may be a deficiency of oxygen where the air is confined in a blind end or in a sealed region; much more rarely there are found in coal mines in relatively small percentages, ethane, or other hydrocarbons with odor of ether, gasoline or kerosene, or there may be minute percentages of hydrogen sulfide. In time of coal mine fire or explosion, there is likely to be high carbon monoxide (4 per cent. or over in some cases) and if the coal contains much sulfur, there may be some sulfur dioxide in the fire fumes. In metal mines there are a number of cases of occurrence of methane and attendant explosions; some metal mines have appreciable percentages of the decidedly explosive hydrogen; in some metal-mining regions carbon dioxide flows into the mine, fills the workings and overflows just like water. In other regions, at many working faces there are high-temperature gases containing a mixture of gases of sulfur (sulfur dioxide, hydrogen sulfide and possibly SO3 in some cases) together with carbon dioxide and nitrogen, and the deadly hydrogen sulfide in lethal proportions is found in some high-sulfide metal mines at blasting time. Carbon monoxide constitutes a decidedly dangerous day by day hazard in connection with metal-mine blasting, because of the heavy charges of dynamite that are used and the use of fuse, which in burning gives off much carbon monoxide. The poisonous gas hazard is accentuated because of the relatively small openings where metal-mine blasting is done and to the inefficient ventilation of the usual metal mine.

Jan 1, 1930

By William Laird

The predominent method of coal mining in the United States for years has been room-and-pillar mining. The reason for this has been the advantages of room-and- pillar method which is a relatively flexible system and its capital investment. The room-and-pillar method permits some selectivity in mining, especially where gas wells, faults and possible coal quality may be a factor. The mobility of continuous and conventional mining equipment used to develop entries may also be used for retreat mining of rooms and pillars. Longwall mining of coal takes place along a long straight face, or wall, blocked out between two butt or panel entries. The long faces or walls are normally projected in lengths of 61 to 183 m (200 to 600 ft) in this country. The longwall method of mining had its beginning in the United States during the 1800&apos;s. During that period, pack wall and wood posts were used for roof support. The longwall face was mined by miners using picks to undercut the coal. To keep the coal face from turning over, short wood posts called sprags were set in a slant position as the coal face was undercut to the depth of two to three feet. When the under-cutting cycle was completed, the sprags were removed to permit the coal to fall from the roof pressure. The longwall mining of coal did not take a firm hold during the 18009s, and room-and-pillar prevailed. In the early 19009s, steel jacks were introduced, and along with it, the modified caving theory. In March of 1950, a retreat longwall mining system, utilizing a plow, manually operated props, wood cribs and chock releases, was installed in one of Eastern Associated Coal Corp.&apos;s mines.

Jan 1, 1981

By George W. Hezzelwood

THE Balatoc mine, one of the Haussermann group,† is on the Island of Luzon, the largest of the Philippine group, about 260 km north of Manila, and 12 km from the city of Baguio The Baguio district is the most important gold-mining area of the Philippines, with 14 producing mines in 1939, milling 2,358,804 tons of ore, yielding [P]40,881,048, approximately 55 per cent of the total Philippine production of [P]74,131,216 PRODUCTION HISTORY The Balatoc mine began production In January 1929 with a 150-ton cyanide mill Increases in mill capacity have taken place as follows March, 1932, to 330 tons June, 1933, to 470 tons December, 1933, to ;15 tons July, 1934, to 700 tons December, 1934, to loon tons May, 193, to 1200 tons October, 1938, to 1300 tolls April, 1939, to 2000 tons January, 1941, to 2T50 tons Production during the period of expansion has steadily increased in total value in spite of the fact that grade of ore milled has dropped-from $31 06 in 1929 to $5 78 in1940 Annual reports give production as shown in Table I, the average value, being based on gold at the old price of $20 67 per ounce [ ] GEOLOGY The ore occurs in quartz-calcite veins that vary in width from narrow stringers to mineralized zones 40 to 30 ft wide Wall rocks consist largely of diorites, with some andesite, and a fragmental breccia called locally the "Balatoc plug " Texture of the ore varies widely in the different vents-from a soft, highly altered, gouge material filled with quartz fragments through a soft, unaltered quartz-calcite to a hard, massive quartz ore Three major vein systems have been extensively developed, and smaller amounts of work have been done on several others These veins strike east-west to N 60°, clipping south from 50° to 90°, and are essentially tension breaks between a series of faults or shears striking N 30°E to N 30°E and clipping southeast from 50° to 90° The shear veins and tension veins probably formed more or less simultaneously,

Jan 1, 1942

By John B. Hastings

The occurrellce of such a large amount of gold in the Hart-eel granite, even though the surmised existence of similar areas is not new, brings freshly to mind the pegmatite type of mag-matic differentiation lately brought again to attention by occurrences at Silver Peak, Nev., described by Spurr; and in Alaska, described by both Spurr and Brooks. In both localities granitic rocks or dikes are thought to pass into metalliferous quartz-veins. An interesting association in this connection is the occurrence of diamonds in residual pegmatitic clay of Sail Juao de Chapado, Brazil, described by Derby :&apos; (P. 142) "Bodies of pegmatite are quite common in the older rocks of Brazil, both in the diamond regions and elsewhere, occurring not only in the gneiss and granite, but in the schistose series as well. Those that have been examined are dike-like in their mode of occurrence and granitic in composition.&apos;&apos; (P. 143) &apos;" The question of the eruptive or secretionary origin of pegmatites has long been a subject of discussion among geologists.... The recent studies .. seen] to have clearly established that most if not all of them are essentially eruptive masses, though possibly modified in some way by aqueous agencies. Even before becoming acquainted with the literature of the subject this view had seemed to me to be the only acceptable one as regards the typical pegmatites of Brazil." What is pegmatite ? J. F. Kemp says :2 "... veins or dikes—it is an open question which is the more correct term— are met formed of very coarsely crystalline aggregates of the same minerals that constitute granite. These are called pegmatite and in them is the home of graphic granite, the curious intergrowth of quartz and feldspar, such that a cross fracture of the blades of quartz suggests cuneiform characters.... In regard to the larger veins or dikes it seems improbable that true igneous fusion could have afforded such coarsely crystalline aggregates, and so we are forced to assume such abundance of steam and other vapors, i.e, mineralizers, as to almost, if not quite, imply solution."

Jan 1, 1909