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By J. H. Wernick, D. Dorsi, K. E. Benson

A LTHOUGH a considerable number of experi--ti mental investigations dealing with the roasting of sulfide minerals have been reported in the past,'"" the behavior of the single roasting particle does not appear to have received the attention it perhaps deserves. This is understandable in that the natural sulfide counterpart of the slab or sheet of metal normally used in high temperature oxidation studies is difficult to obtain and prepare, and is, in most cases, virtually impossible to maintain in one piece at roasting temperatures. The employment, on the other hand, of static aggregations of small particles in masses great enough to permit evaluation of the roasting reactions by means of thermobalances or gas analyses introduces other complications, such as localized overheating, sintering, and variable gas-solid contact. In this investigation a compromise between the above extremes was attempted. Closely sized (e.g., 30 to 40 mesh) particles of natural sulfide minerals were isothermally roasted, out of contact with one another, in an air-swept system. The progress of the roasting reactions was followed by examination in polished section of the treated particles and by X-ray and chemical analysis of their residual sulfide kernels. In this way some conclusions respecting the mechanism of roasting reactions were drawn. Roasting Furnace—The vertical tube furnace used for roasting the sulfide particles had a heated zone 10 1/2 in. long in which four retractable light gage stainless steel trays were suspended. Each tray, and an accompanying baffle, was mounted on a 2 in. iength of 3/8 in. stainless steel tubing. These assemblies were axially suspended on a 30 in. length of in. stainless tubing, by means of which they could be lifted from the hot zone to a water-cooled brass chamber at the top of the furnace. Since each tray unit could slide freely on the 30 in. tube, any desired number of the trays could be retained in the cooling chamber by the manipulation of a horizontal plunger during a momentary withdrawal of the four trays from the hot zone. Although three heating coils, each equipped with variable external resistance, were employed, it was found impossible to avoid a drop of 10O to 15OC between the temperature at the top tray and that of the lower three. Consequently, only the bottom three trays were used for roasting. Temperature readings inside the furnace were made by means of a thermocouple inserted down the tray support tube at tray levels, and a separate thermocouple, inserted adjacent to the middle heating coil, was connected to a Micromax temperature control unit. Experimental Method—The sulfide minerals were obtained in a form as free as possible from gangue and contaminating sulfides, and were crushed and screened to the required particle size range. The tray assembly was kept inside the furnace during the heating-up period and, when a steady temperature had been reached, the trays were withdrawn. Each tray was sprinkled with from 200 to 500 mg of the sulfide grains, and the assembly was lowered into the furnace without delay in order to minimize the time required to achieve the operating temperature. The furnace top was then clamped into position and the thermocouple inserted down the center tube to the required level. It was found that, when this procedure was used, the trays achieved their former temperature within 2 min, after which time the flow of dry air was begun at a rate of 1 liter per min, and timing of the run was started. At the required intervals of time the trays were successively withdrawn from the hot zone and stored in the cooling chamber by means of the retention plunger. On completion of the run the treated particles were removed from the trays to be set aside for examination. The roasted particles were mounted in Lucite on a Buehler press operating at a temperature of 146°C

Jan 1, 1958

Extraction under very mild conditions - a few minutes at room temperature with poor solvents - yields results characteristic of surface properties for a variety of coals. Such superficial extractions preferentially remove long-chain aliphatic compounds. As coal becomes more oxidized, less of these yellow- colored compounds is extracted, forming the basis for a simple colorimetric test for coal surface quality. The fact that these aliphatic compounds are responsible for surface hydrophobicity is supported by good correlation between extraction results and floatability, which decreases with decreasing extractability. This extraction test is very sensitive to oxi dationb even the effect of heating for an hour at 100 C can be detected. A second extraction test using mild alkali conditions has shown good correlation with plant dewatering Operations.

Jan 1, 1986

By Henri S. Swolfs

INTRODUCTION In this paper we present preliminary results of a research program in site characterization methodology. We are interested in under- standing the response of discontinuous rock to mechanical, hydrologic, and thermal loadings. To carry out such a study we selected a field site with simple geology, uniform distribution of lithologies, and easily verifiable boundary conditions on temperature, fluid flow and stresses. The spatial distribution of fractures at the site was established and tests were conducted to determine the temperature field, hydrology, rock-mass properties, and in situ stresses. As part of the study selected borehole instruments were compared to assess their performance and reliability. SITE GEOLOGY The study area is in the eastern part of South Table Mountain, a mesa near Golden, Colo. The exposed cap rock is a single lava flow of uniform thickness (6-7 m) that rests on the clastic sediments of the Denver Formation (Van Horn, 1976). The surface of the cap rock (N. 75º E., 3º S.) is topographically featureless and slopes south- southeast; drainage is predominantly downdip and punctuated by occasional contact springs. The age of the lava flow is 64-65 m.y., or early Paleocene. Paleo- botanic evidence confirms the upper part of the Denver Formation as Paleocene (Van Horn, 1976). "Rapid-rock" analyses of core samples from the lava flow at three depths (0.2, 3.3, and 5.8 m) suggest a uniform chemical composition throughout with an increase in the Fe2O3/ FeO ratio (1.05 to 1.60) with increasing depth, reflecting the existence of a perched water table in the lava flow, To identify the rock

Jan 1, 1984

By N Meyer

This paper presents a research project referring to the stability of submerged walls of open pit mines and the actual state of development. Obviously the slope stability analysis is always a rather complex problem, because it is difficult to reduce the problem to a design scheme and to define the available in situ soil strength. Especially the design of submerged slopes represents a problem. The state-of-the-art slope stability analysis is based on a simplified modelling of slope failure and soil behaviour and with this predicted stable slope inclinations of sand slopes below water-table are less then half the angle of internal friction. Slope angles calculated like that canÆt satisfy the mining companies. One of the problems that have to be solved is the reliable determination of the long-term stability of non-cohesive, submerged slopes, which is not only dependant on geotechnical and hydrogeological parameters of the subsoil, but is also significantly influenced by how the slopes are made. The research project points at the relations between mining and geotechnical engineering with the main aim to find a more suitable stability analysis which takes both soil behaviour and mining influences into account.

Jan 1, 2003

By Wenjun Duan, Kun Wang, Qingbo Yu, Qin Qin

"A novel oxygen production technology noted chemical looping air separation (CLAS) was introduced and properties of Cu-based oxygen carriers used were investigated. The oxygen carriers were prepared by mechanical mixing. Al2O3, Fe2O3, ZrO2, TiO2 and SiO2 were used as binders during the preparation. XRD patterns show that spine! oxides are formed using Al2O3 and Fe2O3 as binders. Phases of CuO and binders keep stable using ZrO2, TiO2 and SiO2 as binders. BET values of oxygen carriers increase in the order of ZrO2>TiO2>SiO2>Fe2O3>Al2O3. The effects of temperatures, binders, particle sizes and flow rates on reduction/oxidation reaction rates were studied in TG experiments. The reduction reaction rate increases in the order of ZrO2>TiO2>SiO2. The effect of binders on the reactivity of oxidation is not obvious. The reduction and oxidation reaction rates both have the tendencies of increasing with the temperature increasing and with gas flow decreasing. However, the effects of gas flow and particle size are little.IntroductionChemical looping air separation (CLAS) is a novel oxygen production technology. The oxygen carriers used in CLAS release oxygen in reduction reactor and regenerate in the oxidation reactor. Selecting suitable oxygen carriers is the key for CLAS. Oxides of CuO, Mn2O3, Co3O4, Pb3O4, CrO2, SrO2, PdO2 and CeO2 have the property of releasing oxygen at suitable temperature and oxygen partial pressure [1]. Among these oxides, CuO, Mn2O3, Co3O4 are the most common compositions used to prepared oxygen carriers for chemical looping combustion (CLC) or chemical looping with oxygen uncoupling (CLOU) [2-5]. Moreover, thermodynamic calculations and preliminary experiments were carried out on oxides of Cu (CuO/Cu2O), Mn (Mn2O3/Mn3O4) and Co (Co3OJCoO) by Moghtaderi to ascertain their feasibility for CLAS process [6]. CuO has the highest oxygen transport capacity (0.1 g 02/g CuO compared to 0.03 g 02/g Mn2O3 and 0.06 g 02/g Co3O4). However, agglomeration is the biggest issue for copper oxides used at high temperature because of its low melting point (l 450°C for CuO, 1235°C for Cu2O and 1075°C for the mixture of CuO and Cu2O) [7]. In order to improve the capability of anti-sintering and stability ofCuO, binders (ZrO2, MgAl2O4, TiO2, SiO2, Fe2O3, Al2O3, cement) are added during the preparation of Cu-based oxygen carriers [8]. In this paper, the Cu-based oxygen carriers were prepared by mechanical mixing method. TiO2, Al2O3, Fe2O3, ZrO2 and SiO2 were selected as binder. XRD, BET and SEM were used to analyze the phase, surface area and surface morphology of oxygen carrier prepared. The reactivity of oxygen reduction and oxidation of oxygen carriers prepared were investigated in STA409PC thermal analyzer."

Jan 1, 2014

By Fang-Qui Zu

Understanding the nature of liquid structures and properties remains an open problem for many fundamental and applied fields such as materials sciences and processing. And as well known, there is no other defined phase line above liquidus (TL ) in phase diagrams of ordinary binary systems. However, via different experimental resorts, our research results on over 30 metallic melts including alloys and elements show a novel physical image: temperature induced liquid-liquid structure transition (TI-LLST) can occur hundreds of degrees over TL. On the other hand, the solidification behaviors and structures out of the melts experienced TI-LLST are distinct from those out of the melts before TI-LLST. In this presentation, some characteristic aspects of the TI-LLST and the effects on solidification behaviors and structures are briefly summarized, and the pertinent rules and mechanism are also analyzed.

Jan 1, 2009

By Nobuo Kikumoto

Recently, the treatment of industrial waste materials has been a serious social problem here in Japan. Filling them in ponds is now strictly prohibited due to a limited land area and incineration method is also regulated as not to generate DXN. In these conditions, Onahama Smelter has begun to treat shredder dusts (SD) of car at reverberatory furnaces to recover various metals such as copper, gold, silver and palladium without generation of DXN. The total volume of these dusts is expected more than 1 million metric tonnes a year in Japan. Onahama Smelter is now planning to treat about 20% of them in the near future by using tonnage oxygen. In this paper, the heat balance, control method of DXN and treatment of these dusts in reverberatory furnaces are described. DXN : Dioxin (The generic term of PCDD and PCDF)

Jan 1, 2000

By E. Buehler, E. Berry

HE magnetic properties of dilute palladium alloys are of fundamental interest.''' Neutron diffraction studies3 have indicated that a better understanding of the behavior of these alloys could be realized with the availability of high-purity single crystals of palladium. Crucible melts of 99.999 pct pure palladium were found inadequate for such research. In a successful effort to fill this need, floating zone refining of palladium was undertaken. In this note the results of the initial experiments are reported. Zoning was accomplished in an argon atmosphere using 450 kc rf generator for an energy source. Samples 5 to 6 mm in diam were suspended in a gastight quartz envelope which could be moved vertically through the rf coil. A nominal upward traverse rate of 1.5 mm per min was maintained during a pass. Close coupling was found to be essential for stable retention of the liquid in the zone. Single crystals averaging 3.5 cm in length were obtained. Laue photography showed them to be continuous single crystals without gross imperfections. Several criteria were used for evaluation of the purity of the zoned material: magnetic behavior, low-temperature specific heat and residual resistivity ratios. Table I shows the residual resistance ratios obtained for two samples, one subjected to a single pass, the other zoned four times. It is appilrent that palladium can be zone refined with the electrically active impurities being transported toward the tail end. A decrease in susceptibility for zone-melted specimens over any previously measured material from 1.5" to 80'~ has been obserted by H. J. Williams and R. C. Sherwood4 substantiating the residual resistance data. The specific heat measurements are currently being made3 and will be published at some later date. Discussions with J. H. Wernick and S. C. Abrahams are acknowledged. We also wish to thank G. F. Brennert for the residual resistance measure ments.

Jan 1, 1962

By S. Harvey

The McArthur River deposit is a structurally-controlled unconformity-related uranium deposit. The mineralization is situated at the intersection of a pronounced fault zone, referred to as the P2 fault zone, and the unconformity between Paleoproterozoic Wollaston Group metasedimentary rock and Paleoproterozoic to Mesoproterozoic Athabasca Group. Mineralization is variably hosted within the Athabasca Group fault wedge and the faulted basement, consisting of twelve zones covering a strike length of 2,700 m. The main P2 fault zone consists of several reactivated foliation-parallel faults containing narrow seams of graphitic clay gouge that are separated by highly cleaved, graphitic wall rock. The mine grid east-dipping P2 fault zone is characterized by reverse offset of the unconformity surface. It varies from a single discrete fault to splay offsets consisting of two to three individual splays. The combined vertical offset along the P2 fault zone is a maximum of about 80 m. The fault has emplaced a wedge-shaped sequence of Wollaston Group metasedimentary rocks into the Athabasca Group. Foliation-oblique faults occur throughout the McArthur deposit trend. Steep east-northeast trending faults generally exhibit apparent oblique dextral sense of shear. Less common, and possibly conjugate, are steep faults trending east-southeast with an apparent sinistral sense of shear. Offsets are generally less than 10 m on these structures. South-trending and shallow west-dipping brittle faults with offsets less than 1 m are also observed while rare steep, north-trending faults are also noted locally and played a critical role in development of the Zone 2 basement-hosted mineralization.

Jan 1, 2020

By Poplawski R. F

A 32-channel PSS seismic monitoring system was commissioned at Mt Charlotte mine in 1994, and at the time it was the first such system in Australian mines. The system continuously observes the occurrence of seismic events and locates them accurately in space and time. Mt Charlotte has a history of seismicity, with the largest event in recent years of Richter magnitude 4.3. The decision to 'go seismic' was made despite some uncertainty regarding its potential usefulness. However after the first year of operation, benefits have been realised in terms of less production downtime, improved mine safety and mine planning, and better understanding of the nature of Mt Charlotte seismicity. The seismic network has performed well, recording 550 events in its first year of operation to a location accuracy averaging ¦ 12 metres. System reliability is excellent, with very little downtime, and acceptable operation and maintenance times and costs. Observations show major distinct changes in the rate of mining induced seismicity over time periods of weeks and months. Events have tended to cluster in specific mine areas and on particular faults and structures. Case examples of pillar preconditioning, breakout around an orepass, and a major stope rockburst, illustrate the role of seismic data and the benefits it brings to safety, productivity and planning.

Jan 1, 1995

By Y. Pokhvisnev, S. Vandariev, A. Yatshenko-Juk, V. Valavin, V. Romenets

The technology of the liquid-phase reduction process known as Romelt was developed in the Moscow Institute of Steel and Alloys in 1979. The pilot plant was constructed at the Novolipetsky Steel Works (Russia) in 1984. Investigations into processing zinc-containing blast oxygen furnace dust and slag from the Lead and Zinc Works at the pilot Romelt plant proved the perspective of using this technology for processing zinc and lead-containing materials. In this article, the description of Romelt technology, basic technological information of trials at the Romelt plant using zinc-containing materials, compositions of charging materials, metal, slag, gas and dust are presented. The influence of flue gas composition on the composition of zinccontaining dust is shown.

Jan 1, 2000

By S. Markstrom

The Boliden AITIK copper mine is located 100 kilometres north of the Arctic Circle in northern Sweden. A pre-feasibility study was conducted in 2005 with the aim of increasing the capacity of the existing processing plant. After analysis, options to upgrade the existing plant were abandoned in favour of building a new processing plant, with higher capacity and therefore greater profitability. A new plant could be designed with greater flexibility to make potential future expansions easier. A feasibility study for a new 36 Mt/y processing plant including fully AG grinding circuits and flotation was completed in 2006. The project was approved by the Boliden board shortly thereafter. Construction started in the beginning of 2007 and was completed during 2009. Commissioning of the new plant was undertaken in the first half of 2010. The grinding circuit consists of two lines with each line consisting of a 22.5 MW AG mill and a 10 MW Pebble mill in closed circuit with a spiral classifier. The nominal production level is 2 200 t/h for each grinding line. This paper presents the start-up and operation of the grinding circuit.

Jan 1, 2012

By Hamid Maleki

The U.S. Bureau of Mines implemented a monitoring program in a western U.S. coal mine for the evaluation of both conventional and alternative support systems. The conventional support consisted of 2.5-m-long vertical bolts installed in an 5.5-m-wide entry. The alternative system consisted of 2.5- and 3-m vertical and inclined bolts installed at a higher density during widening of a cut from 3.6 to 5.5 m. Roof deformation, roof stress, rib deformation, and bolt loads were monitored during the 2-month test period. In addition, roof failure patterns and lithology were characterized within the six-entry main test section. Results were analyzed using roof deformation and failure profiles, roof stress profiles. bolt loading and bending moment diagrams, and numerical models. The mechanics of roof deformation, failure, and support reaction in three zones in the mine roof were characterized. Significant improvements were shown in roof stability in the section using the alternative system. Results are encouraging and indicate the effectiveness of alternative support systems and excavation techniques for limiting inelastic deformation of roof in highly stressed underground mines.

Jan 1, 1994

By S. F. Shaw

MINING conditions in Mexico during the current year have been most unfavorable, synchronizing with conditions in the United States, but the outlook for the near future is improving. The chief difficulties met with are because of the following conditions: severe drop in prices of metals; high smelting rates; high prices of supplies; inadequate means of transportation; low efficiency of labor. In comparison with pre-war prices for metals it cannot be said that prices are low, particularly for silver, which recently has gone to a level that would have been considered exceedingly good in 1912. But conditions have changed so greatly that only the most favorably situated properties can operate without loss.

Jan 1, 1921

By James W. Myers

The Bureau of Mines studied factors affecting ignition of coal mine refuse and on methods for control of burning. Laboratory experiments showed that air permeates more readily through segregated than through nonsegregated refuse and that air permeability is greater through coarse than through fine particle refuse. Minus 3-1/4-inch refuse ignites spontaneously more readily than minus 1/4-inch refuse. The burning of a 1,000-pound conical coal pile was con-trolled by capping with an 18-inch-thick layer of minus 1/4-inch refuse containing 37 percent combustible. In field trials, the burning of refuse at operating mines was controlled by capping with a layer of fine refuse. Water, applied as a spray or by injection, quenched surface flames and cooled the burning waste. Inspection of refuse piles at operating mines showed that the spontaneous ignition tendency is affected by the exposed surface relative to the total volume and the segregation of particles during dumping.

Jan 1, 1966

By John O. Farmer

The wire-line tubing perforator is a mechanically operated tool that is run on an ordinary steel measuring line into the tubing of a well, under pressure, to drive into the wall of the tubing, and securely lock in place, a tapered, cylindrical insert containing an orifice. Use of the perforator obviates the necessity of pulling and rerunning the tubing to install jet collars or flow valves, reduces the cost, and simplifies the task, of placing an oil well on gas-lift operation. More important, however, is the use of the tool with a removable check valve and stop, to provide a means of washing drilling mud from the annulus between the tubing and casing, and to complete the well for gas lift operation without exposing the producing formation to the mud column and without moving the tubing string. This paper discusses the origin, development, and mechanics of the wire-line perforator, the various purposes for which the tool was designed, and the method of selecting orifice sizes for any depth, and gives the results obtained thus far in practical application. Origin and Development Several years ago, a tool that could be lowered on an ordinary steel measuring line into the tubing of a well under pressure was designed and constructed for the purpose of punching a hole in the tubing walls above a shale bridge that had completely plugged the tubing of a well in the Long Lake field, East Texas. The well was in a low, swampy area, which excessive rainfall had caused to be in- accessible by car or truck for about four months. The only equipment at the well site consisted of an ordinary steel wire line that had been carried there to measure the depth of the bridge. Since a pulling unit could not be moved to the well site, and as the pressure on the casing was 2100 lb. per sq. in., it became apparent that the only way out of the predicament was to make a perforating tool that could be lowered into the tubing on a measuring line and operated under Pressure. Thus, the first wire-line tubing perforator was designed and built as an expedient, and was not used extensively until it had been redesigned to meet more frequent and increasingly urgent needs. Until recently, it was necessary to pull the tubing to install jet collars or flow the when a well was to be placed On gas lift. Because most companies either maintained or had access to pulling units and crews for this work, little or no thought had been given to eliminating or even simplifying this task. When the manpower and steel shortage became so acute, however, many operators suddenly found themselves without facilities to equip their wells for gas lifting. The wireline tubing perforator already had been tried and proved successful, therefore operators immediately requested its use to punch gas-jet holes in the tubing, to eliminate the pulling and running of tubing strings. The first deficiency revealed by more general use of the perforator lay in the inability to regulate the size of the hole punched through the tubing. The size could not be controlled to any degree of

Jan 1, 1946

By John O. Farmer

The wire-line tubing perforator is a mechanically operated tool that is run on an ordinary steel measuring line into the tubing of a well, under pressure, to drive into the wall of the tubing, and securely lock in place, a tapered, cylindrical insert containing an orifice. Use of the perforator obviates the necessity of pulling and rerunning the tubing to install jet collars or flow valves, reduces the cost, and simplifies the task, of placing an oil well on gas-lift operation. More important, however, is the use of the tool with a removable check valve and stop, to provide a means of washing drilling mud from the annulus between the tubing and casing, and to complete the well for gas lift operation without exposing the producing formation to the mud column and without moving the tubing string. This paper discusses the origin, development, and mechanics of the wire-line perforator, the various purposes for which the tool was designed, and the method of selecting orifice sizes for any depth, and gives the results obtained thus far in practical application. Origin and Development Several years ago, a tool that could be lowered on an ordinary steel measuring line into the tubing of a well under pressure was designed and constructed for the purpose of punching a hole in the tubing walls above a shale bridge that had completely plugged the tubing of a well in the Long Lake field, East Texas. The well was in a low, swampy area, which excessive rainfall had caused to be in- accessible by car or truck for about four months. The only equipment at the well site consisted of an ordinary steel wire line that had been carried there to measure the depth of the bridge. Since a pulling unit could not be moved to the well site, and as the pressure on the casing was 2100 lb. per sq. in., it became apparent that the only way out of the predicament was to make a perforating tool that could be lowered into the tubing on a measuring line and operated under Pressure. Thus, the first wire-line tubing perforator was designed and built as an expedient, and was not used extensively until it had been redesigned to meet more frequent and increasingly urgent needs. Until recently, it was necessary to pull the tubing to install jet collars or flow the when a well was to be placed On gas lift. Because most companies either maintained or had access to pulling units and crews for this work, little or no thought had been given to eliminating or even simplifying this task. When the manpower and steel shortage became so acute, however, many operators suddenly found themselves without facilities to equip their wells for gas lifting. The wireline tubing perforator already had been tried and proved successful, therefore operators immediately requested its use to punch gas-jet holes in the tubing, to eliminate the pulling and running of tubing strings. The first deficiency revealed by more general use of the perforator lay in the inability to regulate the size of the hole punched through the tubing. The size could not be controlled to any degree of

Jan 1, 1946

By Jean Osorio

A pesar de que en la práctica no es aplicada por las autoridades ni por los concesionarios mineros, la servidumbre minera legal es una figura jurídica vigente en nuestra legislación. Independientemente de los motivos por los cuales hoy en día no se constituyen este tipo de servidumbres, se citan algunas ideas que pueden dar explicación a esta problemática e incluso proponer, a través del derecho comparado, una posible solución para obtener la reactivación de este mecanismo que permitiría, entre otros logros, el crecimiento y desarrollo económico del país e inversión privada.

Sep 20, 2019

By Pedro Alca F

El presente texto refiere el análisis ecónomico en la industria minera privada a través de la estadística financiera como método de medición y gestión empresarial. Para ello, se evaluaron 33 empresas representativas de la mediana minería durante el período de 1975-1979, obteniendo 12 índices standars de tipo financiero y económico para así preveer mediante una administración financiera, el objetivo económico de la empresa. En este sentido, se busca hallar no solo los índices standars en la industria minera, a partir de los datos generados por la correlación de principales cifras de los balances generales, estado de pérdidas y ganancias de los 5 últimos años de operación, sino que se realiza el análisis en conjunto de toda la compañía.

Oct 14, 1980

By Frank M. Monroe, James R. Cost

The solubility of nitrogen in vanadium is determined from 275" to 575°C by measuring the height of the nitrogen internal friction peak of equilibrated V-N alloys. The proportionality constant at 275°C between the internal friction peak height (Q- 1) and the atom percent nitrogen in solution is found to be 0.095 per at. pct for nitrogen concentrations up to 0.8 at. pct. The heat of solution of the nitride in vanadium is 5500 cal per mole. The solubility of nitrogen in the Group V metals is discussed. LITTLE work has been performed on the vanadium-nitrogen terminal solid solution. Hahn1 found the solubility for nitrogen to be very small and reported the existence of a hexagonal phase of composition near that of V2N at the solubility limit. Rostoker and Yamarnoto2 reported the solubility to be at least 3.5 at. pct at the melting point and to be less than this value at 900°C. In addition, they reported from X-ray diffraction studies that nitrogen in solution produces tetragonality in the vanadium lattice. An X-ray study by Schonberg3 has confirmed the results of Hahn but indicated that the tetragonality observed by Rostoker and Yamamoto was due to the presence of oxygen in their specimens. Beatty4 has performed lattice parameter and hardness measurements on terminal solid solutions and found the upper limit of the solubility to be at least 0.66 at. pct N. No measurements have been made of the pressure-temperature-composition relationships (P-T-X) for the terminal solid solution. As a part of a research program on gas-metal equilibrium, an attempt was made to study the P-T-X relationships in the V-N system using both the internal friction and the gas equilibration methods which have been successful with the Nb(Cb)-N and Ta-N systems (see Ref. 5 for a review of this work). Extensive investigation, using the gas equilibration methods, showed this method not to be applicable with vanadium This was presumably due to the gettering action of vanadium sublimed on the walls of the Sieverts apparatus. Thus, the nitrogen pressure relationships with temperature and composition were not obtained. The internal friction methods were, however, found to be applicable, and the temperature-composition relationships are reported in this paper and compared with similar results for the Nb-N6 and Ta-N7 systems. The existence of a Snoek internal friction peak due to nitrogen in solution in vanadium has been clearly demonstrated. 8-10 Powers and Doyle found the peak to be at approximately 275°C for frequencies near 1 cps.8 In a subsequent paper10 they reported the proportionality constant at 275°C between the internal friction peak height (Q-1) and the concentration of ni- trogen in solution (in atom percent) as 0.06 per at. pct. The studies of Stanley and wert9 indicated qualitatively that the height of the Snoek peak decreased with aging at the peak temperature and thus suggested that internal friction methods were suitable for study of the solubility. EXPERIMENTAL METHOD The vanadium for this investigation was of particularly high purity. It was obtained from the Ames Laboratory of the U.S. Atomic Energy Commission, Ames, Iowa in the form of a 1/2-in. diam, three pass zone-refined ingot. The electrical resistivity ratio (p300ºk/p4ºk) was 160. The initial composition was determined as follows: Carbon 200 ppm Oxygen 150 ppm Chromium <50 pprn Iron 125 ppm Silicon <50 ppm Other metallic 100 pprn The initial vanadium ingot was fabricated to 30-mil wire by swaging and wire drawing without the need of intermediate annealing. Lengths of this wire were then further purified (particularly for oxygen) by outgassing at 10-6 torr at 1400°C for 4 hr. The outgassing treatment resulted in specimens with a bamboo grain structure and a lustrous appearance. Desired amounts of nitrogen were added to the outgassed wires in a Sieverts apparatus in which known amounts of nitrogen were equilibrated with the wire at 1300°C. Nitrogen concentrations were produced in the desired range from less than 1 to 10 at. pct N. Monitoring of the partial pressure of nitrogen in the Sieverts apparatus indicated that at 1300°C equilibrium between the nitrogen gas and the vanadium was obtained within 10 min. Relatively rapid cooling from the nitrogen addition temperature was obtained simply by turning off the specimen heating current and cooling to room temperature in the partial pressure of nitrogen. Internal friction measurements of wire specimens were made under forepump vacuum in a torsional pendulum at frequencies near 1 cps. The torsional pendulum was of low thermal inertia and was designed so that specimens could be heated both by a conventional tube furnace and by the joule heating of a separate current through the wire specimen." Use of a static atmosphere of helium gas as a quenching medium made it possible to cut the specimen current, rapidly cool the specimen to the measurement temperature, and make a measurement of the internal friction in less than 1 min. Because of the large solubility of vanadium for nitrogen, the internal friction peak heights were in some cases greater than Q-1 = 0.1. This high damping resulted in an estimated relative uncertainty in the damping measurements of approximately 10 pct. X-ray analyses made to identify the precipitated ni-

Jan 1, 1970