Search Documents

By A. R. Calawa, T. C. Harman, M. Finn, P. Youtz

A study has been made of the growing, annealing, and diffusion parameters in PbSe, Pb1-ySnySe, and Pb1-xSnxTe. Single crystals of these materials have been grown using the Bridgman technique. For all of the above materials the as-grown crystals are p type with high carrier densities. To reduce the carrier concentration and increase the carrier mobility, the samples are annealed either isothermally or by a two-zone method. From isothermal anneals, the liquidus-solidus boundary on the metal-rich side of the stoichiometric composition has been obtained for some alloys of Pb1-xSnxTe and on both the metal- and seleniunz-rich sides for PbSe and alloys of Pbl-ySnySe. In Pbo.935 Sno.065 Se carrier concentrations as low as 5 x1016 Cm-3 and mobilities as high as 44,000 sq cm v-1 sec-1 at 77°K have been obtained. Inter diffusion parameters mere also studied. The ddiffusion experiments mere identical to the isothermal or two-zone annealing experiments except that the samples were removed prior to complete equilibration. The resulting p-n junction depths were determined by sectioning and thermal probing. Inter diffusion coefficients for various temperatures were calculated for both PbSe and Pb0.93Sn0.0,Se. RECENTLY, there has been considerable interest in the PbTe-SnTe and PbSe-SnSe alloys with the rock salt crystal structure. The unusual feature of these systems is the variation of energy gap EG with composition. Several investigations1-3 have shown that EG for the lead chalcogenides decreases as the tin content increases, goes through zero, and then increases again with further increase in tin content. The possibility of obtaining an arbitrary energy gap by selecting the composition is an especially attractive feature of these alloys for applications involving long-wavelength infrared detectors and lasers. In addition, some unusual magneto-optical, galvanomagnetic, and thermomag-netic effects should occur for alloys with low band gaps. If uncompensated low carrier density crystals can be obtained, then a small carrier effective mass, a large dielectric constant, and the resultant high carrier mobility should yield enormous effects at low temperature in a magnetic field. The relative variation of the energy gap with pressure should also be very large for these low gap materials. The primary purpose of this paper is to provide some information concerning the preparation of low carrier concentra- tion, high carrier mobility, and homogeneous single crystals with a predetermined alloy composition. I) DETERMINATION OF ALLOY COMPOSITIONS In all of the work described in this paper, the composition of lead and tin chalcogenides in the alloys was determined by electron microprobe analysis. Separate X-ray spectrometers are used to make simultaneous intensity measurements of the Pb La1 and Sn La1 lines emitted by the sample under excitation by a beam of 25 kev electrons focused to a spot about 2 µm in diam. These intensities are compared to the intensities of the same lines emitted by standards under the same conditions. The standards used are the terminal compounds of each pseudobinary system, i.e., PbTe and SnTe for Pbl-xSnxTe alloys, PbSe and SnSe for Pbl-ySnySe alloys. The composition of the sample is then obtained from theoretical calibration curves which relate the weight fractions of lead and tin in the alloy to the measured ratios of X-ray intensities for the sample and the standards. The lead and tin calibration curves for each alloy system were calculated by using corrections for backscattered electrons,4 ionization,5 and absorption,6 and assuming that the atom fraction of tellurium or selenium in the sample and standards is exactly +. Results obtained by using the microprobe are in good agreement with those obtained by wet chemical analysis. II) CRYSTAL GROWTH FROM THE VAPOR Early work on the vapor growth of PbSe was carried out by Prior.7 He used small chips of Bridgman-grown single crystals as the source material and frequently converted the whole charge of a few grams into one crystal. In the present work, vapor growth occurred using a metal-rich or chalcogenide-rich two-phased alloy powder as the source material. Small, nearly stoichiometric crystals are formed on the walls of the quartz tube. The procedure will now be described in detail. Initially, a 100-g charge containing (metal)o.51(chalco-genide)o 49 proportions or (metal)o.49(chalcogenide)o. 51 proportions of the as-received elements in chunk form are placed in a fused silica ampoule. After the ampoule is loaded, it is evacuated with a diffusion pump and sealed. The sealed ampoule is placed in the center of a vertical resistance furnace. The region containing the ampoule is heated to about 50°C above the liquidus temper-ature for the particular composition used. After about one-half hour at temperature, the elements are reacted and the molten material homogenized. The ampoule is quenched in water. The quenched ingot is crushed to a coarse powder for vapor growth experiments and to a fine powder for the isothermal annealing experiments which are discussed in a later section. Vapor growth experiments were carried out using the powdered, metal-rich or chalcogenide-rich alloys

Jan 1, 1969

By F. F. Craig

Many full-scale waterflooding operations are preceded by pilot floods, one purpose of which is to provide an estimate of recoverable oil. A laboratory model study was made to determine the influence of the producing wells' effective productivity on the oil recovery efficiency of single five-spot pilots, as well as single injection well pilot floods. The effective productivity is indicated by the value of Condition Ratio, defined as the actual well productivity to that of on undamaged and non-stimulated, normal-sized well in the same formation. The effects of initial gas satrcration and mubility ratio on recovery eficiency were also investigated in this model study. Model test results skowed that at favorable mobiliry ratios, a five-spot pilot flood can provide a direct quantitative estimate of the recoverable oil in the pilot area. If the pilot producer's Candition Ratio is 2.2 or more, upwards of 90 per cent of the recoverable oil in the pilot area is recovered from the inside producer, regqrdless of the mobility ratio or initial gas saturation. This Condition Ratio can be achieved with preyent fracturing techniques. Model studies also showed that over the range of imposed injection pressure differences and regional pressure gradients normally encountered in field operations, there was no effect on the recovery efficiency of a five-spot pilot waterflood. Model studies of single injection well pilot waterfloods showed that with no initial gas saturation, the total oil recovery at the offset producing wells can indicate the oil recovery possible by full-scale waterflooding. It is essential that the Condition Ratios of the offset wells be above 1.4. If an initial gas saturation exists prior to water injection, the recoverable oil cannot be directly evaluated by a single injection well pilot flood. However, the production per formance of such a flood can be used to provide information on volumetric sweep efficiency. INTRODUCTION Oil reservoirs are conlplex structures and cannot always be fully studied in the laboratory. Therefore, many operators consider it prudent to evaluate a waterflood prospect by means of a pilot flood. Pilot waterfloods generally involve one of two well arrangements: a single five-spot pilot waterflood, involving four injectors and an internal pilot producing well; and a single injection well pilot flood (sometimes called an inverted five-spot pilot) having one injector and four sur- rounding pilot producers. Some pilot floods are composed of multiple five-spot pilot patterns. To yield information applicable to field-wide performance, the pilot must be located in a representative portion of the reservoir. Pilot floods generally are conducted for one or more of the following reasons: (1) to determine whether water could be injected at desirably high rates, (2) to determine whether an oil bank or zone of increased oil saturation is formed by water injection, and (3) to estimate the oil recovery by waterflooding. Many of the early pilot water-floods were conducted for only the first two reasons. As soon as a buzz in oil production was obtained in the pilot, water injection was initiated throughout the entire lease or field. A number ot laboratory studies have been directed toward determining conditions under which a pilot flood could yield a quantitative estimate of the oil recovery possible by full-scale pattern flooding. One of the early studies of single five-spot pilot flooding' showed that well damage to the inside pilot producer could reduce the total amount of oil recovered. In a study of the single injection well pilot flood pattern,' the results indicated that if the model boundaries were no closer than a half-well spacing beyond the pilot pattern, the pilot performance in the laboratory is unaffected by these boundaries. In another study,? he effect of initial gas saturation and mobility ratio on the ratio of production to injection rate for various groupings of five-spot patterns was defined by mathematical and analog methods. In a study4 involving both potentiometric and flow model experiments at a mobiliry ratio of unity, four different pilot patterns were studied. These included a single five-spot, a single injection well pilot, a cluster of four single injection well pilots and six inverted five-spots. In this study the ratio of well diameter to the distance between injection and producing wells was held constant at 1:1000. The effect of the 7 ratio-—the ratio of the pressure drawdown at the producing wells to the pressure build-up at the injection wells on the pilot performance-was studied. The values of 7 ratio ranged from 0 to 0.34. Results showed that both the total oil recovery and the total fluid production from the pilot relative to the cumulative injection increased with increasing values of the 7 ratio. The effect of both the ratio of injection to producing rates and mobility ratio on the oil recovery performance of a liquid-saturated single five-spot pilot flood was studied in a series of flow model tests.5 Rate ratios ranged from one to four, and mobility rates ranged from 0.1 to 10. Resulls of these tests showed that at low rate ratios, the pilot producers may recover up to four times the recover-

Jan 1, 1966

By E. L. Corp, J. C. Johnson, W. G. Pariseau, M. Poad, M. E. Fowler

This paper describes a comprehensive geomechanics case study of a full¬scale test stope at the Carr Fork Mine. The mine is owned by Anaconda Miner¬als Company and is located near Tooele, Utah. Large diameter blast holes were used in a new method known as blast hole post-fill (BHPF). The new design proved highly successful in contrast with earlier experience with vertical crater retreat (VCR) stopes. The main geomechanics objective was the estab¬lishment of a design procedure for optimizing stope and pillar dimensions with respect to productivity and recovery. An integrated three-part approach consisting of mine measurements, laboratory testing and finite element calcu¬lations was taken. Independent correlations of 0.88 and 0.89 between calculated and measured displacements and between estimated and observed yield :ones substantiate the finite element design approach using UTAH-II. Subse¬quent stope and pillar design analyses indicate that doubling of the original stope width at 50% extraction is quite possible without sacrifice of safety or stability.

Jan 1, 1984

By Charles H. Jacoby, Leo E. Read

IN diamond coring salt beds to evaluate deposits, special techniques are applied to standard slim hole drilling to obtain a representative sample of the water soluble sodium chloride. Industrial consumers generally require a run-of-the-mine material of 98.0 pct sodium chloride. Since no commercial beneficiation has yet been devised to upgrade the lower quality salt beds, the only processing is crushing and screening to the size required by the customer. Coring salt sections has recently become important not only in dry mining, but also in the development of brine cavities by hydraulic fracturing and the formation of jugs for storing liquid petroleum products. Drilling Fluid: The fluid used in coring salt beds in New York, Ohio, and Michigan is a thoroughly saturated brine made from 3.0 lb rock salt per gal of make-up water. This mined rock salt, -4 mesh +10 mesh, is dissolved in a lixator, a double-bottomed cone hopper that turns fresh water to fully saturated brine.

Jan 5, 1957

By David Burgess, Hershiel H. Hayden

Experiments at the Somerset mine, Colo., under an agreement between US. Steel Corp. and the US. Bureau of Mines are described. A test was made of the tube bundle method of mine air sampling which was developed for European longwall mines; some 300,000 running feet of tubing provided continuous monitoring at 38 locations. Carbon monoxide concentrations were obtained with standard deviations of less than 1 ppm and oxygen concentrations with standard deviations of less than 0.2%. A base level of CO index (ppm CO evolved per percent 0, removed) was determined to be zero to 20 through most of the passageways of the mine. However, in one working section where the coal was initially hot (about 180°F within a pillar) the CO index was demonstrably higher, 120 trending upward to about 60 when smoke appeared and the section was sealed. The data are discussed in terms of laboratory experiments on CO evolution from coals.

Jan 1, 1977

By B. J. Steblay

Roof bolts are the primary means of supplemental support in coal mines and are widely used in other mines. Presently, post installation loads are measured infrequently on only about 10% of the bolts by using standard torque wrenches that limit accuracy to about ± 30%. Because mine roof bolts are long, slender, non-uniformly sized, roughly forged, placed in a difficult environment, and subject to severe bending on installation, researchers have been unable to use ultrasonic reflection techniques to measure strain. A complete measurement system has now been assembled by the US Bureau of Mines, Denver Research Center. Obstacles such as bolt preparation, transducer mounting, reliable reflection, and calibration have been dealt with. The seemingly simple concept of measuring the time of flight of an ultrasonic pulse to a reflector is actually complex due to the need to measure to 0.0025 mm (0.0001 in.) accuracy, the sensitivity of velocity to temperature, and stress, and the stability required to make measurements over several years.

Jan 1, 1986

By Robert G. Woolery, S. Ramachandran, James A. Weber, Donald J. Hansen

Union Carbide began looking seriously at heap leaching in 1971. At that time some 1.6 million tons of mineral averaging 0.40 kg U308 /t) (0.80 lb U308) were stockpiled at various sites around the Gas Hills, Wyoming, uranium facility. Several alternatives for economically exploiting these reserves were considered and heap leaching seemed the most attractive. At the time, Western Nuclear Inc. was operating a heap leaching project nearby in which the low-grade ore was leached with sulfuric acid, the product liquor treated in an on site solvent extraction circuit, and the stripped product liquor re-acidified and recycled. The operators were most generous in allowing us to visit their site and in answering our questions. They were also helpful in discussing the problems associated with heap leaching. Their experience confirmed our belief that it was possible to operate a heap leach profitably on material too low grade for conventional milling.

Jan 3, 1978

DISCUSSION, A. Y. Bethune presiding M. E. Wadsworth and W. M. Fassell (University of Utah, Salt Lake City)—The authors of this paper should be complimented on the experimental techniques they have employed to investigate the rate of solution of galena in sodium hydroxide solution. Studies of this type are important not only as a practical means of leaching normally non-leachable substances, but also to determine the mechanism of solution at the solid-aqueous solution interface. There is some question, however, as to the conclusions which have been drawn by these authors concerning their proposed mechanism. Unfortunately, the contribution of OH- was not definitely established in their work, and concentrations less than 0.5 N NaOH evidently were not investigated. The pressure data at 123°C and 0.5 N NaOH were used to determine pressure dependency and the subsequent model proposed was taken as correct on the basis of the three points presented in Fig. 5 of the paper. In developing the

Jan 1, 1954

By R. P. Smith

THE carbon content of iron-silicon and of iron-manganese alloys at fixed activities of carbon has been reported previously.' It seemed desirable to investigate a system which allows a more extended range of alloy composition within a single phase region. The iron-nickel system is ideal in this respect, in that all alloys from 100 pct Fe to 100 pct Ni are face centered cubic ("austenitic") at 1000 °C. The experimental procedure was similar to that previously described.1,2 The alloys, in the form of pieces about 2 by 2 by 0.2 cm thick, together with a similar specimen of pure iron, were equilibrated with each of a series carbon monoxide-carbon dioxide tnixtures of fixed composition, quenched in the carburizing gas in the top of the furnace and then analyzed for carbon. The carbon content of samples containing more than 0.3 wt pct C was determined by the usual combustion method; those with less carbon

Jan 1, 1961

By J. D. Cannon

SLAGS studied in this investigation were from 0.25 to 0.35 pct plain carbon steels and were melted in a 3-ton acid-lined Lectromelt furnace with a 2500-kva transformer. The melting process employs a short, violent boil, which is partially blocked, and the desired carbon content is adjusted by pig iron or iron ore, depending on the preliminary carbon. A relatively small volume of slag is used in refinement. Bottom is here defined as that portion of the furnace that comes in contact with the molten metal, or all the surface below the slag line. Bottom trouble-i.e., holes in the bottom lining-is very seldom experienced at our plant. We have been watching the bottom lining over a period of some boo heats in the hope of having holes large enough to supply data for this report, but none occurred during that period. The bottom is eroded uniformly, occasionally with slightly deeper depressions around the taphole.

Jan 1, 1947

By Frank A. Crossley

The work described has one serious shortcoming: grain size was not monitored during heat up to the temperature (1675°F) of isothermal anneal. The chief obstacles to p grain growth in titanium a-ß structures are the a grains. Heating a structure such as that shown in Fig. 1 to a temperature close to ß transus causes dissolution of a grains in order to adjust the a/ß ratio, compare Figs. 1 and 2. During this process there is a concomitant growth of the ß grains—otherwise ß grains would have to be nucleated in order to adjust the a/ß ratio. When the annealing temperature is reached the a/ß ratio stabilizes and this initial phase of ß grain growth ceases. After an incubation period growth resumes as described. Some 0 grain boundaries can be clearly seen in Fig. 1. (Skilled metallography commonly produces photomicrographs which show more structural detail than direct observation.) These boundaries suggest that the average ß grain size is approximately 0.002

Jan 1, 1970

By L. H. Lange

It is the author's opinion, based on many field experiences over several years, that it is usually better to design a rougher flotation circuit with long rows of rougher cells for high tonnage capacity for maximum recovery and better operating efficiency than the alternative of a greater number of shorter rows with proportionately less tonnage of feed per row. Recent plant studies and tests in the 12,000 ton per day flotation plant of the Atlas Consolidated Mining and Development Corp., Cebu, P. I., have given further substantial support to this opinion. There are two flotation sections in this concentrator: 1) Section 1, treating half the tonnage to the total mill, has eight rows of rougher cells, each row containing 360 cu ft of cell volume. Accordingly, each row of cells receives, on the average, 750 tons per 24 hours which assays about 0.65 to 0.75% copper. The main copper mineral is chalcopyrite with minor

Jan 11, 1963

By George W. Lower, Robert B. Booth

The use of cyanides in the extraction of gold and silver is well known1 Such extractions employ concentrations of cyanide in the range of 0.02-0.25% sodium cyanide equivalent in leaching cycles of 24-48 hr and frequently longer. Copper minerals, even though minor components of precious metal ores, dissolve in these cyanide leaching solutions, consume cyanide, cause fouling of mill solutions, and thus interfere with the precipitation and recovery of gold.2,3,4 This paper presents a summary of laboratory investigations on the use of cyanide solutions as extractants for copper from various copper-bearing ore fractions. In view of the metal contents involved, it will be apparent that larger quantities of cyanide are required to extract copper than for the extraction of precious metals. In cyanide solutions of concentrations generally favorable to copper extraction, sulfide and oxide copper minerals were found to dissolve rapidly at room temperature and atmospheric pressure.

Jan 11, 1965

By J. S. Browning

The pegmatites of the Kings Mountain-Lincolnton, N. C., area constitute the largest known domestic reserve of beryl and spodumene. The reserve is estimated to contain 90 million tons of pegmatic material with 1,280,000 tons of recoverable Li2O (lithia) as spodumene.1 The pegmatites also contain 0.4 to 0.5 pct beryl disseminated throughout the orebodies. The pegmatites may contain a potential reserve of 240,000 tons beryl, equivalent to approximately 34,000 tons of BeO. Different flotation methods for separating beryl from feldspar or quartz, or both, have been developed by various investigators.2,3,4,5,6,7 On the other hand, published information is limited on concentration of spodumene-beryl ores. As the response of beryl and spodumene to flotation is essentially the same, a successful separation of the two minerals depends upon use of a selective depressant or a selective collector for one of the minerals.

Jan 7, 1961

By Charles H. Addison, Robert W. Shields, James W. Sweeney

GIPSY: Is user oriented. Is flexible in applications. Is an ITERATIVE question answering system. Has an adaptable retrieval mechanism. Has both a batch and a teleprocessing version. Allows the user to "browse" through his information. Has ability to answer "ad hoc" queries. Is a currently working and proven system.

Jan 1, 1969

By Philip D. Wilson

WHEN the United Nations win the war and the decision has been made to control future armament in the Axis countries, plans for the extent and operation of such control must have been prepared, to be ready to put into immediate execution. Such control to be effective must be premised upon complete military occupation of the two countries for a substantial period, with an arrangement at the end of such occupation for continued supervision of these industries into an indefinite future.

Jan 1, 1944

By Earl Oliver

IN times like these, the A. I. M. E. and similar societies have their greatest usefulness. . . . Individuals and companies acting alone in the development of public opinion are merely voices crying in the wilderness. United and organized they make a great force that can and does influence public action. . . . What part, if any, then, shall the A. I. M. E. take in these great stabilization processes of civilization? Shall it help to give direction and force to scientific knowledge which comes within its field of activity or shall it merely develop more of it? . . . Is it the A. I. M. E.'s function to help bring system, order and direction out of this situation so that the world can again have forward economic movement, or should it rest on its oars until other agenciess develop that public understanding and direction so necessary for economic progress? As we understand the functions of the A. I. M. E. Petro¬leum Division, they are to discover and promote knowl¬edge for the benefit of society on the mining of oil and gas. To the individual member of the Petroleum Division, there are certain advantages of social and professional contacts, but the collective purpose is that described. And the individual is benefited by membership only as the Division measures up to the purposes of its existence. Consequently, the welfare of this Division and that of its members depends on the extent to which it keeps pace with the needs of society on matters relating to the mining of oil and gas.

Jan 1, 1932

By R. S. McClellan

Western Talc Company, Inc., with headquarters in Los Angeles, Calif., has just completed an extensive modernization and expansion program at its talc mine near Tecopa, Calif., and at its talc and clay mills at Dunn Siding, Calif., the nearest rail shipping point to the mine. The basic objective of the program was to provide facilities necessary to produce 300 tpd of a wide range of ground talc and clay grades for the ceramic, paint, paper, rubber and other industries. In the planning of the program every effort was made to provide a system which would permit a high degree of quality control and uniformity of the finished products, along with efficient operation. Several years ago, R. T. Vanderbilt Co., Inc. purchased Western Talc Co. after a comprehensive investigation of its properties, including an extensive diamond drilling campaign. Western Talc's properties embraced a number of claims in the Resting Springs mining district in the northern part of San Bernardino Co. and the southern part of Inyo Co., Calif., some seven miles southeast of the town of Tecopa. Operations by the original company were started on a small scale in 1913 and production from that date to the time of purchase of the company by Vanderbilt is estimated at 250,000 tons. The major part of this output was sold to the ceramic wall tile industry.

Jan 3, 1968

By Ernst F. Eurich

(Cleveland Meeting, October, 1912.) ALEXANDER PARKES patented in England in 1851-52-53 a process for desilvering lead by means of zinc, making use of the greater affinity of silver for zinc than for lead, discovered by Karsten in 1842. The efforts in England to develop it commercially were not particularly successful, nor was the attempted introduction into the United States. This last was not surprising, as it was about the beginning of our Civil War, and at that period there was very little lead-bullion produced in the united States and there was no field for the process here. There was at that time on Staten Island an establishment that pattisonized lead, probably from Rossie, N. Y., and Chester, Pa., and possibly some Spanish lead, but the production of lead-bullion in the Far West had not yet begun. In 1864, Edward Balbach, of Newark, N. J., patented in this country a process for desilvering lead by means of zinc, and in 1867 Edward Balbach, Jr., patented a " movable black-lead retort with a neck, placed in a furnace," for the purpose of distilling the alloy of zinc, lead, and the precious metals. A brief comparison of the Parkes and the Balbach processes is interesting. The Parkes process as practiced in England consisted in stirring into silver-bearing lead, melted in a kettle, from 1 to 2 per cent. of zinc, cooling, skimming the alloy of lead, zinc, and silver that rose to the surface, liquating it in an iron retort, distilling the residual rich alloy in fire-clay retorts, thus regaining the zinc, and refining the desilvered lead at a low heat in a shallow cast-iron pan that formed the hearth of a reverberatory furnace. If the lead was too impure, it was first softened * Presented also at the Joint Meeting of the Institute and Section IIIa, Metal¬lurgy and Mining, of the Eighth International Congress of Applied Chemistry, New York, September, 1919, and here published by mutual agreement.

Dec 1, 1912

By A. Steiner, K. L. Komarek

Activities of aluminum in solid Ni-A1 alloys have been determined between 20 and 60 at. pet Al and 1200" and 1400°K by an isopiestic method in which nickel specimens, heated in a temperature gradient, are equilibrated with aluminum vabor in a closed all-alumina system. The activity of aluminum shows a strong negative deviation from Raoult's law at low concentrations but increases by three orders of magnitude within the ß(NiAl) phase. The partial molar enthalpy and entropy of mixing are negative. Using Wagner and Schottky's theory of ordered compounds, a degree of disorder of 4 x 10 -4 for NiAl and 1.25 X 10-2 for FeAl has been calculated THE Ni-A1 system has been studied by a great number of investigators, and the results, as far as the phase diagram is concerned, have been compiled by Hansen.1 The phase boundaries from 0 to 50 at. pet Ni are well-established. At higher nickel contents the boundaries are still in dispute and an additional phase, A12Ni3, has been reported.' The phase diagram is dominated by a very stable high-melting compound, NiA1, with a relatively wide range of homogeneity. Heats of formation of solid alloys have been determined calorimetrically by Oelsen and Middel3 from 20 to 95 at. pet Ni and by Kubaschewski4 from 25 to 80 at. pet Ni. According to the most recent compilation5 no other thermodynamic investigations have been reported for the Ni-A1 system. Due to the corrosive nature and the low vapor pressure of aluminum, a method has been employed for determining activities of aluminum which was previously developed for the Fe-A1 system.= Nickel specimens, heated in a closed evacuated alumina system in a temperature gradient, were equilibrated with aluminum vapor from a source within the system kept at constant temperature. After complete equilibration the specimens were analyzed and activities calculated from the known vapor pressure of aluminum. APPARATUS AND EXPERIMENTAL PROCEDURE Materials. The nickel specimens were made from wafers of electrolytic nickel (International Nickel Corp.) of 99.99 pet purity which were rolled to a 0.001-in.-thick foil by Driver-Harris Co. and to a 0.005-in.-thick sheet in our laboratory. The aluminum (Aluminum Corp. of America) had a purity of 99.99+ pct. The alumina tubes and crucibles were made of impervious recrystallized alumina with an alumina content of 99.7 pet (Triangle RR, Mor-ganite Inc.). Experimental Procedure. Annular specimens were punched from the sheet, the punching burrs removed, and the specimens degreased in carbon tetrachloride and acetone and weighed on a micro-balance to within an accuracy of ±0.01 mg. The specimens were positioned with alumina spacers along an alumina tube, and the positions measured. Aluminum metal was machined into cylindrical shape, and placed into an alumina crucible. The tube with the specimens was then inserted into a hole drilled into the aluminum metal. An alumina tube with its closed end at the top was slipped over the specimens so that its lower end fitted snugly into the alumina crucible. The assembled reaction tube was inserted into a mullite tube with a water-cooled brass head which had an opening for a quartz thermocouple protection tube and a metal-to-glass connection to a conventional vacuum system. A Pt-Pt 10 pet Rh thermocouple could be raised and lowered in the quartz tube which was placed along the outside of the alumina reaction tube. The mullite tube was heated by two separately controlled resistance-tube furnaces so that in the experimental temperature range an over-all temperature gradient of approximately 150o to 250°C could be imposed on the reaction tube. The position of the mullite tube was adjusted so that the surface of the aluminum metal was always at the temperature minimum. The reaction tube was thoroughly evacuated before and during slowly heating the assembly up to the melting point of aluminum. A pressure of less than 2 µ (Hg) was maintained during an experiment. Once the aluminum had melted, it isolated the contents of the alumina tube from the surroundings. Several times during an experiment the temperature gradient was carefully measured. An experiment lasted from 3 to 6 weeks and it was terminated by air cooling the evacuated mullite tube. For further details of the experimental procedure the paper on the Fe-A1 system6 should be consulted.

Jan 1, 1964