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By K. M. Rolls, J. Wulff, D. A. Colling

Solid-solution alloys of the Ta- Ti system containing up to 70 at. pct Ti were melted and fabricated into wire. Steady magnetic-field measurements of cold-worked wires at 4.2°K indicate that the resistive critical field increases smoothly with increasing titanium, reaching a maximum of 93 kG (J = 1 amp per sq cm) for a composition of about 50 at. pct Ti. The composition dependence of the resistive critical field indicates it is largely paramagnetically limited for alloys containing more than 35 at. pct Ti. For cold-worked wires the value of the critical current density, Jc , was found to be insensitive to composition changes for compositions in excess of 20 at. pct Ti. It was observed that Jc could be increased by final-size heat treatment at 400°C without altering the value of- the resistive critical field. Experimental data are used to calculate the electronic specific-heat coefficient and the "upper critical field" for the alloys studied. THE effect and importance of metallurgical structure on superconducting properties have been summarized by Livingston and Schadler.1 Specific work on solid-solution alloys such as Nb-zr2-7 and Nb-Ti5-7 have shown that critical current density (Jc) and superconducting transition temperature are structure-sensitive. Berlincourt et al.6,8,9 in their studies of transition-metal alloys find that Ta-Ti alloys remain superconducting at fields comparable to Nb-Ti alloys. 6,8 Transverse critical current tests of a Ta-10 at. pct Ti alloy10 and longitudinal critical current tests of a Ta-25 at. pct Ti alloy1' indicate that such alloys are capable of carrying high currents at intermediate fields (-40 kG). The work reported in the present paper was undertaken to explore the superconducting properties of further compositions in the Ta-Ti alloy system as well as the structure sensitivity of the superconducting properties. I) EXPERIMENTAL PROCEDURE Alloys were prepared by melting tantalum (Fansteel Metallurgical Corp., 99.96 pct purity) and iodide, crystal bar titanium (Foote Mineral Co., 99.92 pct purity) mixtures in an arc furnace on a water-cooled copper hearth using a tungsten electrode. Melting was accomplished in a purified, gettered argon atmosphere at pressures from 250 to 400 Torr. Each alloy was turned and remelted fourteen times to assure complete mixing of tantalum and titanium. Ex- cessive coring in the cast samples was, nevertheless, observed. This was somewhat reduced by annealing in vacuo at 1000°C for 13 hr. The ingots were then machined to 0.250 in. diam, jacketed in Type 304 stainless-steel tubing, and swaged to 0.140 in. diam. They were then drawn to 0.010-in.-diam wire. Alloys containing up to 70 at. pct Ti were readily cold-drawn to wire in this manner. Later experiments showed that oxygen additions up to -3000 ppm could also be cold-worked into wire. Test samples for superconductivity measurements in the 2-in, air-core Bitter solenoids of the M.I.T. National Magnet Laboratory were prepared from 10-in. lengths of 0.010-in.-diam wire, cleaned of residual wire-drawing lubricant. Current contacts were made by clamping clean copper tubing over both No. 18 current lead wire and the ultrasonically indium-tinned ends of the specimen wire.12 Potential leads of No. 32 copper wire were connected to the specimen by ultrasonic soldering in an indium bath. The potential lead separation was about 4 cm, corresponding to the circumference of the Bakelite rod to which the wire was affixed with half-mil Teflon tape. The final specimen configuration is shown in Fig. 1. Specimens were lowered into a liquid helium bath (4.2oK) in a double solenoid dewar and positioned so that the maximum magnetic field was oriented transverse to the wire axis of the gage section. Measurements were made by passing a current through the specimen at a preset solenoidal magnetic field. The current was increased until a 1-pv potential difference appeared across the gage section (1/4 µv per cm). At low magnetic fields, however, it was not possible to use this criterion because power-dissipation difficul-

Jan 1, 1967

By Hans Lundberg

IN ORDER to comprehend the help and information that may be expected from electrical prospecting, it is necessary to have at least a general knowledge of the methods and principles involved in preparing and interpreting results obtained in the field. Electrical prospecting is rather complicated, both in theory and practice, and in order to make a brief description clear to the practical mining man it has been necessary to idealize and generalize the problems, at the risk of having such simplification criticized by the theoretical man. This simplification must not be misinterpreted as showing a lack of theoretical knowledge. FIG. 1.-FLOW OF CURRENT IN AND AROUND A CONDUCTING BODY. For its operation, electrical prospecting mainly depends on the fact that most metallic ores conduct an electric current much more readily than barren rocks. If an electric current flows through a block of ground within which a body of chalcopyrite is enclosed in country rock of schist, the current will find less resistance to its passage through the chalcopyrite than through the schist, even though the passage through the latter be much shorter. This is because the longer path through the chalcopyrite offers less resistance, owing to the superior electrical conductivity of the chalcopyrite (Fig. 1).

Jan 1, 1928

By L. Zwell, H. A. Wriedt

In describing their procedure for measuring the lattice parameters of solid solutions, Abrahamson and Lopata report (p. 77) the final heat treatment of their alloy specimens as "700°C for 100 hr, followed by a furnace cool". The isothermal part of this treatment may be expected to precipitate solute in excess of the stable a solid-solution limit at 700°C; the subsequent slow cooling is likely to reduce the dissolved solute still further. Fig. 1 (upper) presents the data for titanium alloys so he;rt-treated and shows the lattice parameters of solid solutions containing up to 3.5 at. pct Ti; Fig. 17 (lower) shows 2 at. pct Ti as the solubility limit in a iron at 700°C. Figs. 1 and 17 are thus incompatible. The paper contains comparable incon~patibilities for zirconium alloys, for niobium alloys, and for tantalum alloys. The final heat treatment at 700°C may also be responsible for the anomalous "knee" in the lattice-parameter data for nickel alloys, Fig. 3. The "knee" composition is located near the 700°C limit of the stable a solid-solution field;37 alloys of the experimental composition range with more nickel than the "knee" composition are two-phase at 700 C and prolonged heat treatment of them at 700°C would tend to produce inhomogeneity rather than homogeneity. In Figs. 4 and 7, the composition ranges of the zirconium, hafnium, and niobium alloys examined terminate at alloy concentrations of 0.1 to 0.2 at. pct. These metals form very stable oxides and their partial removal from solid solution in iron by impurity oxygen may be expected. We believe that the authors should have reported the procedure by which they distinguished the amounts of alloying elements in solution and in oxide. The diagrams pertaining to copper in Figs. 3 and 18 (lower) are almost certainly incorrect. Three recent investigations of this system38-40 all substantially agree on the solubility of copper in a iron, finding it to be much larger than that reported by Abrahamson and Lopata. The change of the lattice parameter with composition reported by Abrahamson and Lopata is too large by a factor of three to five, as seen by comparison with the findings of other investigators.41738 Moreover, the authors violate, in Fig. 18, the accepted Fe-Cu constitution diagram37 by ignoring the eutectoid at about 850°C.

Jan 1, 1967

By O. B. Buchlen, J. W. Smith

The Coal Research Bureau of the School of Mines at West Virginia University, using an experimental flotation cell designated an airlift-cyclone was able to obtain a clean coal product containing 7.64% ash with 94% yield and 97% coal recovery. This favorable performance was obtained with the experimental flotation cell operating as a simulated three-stage unit on slurry taken from the fine coal circuit of a coal preparation plant. This experimental device, consisting of a sheet metal cyclone-like unit mounted on a U-shaped uplift pipe, uses a combined flotation and cyclone action to beneficiate the minus 14 mesh partially cleaned feed product. In addition to providing comparable analytical results, the airlift-cyclone possesses other attractive features among them being a low capital expenditure, utilization of moderate plant floor space, efficient operation on high density feed slurry, and absence of moving parts. The primary shortcoming of the experimental cell is its limited capacity. The Coal Research Bureau presently has under construction a larger unit which, it is hoped, will provide the capacity and quality to establish the airlift-cyclone as a commercially feasible unit. Froth flotation of fine coal is a practice which has only recently gained wide acceptance in this country. Various explanations can be put forth for this delayed acceptance of a very selective and efficient system of coal preparation. Among these reasons would be the advent of continuous mining machines resulting in the increased production of coal fines, the change in market patterns from domestic and rail consumers who did not want fines to a predominantly utility market which normally consumes fines, and also the imposition of legal restrictions in regard to stream pollution. However, the major detriment is probably the high cost involved both in installation and operation of the flo- tation unit and auxiliary systems. These facts assume greater emphasis when considering that froth flotation installations normally process a low quality feed product. A recent estimate' of installation costs including dryers, filters, and other auxiliary equipment for a flotation system was $5000 to $7000 per ton of capacity while the operating costs, exclusive of auxiliary equipment, were estimated at 10 to 306 per ton of feed. The Coal Research Bureau of the School of Mines at West Virginia University is currently developing a simplified froth flotation cell, designated an airlift-cyclone, which may provide considerable savings in capital and operating costs without sacrificing product quality or recovery. This experimental cell consists of three primary components: 1) a vertically mounted U-shaped pipe; 2) an air injector device; and 3) an integrally mounted cyclone-like unit (Fig. 1). A feed slurry is introduced at the top of one leg of the U-pipe while compressed air is injected near the base of the other leg. The air serves both to aerate the pulp and to cause it to flow upward into the base of the cyclone unit where the floated clean coal is separated from the reject material and unfloated coal which remains in slurry. The Coal Research Bureau's experimental airlift-cyclone is somewhat similar in principle to a flotation device developed by Russian engineers in the late 1950's. In tests upon a two-stage pilot-size device, the Russians obtained very favorable cleaning efficiencies.' However, later experience with production models demonstrated that rated capacities and acceptable product quality could not always be maintained.3 Because of these limitations, Russian engineers subsequently recommended that conventional, mechanical cells be used when cleaning difficult to float slurries. Engineers at the Coal Research Bureau felt that such a device utilizing the combined actions of a cyclone and a froth flotation machine offered numerous attractive features and merited investigation. Accordingly, a small capacity experimental airlift-cyclone was designed and, with the permission of the Christopher Coal Company Div. of Consolidation Coal Co., installed in Christopher's Humphrey preparation plant near Morgantown, West Virginia.

Jan 1, 1964

By J. A. Hren, G. Thomas

A high-temperature stage has been used to study precipitation and dissolution in thin foils of Al-20pct Ag alloy directly in the electron microscope. The results show that the aging characteristics are similar to those observed for bulk materials, and in addition, direct evidence is presented for clustering at the solid solution temperature. The limit of solubility of G. P. zones is-350°C. The heterogeneous precipitation, the growth and dissolution of ?&apos;have been studied in detail. Growth of ?&apos; parallel to the basal planes, occurs by continuous motion of inter -facial partial dislocations. Growth stops at intersecting particles due to formation of sessile a/6 <110> interfacial dislocations. Growth normal to the habit plane occurs by the spontaneous nucleation of partial dislocations on alternate (111) planes and the thickening rate is --10-3= times the lengthening rate. The precipitates dissolve in layers and the final product is a whole a/2 <110> dislocation . The nucleation -growth -dissolution processes are thus completely reversible. Kinetic data obtained from the dissolution rates of ?&apos;particles enable the diffusion coefficient to be determined and the activation energy is found to be 37.5(±4) kcal mol-1, which is that expected for dzffusion of silver in aluminum. The velocity of the interfacial dislocations is thus dependent solely on the rate of diffusion of silver atoms. RECENTLY it was demonstrated that a high-temperature stage could be effectively used in the electron microscope to follow directly the processes of precipitation and dissolution in thin foils of A1-4 pct Cu alloy.&apos; These experiments also provided kinetic data which enabled the diffusion coefficient to be estimated. This new development of electron metallography opens up many fruitful areas of research and it was decided to investigate the aging behavior in thin foils of A1-20 pct Ag alloy, particularly the mechanism of heterogeneous precipitation (i.e., precipitation on lattice defects). This system was chosen because the aging characteristics of bulk specimens are now well known,2"7 and because we wished to obtain more details of the role played by partial dislocations and stacking faults in the nucleation growth and dissolution of the hcp ?&apos; phase. This is of interest for the general case of fcc-- hcp transformations. Part of the A1-Ag phase diagram is shown in Fig. 1. The use of a high-temperature stage also enables a study to be made of the clustering process (formation of G. P. zones) and to determine the structure of the solid solution prior to the usual quenching and aging procedures. It is also possible to obtain kinetic data from measurements of the rates of dissolution of precipitate particles. Unlike the results of previous experiments on A1-4 pct CU 1 where much of the initial precipitation occurred on the foil surfaces, the results on the A1-20 pct A1 alloy were identical to those reported for bulk specimens6,7 and no surface precipitation was ever observed. Thus, it was possible to follow the aging sequence: G.P. zones — ?&apos; — ? directly in the thin foils. This paper is concerned with the formation and dissolution of zones and the ?&apos; phase, and no attempt has been made so far to follow the mode of discontinuous precipitation of ?. I) EXPERIMENTAL DETAILS The high-purity A1-20 pct Ag alloy was prepared by the Aluminum Co. of America in the form of 0.001-in.-thick sheets. These were cold rolled with intermediate anneals to a thickness of 0.0004 in.,

Jan 1, 1963

Jan 1, 1932

By Lawrence P. Bonicatto

The steel industry&apos;s increased demand for higher grade pellets has caused the pellet producers to investigate methods of upgrading their product and the Hanna Mining Co.&apos;s Groveland plant on the Upper Peninsula of Michigan is no exception. The low grade iron deposit is a complex mixture of magnetite and hematite with chert, quartz, jasper and various iron silicates.1 Beneficiation is by Humphrey spirals and anionic flotation of the iron minerals.2 Flotation of the spiral tailings makes up about 75% of the concentrate, while a minor amount of concentrate (less than 3%) is produced in magnetic circuits. The concentrate is pelletized at the rate of 1.6 million tpy. The initial concentrating facilities were constructed in 1958 and the concentrate was marketed as sinter feed until a pelletizing plant was added early in 1963. Grade improvement soon became a high priority research project, and several methods of concentration were investigated.

Jan 3, 1968

By Harry Seltz, J. C. DeHaven

InteRmetallic compounds are formed in many binary metal systems. Some compounds are stable to their melting points, and others decompose at lower transition temperatures. Even those of the first class are dissociated in the liquid state, as indicated by the continuous form of their solubility curves at their melting points1. While the lattice structures of some of these compounds have been determined, their thermodynamic properties have not been investigated. In this paper is described the determination of the free energy and heat of formation of the compound CdSb, which is of the first class mentioned above, melting congruently at 455&apos; C. This compound shows a rhombic structure, and the lengths of the edges of the elementary cell containing four molecules are: a = 6.52, b = 8.60, c = 4.16 A.&apos; There are three possible methods of determining the free energy of formation of a compound of this type. The first method, applying the third law of thermodynamics, requires the measurement of its heat capacity preferably to liquid hydrogen temperatures, and a calorimetric determination of its heat of formation. The second method involves the study of the equilibrium of the compound in some gas reaction, such as: CdSb + CO² = CdO + CO + Sb From the known free energies of formation of CdO, CO² and CO the free energy of formation of CdSb could be calculated. The third method measures the electromotive force of a galvanic cell in which the cell reaction is the reversible formation of the compound from the elements. The first method is generally applicable, but requires elaborate experimental equipment. The second method can not be used for compounds melting at low temperatures, owing to the difficulty in establishing equilibrium. The electromotive force method, therefore, seemed to offer

Jan 1, 1935

By J. C. DeHaven, Harry Seltz

InteRmetallic compounds are formed in many binary metal systems. Some compounds are stable to their melting points, and others decompose at lower transition temperatures. Even those of the first class are dissociated in the liquid state, as indicated by the continuous form of their solubility curves at their melting points1. While the lattice structures of some of these compounds have been determined, their thermodynamic properties have not been investigated. In this paper is described the determination of the free energy and heat of formation of the compound CdSb, which is of the first class mentioned above, melting congruently at 455&apos; C. This compound shows a rhombic structure, and the lengths of the edges of the elementary cell containing four molecules are: a = 6.52, b = 8.60, c = 4.16 A.&apos; There are three possible methods of determining the free energy of formation of a compound of this type. The first method, applying the third law of thermodynamics, requires the measurement of its heat capacity preferably to liquid hydrogen temperatures, and a calorimetric determination of its heat of formation. The second method involves the study of the equilibrium of the compound in some gas reaction, such as: CdSb + CO² = CdO + CO + Sb From the known free energies of formation of CdO, CO² and CO the free energy of formation of CdSb could be calculated. The third method measures the electromotive force of a galvanic cell in which the cell reaction is the reversible formation of the compound from the elements. The first method is generally applicable, but requires elaborate experimental equipment. The second method can not be used for compounds melting at low temperatures, owing to the difficulty in establishing equilibrium. The electromotive force method, therefore, seemed to offer

Jan 1, 1935

By Thomas E. Garnar

Zirconium and hafnium are curious elements because they are almost always found together in nature. Zirconium was discovered by Klaproth in 1789 and isolated 35 years later by Berzelius. Because hafnium&apos;s chemical properties are so close to those of zirconium, it was not discovered until 1923 when Coster and Von-Heresey detected it using x-ray spectrographic analysis. These elements occur most commonly in nature as the mineral zircon (ZrSiO4) and less commonly as the oxide baddeleyite (ZrO2). They also are found as a variety of other silicates. Zircon was identified as a component in alluvial and beach sands in 1895, but it was not produced in any quantity until 20 years later. Zircon is always a coproduct from TiO2 mining and processing. During World War I it was produced as a coproduct of beach sand mining for titanium minerals just south of Jacksonville Beach, FL, and was patented as a refractory. It was not until the 1930s when Zircon Rutile, Ltd. began mining at Byron Bay on the east coast of Australia that zircon was first used as a foundry sand. Later in the 1940s, NL Industries, Humphreys Gold Corp., and E. I. du Pont de Nemours & Co., Inc. began production of zircon sands from fossil beaches in northeast and northcentral Florida. Baddeleyite first became available as a commercial product in 1916, but never in the quantity of zircon. Zircon holds a unique position as an industrial mineral because it is used for both its physical and chemical properties as well as an ore of zirconium and hafnium metals. Australia is the major zircon producer followed by South Africa and the US. Zircon is also produced in India, Sierra Leone, Sri Lanka, Malaysia, China, Thailand, and Brazil. Undeveloped heavy mineral beach sand reserves containing zircon are known to occur in Egypt, Malawi, Senegal, and Tanzania. Locations are shown in Fig. 1. Mineralogy Zirconium and hafnium are always present together in naturally occurring compounds. Most commonly they form as the silicate sometimes containing iron, calcium, sodium, manganese, and other elements. Less commonly they are found as oxides in combination with titanium, thorium, calcium, and iron. Zircon is the most common form. It is extremely resistant to weathering, therefore, often it is present in ancient beach sands and placer deposits. Although resistant to alteration from external sources, it is vulnerable to internal alteration as the result of thorium and uranium substituting for zirconium either in the zircon lattice or in solid solution. Alteration to the metamict state takes place as radioactive emanations from these elements disorder the crystal lattice, accompanied by hydration, reduction in specific gravity, and changes in color. The mineralogy of zircon and baddeleyite and variation of physical and chemical properties are shown in Table 1. The effects of zircon&apos;s internal alteration and darkened color can be corrected by heating to 1000°C for 30 min or so. A certain time-temperature relationship makes it possible for decolorization and reordering of the crystal lattice to take place when heating at higher temperatures for shorter periods or at lower temperatures for longer periods. After heating, x-ray diffraction patterns are sharper, the grains may be harder, and except for particles of malacon, the grains will be white or colorless in the absence of grain surface coatings. The color change is only temporary and the particles slowly darken with time. Zircon fluoresces light yellow in shortwave ultraviolet light. If exposed to ultraviolet light for extended periods of time, white (calcined) zircon turns purple. With time the induced color begins to fade and eventually disappears (e.g., calcined Florida zircon exposed to ultraviolet light for 24 hr still retains faint, but discernible, purple color after six months).

Jan 1, 1983

By Albert Sauveur

Some writers believe that when austenite transforms completely into pearlite on slow cooling through the thermal critical range, such transformation does not imply the formation of any of the so-called transition constituents: martensite, troostite and sorbite. Might it not be claimed with as much justification that when water freezes it does so suddenly, solid ice being obtained without passing through the intermediate stages of ice and water? Obviously, regardless of the speed of solidification, this would be erroneous. Before reaching the completed solid condition, this must of necessity pass through an unbroken series of stages when the system consists of mixtures of water and of ice, the former decreasing and the latter increasing in amount. Are not these "transitionV stages in the freezing of water similar to the transition stages occurring in the transformation of austenite into pearlite? To clarify, let us consider in Fig. 1 the mechanism of the transformation of eutectoid steel from its austenitic to its pearlitic condition as it cools slowly through its thermal critical range. It is generally admitted that this transformation is the result of two distinct phenomena: (1) the allotropic change of gamma iron into alpha iron and (2) the crystallizing out of solution of the carbide Fe3C. Whether this crystallizing of Fe3C implies also its formation is immaterial for our purpose. In other words, whether it is the carbon in atomic dispersion which is present in gamma iron or molecules of Fe3C has no bearing upon the matter to be discussed. The transformation of gamma iron into alpha iron cannot take place suddenly. It must of necessity be progressive, regardless of the speed with which it may take place. At A, for instance, there would be present AB gamma iron and BC alpha iron. The distance MN does not refer to falling temperature, but to the passage of time. It may be assumed that the transformation takes place at a constant temperature (the Ar321 point). In a similar way, the crystallization of Fe3C out of the austenite solid solution must be progressive as depicted between M and N. At A there would be present AB gamma iron, BC alpha iron, CD carbon dissolved in gamma and in alpha iron and DE Fe3C. This condition may be described according to individual preference as martensite or troostite. To sum up, can the metal pass from condition

Jan 1, 1931

By J. H. Kittel

THE properties of the metal molybdenum have been the subject of recent investigations1,2 = which have included studies of the changes that occur in the metal when it is annealed after having been cold worked. Most of the data which have been reported have pertained to only one aspect of annealing, that is, the conditions under which recrys-tallization has been observecl. The process of recovery which may precede recrystallization docs not appear to have been investigated, and it is the purpose of this note to report observations on the recovery process in cold-worked molybdenum as determined by changes ill the thermoelectric power which occur as the metal is annealed. The measurements were made on commercially pure molybdenum wires which, after annealing at 1035°C in dried hydrogen for 1 hr, were swaged to give a series of reductions up to a maximum of 84.5 pct. The variously cold-worked wires were then annea1c.d in dried hydrogen for periods of 16 hr at progrc:ssively highel. temperatures from 200" to 1000 c with a final annealing treatment of 70 hr at. 1100°C. After each annealing treatment the ther.ma1 emf&apos;s were determined against a length of original unwo~,ked material that had received the initial hydrogen anrit,aling treatment. The difference in temperature between the hot and cold junctions was maintained at about 75&apos;C. and. the thermal emf&apos;s were measured with a potentiometer that could be read. to 0.01 microvolt. Fig. 1 shows the thermoelectric power. (dE/dT) in microvolts per C between annclalcd and cold-worked molybdenum as a function of the degree of cold work. The effect of annealing is shown in Fig. 2. The general shape of the curves in both figures is similar to results which have been obtained for copper." It was observed that after annealing at temperatures as low as 200°C recovery was well under way. The rapid changes irt thermoelectric power observed near 900 C are probably associated with recrystallization, since such a relation has been observed with copper. Beyond 900°C the thermal emf&apos;s changed in polarity. indicating that from this point or1 the specimens were more highly annealed than the standard. Annealing treatments could not be given at temperatures higher than 1100°C due to limitations of the furnace, and it is evident that, since equilibrium values of thermoelectric powers were far from having been attained, temperatures considerably higher are required to fully anneal molybdenum. References Robert M. Parke: Molybdenum, A New High-Temperature Material. Metal Progress (1951) 60, pp. 81-96. * R. A. Long, K. C. Dike, and H. R. Bear: Some Properties of High-Purity Sintered Wrought Molybdenum Metal at Temperatures up to 2400 °F. NACA TN 2319 (March 1951): G. W. Brindley: A Thern-io-Electric Study of the Cold-Rolling and Heat-Treatment of Copper, Report of a Conference on the Strength of Solids. Physical Society, London (1948) pp. 95-106.

Jan 1, 1953

By Alexander Knoll, Dwight L. Baker

THIS paper is a report on work undertaken to investigate the results and conclusions of Ravitz and Porter1,2. that galena freed of surface oxidation products and lead carbonate ("clean" galena) is water-repellent, and that the action of xanthates in flotation is the action of a cleansing agent, enabling oxidized galena particles to expose a pure lead sulphide, water-repellent surface. The apparatus, in construction and use, was essentially that of Ravitz and Porter. The only significant modification introduced by the present authors was the substitution of a three-necked flask for the flotation cell as the "reaction vessel." Our procedure was to place 50 grams of freshly ground, minus 200-mesh galena in the reaction vessel, sweep out all molecular oxygen from the system with oxygen-free nitrogen, and proceed to wash the galena surface free of its oxidation products with repeated small portions of (I) ammonium acetate (500 c.c. of water, 200 grams of ammonium acetate) or (2) ammonium chloride, hydrochloric acid (2 liters containing 200 grams of ammonium chloride and 25 c.c. of 1.18 sp. gr. hydro chloric acid). The galena was next washed with many 100-c.c. portions of oxygen-free, distilled water. The galena was finally considered free of soluble salts when wash water that had been in contact with the mineral for at least 48 hr.* gave negative tests for: (I) lead ion with sulphide; (2) chloride with silver ion; (3) acetate with cuprous chloride, sodium chloride; and (4) ammonium ion with Nessler&apos;s reagent. Next 500 c.c. of potassium ethyl xanthate solution, free of dissolved oxygen, was run onto the "clean" galena particles. For this system there were determined: I. The wetting properties of the clean galena particles by shaking the reaction flask and noting the degree of mineral collection at the liquid-air interface. This was, of course, simply a qualitative test, but it proved adequate for our purpose. 2. The removal of xanthate ion from the potassium xanthate solution on being shaken with the "cleansed" mineral. Xanthate concentrations were determined by iodine titration according to the methods of Taylor and Knoll.3 3. The pH of the xanthate solution after having been shaken with the "cleansed" galena. The pH was determined colorimetrically.4 The results of five experiments of the type mentioned above are given in Table I.

Jan 1, 1941

By Albert Sauveur

SOME writers believe that when austenite transforms completely into pearlite on slow cooling through the thermal critical range, such transformation does not imply the formation of any of the so-called transition constituents: martensite, troostite and sorbite. Might it not be claimed with as much justification that when water freezes it does so suddenly, solid ice being obtained without passing through the intermediate stages of ice and water? Obviously, regardless of the speed of solidification, this would be erroneous. Before reaching the completed solid condition, this must of necessity pass through an unbroken series of stages when the system consists of mixtures of water and of ice, the former decreasing and the latter increasing in amount. Are not these "transition" stages in the freezing of water similar to the transition stages occurring in the transformation of austenite into pearlite? To clarify, let us consider in Fig. 1 the mechanism of the transformation of eutectoid steel from its austenitic to its pearlitic condition as it cools slowly through its thermal critical range. It is generally admitted that this transformation is the result of two distinct phenomena: (1) the allotropic change of gamma iron into alpha iron and (2) the crystallizing out of solution of the carbide Fe3C. Whether this crystallizing of Fe3C implies also its formation is immaterial for our purpose. In other words, whether it is the carbon in atomic dispersion which is present in gamma iron or molecules of Fe3C has no bearing upon the matter to be discussed. The transformation of gamma iron into alpha iron cannot take place suddenly. It must of necessity be progressive, regardless of the speed with which it may take place. At A, for instance, there would be present AB gamma iron and BC alpha iron. The distance MN does not refer to falling temperature, but to the passage of time. It may be assumed that the transformation takes place at a constant temperature (the Ar321 point). In a similar way, the crystallization of Fe3C out of the austenite solid solution must be progressive as depicted between M and N. At A there would be present AB gamma iron, BC alpha iron, CD carbon dissolved in gamma and in alpha iron and DE Fe3C. This condition may be described according to individual preference as martensite or troostite. To sum up, can the metal pass from condition

Jan 1, 1931

By N. A. Ziegler

A CERTAIN amount of interest has been indicated recently in the resistance to oxidation at high temperatures of iron-aluminum alloys (rich in iron). Hautman1 published a paper in which some interesting results are given. According to his paper, only alloys containing at least 8 per cent aluminum indicate a marked improvement in their resistance to oxidation. At about this aluminum content, however, alloys become brittle, which considerably reduces their commercial value. About two years ago the author performed a series of experiments, the results of which are presented here. A series of iron-aluminum-carbon alloys was prepared by melting electrolytic iron, aluminum and high-carbon iron alloy in an induction vacuum furnace.2 The list of these alloys is given in Table 1. Each alloy was forged in the ordinary way to

Jan 1, 1932

By H. B. Heller, T. J. LaChapelle

Phosphorus nitride has been used as a diffusant for introducing phosphorus into silicon under various conditions. It has a temperature -dependent rate of decomposition beginning in the 500°C range, increasing very rapidly above 1000 C, producing gas -eous phosphorus and nitrogen. Best control was obtained with a two-temperature arrangement, with silicon at the proper higher diffusion temperature. It is an easier compound to use than the usual P2O5 because it is nonhygroscopic and yields temperature-controlled surface concentrations together with excellent final surfaces. Surface doping nearly as high as that produced by phosphorus pentoxide has been observed for sources at 850" to 900°C. Reproducible high sheet resistances were obtained by using slow flow rates (1 linear in. per min) and staggered-baffle gas mixing with the nitride at 550°C. Both inert gas (argon, nitrogen) and oxidizing ambients have been examined. Oxygen reacts to produce anhydrous P2O5, consuming the source at a rapid rate. Nitrogen, except for short diffusion times, suppressed the dissociation reaction and sometimes produced inferior surfaces. Argon appears to be a more useful ambient. PHOSPHORUS is a common impurity atom which may be introduced into a semiconductor lattice to create a p-n junction or an nn contact region. Various investigators1-4 have described techniques which can be used with either elemental phosphorus or certain of its compounds. This paper discusses a newly available compound of phosphorus, phos- some processes silicon wafers are precoated with a phosphate glass which acts as the doping source. Although a nonoxidizing form like elemental phosphorus or a phosphine can be used, most diffusion methods usually involve the use of phosphorus pentoxide. Because of the rapid volatility of this compound, a two-step process is often used, combining a gaseous deposition to introduce a predetermined quantity of phosphorus into the silicon with a later redistribution to obtain the desired distribution and surface concentration. Such a process usually involves predepositing phosphorus at surface concentrations greater than 1020 cm-&apos;. At such doping levels the phosphorus-diffusion coefficient appears to be strongly concentration-dependent.596 Distribution profiles5&apos;9 for these high concentrations of phosphorus do not follow Fick&apos;s laws, having extended subsurface regions which appear electrically to be nearly uniformly doped with ionized impurity atoms. Radioactive-tracer experiments also show near-surface anomalies in the distribution profile. Additionally, it has been shown1&apos; that the introduction of very high surface concentrations of impurity atoms into silicon (a step necessitated by the subsequent lowering of concentration during the redistribution) creates dislocations, even in material having no dislocations originally. For device fabrication the use of oxide masking introduces certain difficulties and limitations.7&apos;8 The standard practice of using phosphorus pentoxide as an impurity source adds other problems to these because of the speed and ease with which this compound reacts with moisture present in any gas in contact with it. In fact, P2O5 is one of the fastest and most effective drying agents for gases. Because it is such an excellent desiccant, completely anhydrous phosphorus pentoxide is difficult to obtain and is even more difficult to keep dry. Adequately dry gloved boxes must be used for storage and transfer of the chemical. The presence of even traces of moisture will cause formation of phosphoric acids which, during the high-temperature diffusion, results in polyphosphoric acids of variable composition. Such reaction by-products end up as gradually accumulating viscous fluids in the cooler parts of the diffusion furnace. The calculation of the final solute distribution for

Jan 1, 1964

By E. O. Lilge, H. Siebert

A design of a multiple-bomb leaching unit particularly suited for the study of heterogeneous reactions, i.e. sol id-liquid-gas interfaces at high temperatures and pressures is presented. The component parts and overall design are described and illustrated in detail. The system has been tested by a limited number of experiments and found to work satisfactorily. Heterogeneous reactions at solid-liquid-gas interfaces, at high temperatures and pressures, are studied in either autoclaves1&apos;4 or bombs5&apos;9. Autoclaves are usually fairly large vessels which have a stirring arrangement incorporated in the design. Mechanical design limits the use of these vessels to relatively low temperatures and pressures. They are particularly well suited to rate or kinetic studies. Bombs can be designed to be operated at high temperatures and pressures, and are smaller vessels; because of this, stirring arrangements are not easily incorporated. In this paper a multiple-bomb system is described, that has been designed to incorporate the desirable features of both the autoclave and the bomb. The described unit has flexibility for an over all study of leaching. Most of the component units in this assemblage are standard equipment, designed and produced by well known manufacturers. No claim is made to the design of this equipment, and although described in some detail, this is done merely for clarity in the elucidation of the system presented. The general layout of the multiple-bomb assemblage is shown in Fig. 1A and 1B. The basic units in this system are: 1) 6 stainless steel 100 ml bombs (Fig. 4)

Jan 1, 1964

By Alexander Knoll, Dwight L. Baker

THIS paper is a report on work undertaken to investigate the results and conclusions of Ravitz and Porter1,2 that galena freed of surface oxidation products and lead carbonate ("clean" galena) is waterrepellent, and that the action of xanthates in flotation is the action of a cleansing agent, enabling oxidized galena particles to expose a pure lead sulphide, water-repellent surface. The apparatus, in construction and use, was essentially that of Ravitz and Porter. The only significant modification introduced by the present authors was the substitution of a three-necked flask for the flotation cell as the "reaction vessel." Our procedure was to place 50 grams of freshly ground, minus 200-mesh galena in the reaction vessel, sweep out all molecular oxygen from the system with oxygen-free nitrogen, and proceed to wash the galena surface free of its oxidation products with repeated small portions of (I) ammonium acetate (500 c.c. of water, 200 grams of ammonium acetate) or (2) ammonium chloride, hydrochloric acid (2 liters containing 200 grams of ammonium chloride and 25 c.c. Of 1.18 sp. gr hydrochloric acid). The galena was next washed with many 100-c.c. portions of oxygen-free, distilled water. The galena was finally considered free of soluble salts when wash water that had been in contact with the mineral for at least 48 hr.* gave negative tests for: (x) lead ion with sulphide; (2) chloride with silver ion; (3) acetate with cuprous chloride, sodium chloride; and (4) ammonium ion with Nessler&apos;s reagent. Next 500 c.c. of potassium ethyl xanthate solution, free of dissolved oxygen, was run onto the "clean" galena particles. For this system there were determined: I. The wetting properties of the clean galena particles by shaking the reaction flask and noting the degree of mineral collection at the liquid-air interface. This was, of course, simply a qualitative test, but it proved adequate for our purpose. 2. The removal of xanthate ion from the potassium xanthate solution on being shaken with the "cleansed" mineral. Xanthate concentrations were determined by iodine titration according to the methods of Taylor and Knoll.3 3. The pH of the xanthate solution after having been shaken with the "cleansed" galena. The pH was determined colorimetrically.4 The results of five experiments of the type mentioned above are given in Table x.

Jan 1, 1941

By J. H. Jensen

Bromine is the intermediate member of the halogen family of elements between iodine, a solid: and chlorine, a gas. The name is derived from the Greek "bromos," meaning stench. Bromine is the only nonmetallic element that is liquid at room temperatures with a melting point of -7.2" C and a boiling point of 58.78" C. Reddish brown in color, it dissolves easily in water to yield a red solution. Bromine volatilizes at ordinary temperatures to a red vapor that is very irritating to the eyes, nose, and throat. Density of the liquid is 3.12 and gas weighs 7.59 gpl at standard conditions. As the element is highly active, it exists in nature only as bromide compounds. Bromine was discovered by Antoine Jerome Balard in seawater bitterns in 1826 and first prepared in quantity in 1860. Distribution Bromine is widely distributed in nature and compounds occur in solution in natural brines, in seawater, saline lakes, oil and gas well brines, and in evaporite chloride minerals. The concentration of bromine salts ranges from 60- 65 ppm in seawater to several thousand ppm in oil well brines and saline lakes. The distribution of bromine in marine evaporite minerals and in the solutions from which they crystallized was determined many years ago by H. E. Boeke (1 908). Theoretical aspects regarding the geochemistry of bromine have been published in numerous papers (Raup and Mite, 1969). Bromine occurs in solid solution in carnallite and sylvite associated in potash de- posits; in halite in salt beds; salt in oil shales; and in trona deposits. Its presence is useful as a guide in geochemical exploration. The analysis of small amounts of bromides in the presence of large amounts of chlorides is discussed by W. Schwerdtner (1963). Manganese, iron, and iodine may interfere with the determination. Other analytical methods are discussed at length in the literature (Stenger and Atchison, 1964). Sources and Reserves The sources and reserves of bromine, given in [Table 1], appear ample to meet present and foreseeable requirements in all producing countries. With the occurrence of bromine salts in sea-water and other brines, the potential for bromine production is worldwide. It has been estimated that 99% of all commercially recoverable bromine is in the ocean. However, actual subterranean brines having a higher bromine content than seawater will continue to be the preferred sources of bromine for the foreseeable future. Markets and Prices About 17% (1968) of bromine produced is used in its elemental form, with the balance consumed as bromides and bromates. The largest use for bromine is ethylene dibromide which, together with tetraethyl lead, are used as an antiknock additive in gasoline. Tetra-ethyl lead is the antiknock agent. Ethylene dibromide combines with the lead after combustion in the engine to form a volatile com- pound that escapes from the engine with the exhaust gases.

Jan 1, 1975

SHELBY M. HARRISON,* New York, N. Y. (written discussion ?).¬Your secretary requested a brief description of the Russell Sage Foundation, in order that members of the Institute, if they should desire to avail themselves of it, would know what type of service is offered to them through our institution. The foundation was established in 1907 by the gift of Mrs. Russell Sage of $10,000,000 as a capital fund, the income of which is to be spent for the improvement of social and living conditions in the United States. One of the lines of activity which the foundation has felt would lead toward this end is the development and promotion of community surveys; and because the scope and methods followed in these surveys are very similar to the scope and method of much of the institution&apos;s work in general, an idea of its main activities can perhaps be given best by describing one of our surveys. Incidentally, it may be pointed out that antecedent to the survey stand at least two important facts: first, the recognition. that communities are active, not static forces, that they develop, that changes in. material and human relationships occur continuously, and that with them come new social and civic problems which must, in many cases, be diagnosed and prescribed for anew; and second, the reality of scientific advances along lines which make possible at least some measure of solution of the problems. Evidences of these changes are abundant; many of them are found in the rapid growth of cities in the last few decades. Villages in agricultural districts, places where everybody knew everybody else, where the pulpit had been long the chief or only influence molding public opinion, where the air was unclouded by the smoke from factory stacks, where the water supply was not affected by pollution, where sunlight and building

Jan 5, 1918