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By Cyril Stanley Smith

For many years sulphur and its congeners selenium and tellurium have been regarded as very harmful elements in copper and copper-rich alloys. Like many similar prejudices, this has been found to be partly wrong. All three of these elements actually have no great effect on the working properties of copper and its alloys, and are desirable additions in that they considerably enhance the machinability of alloys in which they are present. Because of their possible commercial importance, a study of the machinability and other properties of the pure binary alloys was made, as described in this paper, and the effect of selenium on a large number of copper alloys was determined. The current opinion regarding the deleterious effects of elements in this group undoubtedly arose because of occasional failures of tough-pitch copper containing unusually high tellurium, and because of the well-known fact that sulphur causes spewing and unsoundness in tough-pitch copper. Siebe,1 also Deretchey and Margolina,2 studied the effect of sulphur on copper and showed that in the absence of oxygen it was present in the form of copper sulphide, which was less harmful to the properties than an equivalent amount of copper oxide. No data have been published on selenium and tellurium, although the statement is often made, following Eggleston,3 that tellurium makes copper hot-short. Copper specifications call for only traces of these elements. Skowronski and Mosher4 give data on the effect of selenium and tellurium on the conductivity of tough-pitch copper. In private communication Mr. Skowronski says that the samples were hot-forged from small castings and drawn to 0.081 in. diameter, but it should not be inferred from this that these elements are harmless to the working properties of wirebars and commercial shapes. Constitution and Microstructure Constitution.—Sulphur, selenium and tellurium exist in their alloys with copper in the form of copper sulphide, selenide or telluride. These compounds are practically insoluble in the solid state and possess limited

Jan 1, 1938

By A. H. Willis

In this paper the results of an exploratory study conducted by personnel of the Knolls Atomic Power Laboratory on 18.6, 22, and 40 wt pct uranium-zirconium alloy will be presented. LARGE power output and long life or endurance from small, compact nuclear reactors require the use of enriched uranium for a fuel material. However, the ability to remove heat from the element, the tolerable fission product concentration, or some physical limitation of the system can limit the allowable fuel enrichment, or the volume of the fuel. In such an event, the fuel-element designer must find a suitable diluent for the uranium. Zirconium is an attractive material for such a purpose as it has good nuclear properties and a low absorption cross section. Because it has a good corrosion resistance in water, zirconium is a suitable cladding and the uranium-zirconium alloy makes a good core material. The alloy has a high thermal conductivity, a low elastic modulus, and a low thermal-expansion coefficient, all of which tend to minimize the thermal stresses in the core. Furthermore, the unirradiated material is reasonably ductile and has adequate strength. DESCRIPTION OF SAMPLES Two types of cylindrical samples were used in this study 1) short, 1/2-to 1-in.-long samples to test the irradiation stability of the alloy and 2) 2-ft-long samples to investigate the resistance of an element to longitudinal deformation. Composite samples having 0.060-to 0.140-in. core diameters and clad with a 0.010-in. thick zirconium jacket were fabricated by coextrusion and by hydrostatic pressure bonding of the cladding to the preformed core material. Both fabrication processes produced the uniform metallurgical core-to-cladding bond which was felt necessary to minimize the uncertainty of the central core temperature. Both consumable-arc and induction-melting techniques were used to melt the uranium-sponge zirconium core alloy. Since a graphite crucible was used in induction-melting this alloy contained more carbon impurity, which resulted in a finer grain size than the arc-melted alloy. The core to cladding interface was uniform in elements coextruded from the fine-grain, induction-melted core material, while those elements fabricated using arc-melted core material had very irregular interfaces because of the coarser grain size. Both cold-worked and heat-treated fuel materials were irradiation tested. Cold-worked alloys were swaged to about a 5 pct final reduction in area without subsequent annealing. The heat-treated alloys were heated to 800°C, held at temperature for 15 min and furnace-cooled to about room temperature. This

Jan 1, 1960

By N. N. Breyer

A specially built "hard" tensile machine with characteristics permitting the precise detertnination of the drop of the load at the yield point has been used to study the magnitude of the yield-point phenotnenon in prestrained martensitic 4340 steel. A new phenonzenon, the appearance of a secondary yield point, has been observed by holding the specimen at constant strain in the plastic region. Furthermore, it has been found that a series of yield-point drops could be introduced by successive constant strain holds in the plastic region. The isothermal kinetics of the development of the secondary yielding point lave been studied at four temperatures: 24° 0° -18°, and -79°C. From the results of the kinetic investigation, equations for the In a previous investigation1 it was shown that, contrary to generally held opinion, steels of medium carbon content, such as 4340, 4140, and 86B30, in the as-quenched martensitic condition, can be cold-drawn through a die with reductions in area of up to 10 pct without cracking. Tensile specimens of 4340 machined from bars quenched and prestrained in this manner exhibited tensile strengths of about 400,000 psi coupled with 30 pct reductions in area. In addition, it was found that each sample of such steels exhibited a yield point in the quenched, cold-drawn condition. Since these studies were conducted on a commercial hydraulic testing machine of a type which is not well-suited to detailed study of yield-point behavior, it was decided to study this phenomenon more thoroughly on a rigid straining machine. In this new investigation, use of such a "hard" machine not only allowed study of the magnitude of the yield-point drop but also revealed a new phenomenon—secondary yielding of the martensite introduced by stopping crosshead motion after plastic deformation of the sample had begun. The present paper is a report of these findings. MATERIALS AND PROCESSING The material used was a commercial 4340 steel of the composition shown below: 0.41 0.80 0.013 0.019 0.31 0.85 1.76 0.28 1 0.42 0.77 0.015 0.024 0.30 0.84 1.69 0.28 0.08 2 1 = Ladle analysis. 2 = Laboratory analysis. Bars of this steel were processed in the following way: 1) machined to predetermined diameters; 2) austenitized at 870°C for 1 1/2 hr; 3) oil-quenched; 4) cooled to -115°C for 1/2 hr; onset and increase in magnitude of the secondary yielding in this temperature region have been found to fit the relationship ?Ys = Atn where ?Ys is the magnitude of the secondary yield Point in psi, t is the time in seconds, and A and n are parameter characteris-tics of the material. Although the occurrence of the primary and secondary yield points could be rationalized qualitatively on the basis of stress-induced ordering of carbon atoms in the stress fields of dislocations, as postulated in an earlier paper, the kinetics of the secondary-yield-point development were interpreted to indicate that the ordering involves more than just single jumps of carbon atoms from high-energy to neighboring low-energy sites. 5) pickled and lime-coated; 6) drawn through a carbide die. The predetermined diameters were chosen so that drawing through the same die gave the various reductions desired. Tensile specimens of 0.252 in. diam with a 1 1/4 in. gage length were then prepared from the drawn bars and tested. In order to study the stress-strain behavior at the yield point in detail, a rigid tensile machine with a high spring constant was constructed. Columns of large cross section (relative to the specimen cross section) constituted the machine frame. A dc motor was used to drive a screw via a gear reducing train and a "crane" thrust bearing. In this relatively simple device small deformations could be observed un-blurred by the slow response and lower spring constant inherent in hydraulic machines.' A strain-gage dynamometer permitted load changes as small as 8 lb to be read. RESULTS Tensile test samples machined from bars in the as-quenched condition with no subsequent drawing and samples from bars with 3.8 pct reduction after quenching gave stress-strain curves typified by those shown in Figs. I and 2. The time lapse between predrawing and tensile testing varied but usually ranged between 3 to 6 days at room temperature. The strain rate during testing was 0.003 in. per in. per min. The as-quenched curve is seen to have a broad serrated maximum whereas the stress on the specimen prestrained 3.8 pct rose linearly to point A, Fig. 2, fell abruptly to B, and then gradually to C. The abrupt drop to B was accompanied by evidence of incipient necking. The drop of the stress at the yield point in the prestrained samples (A to B in Fig. 2) changed with the percent prestrain, as illustrated on Fig. 3. Although the tensile strength increased continuously with the amount of previous cold drawing, the magnitude of the yield point drop first increased—up to about 6 pct prior reduction—and then decreased. Specimens from bars predrawn more than 8 pct broke in a brittle fashion in the elastic portion of the stress-strain curve.

Jan 1, 1967

By Persifor Frazer

IN his “Final Report," Vol. II, part second, p. 763, Prof. Rogers sums up the metalliferous veins of the mesozoic sandstone by remarking that these are not associated with dykes or trap-rock, but are independent metalliferous injections. But singularly enough, in enumerating the different kinds of ores, no mention is made of

Jan 1, 1877

By R. K. Buhr, H. Thresh, M. Bergeron, F. Weinberg

The microsegregation of nickel and chromium in directionally solidified AISI 4340 steel castings has been measured using electron probe microanalysis. Minimum concentrations were observed to occur at the center of the dendrite stalks, as reported previously. However, the position of the maximum concentrations could not be determined from the dendrite configuration. An etching technique has been developed which shows the position of maximum concentration. Measurements were made of the distribution of nickel and chromium in the dendritic structure. The ratio of maximum to minimum concentration was determined as a function of primary dendrite arm spacing for both as-cast and partially homogenized materials. The results are compared with observations reported in the literatuve. A S part of an investigation of solute segregation in directionally solidified AISI 4340 steel casting, electron probe microanalysis was used to measure the distribution of nickel and chromium in the dendritically segregated material. This complemented the observations on the segregation of radioactive phosphorus obtained by autoradiographic techniques in the same castings.' Kattamis and I?lemings2 have reported similar measurements, using electron probe microanalysis, on dendritically segregated AISI 4340 steels. They found minimum solute concentrations occurred at the center of dendrites, maximum concentrations occurred in the center of interdendritic regions, for symmetrically oriented dendrites, and a regular variation of concentration within dendrite arms. The ratio of maximum to minimum concentration was found to be essentially independent of position in the castings, except near the chill surface where it was somewhat higher. Assuming complete diffusion in the liquid and no diffusion in the solid during freezing, they considered that isoconcentration curves in the steel were homothetic. As a result, isoconcentration curves of the various elements, contour surfaces of dendrites produced by isothermal-transformation studies, and the contour of the solid-liquid interface would all be similar, and could be superimposed by a uniform expansion or contraction of the contours. Preliminary results of the present investigation suggested that isoconcentration curves were not homothetic. It was also evident that points of maximum concentration could not be predicted from the dendrite configuration. Since the ratio of maximum to minimum concentration appeared to be an important parameter in defining the overall segregation in a casting, other techniques for determining the point of maximum concentration were investigated. In addition the overall solute distribution associated with the dendritic structure was examined for both nickel and chromium, and the consistency of the distribution for neighboring dendrites was determined. METHOD Fifty-pound heats of AISI 4340 steel were cast in a manner similar to that used by Flemings et al3 with a water-cooled copper base plate and exothermic sides and top. The nominal composition of the material was C, 0.41 pct; Mn, 0.66; Si, 0.35; S, 0.012; P, 0.010; Ni, 1.88; Cr, 0.95; Mo, 0.28. The steel solidified directionally from the chill surface, with a dendritic structure which increased in dendrite arm spacing with increased distance from the chill. Results of the general investigation of the cast structure and segregation of radioactive phosphorus in these castings have been reported elsewhere.' For the present measurements, sections were cut from the casting at several distances from the chill surface. The sections were subsequently heat-treated, mounted, and then polished on a plane perpendicular to the general freezing direction of the casting. Electron probe microanalysis was carried out with the JEOL-JXA3 microprobe using a voltage of 25 kev and beam current of 0.15 µa. The take-off angle is 22 deg. Quartz crystals were used in the spectrometers and measurements made for Ka radiation from both nickel and chromium simultaneously. A thin layer of carbon was deposited on all specimen surfaces prior to examination in the microprobe. Early measurements were made on polished surfaces, with indentation marks produced by a hardness tester to indicate the area of interest. It was found desirable to use etched surfaces, as opposed to polished surfaces, to reduce sample preparation time and more readily relate the microprobe scan to the structure. To determine if this could be done, without introducing significant errors, a series of measurements were made on polished and etched surfaces of the same specimen. Both polished and etched surfaces produced similar results within normal scatter as shown in the observations. Subsequent measurements were then made on etched surfaces. Measurements with the microprobe analyzer were made by point counting, for periods of 100 sec, at 10-µ intervals. Ten-second counts were made on pure nickel and chromium standards, incorporated in the specimen mount before and after each set of measurements. The results were adjusted for background, then corrected for dead time using the expression:

Jan 1, 1969

By William Wraith

At the Washoe smelter, Anaconda, Mont., the blister-copper from the converters is transferred, by means of a crane, to a re-fining-furnace, in which it is brought to proper pitch by means of air and poles. From this furnace the refined copper, containing gold and silver, is poured into cast-iron molds placed on a platform-convejor, giving an anode 36.75 in. long, 35 in. wide, and 2 1/16 in. thick. By reason of a disagreement between the smelter and the refinery, in reference to the silver-content of the anodes, it becanle necessary to investigate the methods of sampling used. 11. SMelter Method of SampliNg. At the smelter the sampling is done by " shotting " into water a small portion of the molten stream of copper as it flows from the furnace, by " batting " the stream'with a wooden paddle. The first sample is taken 30 min. after the pouring i.: started, three other samples being taken at 1-hr. interrals, each sample Weighing from 4 to 6 oz. The samples are dried, esamined for particles of burnt wood, screened on a 10-mesh screen of NO. 8 wire to remove the fines, the oversize then screened on a 4-mesh screen of No. 20 wire to remore the coarse, the undersize of this screen being taken as the sample. The four portions thus obtained are thoroughly mixed and split in half by passing over a 16-slot splitting-device, slots being 0.5 in. wide. One-half of the sample is sent to the laboratory for analysis and one-half kept as a duplicate. 111. Refinery Method of Sampling. The method used at the refinery and also used in this in1-estiyation is the one developed by Dr. Edmarcl Keller, of

Jan 1, 1911

By N. F. Mott

Jan 1, 1961

COUNCIL OF SECTION DELEGATES Nicholas A D'Arcy, Jr, Chairman (Southern California Section) Charles Chapman, Vice-Chairman (Florida Section) Ben H Parker, Secretary (Colorado Section) Frontier Refining Co Boston Bldg Denver 2, Colorado

Jan 1, 1956

Jan 1, 1893

Jan 1, 1915

By D. E. Swets, R. C. Frank

It is well known that hydrogen is introduced into iron or steel as a result of many chemical processes (acid pickling, electrolytic cleaning, plating, etc.). One of the reactions that has been of recent interest1 is the reaction between an iron surface and water vapor. It was shown a few years ago2-4 that hydrogen can be introduced into steel at an accelerated rate during abrasion as a result of this reaction. Grun-berg and Scott have also observed that water in mineral oil lubricants increases pitting failure in ball bearings5 and they have suggested that hydrogen from the water is the primary cause of this effect.' In this laboratory, the question was raised as to whether or not hydrogen is also introduced into the metal surface of a bearing as a result of the decomposition of the hydrocarbon lubricant itself, and an experiment was performed to try to find a satisfactory answer. All steel parts contain some residual hydrogen. Therefore, it appeared that the best way to carry out this experiment without the need for highly accurate quantitative analyses was to use deuterium as a tracer. The natural abundance of deuterium in H2 is only 0.015 pct. The tracer was obtained in the form of deuteroparaffin (CD,(CDJ, CD,) and 0.25 g were dissolved in 20 cc of mineral oil to form the lubricant to be used in the tests. The bearings used were New Departure Type QOLOO ball bearings with a ball diam of 0.187 in. Prior to adding the mineral oil-deuteroparaffin lubricant, the bearings were cleaned in warm trichloroethylene to remove the packing grease. After packing with the new deuterated lubricant, the bearings were operated in a bearing fatigue test machine under a radial load of 190 lb and a thrust load of 190 lb at a speed of 3800 rpm. The expected life under these conditions is about 500 hr. Two tests were made; one for a period of 27 hr and the other for a period of 102 hr. The bearings achieved a temperature of 120o F during the tests. When the tests were stopped the balls were mechanically removed from the bearings and were immediately placed in liquid nitrogen to reduce degassing until the analysis for deuterium could be made. Before analyzing, the balls were warmed to room temperature and scrubbed with several degreasing agents to remove all traces of the deuteroparaffin mixture. This cleaning procedure was shown to be satisfactory by running a control test in which one ball bearing was subjected to all parts of the test except running in the fatigue machine. The hydrogen and deuterium were removed from the balls using a hot extraction apparatus attached to a mass spectrometer. Four balls from each bearing were analyzed. Each one was analyzed separately by removing it from a cold storage volume of the hot extraction apparatus and transferring it to the oven tube with a magnet. As the gases were evolved they were analyzed with the mass spectrometer. Since the hydrogen and deuterium pass through steel in the atomic form and since there are many more hydrogen atoms than deuterium atoms in the sample, the probability of forming an HD molecule is greater than forming a D2 molecule. For this reason the evolution of HD and H was followed as each ball was placed in the oven. The results showed that as each ball from the test bearing was dropped into the oven, the mass spectrometer recording of the HD evolution increased by about ten divisions. When balls from the control test bearing were dropped into the oven, the increase was about one division or less. The hydrocarbon background in the mass spectrometer was also monitored to see if hydrocarbons or deuterocarbons were given off when the balls were dropped into the oven, but no change in the hydrocarbon peaks was observed. Since the balls contained a fair amount of residual hydrogen, isotope ratio measurements were made on the gas obtained from each ball. The D/H value found for those balls which had been operated in the fatigue testing machine was consistently about 0.3

Jan 1, 1962

By John Wulff, J. H. Hollomon

THE opinion has been widely held that the corrosion of alpha brass occurs by the selective solution of zinc. As late as 1939, Fink1 and Evans2 suggested that in the initial stage of the corrosion the selective solution of zinc produces copper-rich areas, which subsequently act as cathodes that facilitate the deposition of copper. Previously Abrams3 had shown that most of the copper found on corroded brass was redeposited and not residual, although he did not consider the nature of the initiation of the corrosion process. Enough data exist to indicate that any metal surface is sufficiently heterogeneous to provide the anodes and cathodes necessary for the initiation of corrosion.4,5 Thus, for alpha brass we need postulate not an initial selective solution of zinc, but only the existence of local differences in electrochemical potential. The heterogeneity responsible for potential differences may arise from oxide and other films as well as from alloy concentration gradients. Even though selective corrosion may be possible in some alloy systems, previous data on alpha brass as well as the experimental work reported in this paper do not require this supposition. Bengough and May,6 in a discussion of Abrams' paper, first suggested the addition of small amounts of arsenic (0.03 per cent) to alpha brass to prevent the redeposition of copper (dezincification). This suggestion was later substantiated by Nixon.7 In their studies of the inhibiting influence of arsenic, Evans and Fink were led to the selective-solution hypothesis in order to explain the initial corrosion of such alloys. They believed that an arsenic film covered anode areas and prevented the formation of copper-rich spots capable of acting as cathodes for the deposition of copper. They did not consider, however, the mechanism by which the arsenical film was formed. Bengough and May,8 in another publication, suggested that the commonly found gray or black arsenical film may act to: (I) carry oxygen to the brass surface, (2) increase the discharge potential of copper on brass, (3) precipitate cuprous chloride from colloidal suspension in chloride solutions. Masing9 assumed that the film found upon arsenical brass was metallic arsenic. His measurements of hydrogen overvoltage of bulk arsenic led him to believe that the inhibition of dezincification occurs because the overvoltage of a brass surface is lowered by the arsenic film. He reasoned that this film would permit the more rapid reduction of hydrogen at the cathode, which would prevent the redeposition of copper. In a recent paper,10 we have pointed out that the film formed during the corrosion of arsenical brass and copper in stagnant solutions is essentially arsenious oxide (As203),

Jan 1, 1942

By Persifor Frazer

In his " Final Report," Vol. 11, part second, p. 763, Prof. Rogers sums up the metalliferous veins of the mesozoic sandstone by remarking that these are not associated with dykes or trap-rock, but are independent metalliferous injections. But singularly enough, in enumerating the different kinds of ores, no mention is made of

By K. Stout, E. Van Eeckhout, L. Friel

Previous research at the Montana College of Mineral Science and Technology indicated that it is practical and economically feasible to place stiff back- fill in a cut-and-fill stope. This backfill would reduce wall closure and high stress buildup in pi1llars, thus alleviating rockburst potential. Three ;topes from the Sunshine Mine, of the Coeur d’Alene Mining District, were chosen for a test verification of this concept. Although the first stope was lever mined beyond the initial cut (for economic reasons), some vibrating wire stressmeter results were obtained and found to compare favorably with numerical predictions. Some other instrumentation devices were built and tested, but never installed .

Jan 1, 1984

By A. Keil

TO measure the absolute conductivity of metallic specimens it is generally necessary to have exact geometrical shapes and good electrical contact with the test-piece. To overcome limitations of the standard methods, an electronic conductivity-meter* Trade name, Sigmatest; model Dr. F. Forster; Reutlingen, Ger-many. has been developed, which works on the principle of inducing high frequency eddy-currents in the specimens and measuring the reaction of these curients on a measuring coil.',' To attach the instrument to the test specimen, a flat area of about 10 mm diam is all that is necessary. The reading is taken off a scale calibrated in pet of International Annealed Copper Standard. The induced eddy-currents are propagated in a circular motion parallel to the surface. Thickness of the layer included in a measurement depends on the frequency used. With a frequency of 60 kc per sec, the penetration of the currents was 0.8 mm at the upper limit of the scale, and 2 mm at the lower limit. The method is limited to nonferrous metals and other applications have been described elsewhere." The object of the present investigation was to detect the formation and growth of surface layers of differing conductivity, and to determine the depth to which these changes could be observed. A well known phenomenon which illustrates the problem is the internal oxidation of certain silver alloys containing base metal solutes, such as copper or cadmium, when they are annealed in an oxidizing atmosphere.4, 5 Until now, the only methods available for following these phenomenon have been metallo-graphic examination and hardness tests.0, 7 Changes in mechanical properties of copper alloys by internal oxidation were recently discussed in a more general way by Martin and Smith." When measuring these conductivity changes it must be remembered that the only absolute values of conductivity are those of 1) the nontreated homogeneous specimen, and 2) the final values obtained with a surface layer of depth comparable to the penetration of the eddy-currents. All intermediate values refer to the mixed conductivities of the transformed surface layer and the untransformed alloy, and are thus readings of relative value only. Experimental Results Specimens were annealed for 1/2 hr at 800°C in hydrogen, and the internal oxidation was carried out by thermal treatment in air at 800°C. Fig. 1 shows the results of the first series of experiments. With internal oxidation of a solid solution of 8 pet Cd in silver, the conductivity rises continuously until the surface layer formed has become thick enough to be the deciding factor (about 400µ). Precipitates of CdO are mainly in the form of points, Fig. 2, and, as a result, the electric contact between the silver crystals is not distorted by them. Brine11 tests were run with a 1.25 mm ball and a 7.812 kg load. The specimen annealed in hydrogen and oxidized to a depth of 400µ had a hardness of 40 Bhn,

Jan 1, 1959

By John F. Elliott

STAFF: Editor, Gerhard Derge Acting Editor, Poul G. Shewmon Carnegie lnstitute of Technology Schenley Pork Pittsburgh 13, PO. Editorial Assistant, M. A. Redmerski Production Editor, Otto T. Johnson THE METALLURGICAL SOCIETY: Rich-ard C. Cole, President; Karl L. Fetters, Past-President; J. H. Scoff, Vice President; R. L. Henneboch, Treasurer, R. W. Shearman, Secretary. PUBLICATIONS COMMITTEE OF THE METALLURGICAL SOCIETY: R. E. Lund, Chairmon; T. E. Dancy, P. R. Gouwens, W. A. Krivsky, F. C. Longenberg, E. R. Morgan, R.R. Nosh, Poul Queneou, W.O. Philbrook, J. H. Scoff, L. L. Seigle, and M. E. Wadsworth. Review and selection of manuscripts is under the supervision of the following Publications Committees: Extractive Metallurgy Division: M. E. Wadsworth, Chairmon; R. E. Grace, Vice Chairman; D. H. Baker, Jr., G. M. Bell, D. H. Bridges, J. M. Cigon, G. W. Healy, R. A. Lewis, C. E. O'Neill, A. W. Schlechten, R. E. Shinkoskey, and W. W. Stephens. Iron and Steel Division: T. E. Dancy, Chairman; A. Muan, D.W. Murphy, R. D. Pehlke, J. M. Uys, J. 5. Wagstoff, and R. G. Word. lnstitute of Metals Division: R. R. Nash, Chairman, H. H. Johnson, Jr., Vice Chairman; M. R. Achter, P. A. Beck, J. J. Becker, G. F. Bolling, J. 0. Brittain, J. 8. Clark, R. 5. Davis, A. E. Dwight, R. W. Fountain, L. A. Girifalco, E. L. Harmon, J. J. Heger, A. A. Hendrickson, L. Himmel, J. P. Hirth, R. H. Richmao, H.C.Rogers, W. Rostoker, 0. D. Sherby. E. A. Steigawald, R. Steinitz, H. C. Stumpf, R. A. Swalin, W. A. Tiller, W. R. Upthegrove, D. Walton, H.W. Weart, and D. Wilsdorf. Published bimonthly by the American lnstitute of Mining, Metallurgical, and Petroleum Engineers, Inc 345 East 47th Street, New York 17. N. Y. Telephone PLaza 2-6800. Subscription $30 per year for non-AIME members in United States and North, South, and Central America; $32, foreign;$30per $7 50 for AlME members. Single copies, $6.00, single copies foreign, $6.50. The AlME is not responsible for any statement made or opinion expressed in its publications ... Copyright 1963 by the American lnstitute of Mining, Metallurgical, and Petroleum Engineers, Inc....Registered cable address, AlME New York . .. Indexed in Engineering Index, Industrial Arts Index, and Chemical Abstracts . . Second class postage paid ot New York, N. Y., and Ann Arbor, Mich. Volume 227, Number 4.

Jan 1, 1963

By B. C. Allen

The solubility of chromium in liquid silver and that of molybdenum and tungsten in liquid tin have been determined by equilibrating Ike Liquid in a crucible of the solule metal. Generally the weight of solute in solulion was delermined both chemically and from crucible weight losses. The resulting weight percent solubilily of chromium in silver as a function of absolule temperature T is given by log w = -6660/T + 4.02 in the range 960° to 1445°C, and that of molybdenlttrl in tin by log w = —5050/T + 1. 79 in the range 1200° to 2200°C. The values appear unaffected by minor changes in solute composition. Calculations aye made of the parlial molar heal and excess entropy of mixing. The estimated solubility of tungsten in tin is 0.001 pct at 2000°C. Evidence is presented that molybdenwm dissolves in tin without compound for mation and that tungsten and tin form W10Sn. RECENT developments in coatings, heat transfer, and brazing require a knowledge of equilibrium solubilities in a variety of systems at elevated temperatures. Of particular interest are solid-liquid interactions in metal systems involving dilute solutions. This investigation was undertaken since little is known about the phase relations or solubility of chromium in liquid silver or of molybdenum and tungsten in liquid tin.1,2 EXPERIMENTAL WORK As indicated in Table I, high-purity metals or those of known impurity levels were used. Crucibles were machined from chromium, molybdenum, and tungsten bar stock 1.3 cm diam and 2.2 cm long. Chromium rod was prepared by arc melting and extruding iodide process crystals.3 The five chromium impurity alloys were in the form of 0.6-cm-diam swaged rod. A Cr-0.06N* alloy was prepared by exposure to NH3 at 1150°C in a closed quartz capsule for 24 hr. Because significant nitrogen was lost during annealing in argon at 1600°C,4 the estimated level was 0.01 pct N. Chromium and Mo,W crucibles were outgassed at 1200" and 1600°C, respectively, at 3 X 10-5 mm. The solvent was placed In crucibles of the solute metal- 6 g Ag in chromium, 0.4 g Ag in the five chromium impurity alloys, and 4 g Sn in Mo,W crucibles. The silver and tin series were outgassed at 900" and 110O°C, respectively, and held at the desired solution temperature in a tantalum resistance furnace under 1.05 atm 99.995 pct Ar. An equilibration time of 0.5 to 1 hr was chosen since 0.3-, I-, and 4-hr anneals at 1235°C for Cr-Ag yielded similar results. Temperatures were measured optically to +10°C under essentially black body conditions which were checked against the melting point of silver. The Cr-Ag and Mo-Sn,W-Sn series were respectively equilibrated at 990° to 1400°C and 1200" to 2000°C. Vaporization losses were generally held to <1 pct by the argon. In the 1800" and 2000°C anneals for 0.5 hr, the crucibles were placed in tightly sealed tantalum cans which kept tin losses to <5 pct. After the anneals, the specimens were furnace-cooled. One anneal was made on small Mo-0.02 C, Mo-0.5Ti-0.lZr, and tungsten crucibles containing tin at 2200°C. The metals were sealed in an electron-beam-welded tantalum can of minimum volume. After the anneal, tin was still present in each crucible, none of which was severely attacked. After equilibration, the saturated solvent metal was selectively removed from the crucible by acid leaching. Weight losses sustained by the crucibles were determined from the initial weight minus the final blank-corrected weight after acid leaching. Chemical analyses were performed on some of the samples. Hot 1:l HNO3-H2O removed silver from chromium with the blank running <0.1 mg or <0.002 pct on measured solubility. Tin was removed from molybdenum and tungsten by hot concentrated HC1 with the respective blanks amounting to -0.004 and -0.0004 pct in the presence of tin. The insoluble residues were weighed and checked for composition. The leaching solutions contained traces of the solute metals which were analyzed by colorimetric methods, Diphenyl Carbazide for chromium, Thiocyanate for molybdenum, and Dithiol for tungsten. The total of the two percentages found from the residue and leaching solution minus the blank gave the desired solubility values. On the basis of annealing empty molybdenum and tungsten crucibles, weight losses due to MoO3 or WO3 volatilization were found to be generally 10.4 mg and affect measured solubilities by <0.01pct. RESULTS AND DISCUSSION Chromium-Silver . Since no intermediate compounds are reported to form in the Cr-An system,&apos; crucible weight losses and chemical analysis of the entire melt should provide reliable measures of the chromium in solution. Values obtained by the two methods are in agreement as shown by the results for unalloyed chromium in Table II and plotted in Fig. 1. Furthermore, the results are consistent with those previously determined by melting equilibrated silver out of the crucible and analyzing calorimetrically for chromium.&apos; On the basis of limited thermal analysis data, the solubility of chromium in silver has been quoted as 8 pct at the monotectic temperature of -1445°C.1 This investigation indicates an extrapolated solubility of 1.38 pct which is believed to be more reliable. At the eu-

Jan 1, 1968

By R. Stratton-Crawley

Flotation-related processes utilizing an oil phase for processing fine mineral particles have been described and various applications discussed. The problems associated with the techniques are varied, but may be summarized by the following areas; (1) applicability to fine particle beneficiation, e.g. collector extender and emulsion flotation. (2) major &apos;mechanical&apos; problems, e.g. emulsion breakage and oil recovery in oil flotation. (3) complex interfacial chemistry, e.g. empirical nature of pigment flushing .

Jan 1, 1979

By Thys B. Johnson

Traditional mine planning concepts are discussed and suggestions for improvement through use of the developed model are proposed. The approach developed in this paper allows optimal planning of the complete mining-concentrating-refining system over the entire planning horizon and permits the system to dictate how and when to process a block of material, i. e., a dynamic cutoff.

Jan 1, 1969

By S. K. Nicol, A. R. Swanson, J. C. Day

Addition of oil to a suspension of hydrophobic coal particles can influence its dewatering characteristics. An agglomeration process occurs in which coal particles are held together by negative capillary pressure at particle/oil/water contacts. Consequently, the units round which flow can occur are enlarged and this improves dewatering parameters such as drainage rate, solids recovery, and equilibrium moisture content. This paper discusses processes which attempt to use this principle, in terms of metallurgical and economic efficiency. The discussion is augmented by results of recent experiments on the effect of oil addition to centrifuges and vacuum filters.

Jan 1, 1980