Search Documents

By J. H. Brophy, J. Wulff, H. W. Hayden

The mickel-activated sintering of tungsten occurs in two stages of densification. A kinetic analysis of the second stage has been based on an appropriate model of the process. As in the first stage, the rate-controlling mechanism for the second stage is also the solution of tungsten in the nickel carrier phase. The transition from the relatively rapid first-stage results from the spherozdization of pores and the initiation of grain growth. Finer grain size due to higher-nickel content leads to more rapid and higher degrees of densification 1 HE sintering of tungsten is accelerated by small additions of nickel, cobalt, and iron.' Experimental evidence in detail has shown that nickel-coated, hydrogen-reduced tungsten powder may be sintered to more than 90 pet of theoretical density at l100o C.2, 3 Simultaneously, a kinetic analysis of the process showed that it took place in two distinct stages. In the first stage, nickel evidently served as a carrier phase through which tungsten atoms could move. This stage was kinetically similar to the "solution-precipitation" step postulated when the carrier phase is a liquid,4 although in the Ni-W case, there is no evidence of the existence of a liquid phase either in equilibrium phase relationships or in microstruc-tures at the temperatures under consideration. It has been shown that this stage corresponds to a process which is rate controlled by a phase boundary reaction.3 More recent evidence has been presented5 showing that after the initial rapid stage of sintering, densification continues in the final stage but at a slower rate, although no mechanism for this stage of densification was defined. An analysis of later stages of densification in solid state sintering has been presented,6 but it is not directly applicable in the present case of activated or carrier phase sintering. It is the purpose of this investigation to study the final stage of nickel activated tungsten sintering in greater detail The effect of varying nickel content has been examined, and a possible kinetic mechanism defined. EXPERIMENTAL PROCEDURE AND RESULTS Commercial hydrogen-reduced tungsten powder from Wah-Chmg Corp., having a nominal particle size of1 µ and a B.E.T. specific surface area of 5500 sq. cm per g was mixed with aqueous solutions of hydrated nickel nitrate in proportions sufficient to produce nominal compositions of 0.25, 1, 3, and 5 wt pet Ni. This solution was then evaporated to dry-ness at approximately 150" C for 15 hr. Following evaporation, the resulting powder cake was broken with a mortar and pestle and reduced in hydrogen at 800oC for 1 hr. Following reduction, the powder

Jan 1, 1962

By David A. Thomas, Eugene S. Meieran

MECHAMCAL, electrical, and other property measurements are often more easily made on wires than on sheets. In order to carry out transmission electron microscopy on the same material used for property determinations, we have developed a method for preparing thin foil specimens of wires. The technique was developed for 0.030 in. diam tungsten wires, and is a modification of the thinning techniques used by Wilsdorf, et al 1 A length of wire is first ground to about 0.010 in. thick by mounting the wire in low melting temperature wax, hand grinding a longitudinal flat, removing and reversing the wire in the mount, and then grinding a second parallel flat. The 0.030 in. wide and 0.010 in. thick strip is cut into 1/8 in. lengths to fit in the specimen holder of the electron microscope. Next the specimen is gripped in platinum-tipped tweezers (the anode) and placed 2 mm below a hol- low copper cathode with a 0.010 in. ID nozzle. Electrolyte, 10 pct NaOH, flows by gravity feed through the nozzle onto the specimen, as shown in Fig. l(a). Polishing is carried out until a shallow impression is made on one surface, and then the specimen is turned over and the opposite surface indented. The metal between the two impressions should be about half the specimen thickness, as is shown by the heavy line in the cross section in Fig. l(b). The entire specimen is then electropolishedin 2 pct NaOH until a hole appears at the location of the indentations. The apparatus is shown in Fig. 2, and is essentially the same as that used by Wilsdorf et al. at The Franklin Institute. Light is reflected by a mirror onto the bottom surface of the specimen! which is viewed by a stereoscopic microscope placed above it. Polishing is carried out until light is seen, indicating that a hole has formed, and then immediately stopped. The specimen is washed in water. alcohol, and ether, and is then ready for examination. The specimen should be reversed in its platinum clip during electropolishing to insure equal polishing on both sides of the impression. For tungsten, indenting at 120 v and 0.04 amp takes less than 1 min, and final polishing, at 10 v and 1 amp, less than 5 min. The portion of the specimen available for transmission microscopy surrounds the hole, as is seen by the dashed lines in Fig. l(b). Slight electroetch-ing accompanying electropolishing reveals the mi-crostructure, as seen in Fig. 3(a) by light microscopy. Low-magnification electron microscopy, as in Fig. 3(b), enables the same areas and grains to be viewed and identified when subsequently examined at high magnification. Fig. 4 is a typical structure of

Jan 1, 1963

The Carlin gold deposit is located in northeastern Nevada about thirty-five miles by road from the town of Elko. Following the staking of six square miles 'of ground, a drilling program outlined a fine ore body mineable by open pitting. The resulting mine turned out to be the largest open-pit gold operation in the world, until the Rosario Pueblo Viejo operation was started in 1975. Because of the high profitability forecast at the then $35 gold price, construction of a 2000 stpd mill was commenced on a crash program and was completed for Newmont Mining Corporation by Bechtel Corporation in ten months. Production was started in early 1965. The gold mineralization occurs in marine-type sediments, chiefly silt- stones and limey shales, and the ore characteristics make for a difficult materials-handling problem. At 5% to 6% moisture the ore is dusty during crushing, but even a light rain or snowfall virtually turns the material into a slurry. Crushing this sticky ore below 314 in. (19 mm) in the dry season and 1 in. (25.4 m) during the winter is extremely difficult and leads to problems with conveyors, chutes, and fine ore storage. The initial flowsheet for Carlin's crushing plant used a 5 ft by 22 ft (1.52 m by 6. 7 m) vibrating feeder -grizzly under the 60 -ton dump pocket for feeding the 42 in. by 48 in. (1067 mm by 1220 mm) single toggle jaw crusher and a 5 ½ ft (1.52 m) standard cone crusher in closed circuit with a 6 ft by 12 ft (1.83 m by 3.66 m) vibrating double - deck screen. Because continual packing of fines in the vibrating feeder pan would cause frequent plant shut-downs to remove the fines with jack hammers, the decision was made to replace the vibrating unit with an apron feeder and stationary grizzly ahead of the jaw crusher. A dribble belt was also installed under the apron feeder. This installation has greatly improved the feeding of the pit run ore to the .primary jaw crusher. Mining at Carlin is done by a 5 yd shovel and 7 ½ and 10 yd front-end loaders, and ore transport is by several sizes of trucks from 30 to 75 tons capacity. These pit haulage trucks dump onto stockpiles adjacent to the primary crusher. Ore is then fed to the dump hopper by front- end loaders only when the crushing plant is operating. This extra handling procedure is necessary because plant delays caused by problems with wet ore in the secondary crusher resulted in the ore setting up or packing in the dump pocket. Solidified material in the dump pocket would in turn delay truck haulage. The substitution of an

Jan 1, 1978

By K. K. Rao, M. E. Nicholson

IN a recent paper on the solubility of carbon in Ni-Cu alloys,' Nicholson reported that the carbon solubility appeared to be limited by the electronic structure of the alloys and that the solubility was propor- tional to the density of states at the Fermi surface of the "3d" band. In order to determine whether or not this relationship is a general one, the study has been extended to other systems. One of these is the CO-Ni system. This system was chosen for study because 1) it is adjacent to Ni-Cu system in the periodic table, 2) the alloys of cobalt and nickel do not form stable carbides at 1000°C, and 3) the system exhibits no pronounced change (less than 1 pct) in lattice parameter from cobalt to nickel,' see Fig. 1. The alloys were prepared from -200-mesh 99.92 pct Ni furnished by the International Nickel Co. and spectroscopically pure -200-mesh cobalt sponge obtained from Johns on-Matthey and Co. The powders were weighed, mixed, and pressed using a pressure of 40,000 psi. The samples were sintered for 24 hr at 900° C in dry hydrogen and then cold rolled to a thickness of 0.010 in. (Samples containing more than 70 wt pct Co had to be annealed after cold reductions of about 20 pct to avoid cracking.) The alloys were carburized at 1000°C in an alun-durn boat containing Acheson AUC powdered graphite in an atmosphere of carbon monoxide cylinder gas which had been passed through Ascarite to remove carbon dioxide. After carburizing for either 12 or 24 hr the samples were moved to a cool zone of the furnace to cool. Cooling required about 5 min. The samples were filed to remove about 0.005 in. from the surface and then analyzed using a conventional combustion-gravimetric analytic method. The results of this investigation are shown in the lower portion of Fig. 1 and Tabulated in Table I. The nickel percentages for these alloys were determined from the weights of the powders from which the alloys were made. The solubility of carbon in pure cobalt at 1000°C (fcc) is 0.25 wt pct. This is somewhat less than the 0.33 wt pct measured by Boecker.3 From his data, it would appear Boecker's samples were supersaturated before the equilibrating treatment and that a 20-min treatment was not long enough to achieve equilibrium. Since in the present investigation the 12 and 24 treatments produced essentially equal carbon contents, our figure is presumed to represent more nearly the equilibrium value. The solubility of carbon in nickel of 0.19 wt pct agrees quite well with the value of 0.21 wt pct

Jan 1, 1963

By R. D. Fisher, A. G. Metcalfe, F. A. Crossley

AN investigation of the application of magnetic stirring to the consumable arc melting of aluminum and nickel demonstrated that grain refinement could be obtained when there was sufficient stirring force. Also, it was found that grain refinement could be obtained in aluminum by alternately reversing the polarity of the current through the magnetic stirring coil. The effect of the latter was to periodically reverse the direction of rotation of the molten metal.' Because of their promise, these findings were applied to conventionally cast aluminum. Shortly after this work was begun, Kondic2 reported experiments in which aluminum cast with 40° C (72° F) of superheat exhibited a grain size of 10 to 20 grains per cm2. When interrupted rotation was applied during solidification by mechanical means, a grain size of 800 to 1000 grains per cm2 was obtained. Magnetic Stirring Applied to Conventional Casting— The applicability of magnetic stirring to producing grain refinement in conventionally cast metal was evaluated in the following way. Three pounds of aluminum were cast into a clay-bonded graphite mold. The mold was surrounded by a magnetic stirring coil of 1000 turns. A direct current of 200 amp was passed through the casting by means of a graphite electrode which was immersed from the top. A current of 5 amp was passed through the stirring coil. The aluminum (1100 or 25) was superheated to 1600° F (871° C) and fluxed by passing chlorine gas through the melt for 2 min prior to casting. Two additional castings were made for comparison: 1) a conventional casting of metal superheated to 1600° F and 2) a similar casting through which 200-amp current was passed during solidification, but without current in the magnetic coil. Macrosections of these three ingots are shown in Fig. 1. Very remarkable grain refinement resulted in the magnetically stirred casting. It may be noted that the casting through which 200-amp current was passed has a coarser structure than the conventional casting. It would appear that this is due to the additional heat input generated by the current to the former casting. Mechanical Rotation Applied to Conventional Casting—A casting temperature of 1600° F was used throughout. Some 1 1/2 -lb castings rotated at 150 rpm were predominantly columnar with small areas of coarse, equiaxed grains close to the lower mold wall. Following these, a series of 3-lb castings was made. Macrosections of these ingots are shown in Fig. 2. The imposed rotational speed was 250 rpm. Turbulence or acceleration in the solidifying liquid was the significant factor. Fine grain size resulted in the material solidified during the period of acceleration of the liquid to the imposed rotational speed. When uniform rotational motion was achieved, the grain structure reverted to columnar. The final casting shown in the lower right-

Jan 1, 1962

By Frederick C. Langenberg

IT has been shown1 that copper can be removed from iron-base alloys by solvent extraction with molten lead and sodium sulfide slags. In these processes copper removal is favored by a positive deviation of copper in iron from ideal behavior. Chou' determined the distribution of copper between liquid silver and iron and obtained a value for the activity coefficient of copper in iron at 1600°C, y°, of 9.12. Chipman" calculated the activity coefficient from the Fe-Cu phase diagram to be 12 at 1600°C. More recent work by Koros and Chipman" yields a value at 1600°C for y V equal to 8.0. In this latter work, the distribution of copper between silver and iron was measured at 1600°C, while the activity of copper in the silver phase was determined from calculations based on the Ag-Cu phase diagram. The present work presents another value of based on calculations from the Cu-Pb phase diagram, on the heat of mixing data for the Cu-Pb system, and on an experimental study of the distribution of copper between iron and lead at 1600°C. These experiments were part of a larger research on the removal of copper from iron-base alloys conducted at The Pennsylvania State University. Experimental Procedure—The distribution of copper between pure iron and lead at 1600°C was made in the furnace assembly shown in Fig. 1. The melts were made in high purity alumina crucibles under an atmosphere of prepurified argon. Temperatures were read with an optical pyrometer sighted into a %-in. hole drilled in the inductor. Extensive calibration of the optical readings with immersion readings had been carried out previously. The initial charges consisted of 100 g of electrolytic iron and varying weights of copper. The melts were brought rapidly to 1600°C and 75 g of lead added. The temperature was quickly readjusted to 1600°C, and the melts were held for 10 min at this temperature. A sample was then drawn from the iron layer in a fused silica tube. This sample was analyzed to determine the copper content of the iron layer at equilibrium, while the copper content of the lead layer was determined from a material balance. The validity of the material balance was confirmed by a chemical analysis of the entire lead layer for one heat in which the crucible was removed and quenched after the iron sample was taken. The calculated copper content of the lead-rich phase was 1.18 pct; while the entire lead layer analyzed 1.20 pct Cu. The distribution results are shown in Fig. 2. The distribution constant, N,.'r'"/N, is equal to 3.95. Discussion—From the Cu-Pb phase diagram' it can be seen that lead-rich liquid Pb-Cu solutions

Jan 1, 1957

National Slate Association, Drexel bldg , Philadelphia, Pa. This Association has published a book entitled "Slate Roofs " It is primarily intended for users of slate but it contains some information on the geology, analysis, quarrying and origin of slate It may be had from the office of the Association for $1 50

Jan 1, 1933

PRESIDENT GEORGE OTIS SMITH, District 4 WASHINGTON, D. C. PAST PRESIDENTS SAMUEL A. TAYLOR, District 3 PITTSBURGH, PA. E. DEGOLYER District 0 NEW YORK, N. Y. FIRST VICE-PRESIDENT W. H. BASSETT District 1 WATERBURY, CONN. TREASURER KARL FILERS NEW YORK, N. Y.¬ SECRETARY H. FOSTER BAIN NEW YORK, N. Y.

Jan 1, 1923

By R. J. Sherman, M. R. Achter

IT has often been reported that coatings may strengthen single crystals and polycrystalline specimens of coarse grain size. This note reports the effect of a surface layer of fine grains on the creep-rupture properties of coarse grained nickel 99.8 pct pure. Sheet specimens were machined from cold-rolled material, finished by surface grinding and annealed at 1230°C in vacuum for 4 hr. Half of them were re-ground on faces and sides and annealed at 925"C for 1 1/4 hr. The double grind-anneal treatment produced a structure consisting of a surface layer of fine grains of 0.02 mm diam on a coarse-grained substrate of grains of 0.40 mm diam. Comparison with specimens which received only the single grind showed that the second grind-anneal did not alter the structure of the substrate. Several modifications were made in specimen design to eliminate erratic rupture behavior outside of the gage length. In the final design the gage section, oriented parallel to the rolling direction, was 1.00 in. long, 0.4 in. wide, and 0.0625 in. thick. End tabs were pinned in place. Although other configurations (welded end tabs, transverse orientation, and wider gage section) showed similar effects of a layer of fine grains, because of the erratic rupture behavior, only the data from the final design are reported here. Creep tests were performed at 650°C in air and in a vacuum of 10~5 mm Hg. Creep rates were measured from the movements of the lever arm. Since the broken sheet specimens could not be fitted together, elongations at fracture measured by means of gage marks, do not include the necked portions adjacent to the fracture. Results of the creep tests with and without the fine grained surface are given in Table I. An explanation for the lower strength in air than in vacuum has been proposed previously in terms of the reduction of crack propagation energy by gas adsorption.l In both environments the fine-grained layer produced a small decrease in minimum creep rate and, except for the shortest test in air, a substantial increase in rupture life. The elongation values at rupture, as they are measured here, do not demonstrate an appreciable effect of the grain structure but do show much smaller ductilities in air than in vacuum. Greater elongations maybe associated with the finegrained layer, however, especially in vacuum, in creep curves such as those in Fig. 1. Duplicate tests were not run to determine the re-producibility of the data. It is felt, however, that, in view of the consistent behavior, the prolongation of rupture life may be attributed to the effect of the fine-grained surface. In the data not reported be-

Jan 1, 1962

By R. D. Vaughn

The limiting cases of non- Newtonian fluids flowing inside a concentric annular duct are developed without using a model of the fluid behavior. The solutions provide limits with which to test the various models of fluid behavior such as the power law and Bingham plastic models. The results of previous theoretical work are discussed in terms of limiting cases. This limiting case study also shows that experimental work on flow of non-Newtonian fluids in annular ducts should be confined to ducts for which the ratio of the radius of the inner wall to that of the outer wall is less than 0.3 and preferably less than 0.2. INTRODUCTION During the last 10 years the problem of laminar flow of non-Newtonian fluids in concentric annuli has received much attention large1y because of its application to the hydrodynamics of the wellbore. Recently solutions utilizing the power law1,2 and Bingham plasticl,3,4 models have been published. In this paper the method of limiting cases, which has been successfully applied to laminar-flow heat transfer516 will be applied to the problem of flow of non-time dependent, non-Newtonian fluids through annuli. This method permits solutions for the limiting cases to be made without using a model of unknown validity. The solutions, therefore, provide limits with which to test the various models which have been or will be proposed. A pertinent conclusion concerning the region of experimental work is also provided. DEVELOPMENT OF LIMITING CASES The limiting cases for the axial flow of fluids in concentric annuli may be defined with reference to Fig. 1. It is possible to define two limiting cases which pertain to the physical dimensions of the annulus. First, the annulus must degenerate to a circular pipe as the radius of the inner wall decreases or, as k = (k R/R) ? 0. Second, the annulus must approach the limit of parallel plates of infinite extent as the spacing between the inner and outer tubes becomes small in comparison with the radius R of the annulus, or as k?1. It is also possible to ascertain three limiting cases which pertain to fluid behavior. With reference to Fig. 2, as a fluid becomes progressively more pseudoplastic, the shear stress-shear rate relationship progressively approaches the indicated horizontal line more closely. At this limit the shear stress becomes independent of the shear rate. At the other extreme of increasingly dilatant behavior, the vertical asymptote is approached. Intermediate between these two limiting cases lies the case of the Newtonian fluid. Fluids which exhibit a yield shear stress also approach the limiting case of "infinite" pseudoplastic behavior. The remainder of the theoretical development is concerned with the description of and the solutions

By J. R. Cahoon, W. V. Youdelis

FOR the diffusion of copper in silver-rich alloys, there have been only two previous investigations, that of Seith and Peretti in 1936, and that of Sawatzky and Jaumot2 in 1957. Seith and Peretti obtained a value of 24.8 keal per g-atom for the activation energy of diffusion whereas Sawatzky and Jaumot obtained a value of 46.1 keal per g-atom. Admittedly, Seith and Peretti used relatively high concentrations of 2 at. pet Cu and polycrystalline diffusion couples, while Sawatzky and Jaumot investigated tracer diffusion in single crystals of silver. The difference in the results, however, seems too large to attribute solely to solute concentration, as a change of over 20 keal per g-atom in the activation energy suggests a change in the mechanism of diffusion. Therefore, in the present investigation the diffusion coefficient for copper in polycrystalline Ag-2 at, pet Cu alloy is re-established using conventional sandwich-type diffusion couples and electron-probe microanalyses, and the results are compared with those of the previous studies. The diffusion couples were prepared from high-purity silver (99.999 pet) and high-purity copper (99.999 pet). The silver disks, 1/4 in. long and 4 in. in diam, were machined from an ingot which had been solidified in a dynamic vacuum of 10-3 mm of Hg to eliminate oxygen absorption which otherwise would result in copper oxide precipitation in the weld zone. The alloy disks of similar dimensions were machined from an alloy ingot (nominal composition 2 at. pet Cu) which had been unidirectionally solidified to obtain a predictable solute concentration,3 and homogenized for 1 week at 800°C. Sandwich diffusion couples were made by pressure welding an alloy disk between two silver disks in an induction heating coil. The couples were diffusion-annealed at temperatures of 800°, 756°, 699°, and 630°C in tube furnaces in which the temperature was controlled to better than ± l°C. The diffusion couples were examined metallographically for weld defects, and couples showing even minute defects at the weld interfaces were rejected. Concentration penetration curves were established using an A.R.L. Microprobe analyzer. CuKO radiation was counted and converted to concentration using 0.5 and 1.0 wt pet Cu chemically analyzed standards. Initially, four continuous profiles were obtained, and averaged to obtain the final diffusion curve. The initial analysis was performed commercially and the welds were not located with respect to the profile. Therefore, the results were rechecked by the authors using the Mellon Institute A.R.L. probe. In the latter case, concentrations were obtained at 10-µ steps for four different traverses, and then averaged to obtain

Jan 1, 1968

Through the generosity of Sir Robert Hadfield, Honorary Member, the Directors of the American Institute of Mining Engineers are enabled to announce the Hadfield Research Prize of $1,000 for the best contribution to the publications of the Institute upon the general subject of The Different Forms and Combinations of Carbon with Iron, including those in Iron Alloys. The prize will be awarded at the Annual Meeting of the Institute in February, 1916, to the best paper upon this subject which is presented to the Institute before Nov. 1, 1915, provided such paper is deemed worthy by the Institute's Iron and Steel Committee. The following suggestions are also added for the guidance of those who may take part in this research. While it is not desired to define closely the exact lines or scope of the proposed research, as it is advisable to make these as broad as possible, the object in mind may be said to be generally as follows: To elaborate and find out the best methods of determining the forms of carbon in steel or iron, including those in iron alloys. A portion of the work would probably be a continuation of the researches which have in the past been carried out by Jullien, Abel, Muller, Ledebur, T. Sterry Hunt, Akerman, Arnold, Stead, E. D. Campbell, Hogg, Parry, Upton, and others.Through the generosity of Sir Robert Hadfield, Honorary Member, the Directors of the American Institute of Mining Engineers are enabled to announce the Hadfield Research Prize of $1,000 for the best contribu¬tion to the publications of the Institute upon the general subject of The Different Forms and Combinations of Carbon with Iron, including those in Iron Alloys. The prize will be awarded at the Annual Meeting of the Institute in February, 1916, to the best paper upon this subject which is presented to the Institute before Nov. 1, 1915, provided such paper is deemed worthy by the Institute's Iron and Steel Committee. The following suggestions are also added for the guidance of those who may take part in this research. While it is not desired to define closely the exact lines or scope of the proposed research, as it is advisable to make these as broad as possible, the object in mind may be said to be generally as follows: To elaborate and find out the best methods of determining the forms of carbon in steel or iron, including those in iron alloys. A portion of the work would probably be a continuation of the researches which have in the past been carried out by Jullien, Abel, Muller, Ledebur, T. Sterry Hunt, Akerman, Arnold, Stead, E. D. Campbell, Hogg, Parry, Upton, and others.

Jan 1, 1917

By John Chipman

DESPITE the rapidity of chemical reactions at steelmaking temperatures, deoxidation reactions cannot be expected to reach equilibrium immediately after addition of a deoxidizing agent. A considerable period of time may be required merely to obtain complete mixing of the deoxidizing element throughout the volume of steel to which it is added. Evidence in the literature indicates that in some cases the time is long compared with that allowed for completion of the experiment or for teeming of the heat. The great turbulence observed during the filling of the ladle is no guarantee of complete dispersion on a fine scale throughout the heat. During the process there are initially certain volume elements which are high in deoxidizer and others which retain substantially their original oxygen content. Mixing consists of the subdivision and ultimate destruction of these liquid segregates through the process of shear and elimination of concentration gradients by diffusion. The shear process does not continue indefinitely and a quiescent state may be reached in the ladle before all volume elements of divergent deoxidizer and oxygen content are completely eliminated. In furnace deoxidation the time required for complete mixing may be very long unless continuous stirring is employed.' In Fig. 1, let the circle represent one small volume element of aluminum-rich metal surrounded by oxygen-rich steel in which no stirring movement remains. Further mixing requires inward diffusion of oxygen and outward diffusion of aluminum, resulting in precipitation of A12O3 in the diffusion zone. It is important to note that such a precipitate may itself interfere with the diffusion process. Moreover, if the precipitate forms as a film with even minimal mechanical strength, it may interfere not only with diffusion but with shear as well, thus stabilizing compositional differences in volume elements of greater than microscopic size. A film surrounding such a volume element would have little or no ability to rise or to sink unless it enclosed a liquid whose density differed from that of the ambient. Consider now the effect on the overall composition of the melt. Fig. 2 represents the A1-O equilibrium at the temperature of the bath. High-aluminum elements of composition X may exist alongside high-oxygen elements of composition Y in such proportions that the average composition 2 has a much higher A1-O product than that corresponding to equilibrium. The A1-O product supposedly corresponding to equilibrium at 1600 °C was found by Wentrup and Hieber2 to be 10-10, by Hilty and crafts3 to be 2 X 10-9 and by Gokcen and chipman4 to be 2 x 10-14. Only the last named investigators approached equilibrium by means

Jan 1, 1962

By B. Wilshire, W. J. Evans

W. J. Evans and 8. Wilshire SEVERAL recent investigations1-6 have shown that the strain, c, during transient and steady-state creep is well-represented by the expression: € = e0 + et(l - e-mt) + Esl [l] where Eo is the instantaneous strain on loading, ET the total transient strain, C, the steady creep rate! and m a constant relating to the rate of exhaustion of transient creep. However, it has been noted6 that deviations from this equation occur over the first 10 to 15 pct of the transient stage, when the creep rate, (. decreases more rapidly than is predicted by this equation. This rapid decrease has been attributed to a large change in work-hardening coefficient. It 1s widely accepted that steady-state creep results from a balance between the rate of strain hardcning h and the rate of recovery r (=-s(st) as: dE/dt = Es = r/h [2] Comparison of values obtained for h at the end of the initial extension and during steady creep suggests that h increases several fold during the transient stage. which has the effect of reducing the creep rate proportionally.7 To examine the dependence, on r and h, of the deformation behavior during transient and steady-state creep. a series of constant-stress creep tests was carried out at 413°C at 6000 psi using 70-30 a brass. Prelinlinary investigation showed that. with this material. the transient stage constituted a significant portion of the total creep life (-0.4tf. where tf is the time to fracture). The alloy. obtained from Metals Research Limited. was made from high-purity copper, 99.999 pct. and zinc. 99.99 pct. Heat treatment at 675°C for 4 1/2 gave a uniform grain size of 5 mm-1. Details of specimen preparation and creep testing procedures have been given previously.6 Values of h (?s/?E) were determined by measuring the instantaneous strain. ?E. which occurred on increasing the stress during creep by a small amount. ?s. Similarly. v (= -?s/ ?t) was derived from the incubation period. At, after a small decrease in stress.' Several values of v and h were obtained throughout duplicate creep tests. using different stress increments in the range 300 to 800 psi. The accuracy with which Eq. [I] represents the present creep curves was established by determining the best value of the constants Es, Et, m , and 6, using a digital computer program based essentially on the graphical solution for this equation devised by Conway and Mullikan.9 About 40 strain/time readings were taken during transient and steady-state creep. Over most of the creep curve, the average difference between the measured reading and the calculated strain at the appropriate time was less than 0.0001. However.

Jan 1, 1969

By Tell Ertl, Ernest E. Burgh

The Bureau of Mines is operating an oil-shale mine 10 miles west of Rifle, Colo., as part of its Synthetic Liquid Fuels program. The purpose of operating this mine is twofold: First, to supply oil shale to an experimental Processing plant; and second, to develop practices and select methods for mining oil shale on a commercial scale at the lowest practicable cost. The second purpose—that of finding out how to mine oil shale most cheaply—entails considerable mining research. Since the drilling of oil shale probably will be one of the major items of the mining cost, fattors that influence drilling speeds were investigated. One phase of the drilling program was the development of a successful hard-surfaced rock-drill bit1 that can be used for drilling long holes in oil shale without changing bits. During that phase, drilling speeds were measured and drill cuttings were collected for assay and for screen sizing, when the cuttings from the individual tests were compared, a definite relationship was shown to exist between the drilling speed and the coarseness of the drill cuttings. Procedure Measurement of Drilling Speeds All drilling in the tests was done with a Model UMB-D-99W Gardner-Denver wagon drill. Round-lugged drill steel, 141 in. in diameter was used in 6, 12, and 18 ft lengths with 1/8-in. Timken H-type bits hard-faced with acetylene tube borium. The tests were made in the lower adit of the Bureau of Mines oil-shale mine; the grade of the oil shale drilled ranged from 18.6 to 42.7 gal per ton, During the experiments air pressure varied between 75 and go psi while water pressure remained fairly constant at 75 psi. All holes were drilled almost horizontally. Each drill hole was thoroughly cleaned of cuttings after being collared. The advance of the drill along the carriage was measured and recorded as the drilling speed in inches per minute. Method of Collecting Cuttings TO facilitate the collection of cuttings, each drill hole was collared in a smooth, vertical portion of the oil-shale breast (Fig 1). A galvanized-stee1 sheet was fastened to the breast below the area in which the hole was to be drilled. The cuttings washed out of the drill hole by the drilling water were guided by the steel sheet into a wooden box. The cuttings that remained in the drill hole after the drill was withdrawn were scraped out and placed in the same box as the cuttings washed out of the hole. After the cuttings from a I-min. drilling interval were collected, they were placed in flat metal pans. The fines were allowed to settle and the clear water was decanted. The cuttings then were dried in the sun.

Jan 1, 1949

By Cyril Smith

A STUDY of the mechanical properties of the alloys of copper and silver led to the discovery that the solubility of silver in copper was greatly different from that generally supposed, therefore some work was done to determine the solubility with greater accuracy than had previously been achieved. After the work had been completed, two papers were published1 giving solubility figures which agreed closely with one another and with the work described herein. A detailed comparison of that work with the present will be given later. PREPARATION OF ALLOYS The copper used in making the alloys was electrolytic ingot of high purity. The silver was prepared by precipitation as chloride from nitric acid solution, followed by fusion of the washed precipitate with sodium carbonate and potassium nitrate. This method gives metal containing at least 99.99 per cent silver. The copper was first melted under charcoal in a small electric resistance furnace and the silver added as pure silver, it being unnecessary to make any intermediate alloys. After thorough stirring the metal was poured into a mold of suitable form. The alloys contained between 0.008 and 0.015 percent of oxygen. Small amounts of oxide were visible under the microscope, but it is not believed this would have much effect on the results. Copper-silver alloys are notorious for segregation, consequently a few experiments were carried out to find a form of casting with as little segregation as possible. A mold 6 in. long and 1/2-in. dia. was first used, and an alloy nominally containing 5 per cent silver was cast in it, while some of the same alloy was poured directly into water to obtain the maximum rate of cooling possible. Analyses were made both on this sample and on turnings from the top and bottom of the 1/2-in. dia. casting, the turnings being separated into three parts according to the position

Jan 1, 1931

By John D. Verhoeven, Edward E. Hucke

An experimental technique has been developed for the measurement of the rate of electrotransport to a precision of 1 pct in the molten Bi-Sn system. Results are presented across the phase diagram from 30°C above the liquidus to 520°C. A phenomenological description is presented and the data on Bi-Sn are thereby converted to the effective charge, Analysis of the data indicates the true charge of the migrating tin species in bismuth to be +1.8 at 500°C. The data agree well with the recent work of Belashchmko. fieldintensity. The resistivity of the molten Bi-Sn system is also presented. WHEN an electric field is applied to a metal, a relatively large current is produced due to the ease with which electrons move within the metal. The electric field also produces a force on the ions which might cause them to migrate. Such a migration of metallic ions has been detected under certain conditions. This electromigration of the metallic ions will be referred to herein as electrotransport. The study of electrotransport in metallic systems has a rather long history dating back to the initial work of Gerardin1 in 1861. General reviews of electrotransport in liquid and solid metals have been published by Schwarz,2 Jost,3 Seith,4 and Heumann.5 In reviewing the literature it is apparent that the theoretical developments are not yet complete. The difficulty arises in describing the momentum transfer between the migrating ions and the electrons. In addition, there is a lack of good quantitative electrotransport data at high temperatures, especially in liquid metal systems. This work was undertaken to establish quantitative electrotransport data in a liquid metal system which might serve as a critical test of the theoretical developments. The Bi-Sn system was chosen for analysis, and the rate of electrotransport was determined as a function of temperature and composition. THEORETICAL CONSIDERATIONS If all of the atoms of a metal are considered to be positively charged due to the loss of electrons to the

Jan 1, 1963

By Charles R. Austin, Carl H. Samans

In an earlier serics of studies on 18-8 stainless steel at 600º, 700º, and 800ºC.l one pretreatment was used throughout; viz., 15 min. in hydrogen at 950°C., followed by an air quench. Several manufacturers of this alloy since have expressed doubt as to the suitability of the temperature employed, recommending instead the more customary Strauss treatment as promising superior results. In this subsequent investigation on the effects of the temperature of pretreatment several interesting points have arisen, which are described in this paper. Previous work on our equipment had shown a marked difference between alloys of "similar chemical composition" that had been manufactured by different companies. Accordingly, one mill-bar length was selected from which to prepare all specimens. It could then be assumed that any marked differences in creep characteristics would be due to effects resulting from variations in the pretreatment of the alloy. The material was furnished by the Allegheny-Ludlum Steel Co. in the form of 5/16-in. dia. rod, finished by air cooling from a mill anneal at 1950°F. (1066°C.). It was analyzed only for the elements shown: carbon, 0.07 per cent; chromium, 18.73; nickel, 9.46; manganese, 0.40. Three pretreating temperatures were chosen, the specimens being held for 15 min. in hydrogen at either: (1) 1150°C., to conform to the recommended Strauss treatment; (2) 950°C., to compare with the results of previous tests; or (3) 75Q°C., to initiate precipitation of carbides in the material before testing. As the test cross sections were only 1/8-in. dia., air cooling followed the annealing treatment. These treatments permitted two direct comparisons: (1) between the 1150" and 950°C. treatments to indicate the effect of grain size when all carbides were probably in solution at the start of the test; and (2) between the 950" and 750°C. treatments to indicate the effect of carbide "nucleation" for similar grain sizes.

Jan 1, 1940

By Carl H. Samans, Charles R. Austin

In an earlier serics of studies on 18-8 stainless steel at 600º, 700º, and 800ºC.l one pretreatment was used throughout; viz., 15 min. in hydrogen at 950°C., followed by an air quench. Several manufacturers of this alloy since have expressed doubt as to the suitability of the temperature employed, recommending instead the more customary Strauss treatment as promising superior results. In this subsequent investigation on the effects of the temperature of pretreatment several interesting points have arisen, which are described in this paper. Previous work on our equipment had shown a marked difference between alloys of "similar chemical composition" that had been manufactured by different companies. Accordingly, one mill-bar length was selected from which to prepare all specimens. It could then be assumed that any marked differences in creep characteristics would be due to effects resulting from variations in the pretreatment of the alloy. The material was furnished by the Allegheny-Ludlum Steel Co. in the form of 5/16-in. dia. rod, finished by air cooling from a mill anneal at 1950°F. (1066°C.). It was analyzed only for the elements shown: carbon, 0.07 per cent; chromium, 18.73; nickel, 9.46; manganese, 0.40. Three pretreating temperatures were chosen, the specimens being held for 15 min. in hydrogen at either: (1) 1150°C., to conform to the recommended Strauss treatment; (2) 950°C., to compare with the results of previous tests; or (3) 75Q°C., to initiate precipitation of carbides in the material before testing. As the test cross sections were only 1/8-in. dia., air cooling followed the annealing treatment. These treatments permitted two direct comparisons: (1) between the 1150" and 950°C. treatments to indicate the effect of grain size when all carbides were probably in solution at the start of the test; and (2) between the 950" and 750°C. treatments to indicate the effect of carbide "nucleation" for similar grain sizes.

Jan 1, 1940

By G. U. Greene

The various lead producers have given the subject of lead drosses much attention in recent years but the problem of their economical treatment is yet to be solved. Formerly the copper in the furnace feed was removed from the furnace in the form of matte. The speiss at that time consisted principally of the iron arsenide. The practice today is to roast off most of the sulphur and the copper in the feed forms a dross in the furnace, which is removed from the furnace with the lead. This material is poured into the drossing kettles and allowed to cool down to but slightly above the freezing point of lead. The copper dross, containing almost all of the arsenic and part of the antimony, is skimmed off and treated in a small reverberatory furnace at most plants. This is essentially a liquation process. The skimmed dross contains from 70 to 80 per cent lead, and much of this lead is liquated out. The products from this treatment are: (1) impure lead, (2) speiss and (3) matte. The speiss from the reverberatory furnace was studied in this research. The literature on the subject is of very little assistance, as almost no work has been done on the problem of establishing the exact identity of the various phases present. One author(1)† states that speiss consists of a series of isomorphous compounds of the general formula FexAsy in which the Fe may be replaced by Ni, Co, Cu, Pb, Ag, Au, Pt, Zn, Cd and the As replaced by Sb, S and Bi. Hofman(2) states that the iron arsenide present is Fe5As. Experimental Work In the present research, the author used for methods in an attempt to determine the composition of the various phases: (1) chemical, (2) microscopic, (3) roentgenographic and (4) thermal. Previous to this research, considerable time had been spent making analyses of different speisses, but unfortunately no very definite conclusions could be made as a result of these analyses.

Jan 1, 1937