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By H. C. Chang, N. J. Grant

REEP studies and measurements in most in-V> stances are based on a relatively gross gage length. Even in some recent theoretical studies on the mechanism of creep, changes were followed by means of X-rays and metallography without regard for the behavior of the individual grains and grain boundaries.'" Analytical studies of creep have frequently indicated that more than one competing process is operative and that the ultimate creep performance depends on the effects of temperature, time, and strain rate as well as grain size.'-" he grains and grain boundaries are known to respond differently to these variables but the extent of the response is still little known, especially in poly-crystalline materials where the relative orientations of grains and grain boundaries are important. This paper reports some experimental observations of the behavior of the grain boundaries and their effect on the deformation in the grains. High purity aluminum was used to avoid complications of aging reactions, second phase, inclusions, etc. Experimental Procedure A small vertical nichrome wound furnace was built to permit direct loading on the test specimen. This furnace is capable of operating up to about 1300°F with reasonable temperature distribution. A ground rectangular quartz window, 1.25x0.5 in., is imbedded in the external stainless steel tube to permit observations of the creep process with a microscope. An argon atmosphere ,was provided to prevent oxidation. The quartz window caused a temperature gradient between the back and front surfaces of the specimen of 15" at 700°F. The temperature gradient could be cut down to 3°F along the length of the specimen by adjusting shunts across the furnace windings. An ordinary metallurgical microscope with a working distance of 14 mm was rebuilt so that it could be moved in three mutual perpendicular directions. Visual examination could be made with either a 30X eyepiece or a 15X filar eyepiece. Using an objective of focal length 24.3 mm and a numerical aperture 0.20 a total magnification of 120X or 240X could be obtained. High purity aluminum rated at 99.995 pct was supplied by the Aluminum Co. of America as % in. then the gage portion was further machined to 3/16 in. diam. The ends were Y4 in. diam and threaded to fit available specimen holders. Two opposite flat surfaces of the gage portion were obtained by milling, giving final dimensions of the gage portion of 3/4x3/16x3/32 in. Machined specimens were first electropolished in Jacquet's solution.' Reference marks were produced by pressing a thin sewing needle into the surface of the specimen. The specimen was then annealed at 900°F for 24 hr and at 1150°F for 12 hr. Typical macrostructures of specimens treated in this manner are shown in Fig. 1. The range of the grain size was 1 to 5.5 mm (see Fig. l), but most of the grains were of 2.5 mm and went through the whole thickness of the specimen. The specimen was re-electropolished and etched electrolytically to reveal the grain boundaries. In order to reveal the orientation difference of the grains, etch pits were produced on the surface of the grains by etching in a mixture of hydrochloric and nitric acids (HC1, 45 pct; HNO,, 10 pct; H,O, 45 , by volume). The specimens were very carefully put into the holders and furnace; yet even with this care, fine slip lines were developed on the specimen surface.

Jan 1, 1953

By W. A. Backofen

THE texture of cold-drawn copper wire has been described most often as a composite of [Ill] and [loo] directions aligned parallel to the wire axis.' Hibbard2 suggested that sufficient reduction will result in a single [111] texture and reported that after a reduction in area of 96.4 pct, such a texture was nearly obtained. Other work3-4 has shown that recrystallization within the temperature range of 300" to 1000°C does not alter the texture established by cold-drawing. In general, however, the texture of cold-drawn end annealed copper wire is not as well defined as the deformation texture. In the work reported here it was found that the double-fiber, deformation texture persists even after a reduction in area of 97.3 pct, and after recrystallization the texture is practically all [l00]. The wire used in this work was prepared in the following way. A 3/4-in. diam length of annealed OFHC copper was cold-drawn to a diameter of 1/8 in., a reduction in area of 97.3 pct. Each step in the drawing operation brought about a reduction in area that varied from 6 to 10 pct. Short lengths of this wire were etched in a 50-pct solution of nitric acid to a diameter of approximately 0.01 in. The texture of the cold-drawn specimens was determined with the conventional X-ray transmission diffraction technique using filtered copper radiation. The X-ray beam was directed perpendicularly to the wire axis and the diffraction rings were recorded on a flat film. Fig. la is typical of the photo-grams obtained and reveals that the cold-drawing schedule described above introduces a distinct, double-fiber texture with both [Ill] and [l00] directions aligned parallel to the wire axis. Supplementary measurements with a Geiger-Mueller counter of the intensity of reflection from (111) planes showed that the [111] component was much more predominant than the [l00]. Additional specimens of the drawn and etched wire were annealed in a salt bath at temperatures from 300" to 450°C. The texture of the recrystal-lized wire was studied with the same technique applied to the cold-drawn wire. Fig. lb is an X-ray photogram of a specimen annealed for 1 ½ at 300°C and is typical of those obtained from re-crystallized specimens. The photogram shows that recrystallization of this material is accompanied by the almost complete elimination of the [111] component of the deformation texture. A pronounced strengthening of the [100] component was evident from intensity measurements with a Geiger-Mueller counter. In summary, the deformation texture of cold-drawn OFHC copper wire, after a reduction in area of 97.3 pct, may still be described as a composite of [Ill] and [loo] directions aligned parallel to the wire axis. Recrystallization of such wire at temperatures from 300" to 450°C introduces a texture which consists almost entirely of a [loo] alignment. Acknowledgment Sidney Rolle of the Scomet Engineering Co. generously supplied the OFHC copper used in this work. References 'C. S. Barrett: Structure of Metals. p. 382 (1943) New York. McGraw-Hill Book Co. 2 W. R. Hibbard, Jr.: Trans. AIME (1949) -185, p. 598; Journal of Metals (Sept. 1949) TN 19E. 3 P. 422 of ref. 1. 'E. Schmid and G. Wasserman: Ztsch. Physik (1926) 40, p. 451.

Jan 1, 1952

By T. R. Ingraham

The thermal decomposition of cupric sulfate and of cupric oxysulfate has been examined by deter-mining the equilibrium gas pressure generated over each pure compound. The equilibrium data have been used to calculate the thermodynamic properties of both compounds, and the results have been combined with previously published data to establish a predominance-volume diagram for the Cu-S-O system over the normal range of roasting temperature and gas composition used in the treatment of copper minerals. Copper oxysulfate recrystal-lizes at 1100°K with an apparently irreversible en-dothermic heat requirement of 2.9 * 0.3 kcal per mole. WHEN mixed sulfide minerals containing copper are roasted, either of two procedures may be followed, depending on the nature of the other metals. In the first procedure, the roasting is controlled to produce a maximum amount of water-soluble copper sulfate which may be removed selectively from the water-insoluble compounds of the other metals. In the second, control is directed toward the production of water-soluble sulfates of the other metals and an insoluble salt of copper. Effective control of either of these processes would be enhanced by knowledge of the thermal stability of cupric sulfate and of cupric oxysulfate. In this paper, established data for the thermal stability of cuprous and cupric sulfide and of cuprous and cupric oxide will be combined with new data for the therma1 stability of cupric sulfate and cupric oxysulfate, to designate the volumes of stability of the significant compounds in the Cu-S-O system in the temperature range 750° to 950°K. EXPERIMENTAL Materials, Apparatus, and Procedure. The copper source material used in all experiments was Fisher Certified Reagent Grade "anhydrous" cupric sulfate, for which the following analysis was supplied by the manufacturer: chloride, 0.002 pct; alkalies and earths, 0.2 pct; insoluble, 0.002 pct; iron, 0.020 pct. Cupric oxysulfate was prepared from the normal sulfate by two procedures. In the first, equimolar quantities of cupric oxide (prepared by decomposition of the sulfate) and cupric sulfate were ground together and heated under vacuum in a sealed silica vessel at 800°C. This procedure was subject to failure because of explosion of the silica vessels due to the pressure of the final traces of water released from the sulfate on the initiation of its decomposition. The second procedure involved roasting the cupric sulfate, with frequent rabbling, in a muffle furnace at 725°C for a period of 48 hr. This produced an excellent product, which was confirmed as copper oxysulfate by X-ray and chemical analyses. The experimental technique used was that of measuring the total pressure exerted by the sulfur trioxide, sulfur dioxide, and oxygen produced by the following reactions: 2 CuS04 = cuo • CuSO4 + SO3 [1] cuo . CuSO4 = 2 cuo + SO3 [2] SO3= SO2 + 1/2 O2 [3] The apparatus used in the experiments has been described previously.1-3 Its main feature of a U-tube mercury manometer in which the mercury is protected from corrosion by enclosure in a flexible Pyrex bellows. Before beginning a run, the interior of the apparatus, including the bellows-manometer and all connecting tubing, was thoroughly washed with hydrochloric acid and distilled water to remove any

Jan 1, 1965

By T. P. Papazoglou, N. A. D. Parlee, W. C. Phelps

PRACTICAL designs for good "home made" molybdenum furnaces are hard to find in the literature. The one described briefly below left something to be desired but was good enough to operate as a rather long (30 in.) two-zone furnace for periods of over 2 months at temperature (1400° to 1600°C) without shutdown. The principal problem in our application was to establish a temperature profile with two distinct constant-temperature zones and no dip between the zones. This and other problems mentioned below would not arise, however, if both zones were operated at the same temperature and if a shorter furnace were acceptable. Since molybdenum windings oxidize very rapidly when heated in air, impervious refractory tubes were used for both the furnace core and the outer jacket tube shown in the accompanying figures. A protective atmosphere of forming gas (10 pct H2, 90 pct N2) was continuously passed through the gas-tight annular volume between the core and outer jacket. The water-cooled copper ends shown in Figs. 1 to 3 sealed the ends of the tubes. Annealed molybdenum wire (40 mil) was wound on the recrys-tallized alumina core (35.5 mm OD by 28.5 mm ID by 30 in.) at a spacing of 0.36 in. The spacing was reduced to 0.29 in. close to the ends to partially compensate for end heat losses. Fig. 2 shows two molybdenum-ground lead taps off the center of the winding to produce the two independect temperature zones. The ground lead was insulated with 1/4-in. alumina tubing and connected to the grounded copper end by passing the wires through the gas port tube and crimping each wire into notches cut at the mouth. To prevent sagging of the core at high temperatures, refractory "troughs" were cut from alumina and mullite tubing to cradle the core. The support "troughs" which were 6 in. long and located about 5 in. from each end of the annular volume also served as radiation shields. In view of the different expansion coefficients and operating temperatures of the core and outer jacket (3.5 in. OD by 3 in. ID by 30 in.), the ends of the tubes were smoothed and squared to produce good sealing surfaces, and the core was ground 1/32 in. shorter than the outer tube. The power terminals were passed through their respective conductor ports which were internally lined with alumina tubing and sealed with Armstrong adhesive A-6 leaving about 1 in. of protruding lead wire for external connections. (Adhesive A-6 is a two-component system consisting of an epoxy-type resin with a mineral fibrous filler and an amine catalyst.) Figs. 1 and 3 show the entire assembly of concentric refractory tubes, copper ends, and sealing o rings, held together with two brass flanges and 3/8-in. bolts with heavy springs for dimensional flexibility. The furnace shell (19 by 19 by 30 in.) consisted of a steel frame with sheets of transite forming a box. The copper ends protruded through two 3.75-in. circular holes cut at the center of each transite square end. Thermal insulation next to the transite exterior was effected by K-23 B&W bricks alld in a central volume of approximately 9 by 9 by 30 in. a row of K-30 bricks was lined up to support the hot assembly. The rest of the volume around the outer

Jan 1, 1965

By N. J. Grant, B. C. Giessen, R. Koch

The system Nh-Ir was investigated over the complete concentration range by metallography and X-my techniques, using forty one alloys. The solubility limits of terminal and intermediate phases and the solidus temperatures were determined. Five intermediate phases were found: a Nb3Ir, cubic, Cr3O type; tetragonal, ofecr thorhomhic, isostruc-turn1 with (ta-Rh); and a Nhlr3. cubic, AuCu, type. a Nb3lr and a Nbfr3 melt congruently; three eutectic and three pentectic reactions occur. The phase diagram of the Nb-Ir system had not been fully treated in the literature; only surveys of intermediate phases were found.1"5 In this study, the details of the phase boundaries were investigated as well as the crystallography of the intermediate phases. EXPERIMENTAL METHODS The experimental procedures such as arc melting of powder compacts, heat treatments, solidus measurements, X-ray, and metallographic observation were identical with those used in the work on the Nb-Rh phase diagram.&apos; They will therefore not be repeated here except where the conditions differed. The purity of the niobium powder was as stated in Ref. 6; the iridium powder of 99.9+ pct purity from J. Bishop and Co., Malvern, Penn., did not contain impurities exceeding 100 ppm, except rhodium (200 ppm). The melting points and vapor pressures of both elements are very similar. This fact contributed to a very small weight loss on melting and facilitated preparation of homogeneous alloys. As shown in Ref. 6 for Nb-Rh, no oxygen pick-up exceeding 200 ppm had to be considered; this was regarded as valid also for Nb-Ir. A total of forty one alloys were used in the determination of the phase diagram; their concentrations are shown in Fig. l, which presents the phase diagram. The concentration limits as determined by the weight-loss method averaged <0.2 at. pct, and never exceeded 0.5 at. pct. Heat treatments were carried out as described in Ref. 6. Depending on the concentration, only tantalum, tungsten, or iridium containers were employed, avoiding oxide crucibles altogether. Alloys from 0 to 25 and from 65 to 100 at. pct Ir were homogenized at 2095°C for 15 hr, intermediate compositions from 25 to 65 at. pct Ir for 65 hr at 1780°C. A typical annealing-time schedule is presented in Table I. Solidus points were measured as described in Ref. 6 with the modification that samples rich in niobium were held between pieces of tantalum foil and samples of high iridium concentrations were held between rhenium platelets or in iridium wire. After each run it was ascertained metallographically that no reaction with the holder had occurred. Rhenium was selected as holder material after it had been shown in separate tests that the melting points of Re-Ir alloys rise continuously from 2440°C. Metallographic examination was carried out as described in Ref. 6, and the same procedure and etchants were used successfully. While metallographic discrimination between a Nb3lr and o was easily possible, X-ray diffraction was necessary to separate al and ct2. X-ray powder patterns were taken and evaluated as for Nb-Rh6 yielding the error limits indicated in Table 111, to be introduced later. For the determination of the invariant reactions and phase boundaries, the same techniques as for Nb-Rh6 applied. The general accuracy of invariant concentrations is regarded as somewhat higher than for Nb-Rh due to the small slope of most solvus lines.

Jan 1, 1964

By R. G. Powell, R. Schuhmann, E. J. Michal

Liquidus surfaces in the ternary system FeO-Fe2O3-SiO2, were determined from 1250&apos; to 1450°C by the procedure of equilibrating small samples in platinum crucibles, quenching, and microscopic examination. The experimental results were combined with previously published information to construct a ternary diagram for the system showing the entire temperature-composition range of stability of iron silicate slags. Metallurgical applications of the diagram, especially in copper smelting, are discussed briefly. IRON oxides are almost unique among the common oxide constituents of metallurgical slags in that the iron occurs in two different states of oxidation, ferrous and ferric. Moreover, in liquid slags the degree of oxidation of the iron is readily changed by reactions of the slags with oxidizing agents or reducing agents. This behavior of iron oxides in slags accounts, for example, for the effective transfer of large quantities of oxygen through slag layers in open hearth steelmaking. In this process, oxygen supplied by reactions at the gas-slag interface is dissolved in the slag with the oxidation of ferrous iron to ferric. Ferric oxide is transported across the slag layer by convection, and at the slag-metal interface the oxygen reacts with liquid metal while the ferric iron is reduced back to the ferrous state. Another group of processes in which variation in degree of oxidation of iron has great practical importance is in copper smelting. In matte smelting and converting, such large proportions of the iron are oxidized to the ferric state that problems are encountered in preventing or controlling the formation of solid magnetite. The ferrous-ferric relationship also affects the attack of iron oxides on high-SiO2 refractories, which appears to be most severe under reducing conditions for which ferrous iron predominates. Darken and Gurry&apos; determined the chemical properties and phase equilibria of pure iron oxide slags. Their data show that iron oxide melts can have compositions ranging almost all the way from FeO to Fe2O3. The melts of lowest oxygen contents, which exist in equilibrium with metallic iron, approach ferrous oxide in composition but still have a small percentage of ferric oxide. The melts of highest oxygen contents, which have oxygen dissociation pressures of 1 atm, are above magnetite in oxygen content, with over two-thirds of the iron in the ferric state. The previously established phase diagrams for silicate slag systems all show FeO as the iron oxide component. However, Bowen and Schairer? who determined the FeO-SiO2 diagram and many of the other diagrams used by slag chemists, have been careful to point out that their systems always contained both ferrous and ferric iron. Thus, their data are for limiting mixtures with minimum contents of ferric iron, obtained by melting and equilibration in iron crucibles. Under these conditions, the Fe2O3 percentages found by analysis were small enough to justify simplification of the published phase diagrams by calculating the Fe2O3 to equivalent FeO and ignoring Fe2O3 as an additional component. On the basis of experimental measurements of melting points of iron oxides on silica in the presence of various gas mixtures, Darken3 worked out phase diagrams for the Fe-Si-0 system which show the important phase equilibria in terms of temperature and gas composition. This study clarified many aspects of the application of the phase rule to the FeO-Fe2Oa-SiO2 system and was an important basing

Jan 1, 1954

By H. S. Wang, Y. P. Gupta

Diffusion of zinc and germanium in liquid silver is measured in the temperature range 975" to 1400°C by use of the capillary-reservoir technique. The ex-perinzental results are discussed in terms of the fluctuation and the "hole" theories of liquid diffusion, assunzing the solute as a point charge equal to the difference in the valences of the solute and solvent atoms. The additional coulombic interaction term due to the excess solute charge is evaluated in terms of the Thomas-Fenni approximation. The theoretical and experimental results agree with both the fluctuation and "hole" theories of liquid diffusion. No perceptible effect on solute diffusion in liquid silver of the size difference between the solute and solvent atoms/ions is apparent. DIFFUSION in liquid silver of electropositive solutes indium, tin, antimony, and homovalent gold has been previously reported by Leak and Swalin1 and Gupta,&apos; respectively. These solutes have nearly the same atomic size but differ principally from one another in excess valence (+2, +3, +4, respectively). The observed differences in the temperature dependence and the rate of solute diffusion were explained in terms of an added coulombic interaction between the solute and the solvent atoms. In the case of diffusion of gold in liquid silver, the data were found to be consistent with an effective valence for gold of -0.85, as proposed by Le Claire.3 Recently, Wang and Gupta4 have reported a study of diffusion of ruthenium, iron, and cobalt in liquid silver. The results of diffusion of these solutes and their temperature dependence were found consistent with the hole theories and the fluctuation theories of liquid diffusion, if ruthenium, iron, and cobalt were diffusing in liquid silver with relative valences -2, -1.3, and -0.5, respectively, instead of -3, -3, and -2 as suggested by the relative position of these elements in the Periodic Table of Elements. Furthermore, the predicted valences for these solutes were observed to be consistent with the sparsely available information on the magnetic properties of some of the dilute alloys of copper and silver with these solutes. In theoretical calculations of solute diffusivity, the solute was assumed as a point excess charge equal to the difference in the valences of the solute and solvent atoms. Both the assumption of a point excess solute charge and the use of the Thomas-Fermi approximation to calculate the potential of a solute charge are less precise for the case of electronegative solutes. Therefore, it was not possible to infer from the data on ruthenium, iron, and cobalt an effect, if any, on solute diffusion of the relative differences in either the Period or the size of the solute and solvent atoms or the solute atoms themselves. A study of the diffusion of Period 4 elements, specifically zinc and germanium was, therefore, undertaken since zinc and germanium, respectively, have relative valences of +1 and +3 in liquid silver and the data obtained on diffusion of these solutes could be compared with the available data on diffusion of Period 5 electropositive solutes, indium, tin, and antimony in liquid silver. From such a comparison, it was hoped to learn something about the effect, if any, of the ion size or the structure of the ion core on impurity diffusion in liquid silver. EXPERIMENT The diffusion of tracer zinc and germanium in liquid silver was studied by the capillary reservoir technique, modified adequately for use at high temperatures. In principle, capillaries containing liquid silver

Jan 1, 1970

By J. C. Scully

In June, 1965, Sanderson and scully5 reported at the Conference on Environment Sensitive Mechanical Properties of Materials at the Research Institute for Advanced Studies at Baltimore that thin foils of titanium could be prepared by chemical polishing in a mixture of 44 pct HF and 73 pct HNO3 in the volumetric ratio 2:3. The technique is simpler than that since reported by Rice and Orava. As-received annealed titanium (containing 0.8 pct Fe and 30 ppm H) in the form of sheet 0.05 cm thick is placed in the solution and moved up and down. The reaction is violent but suitable foils are obtained very easily and consistently. A typical micrograph is shown in Fig. 3. The small precipitates were not identified. Yamane and ueda6 observed many spotlike features which they referred to as small dislocation loops. While their spots may be due to the reaction of the warm foil with the air as suggested by Rice and Orava, the precipitates in Fig. 3 are also found when foils of titanium are prepared by electro-polishing at low temperatures and subsequently examined in the electron microscope without any inter- mediate warming. Furthermore, they are not a surface effect. It is necessary to add that alloys of titanium cannot be so easily thinned by the chemical polishing solution described above since it contaminates the a, phase with hydrogen and produces y hydride. These matters are described at length in a paper7 and their relevance to stress corrosion is considered elsewhere.&apos;-* Author&apos;s Reply The authors are grateful to Dr. Scully for bringing to our attention his hitherto unpublished technique for thinning unalloyed titanium, and deeply regret the unintended apparent duplication. The chemical thinning solution (7 parts HNO3 and 3 parts HF, by volume) reported by us is the same as that with which, for some period in the past, we had experienced success in the preparation of foils from single and polycrystalline niobium. Its subsequent effective application to titanium was a logical step, which, clearly independently of Scully, was conceived by Mr. Rice, to whom full credit is due. A few comments are warranted concerning some of the details of the preceding Discussion. It is evident to the discerning reader that the two thinning techniques under consideration are chemically almost identical, and in that sense are equally "simple". The chemical aspect is, of course, the one of primary importance in both communications. Thereafter, the relative simplicity is dictated by the mechanics of the actual thinning operation selected by the individual investigator. Our standard dimpling, or dishing, procedure was chosen with a view toward providing, for the electron transparent areas of the sample, the maximum protection from extraneous deformation during handling. That the long, straight dislocations visible in Scully&apos;s electron micrograph of a seemingly recovered structure closely resemble handling dislocations would tend to indicate the merit of our adopted technique. Features similar to those which Scully has attributed to precipitates, without any apparent diffraction contrast confirmation, were not observed in any of our clean foils taken from annealed or deformed specimens. This was admittedly somewhat surprising since the 3700 ppm (nominal) Fe in the A-70 commercial-grade titanium examined should have given rise to TiFe precipitates. Presumably these existed but were un-resolvable. Curiously, Scully&apos;s "precipitate1&apos; density is fairly high although the iron content quoted was less than one-fourth of that in our material. One is forced to conclude from the evidence that prior thermal and mechanical treatments are responsible for the two different types of structure observed.

Jan 1, 1968

By A. Simkovich, R. W. Lindsay

The possibility of using sodium sulfide slags to remove copper from ferrous alloys has been investigated by Jordan1 and by Langenberg.2, 3 In these studies, such slags were determined to be capable of removing copper and sulfur from the melt. The present work represents additional effort to clarify the effects of temperature on copper removal. The experiments were performed in a 17-lb induction furnace. Graphite crucibles contained the melts and kept the baths saturated with carbon. Temperatures were measured with a calibrated optical pyrometer and were controlled by manipulation of power input to the furnace. Estimated accuracy of temperatures in this investigation is ± 10°C (18°F) for measurements prior to slag additions, and + 20°C (36°F) after slag formation. The procedure consisted of melting 800 g of electrolytic iron. During this step, powdered graphite covered the exposed iron surface. After a predetermined temperature was reached, copper shot was added. A sample of the molten alloy for chemical analysis was then aspirated into a silica sheath. Next, a slag-forming mixture of sodium sulfite and graphite was added instantaneously to the melt. The sodium sulfite amounted to one-tenth the charge weight of iron; sufficient graphite was added to combine with oxygen in the sodium sulfite, assuming formation of carbon monoxide and reduction of the sulfite to sulfide. Subsequent to the slag addition, the molten alloy was sampled periodically, with the exception of heat A in which no intervening samples were taken between the slag addition and the end of the run. The iron was poured into a graphite mold, and the ingots sectioned and drilled for samples. Results of selected heats are presented in Table I. Analyses of samples drawn from the iron prior to slag addition are listed under zero time. Two samples from heat D were reported with copper contents greater than the initial concentration in the bath. Owing to the gradual but complete disappearance of slag during this heat, it is believed copper momentarily became more concentrated in the upper portion of the bath while reverting from the slag. This is the region from which samples were drawn. It should be noted that analysis of the ingot was equal to the copper content at the time of slag addition. The terminal temperatures of heats D and E, and the initial sulfur content of heat A are also to be noted. Because of the large temperature drop which occurred when slag was formed in heat D, power input to the furnace was increased in heat E after the slag addition, causing a higher terminal temperature. In heat A, the initial sulfur concentration was relatively high as compared to heats B through E owing to contamination by some slag remaining in the crucible from a previous heat. It is evident from Table I that copper was removed at the onset of slag formation. Roughly 30 pct of the copper was taken into the slag, with the exception of heat D, which had approximately 50 pct removed. For a comparatively short time of slag-metal contact, it appears that no gain is to be made in copper removal through use of high or low temperatures. If the slag initially formed remains in contact with the iron for an extended period, temperature has a marked effect upon copper removal, as can be seen by studying results for the two extremes in temperature. At about 1425°C, the copper level remained relatively constant after the initial removal by the slag. However, in the region of 1670°C, a definite reversion of copper occurred. Reversion was incomplete in heat D, and complete in heat E. The final temperatures of heats D and E differed by about 75°C. This temperature difference is thought to be the reason for only partial copper reversion in heat D. It is believed the effects of temperature noted above are related to the evolution of a white fume, which appeared in every run except heat A. (In the case of heat A, the fume was practically indiscernible.) After each slag addition, a yellow flame formed for about 5 sec. When the flame subsided, a white fume appeared. Upon contact with surrounding cooler surfaces, this fume deposited as a white solid. In the experiments made at 1425°C, evolution of fume continued unchanged to the end of the runs. However, heats D and E exhibited a different behavior. A very noticeable decrease in fume evolution from heat D was observed. Furthermore, this heat had much less slag remaining than did runs A through C when the experiments were terminated. No slag remained at the end of heat E; evolution of fume from this heat ceased prior to pouring. Spec-trographic analysis of the white deposit indicated sodium to be the major metallic element, with the maximum concentration of iron and copper as 0.1 and 0.01 pct, respectively. It is supposed the white fume observed in these experiments is principally sodium oxide (Na2O), formed by oxidation of sodium in the slag and subsequent sublimation. (Sodium oxide is a white to gray substance in the solid state; at 1275oC, it sublimes.4) According to this mechanism, elevated temperatures would accelerate removal of sodium from the slag, sulfur pickup by the

Jan 1, 1961

By Mark E. Smith

To allow recovery of gold values from ore which cannot be economically processed by the mill, Pinson Mining Company has developed a run-of-mine heap leaching facility. In order to estimate production scale recovery rates, reagent consumption and percolation problems, a series of pilot scale tests were performed. These tests typically consisted of 3,630 metric tons (mt) (4,000 tons) leach ore at a grade of .94 to 1.56 grams Au per metric ton (g/mt) (.03 to .05 oz. Au/ton). Test heaps were loader stacked to approximately 4.3 meters (14 feet) high. Information from these pilot scale tests was employed in the design and construction of the production scale facility. Parameters such as spray rate, leach cycle, sprinkler placement, and barren solution chemistry were determined by the pilot tests.

Jan 1, 1984

By D. C. Holloway

Ceramic projectiles made from 94% to 99% alumina with a nominal mass of 3.1 gms were fired into granite blocks. The average compressive strength of the ceramic was 800 MPa and that of the rock was 135 MPa. Flat, ogive, conical and pyramidal nose shapes were evaluated at velocities ranging from 450 to 1400 m/sec. It was found that the conical and pyramidal nose shapes at the higher velocities did a significant amount of damage to the rock. On the average, they removed 10 5mm3 of rock and were six and ten times better than the flat and ogive nose shapes. It was also observed that increases in volume occur in discrete steps. This process is highly dependent on the ability of the projectile to penetrate the rock.

Jan 1, 1984

By T. F. Witherbee

IN the sections, Figures 1, 2, and 3, are shown three crucibles that have been applied to substantially the same furnace, all the conditions having been the same except a variation of one foot of bosh, and a slight variation in the angle of the same. The bosh of No. 3 was originally the same as No. 2, the additional foot in diameter being the result of three months&apos; cutting. Beginning with No. 1, which was 5 feet 6 inches diameter, with tuyeres 5 feet 4 inches high, and cinder-tap four feet from bottom, great trouble was found in holding iron a proper length of time, four hours being the outside limit when working well, and two hours or less if working badly. "Break-outs" through the iron

Jan 1, 1880

By Leon Hart

THE nickel-chromium alloys of importance are those containing iron and those free from iron. The most important alloys containing iron, with regard to high tonnage, are the nickel-chromium steels. Straight nickel steel was introduced about the year 1889, but it was not until 1895, when it was found that the addition of chromium greatly increased the FIG. 1.-RESISTIVITY OF NICKEL-CHROMIUM-IRON ALLOYS. strength and resistance to shock, that nickel-chromium steels came into use. The three types of nickel-chromium steels developed at this time were: Type 1, containing 3.50 per -cent. nickel and 1.50 per cent. chromium; type 2, containing 2.00 per cent. nickel and 1.00 per cent. chromium; and type 3, containing 1.50 per cent. nickel and 0.50 per cent. chromium.

Jan 1, 1921

By J. A. Herbst, J. L. Sepulveda, J. D. Miller

Effective bismuth removal from flue dust residues has been accomplished for flue dusts from both zinc and copper smelters. Selective dissolution of bismuth, with respect to silver and lead, can be achieved by the proper manipulation of temperature, sulfuric acid addition and sodium chloride addition. Optimum levels of these variables were determined using a response surface technique to maximize the objective function: Y = %Bi/(1 + %Ag). In the case of the flue dust residue from a zinc smelter, which contains bismuth as an impurity (0.05%), 86% bismuth removal can be realized with less than 1% combined silver and lead dissolution. Similarly, in the case of flue dust from a copper smelter, which contains bismuth as a primary constituent (3.3%), 93% bismuth removal was obtained with little dissolution of silver and lead values.

Jan 1, 1977

By H. Scott

SINCE Böhler discovered, in 1903, on cooling certain alloy steels, the phenomenon of a new and lower temperature transformation than the usual Ar3_2_1 obtained by increasing the maximum temperature to which the material was heated, much has been published&apos; connecting this phenomenon with a large number of dissimilar steels of high alloy content. From the fact that the transformation divides itself, taking place at two widely separated temperatures, it has been called a "split transformation." The, significant facts established by recent investigators&apos; are: that when the&apos; transformation occurs at the higher temperature Ar&apos;, troostite or a decomposition product is formed, and that when the transformation occurs at the lower temperature Ar", the resulting structure is martensite. The terminology Ar&apos; and Ar" adopted here is that of Portevin.3

Jan 2, 1919

By A. T. Miesch, L. B. Riley

An error occurred in the preparation of Fig. 3, p. 249, of Basic Statistical Measures Used in Geo-chemical Investigations of Colorado Plateau Uranium Deposits. This figure shows the relation of the arithmetic mean: geometric mean ratio to the geometric deviation. Curves for the cases where n, the number of samples, is 100, 10, and 5 are too high with respect to the ordinate. The error is negligible at low geometric deviations, but becomes increasingly greater wi,th higher values of geometric deviation. Arithmetric mean values in Table I1 are not effected by the errors in Fig. 3. The authors will endeavor to supply copies of the revised curves on request; write to: A. T. Miesch, Geologist, Branch of Radioactive Materials, U.S. Geological Survey, Bldg. 25, Federal Center, Denver 25, Colo.

Jan 1, 1962

By T. F. Witherbee

In the sections, Figures 1, 2, and 3, are shown three crucibles that have been applied to substantially the same furnace, all the conditions having been the same except a variation of one foot of bosh, and a slight variation in the angle of the same. The bosh of No. 3 was originally the same as No. 2, the additional foot in diameter being the result of three months&apos; cutting. Beginning with No. 1, which mas 5 feet 6 inches diameter, with tuyeres 5 feet 4 inches high, and cinder-tap four feet from bottom, great trouble was found in holding iron a proper length of time, four hours being the outside limit when working well, and two hours or less if working badly. "Break-outs" through the iron

Jan 1, 1880

By Dorsey A. Lyon, Robert M. Keeney

Page I. Introduction..........234 I1. Chemistry oF Copper Smelting...235 1. Native Copper Ores.......235 2. Oxide and Carbonate Ores....235 3. Sulphide Ores.......236 (a) Elimination of sulphur ...236 III. Reverberatory Copper Smelting...237 IV. Substitution of the Electric Furnace for the Reverberatory Furnace..................... 238 V. Smelting of Fine Michigan Native-copper Concentrates in the Electric Furnace.................. 239 1. Conclusions.................240 VI. Proposed Process for Electric melting of Fine Native-copper Concentrates.................. 241 VII. OrdINary Copper Blast Furnace &apos;Smelting......... 245 1. Prerequisites.................. 245 2. Losses .................... 247 VIII. Experimental Data on the Electric Smelting of Raw Sulphide. Oxidized and Carbonate Ores............. 248 1. Vattier&apos;s experiment................ 248 2. Wolkoff&apos;s experiments................ 249 3. Experiments of Stephan.............. 250 (a) Conclusions of Stephan ............ 251 IX. Smelting of Sulphide Ores in the Electric Furnace...... 251 1. Ores Treated.................. 252 2. Conclusions................... 253 X. ELectric Furnace vs. the Reverberatory Furnace and Blast Furnace as a Melting Agent.............. 253 XI. Smelting of Sulphide Ores without Roasting or Partial Pyritic Smelting............254 XII. The Electric Blast Furnace vs. the Copper Blast Furnace for Partial Pyritic Smelting.......259 1. Metallurgical conditions......259 2. Mechanical considerations......259 3. Comparison of costs.......260 (a) General considerations .....260 (b) Cost of plant........260 (c) Amount of electrical energy...260 (d) Cost of smelting.......261 (e) Cost of electrodes........262 XIII. The Use of the Electric Furnace in the Smelting of PyRITIc ORES : 262 XIV. Summary...................... 264

Jan 1, 1914

CHARLES KIRCHHOFF, Chairman. ALBERT SAUVEUR, Vice-Chairman. HERBERT M. BOYLSTON, Secretary, Abbot Bldg., Cambridge, Mass. John Birkinbine, J. Esrey Johnson, Jr., Felix A. Vogel, William H. Blauvelt, William Kelly, Leonard Waldo, James Gayley, . Richard Moldenke, William R. Walker, Henry D. Hibbard, Joseph W. Richards, - William R. Webster. Henry 1%1. Howe, E. Gybbon Spilsbury, Frederick W. Wood. Robert W. Hunt, A. A. Stevenson, The Board of Directors of the Institute has authorized the holding of a meeting under the auspices of the Iron and, Steel Committee in New York City, October 16 and 17, 1913. Gratifying responses have been received to the request of the Committee for contributions, the following papers being already assured: 1. H. M. Howe, Equilibrium Temperature for A, in Carbon Steel. 2. H. M. Howe, The Divorcing of the Eutectoid in Meteorites. 3. H. M. Howe and A. G. Levy, Determination Of the Position of Ae3, in Carbon-Iron Alloys. 4. G. .K Burgess, J. J. Crowe and H. S. Rawdon, Thermal and Microscopical Examination of Professor Howe&apos;s Standard Commercial Steels. 5. H. Dl. Hove, Discussion of the Existing Data as to the Position of Ae3,. 6. J. H. Hall, Shock Tests of Cast Steel. 7. H. F. Miller, Jr., The Design of Regenerators for Open-Hearth Furnaces. 8. E. Stütz, Paper on the "Scoria Process." 9. Albert Sauveur, Mayari Steel. 10. Felix A. Vogel, Briquetting. 11. J. E. Johnson, Jr., Paper on " Cast Iron."

Jan 6, 1913

By W. J. Babyak, F. N. Rhines

It has long been supposed that, regardless of the mechanism by which grain boundaries increase the hardness of a ductile metal, the effect should be linearly proportional to the grain boundary area. At the present time two methods for determining grain boundary area in an isotropic aggregate are available. The first, derived by Angus and Summers,&apos; presumes that the grain boundary area is equal to 3vn, where n is the number of grains per sq mm in a random section through the metal. This estimate is based upon the assumption that the grains are equivalent to cubes whose faces correspond with the grains as observed in the micro-section. Measurements on copper, bronze, and a brass showed that a nearly linear relation exists between 3vn and hardness. This is illustrated, for the case of brass, in Fig. 1. The second method, developed independently by Smith and Guttman2 and by Duff in, Meussner, and Rhines,3 is absolute and employs a simple linear intercept count for measuring grain boundary area. It involves no assumptions with respect to the shape and distribution of the grain boundaries. The total surface in unit volume is 2 NL , where NL is the number of intercepts between grain boundary and unit length of a test line passed randomly through the sample. In practice, NL,, the average number of grain boundaries intercepted by unit length of traverse across a prepared microsection, is ob-

Jan 1, 1961