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By H. S. Geismer

INTRODUCTION. THERE are three general methods available for obtaining commercial brown iron-ore : hand-screening; washing; and washing and concentrating. Hand-screening has produced a large tonnage of ore in the past, but is rapidly falling into disuse, except as a preliminary step, largely because modern furnace-practice requires all foreign material to be separated from ores before they are delivered to the furnace, and hand-screened ores can rarely be made to fulfill that requirement. Another argument against hand-screening is, that the waste-pile often contains as much ore as the screen recovers. The operation known as hand-screening consists of throwing the ore-bearing material against a stationary inclined screen of 0.5- to 0.75-in. mesh, similar in construction to the screens employed in sand-pits. The recently-prospected brown-ore deposits of Cuba seem to offer possibilities for hand-screening not possessed by the average American deposit, since these ores are not associated with worthless clays. Washing, and washing and concentrating, may be discussed together, since concentrating is never practical on brown iron-ore, except to treat ores that have already been washed. (Strictly speaking, washing might be classed as concentrating, but it is never so designated by brown-ore men.) The various steps of removing ore-bearing material and converting it into ore suitable for blast-furnace use, may be grouped under five heads: loading for transportation ; transporting ; feeding into the washer; washing; and concentrating. These five subjects will be considered in consecutive order. Each of these successive steps may be accomplished in a number of different ways, the choice depending entirely upon the character of the ore-bearing material to be treated.

Aug 1, 1911

THERE can be little doubt in the mind of anyone of the great interest which has been provoked in the mining and petroleum industry by the com-paratively new geophysical methods of prospecting, after the sessions at this year's meeting of the Institute. Not only were the sessions very well attended but every¬one seemed most attentive. Although the discussion was somewhat limited in general, that may well be at-tributed to the newness of the subject. Two sessions on this subject were planned originally, but these gave insufficient time for the presentation of all the papers prepared and a third session was abso-lutely necessary. The first meeting dealt entirely with the gravity methods and was completed in the scheduled time owing to the fact that but two of the five papers listed were read. The second session was devoted to magnetic and electrical methods, the completion of which had to be carried over into the third period of geophysics. The first session on geophysical prospecting, and in-cidentally the first scheduled Institute meeting devoted entirely to this subject, was most appropriately opened by E. L. DeGolyer, the chairman of the session. It was through the efforts of Mr. DeGolyer that the first gravity work, as applied to prospecting, was under-taken in this country. Again most appropriately, the first paper presented was given by Donald C. Barton, who carried on the first work with the Eötvös torsion balance in America and aided materially in its development. A subject, the theory of which is so difficult to understand as it is generally presented, was so clearly illustrated and ex-plained by the speaker that even a novice could grasp the fundamentals. Dr. Barton, in showing actual re-sults obtained in torsion balance surveys with the in-terpretation of the sane and later drilling records, was free in stating that there are many limitations to the field in which this and the other geophysical instruments may be successfully employed. This paper called for considerable discussion relative to the application of the torsion balance to gravity surveys over various types of structures. During the course of this discus-sion a very important point was emphasized by the chairman, namely, that for successful application of any or all of the scientific methods of prospecting, a back-ground of experience is absolutely necessary to serve as a basis for further work. This can only be secured by contributions from the results of actual prospecting work.

Jan 3, 1928

THE committee in charge of arrangements for the meeting of the Institute in September has com-pleted its program. The headquarters of the meeting will be at the Palace Hotel, San Francisco, and the registration committee will be at the hotel all day on Sunday, Sept. 24, and from 8 a.m. until noon on Monday. On Sunday afternoon, automobiles will be available for sightseeing trips around the city. Monday will be devoted to technical sessions. In the morning, there will be sessions on Mining and on Iron and Steel; in the afternoon, sessions on Mining and Milling. At these sessions, in addition to the papers mentioned in the tentative list printed in August, there will be presented three papers on the geology, mining and milling of the Comstock lode; one on the Aztec mine, Baldy, N. M.; one on the Colombian oil fields; and one on charcoal precipitation of cyanide solutions. The luncheon on that day will be Dutch Treat, for men only, at the Engineers Club. On Monday evening, there will be an informal buffet supper at the home of F. W. Bradley. On Tuesday morning, a party of 50 men will leave for Hetch Hetchy. During the four days of the trip, the party will see the Priest tunnel and earth dam under construction by steam-shovel and hydraulic-fill methods, the Big Creek shaft and tunnel, early intake power plant and tunnels and the Hetch Hetchy dam under construction. For those who remain in San Francisco, Tuesday will be "San Francisco Day." There will be motor trips to the Presidio, Cliff House, Golden Gate Park, and other points of interest, and shopping trips to Chinatown. On Wednesday, "University of California Day," the party will be guided through the university by members of the Mining Association, the affiliated stu-dent society, and will see the Greak Theatre and not-able buildings. Thursday will be "Leland Standford, Jr. University Day." Automobiles will leave the Palace Hotel at 10 a.m., and will return from the university at 4.30 p.m. Friday has been reserved for trips to the Selby Smelter, to Mt. Tamalpais, or to other points of interest. Arrangements will be made to visit the mines or gold dredges in California, if members desire to do so, but such trips must of necessity be considered special trips and arrangements will have to be made to suit the convenience of the individual or party. The Golf Committee will make arrangements for those who wish to play golf.

Jan 9, 1922

By D. F. Atkins, B. A. Rogers

The constitutional diagram presented herein is relatively simple. Complete mutual solid solubility exists for an interval below the solidus line, a continuous curve with a flat minimum near 22 pct Cb and 1740°C. Upon cooling, the solid solution breaks up, except at the columbium-rich side, from two causes: zirconium-rich alloys transform under the influence of the ß-a transformation in zirconium; alloys of intermediate composition decompose into two solid solutions below 1000°C. The combined effect is the formation of a eutectoid at a temperature of 610°C and a composition of 17.5 pct Cb. The eutectoid horizontal extends from 6.5 to 87.0 pct Cb. Some age hardening effects have been observed in the zirconium-rich alloys but the positions of the solvus lines remain uncertain. IN recent years, zirconium has been produced in much larger quantities than were available previously. Correspondingly, the incentive for studying its alloy systems has increased, as the number of recent publications on alloy systems testifies. However, only a partial diagram of the Zr-Cb system has been published and relatively few references have been made to alloys of the two metals. Hodge' investigated the Zr-Cb system up to about 25 pct Cb. His data on melting points were not sufficiently numerous to distinguish with certainty between the alternatives of a narrow eutec-tic horizontal and a wide flat minimum in the solidus curve. Although Hodge considered his results on transformations in the solid state to be only tentative, he suggested that the eutectoid in the zirconium-rich alloys lay at about 625 °C and 10 pct Cb and estimated that the solubility of colum-bium in zirconium at 625 °C was near 6 pct. According to Simcoe and Mudge,2 less than 0.5 pct Cb is soluble in zirconium at 800°C. These authors observed an increased strength in both the 0.5 and I pct Cb alloys made with hafnium-containing zirconium. According to Keeler,3 the strength of zirconium is increased by addition of columbium to a content of at least 3 pct. Keeler' also observed a maximum in hardness at about 10 atomic pct Cb and commented on the brittleness of alloys of this composition. Anderson, Hayes, Rober-son, and Kroll5 investigated the tensile properties of Zr-Cb alloys containing 5.1 and 12.9 pct Cb at room temperature and at 343°C. The 12.9 pct alloy had a high tensile strength at room temperature but also a low percentage of elongation. All alloys had high elongation at 343 °C. Littona measured strength and elongation values of annealed alloys containing up to 27.5 pct Cb and found low elongation values for all of the alloys of high columbium content. Some observations on the resistance of Zr-Cb alloys to corrosion in water at high temperature have been published by Lustman, De Paul, Glatter, and Thomas' who found that additions of columbium up to 1 pct had only a minor effect on the corrosion resistance of zirconium. Preparation of the Alloys Raw Material: Zirconium of a relatively good grade was available for making the alloys. It was obtained as scrap pieces that had been left over from an operation that included production by the iodide process, melting under a protecting atmosphere, and fabrication to plates. The individual pieces had hardness values of 24 to 32 Ra and a typical analysis is shown in Table I. The columbium also was scrap trimmed from sheets. It was furnished by the Fansteel Metallurgical Corp. and had a high ductility but its analysis was known only approximately. The metal probably contained about 0.5 pct Ta, perhaps 0.25 pct C, and a few hundredths percent each of iron, silicon, and titanium. Melting: The alloys were melted in a tungsten-electrode copper-crucible arc furnace similar to units that have been described recently in the metallurgical journals.'.' The crucible of this furnace is provided with a cavity in which a getter charge can be melted before the melting of the alloy charges. Hardness measurements on the ingots indicate that the getter charge takes up a considerable fraction of the oxygen and nitrogen from the helium atmosphere of the furnace. The alloys used in the investigation are given with their intended compositions, hardness, and melting points in Table 11. Fabrication: All alloys of the Zr-Cb system appear to be amenable to fabrication. At least, all of the compositions listed in Table II could be reduced to wires in a rotary swaging machine. The starting material was either slabs cut from ingots and ground by hand to rough cylinders or narrow strips trimmed from sheets made by cold rolling slabs. However, not all of the alloys could be fabricated satisfactorily by the same method. From 0 to 4 pct Cb and from 20 to 30 pct Cb or more, the alloys could be swaged cold from ¼ in. cylinders to 0.80 mm wires with only one intermediate annealing, sometimes with none. From 40 to 90 pct Cb, the alloys were difficult to swage either hot or cold but could

Jan 1, 1956

By J. H. Polhems, R. B. Brackin, D. B. Grove

THE heavy media separation process plays an outstanding role in the concentration of 4000 tons of zinc ore per day at the Mascot mill of the American Zinc Co. of Tennessee. Of the total tonnage, 72 pct is treated in the heavy media separation plant to reject 56 pct of the ore as a coarse tailing, which has a ready market. Concentrates from this separation are beneficiated further by jigging and flotation. Approximately 25 pct of the total zinc concentrate production is made in the jig mill. Jig tailings are ground and pumped to the flotation circuit where the balance of the production is made. Fig. 1 shows a generalized flowsheet of the mill. The Mascot ore is a lead-free, honey-colored sphalerite in dolomitic limestone, with lesser amounts of chert and some pyrite. A mineralogical analysis is given in Table I. After 10 years of successful operation with galena medium and treatment of nearly 10,000,000 tons of ore, a decision to convert to ferrosilicon was made early in 1948 because of the increasing price of galena and consequent high operating costs. The conversion was made on Nov. 6, 1948, and the results obtained since that time have shown remarkable improvement over those made with galena. The Table I. Mineralogical Analysis of Mill Feed, Pct Calcium carbonate 49.5 Magnesium carbonate 35.2 Iron oxide and aluminum oxide 1.5 Zinc sulphide 4.5 Insoluble 9.3 100.0 Table II. Comparative Data, Galena and Ferrosilicon Ferro- Diner-Gelenaa siliconb ence Operating costs per ton milled, ct. 21.21 9.12 12.09 Medium consumption per ton milled, lb 0.80c 0.15 0.65 Reagent consumption per ton milled, lb 0.45 0.02 0.43 Tailing assay, pct Zn 0.310 0.297 0.013 Concentrate. oct Zn 12.08 10.33 1.75 Heavy medla ieparatlon recovery. pct 89.38 90.22 0.84 Mill feed rate, tons per hr 153 166 13 Heavy mesa separation feed rate. tons per hr 100 10 0 Tons milled per heavy media separation man shift 350 620 270 Mill feed to coarse tailings, pct 51.0 56.7 5.7 Lost mill time, pct 5.6 5.0 0.6 Power consumption, kw-hr per ton 2.06 1.92 0.14 a 1947. " First 6 months of 1950. c Net consumption after deducting credit for reclaimed waste galena. Consumption of new galena was 1.320 lb per ton milled. For entire life of galena operation, a credit of 40 pct of the value of the new galena added was realized from the sale of waste galena. comparisons given in this report cover the first 6 months of 1950 as representing the ferrosilicon operation, and the year 1947 as representing the galena operation. This was the last full year in which galena was used exclusively and is representative of the best work done during the 10 years of operation with this medium. After only 2 years' operating experience, with ferrosilicon and treatment of 1,807,585 tons many advantages have been revealed and are summarized in Table 11. Development Prior to the introduction of the heavy media process, all the mill feed was crushed through 5/8 in. and treated by jigging. A finished tailing assaying 0.66 pct Zn was made on rougher bull jigs, and cleaner jig tailings were ground for treatment by flotation. The first test work on the sink-and-float method of mineral beneficiation was carried out at Mascot in 1935, using a 3-ft cone and galena medium for batch tests. The following year a 6-ft cone was installed for pilot-plant work. This unit became a part of the mill circuit on March 1, 1936, and handled a gradually increasing tonnage in the next 2 years as the process developed to the point where it could treat all the + 3/8-in. material in the mill feed. Coarse jigging was then discontinued on March 1, 1939, and all coarse tailings have been made by the heavy media separation plant since that time. Feed Preparation: The original feed preparation plant consisted of a drag washer followed by two 4x10-ft Allis-Chalmers washing screens. A surge bin and two additional 5x12-ft AC washing screens were added in 1943. Use of primary and secondary washing screens was found essential to provide the cleanest possible feed for the cone and thereby avoid excessive contamination of the galena medium. Improved washing was obtained by replacing the drag washer with a 7x20-ft Allis-Chalmers scrubber, shown in Fig. 2, which has been in service since May 1944. Throughout the life of the galena operation, delivery of extremely muddy ore to the mill overloaded the medium cleaning system, and it frequently was necessary to cut off the feed and clean the medium for several hours until its normal viscosity had been re-established. The cleaning circuit

Jan 1, 1952

By W. H. Porter, M. E. Wadsworth, J. R. Lewis, K. L. Leiter

The oxidation of Cu2S in oxygen and the sulfating of Cu2O in oxygen-sulfur dioxide atmospheres was carried out under a variety of conditions. The oxidation of Cu2S was found to be retarded by entrapment of SO, and O2, which stabilized internal sulfates for long periods of time. The course of the reaction was followed by measuring weight changes and also by SO, evolution. Sulfating of Cu2O was a maximum at ratios of SO, to O2 approximating maximum SO, production. At elevated temperatures SO, was found to increase the rate of oxidation of Cu2 O to CuO even though sulfates did not form. All sulfating reactions followed the parabolic rate law indicating diffusion. MANY studies of the roasting of copper sulfides have been reported in recent years. Diev et al.1 investigated the roasting of chalcocite (Cu2S) in air, and oxygen enriched air. Lewis et al.2 also studied the oxidation of natural and synthetic chalcocite in air and oxygen atmospheres and their studies indicated that the maximum formation of water soluble sulfates occurred at approximately 450oC. Ashcroft3 reported that oxide production during the roasting of chalcocite resulted only from secondary decomposition of sulfates which were formed as primary products. peretti4 refuted this claim by showing that a layer of Cu2O appeared directly adjacent to the Cu2S during roasting of cylindrical briquettes of cupric sulfide, CuS. The linear advance of the Cu2S-Cu2O interface was used as a measure of the kinetics of the roasting reaction. The reactions proposed were: 2 CuS—Cu2S + 1/2 S2 [4-1] 1/2 S2 + O24 SO2 [4-2] cuzs +3/2 O2 4 Cu2O + SO2 [4-3] cu2o + 1/2 O2—2 cuo [4-4] At temperatures above 663oC, CuO was the only final solid phase reported. Below 663" C increasing amounts of sulfate were found mixed with the CuO. McCabe and Morgan5 investigated the roasting of discs of synthetic chalcocite and reported the following sequence of products beginning at the sulfide surface: Cu2O, a mixture of Cu2O and CuSO4, Cum,, CuO . CuSO4, and CuO. The principal reactions were reported to be: Cu2S + 3/2 O2-Cu2O + SO2 [5-1] CU2O + 2 SO2 + 3/2 O2—2 CUSO4 [5-21 2 CUSO4— CUO . cum, + SO3 [ 5-31 cuo . cuso4—-2 cuo + SO, [ 5-41 Eq.15-11 supports the claim of Peretti, Eq. [4-31, that CuzO is formed directly from Cu2S rather than as a secondary product from a sulfate as suggested by Ashcroft. On the other hand CuO was found to form as a secondary product from the decomposition of copper sulfate and basic copper sulfate, Eqs. [5-31 and [5-41. The formation of sulfates was explained by McCabe and morgan5 to be a direct reaction of Cu2O with 0, and SO, or SO, at distinct regions in which the partial pressures of each were such as to form the sulfate. Thornhill and pidgeon6 roasted both natural and synthetic chalcocite grains in air at temperatures between 420" and 550° C. They found a dense primary oxidation layer in contact with the sulfide. A secondary layer of porous oxidation products was found to expand with roasting time. The oxide products were leached away and the remaining core was studied by X-ray diffraction. The X-ray patterns showed an increased conversion of chalcocite to digenite with time. Digenite,7 a defect structure of cuprous sulfide, occurs naturally as Cu,-,S where x = 0.12 to 0.45, with an average analysis of Cu, ,S. The mechanism of digenite formation was proposed as: Cu2S + oxygen—Cu1-8S + 0.1 Cu2O [6-1] Cuj.eS + oxygen—0.9 Cu2S + SO2 [6-2] It is apparent from the above studies that the oxidation of Cu2S, ultimately ending in CuO, may be divided into ihree general stages (all of which may occur simultaneously): 1) primary oxidation to Cu2O; 2) secondary sulfate formation; and 3) sulfate decomposition. Consequently reactions of O2 and SO, with Cu20 constitute important aspects of the roasting of chalcocite. Virtually no studies have been made regarding sulfating reactions involving Cu,O. Mills and Evans8 noted the effect of sulfur dioxide on the oxidation of copper at low temperatures and low SO, partial pressures. They reported a measurable increase in the oxidation rate of copper when SO2, was present. Interest in the Cu2O-CuO-0, system has been limited predominantly to misciblllty studies and determinations of heats of formation by

Jan 1, 1961

By Y. A. Chang

Phase relationships in the system Cr-Si have been established based on the melting point, X-ray, metallo-graphic, and DTA studies. The three intermediate phases, Cr3Si, Cr5Si,, and CrSi,, melt congruently at 177V ± I@,Cr3Si, 1680"i 20°, and 1490" *20°C, respectively, while the fourth intermediate phase CrSi, melts peritectically at 1413" i 5°C to Cr5Si3 and a melt containing 51 at. pct Si. The temperatures and compositions of the four eutectic isotherms occurring in this system are given below: DTA and metallographic evidences indicate that Cr5Si, undergoes a phase transformation at 1505" i20°C. The high-temperature form of this phase could not be retained by the quenching techniques used in this study. TECHNOLOGICAL interest in the developing of composite systems, consisting of Sic on the one hand as a fiber-reinforced material and metallic substances such as chromium, nickel, or Cr-Ni alloys as a binding agent on the other hand, stimulated the present investigation of phase relationships in the binary system Cr-Si. Earlier works concerning this system have been evaluated and summarized by ansen and Anderko.' Their phase diagram was based mainly on the works of Kieffer, Benesovsky, and schroth2 and Kurnakov.~ According to these authors, the three intermediate phases Cr3Si, CrSi, and CrSi, all melt congruently at approximately 1730°, 1600°, and 1550°C. However, they did not agree on the compositional stability of the fourth intermediate phase between Cr3Si and CrSi. Later Parthe, Nowotny, and schmid4 determined the structure of this phase to be tetragonal T-1 type using the single-crystal method, and concluded that this phase had a formula of Cr5Si3. Since the compilation of Hansen and Anderko,' a new phase diagram for the system Cr-Si has been proposed by Elliott5 based on the works of Goldschmidt and rand,' Guseva and ~vechkin,~ and Trusova, Kuzev, and Ormont8 and the earlier works quoted by Hansen and Anderko.' According to this proposed phase diagram, all four intermediate phases have large ranges of homogeneity and all melt congruently. More recently, Svechnikov, Kocherzhinskii, and yupkog studied the system Cr-Si by the DTA-method. According to their findings, the three intermediate phases, Cr3Si, Cr5Si3, and CrSi,, melt congruently at 1700°, 1720°, and 1475"C, respectively, while the fourth intermediate phase, CrSi, melts peritectically at 1475°C to Cr5Si3 and a melt containing 50 at. pct Si. The temperatures and compositions of the four eutectic isotherms were found to be: In view of the discrepancies existing in the literature concerning the system Cr-Si, it was decided to rein-vestigate the phase relationships in this system. EXPERIMENTAL a) Starting Materials. Chromium disilicide and chromium or silicon powders were used in the present study to prepare the melting point and DTA samples. CrSi, was obtained by directly reacting cold-pressed elemental powders in an atmosphere of Hz at a temperature of about 1250°C. Chromium powder, purchased from Stark Chemical Co., had the following impurities in ppm: Fe, 200; Mg, 1000; and 0, 250; while silicon powder, purchased from the Welded Carbide Co., had the following impurities in ppm: Ca, 700; and Fe, 3500. b) Melting-Point Determination and Differential Thermal Analysis. Cylindrical melting-point samples of approximately 13 mm in diam and 30 mm in length with a rectangular groove in the center were prepared by hot-pressing of well-mixed powder mixtures in graphite dies. Before the melting-point determination, the hot-pressed samples were ground on a sand paper to remove any minute surface contamination of graphite. A small hole of 1 mm in diam, drilled on the center portion of the samples, served as a blackbody cavity for the temperature measurements. DTA samples approximately 13 mm in diam and 15 mm in length were prepared in a manner similar to the melting-point samples. Melting points were determined using the Pirani technique under a helium atmosphere of 40 psi. The design, performance, and operation of this apparatus have been described in detail by Rudy and ~ro~ulski.'~ The temperature measurements were carried out with a calibrated disappearing-filament-type micro-pyrometer. The measured temperature was corrected for losses from the quartz window of the melting-point furnace and for deviations from blackbody conditions of the observation hole. The procedure for temperature correction has also been previously described." The DTA method of Heetderks, Rudy and Eckertl' was also used to check any phase transformations of selected alloys in the system Cr-Si. It was not possible to make remated runs on the same sample once melt-

Jan 1, 1969

By H. Conrad, V. V. Damiano, G. J. London

A method is described for producing single crystals of high-purity beryllium, Be-4.37pct Cu, and Be-5.24 pct Ni. These crystals were prepared for testing in compression parallel to the [0001] by orienting and lapping to within ±3' of arc of the (0001). Microstrain testing apparatus is described along with c axis compression results for ingot purity beryllium, twelve-zone-pass material, and the above-mentioned alloys. Results show no measurable plasticity for the ingot purity material from -196" to 400°C, although some surface traces of (1122) slip was observed at 200°C and above. The twelve-zone-pass material shows substantial microstrain plasticity at 220°C with slip on (1122). Both alloys show significant plasticity at room temperature and above with slip also on (1122) planes. THE two slip systems which normally operate during the plastic deformation of beryllium in the vicinity of room temperature are:' basal slip (0001)(1120) and prism slip . Pyramidal slip with a vector inclined to the basal plane has been reported for elevated temperatures,'-a but occurs near room temperature only at very high stresses.~ A summary of the available data on the effect of temperature on the critical resolved shear stress for slip on these systems has been compiled by Conrad and Perlmutter.~ It has been postulated6'7 that one of the principal factors contributing to the brittleness of poly crystalline beryllium at temperatures below about 200°C is the difficulty of operating pyramidal slip with a vector inclined to the basal plane. Hence, detailed information on the operation of such a slip system is important to understanding the brittleness of beryllium. The operation of pyramidal slip with a vector inclined to the basal plane is best accomplished in beryllium by compressing single crystals in a direction parallel to the c axis. In such a test the resolved macroscopic shear strzss on the basal and prism planes is zero and (1012) twinning which is favored by tension along the c axis does not occur. Hence, in c axis compression of beryllium the normal deformation modes are inhibited and the operation of pyramidal slip with a vector inclined to the basal plane is favored. In the present investigation, c axis compression tests were performed on beryllium single crystal as a function of temperature (77" to 700°K), purity (commercial and twelve zone pass), and alloy content (4.37 wt pct Cu and 5.24 wt pct Ni). Presented here is a description of the test techniques employed and the gross mechanical behavior observed. A detailed analysis of the slip traces developed on the surfaces of the deformed specimens during these tests and the results of electron transmission studies of the deformed crystals are given in a separate paper.B PROCEDURE 1) Materials and Preparation. Single crystals about 1 in. diam were prepared of the following materials: commercial-purity beryllium, high-purity beryllium, and two beryllium alloys, one with 4.37 wt pct Cu and the other with 5.24 wt pct Ni. The commercial-purity single crystals were obtained by cutting specimens from large-grained ingot of Pechiney SR material, which is approximately 99.98 pct pure. The high-purity crystals were prepared by floating-zone refining (twelve passes) a rod (7 in. by 1 in, diam) of Pechiney SR grade cast and extruded beryllium. Although an absolute chemical analysis of the zone-refined material was not established, mass spectro-graphic analysis, emission spectrographic analysis, and y activation analysis indicated that it contained in atomic fractions about 5 to 10 ppm each of carbon and oxygen, 1 to 5 ppm each of nickel and iron, and about 1 to 2 ppm of copper, with the remaining residual impurities being less than 1 ppm. Further indication of the purity of this material is provided by the critical resolved shear stress for basal slip, which was approximately 300 psi. The starting material for the alloy single crystals was 1-in.-diam floating-zone-refined (six passes) rod of Pechiney SR grade beryllium. Two such rods were wrapped respectively with sufficient weight of wire of high-purity copper (99.999 pct) or nickel (99.999 pct) to yield a 5 wt pct alloy. A seventh floating-zone pass was then applied to each of the rods to accomplish the initial alloying and an eighth pass for homogenization. Analytical samples were taken from regions of the rod immediately adjacent to where the mechanical test specimens were cut; these indicated 4.37 wt pct Cu and 5.24 wt pct Ni. 2) Crystal Orientation. To avoid the occurrence of basal slip during c axis compression testing, it is necessary to load the crystals as nearly parallel to the c axis as possible. Preliminary c axis compression tests indicated that plastic flow and/or fracture occurred at stresses of the order of 300,000 psi; hence on the basis of a critical resolved shear stress for basal slip of 300 to 400 psi, the maximum crystal misorientation permitted is about 4 to 5' of arc. Since this accuracy cannot be obtained using the usual back-

Jan 1, 1969

By W. A. Backofen, R. L. Fleischer

Single crystal, bicrystal, and polycrystal tensile tests of aluminum at 4.2°K, 77°K, and 300°K have been used to examine the role of grain boundaries in the deformation process. Results indicate that a grain boundary may affect the extent and slope of easy glide. The stage II hardening rate, on the other hand, is independent of the presence or absence of grain boundaries. This conclusion allows the size of the region of multiple slip caused by an incompatible grain boundary to be determined. For the size of bicyystal sample used in this study, multiple slip occurs in about half of the cross section. PREVIOUS studies of the stress-strain characteristics of bicrystals of face-centered-cubic metals have been limited to aluminuml-5 at room temperature. Recent results, however, indicate that the stress-strain curves of single crystals of such metals may be separated into at least three stages6 in which different deformation processes are occurring7 provided testing is done at sufficiently low temperatures.' Since for aluminum a well-defined stage II develops only below room temperature, previous studies have not been able to relate effects of grain boundaries to all of the three stages of deformation. It is therefore to be expected that low-temperature deformation of aluminum single crystals and bicrystals should clarify the effects of grain boundaries on the different processes of deformation. EXPERIMENTAL PROCEDURE Single crystals and bicrystals were grown from the melt by the standard techniqueg with aluminum reported by Alcoa to be 99.993 pct pure. Ridges in the boat were used to guide the grain boundary during growth, assuring that the boundary would bisect the sample.10 The rate of furnace motion during growth was 1.0 cm per hr. During growth zone purification resulted, as evidenced by the ability of the first material to freeze to recrystallize at room temperature following severe deformation. Samples were approximately 4.4 X 6.6 mm in cross section and 103.5 mm in length between grips. Samples were annealed at 635" i 5°C for 40 hr and furnace cooled over a 7-hr period. They were then electropolished in a solution of 5 parts methanol to 1 part perchloric acid at a current density of 15 amp per sq dm for about 30 min at temperatures below 0°C. Tensile testing was performed at 295" (room temperature), 77" (sample in liquid nitrogen), and 4.2"K (sample in liquid helium) on the hard-type machine indicated schematically in Fig. 1. The machine con- sists basically of a tube surrounding a rod; one end of the sample is attached to each member, and the rod is pulled up the tube to extend the sample. The rod is rigidly mounted and is moved vertically by a system described by asinski." The pulling force is measured continuously by an electrical strain gage load cell, and the relative displacement of the tube and rod is also recorded continuously by a soft cantilever beam with electrical strain gages. Maximum stress and strain sensitivities were ±2g per sq mm and * 3-10-5. In all tests the strain rate was approximately 5.10-5 per sec. The thin wires in the tensile apparatus introduce softness, which may be corrected for, however, by measuring load vs displacement with the sample replaced by an elastic member. For loads greater than 15 kg the spring constant is 1.875.106 g per cm. The flexible wires also served to reduce substantially the large shearing forces which may arise in the case of grips having horizontal rigidity.'' As in any gripping system, however, bending moments will arise in the course of deformation by single slip. Engineering stress, s = (load)/(original cross-sectional area), and strain, E = (increase in length)/ (original length), are used for stress-strain curves unless otherwise indicated. Tables list resolved shear stress, T=mo and shear strain ? = dm, where m is the usual Schmid resolved shear stress factor for the primary slip system at the start of deformation. The first group of samples to be described forms an isoaxial set, all of the crystals making up the single crystals or bicrystals having the same tensile axis, the orientation of which is indicated by the cross in Fig. 2. For this orientation the primary slip plane and slip direction make angles of 45 deg with the tensile axis and the Schmid factor m has its maximum possible value of 0.5. Rotations about the tensile axis are indexed by means of an angle 0 between the small-area surface of the samples and the projection of the primary slip direction onto the cross section, as defined in Fig. 3. In single crystals, values of 0 were 0 and 90 deg, while in bicrystals 0 values were (0 deg, 180 deg), (90 deg, 270 deg), and (0 deg, 90 deg) as indicated in Fig. 4.

Jan 1, 1961

By D. I. Bardos, Paul A. Beck

A MARK, Boren, and westgrenl in their X-ray diffraction study of manganese alloys with 10 to 25 at. pct Si reported the occurrence of a phase with complex crystal structure in a Mn + 14.5 at. pct Si alloy after annealing at 800° or at 600°C. Recently Kuzma and Gladyshevskii2 identified Mn6Si as an R phase,3,4 the second binary R phase known. (A binary R phase was previously found in the Mn-Ti system by Waterstrat.5) A ternary R phase was reported earlier0 near the Mn-Si binary border of the Ti-Mn-Si system at 1000°C. In the light of the Russian work it now appears that this "ternary" R phase may be in fact an extension of the binary (Mn6Si)R phase. As already found by Amark, Boren, and Westgren, the corresponding binary phase is absent at 1000°C; the effect of titanium is evidently to stabilize it up to higher temperatures. In a recent paper Wieser and Forgeng7 gave the boundaries of this binary phase, which they referred to as 6. In order to re-examine the identity of this phase, an alloy of Mn + 14.5 at. pct Si was prepared by induction melting in helium atmosphere and annealed for 3 days at 800°C. The powder pattern, taken with an asymmetrical focusing camera of large dispersion and shown in Table I, was found to be that of the R phase, in agreement with the results of Kuzma and Gladyshevskii. For comparison, Table I also lists

Jan 1, 1965

By F. C. Schora, H. P. Meissner

Iron ore from Cerro Bolivar, Segre', and Sierre Grande was reduced in fluid beds at about SOOT, using gas analyzing 20.5 pct CO, 41 pct Hz, and 38.5 pct N2. Except in the early stages of reduction, the rate of oxygen loss from the bed was directly proportional to the oxygen concentration in the bed, independent of gas composition as long as the gas was reducing, and little affected by temperature. The percentage reduction of the bed solids at any time was independent of particle size. I HE reduction of spheres or cubes of dense iron ore in a slowly moving stream of either pure H, or pure CO has been found to take place at distinct interfaces between well defined layers of iron and the iron oxides.'y4 These interfaces generally penetrate the ore lump in topochemical fashion, remaining parallel to the original contours of the specimen. Thus in the earlier stages of reducing hematite, the specimen's core is Fe,O, surrounded by successive shells of the lower oxides, and finally by an exterior shell of iron. McKewan5 assumed that the rate limiting step occurred at the Fe-FeO interface, with reducing gas penetrating up to this interface through the external porous iron shell, and reduction of the higher oxides within the ore lump occurring by diffusion of iron through the dense FeO shell. He developed an analytical expression based on this model relating the amount of oxygen removed from

Jan 1, 1962

By H. l. Burghoff

THE presence of tellurium in copper and, by inference, in copper alloys, has been considered seriously detrimental and has been avoided. In particular, very small amounts of tellurium have been found to produce red-shortness, although the effects on cold-working and ordinary physical and mechanical properties have not been known so definitely. References in the literature are few, but as long ago as 1881, Egleston1 reported that 0.083 per cent tellurium in fire-refined copper rendered the copper red-short and therefore worthless for hot-rolling. In hot-rolling copper cakes containing this amount of tellurium, he found that fine cracks appeared in the cakes on the first pass through the rolls, the cracks opening further in successive passes. When cold, the metal was said to be tough and malleable. A few years ago, during the course of an investigation in our laboratory on copper-base alloys, it was found that tellurium-bearing alloys could be machined much more freely than similar alloys not containing tellurium. The study was pursued further in this direction, and considerable data were obtained, which indicated that certain tellurium-bearing alloys might have properties of commercial interest. The work eventually led to patent protection,2 a wide range of tellurium-bearing copper-base alloys being covered. This article presents results obtained on the effect of tellurium on the. mechanical properties of three copper-base alloys: commercial bronze (90 Cu, 10 Zn), 1.5 per cent tin bronze (98.5 Cu, 1.5 Sn), and silicon bronze (96 Cu, 3Si, 1 Zn).

Jan 1, 1937

By Haim Chiswik

IN recent years considerable attention has been devoted to the devel-opment of new commercial uses for silver, chiefly because of lowered prices and large stocks of the metal. This has led to increased interest in the phase diagrams of silver alloys. The silver-lead diagram is reported' to be of the simple eutectic type, but no measurements of the solubility of lead in silver have been made. The solubility of silver in lead has been estimated2 from diffusion experiments and resistance measurements to vary with temperature from 0.09 to 0.18 atomic per cent (0.05 to 0.10 weight per cent). Silver-rich silver-lead alloys have recently been recommended as high-strength bearing metals.3 The silver-bismuth diagram is similar.' The solubility of bismuth in silver has been estimated to be about 5.5 weight per cent on the basis of X-ray work.4 Matthiessen5 found a solubility of silver in bismuth from 0.25 to 0.50 per cent by conductivity measurements. Silver and thallium form the same type of diagram,1 with no data on their mutual miscibilities. We have studied the first two of these diagrams by X-ray methods, verifying their main features and determining the solubilities of lead and bismuth in silver at several temperatures. We also determined the solubility of thallium in silver at one temperature. The solubilities of silver in lead and in bismuth were found to be too low to be detectable.

Jan 1, 1940

By E. A. Nesbitt

A new permanent-magnet material has been developed with unusual mechanical as well as magnetic properties. Specimens that have been cast or subjected to a small amount of hot reduction by rolling or swaging may be machined, punched, tapped or drilled. The composition range of the alloys is 30 to 52 per cent iron, 36 to 62 per cent cobalt and 4 to 16 per cent vanadium. After being either quenched, annealed or given the usual cold finishing passes and then heated for 2 hr. at 600°C., such materials have a magnetic energy product of 1.0 X 106 gauss-oersteds. This product is equivalent to that of the well-known Honda steel (36 per cent Co, 4W, 2 Cr, 0.8 C. 0.3 Mn, balance Fe). Material handled in the manner just described does not depend on cold-working for its magnetic properties, and is known as Vicalloy I. The preferred composition for Vicalloy I is 38.5 per cent iron, 52 per cent cobalt and 9.5 per cent vanadium. When the alloys are first hot-worked, then considerably reduced in area by cold-swaging, drawing or groove rolling and then heat-treated, the magnetic energy product measured in the direction of previous extension is increased to 2.0 to 3.5 X 106 gauss-oersteds. These higher values have been obtained only after cold reductions in area of 75 to 95 per cent. Material handled in this manner is known as Vicalloy II and the preferred composi-

Jan 1, 1947

By E. A. Nesbitt

A new permanent-magnet material has been developed with unusual mechanical as well as magnetic properties. Specimens that have been cast or subjected to a small amount of hot reduction by rolling or swaging may be machined, punched, tapped or drilled. The composition range of the alloys is 30 to 52 per cent iron, 36 to 62 per cent cobalt and 4 to 16 per cent vanadium. After being either quenched, annealed or given the usual cold finishing passes and then heated for 2 hr. at 600°C., such materials have a magnetic energy product of 1.0 X 106 gauss-oersteds. This product is equivalent to that of the well-known Honda steel (36 per cent Co, 4W, 2 Cr, 0.8 C. 0.3 Mn, balance Fe). Material handled in the manner just described does not depend on cold-working for its magnetic properties, and is known as Vicalloy I. The preferred composition for Vicalloy I is 38.5 per cent iron, 52 per cent cobalt and 9.5 per cent vanadium. When the alloys are first hot-worked, then considerably reduced in area by cold-swaging, drawing or groove rolling and then heat-treated, the magnetic energy product measured in the direction of previous extension is increased to 2.0 to 3.5 X 106 gauss-oersteds. These higher values have been obtained only after cold reductions in area of 75 to 95 per cent. Material handled in this manner is known as Vicalloy II and the preferred composi-

Jan 1, 1947

By G. Gutierrez, M. C. Fuerstenau, J. D. Miller

The response of pure goethite and two natural iron ores to flotation with potassium octyl hydroxamate is presented. The ores contained 12.5% and 39.7% iron; concentrates containing 69.5% and 61.5% iron, respectively, were obtained with additions of 0.4 lb/ton hydroxamate. Selective flotation of iron oxides from associated gangue minerals has proven difficult in the past with standard collectors, such as sulfonates and fatty acids. As a result, recent work has been directed toward silica flotation with calcium activation after the iron oxide surfaces have been blinded with certain starches.& The results obtained with this technique are encouraging. This method, however, involves depressing a mineral that would normally float under the conditions employed. A preferable method would involve floating the iron oxide because quartz is naturally depressed until activated. Earlier work involved this approach, but in view of the results obtained, collectors that exhibit greater specificity for iron are needed. During an investigation of chrysocolla flotation with potassium octyl hydroxamate, a metal chelate former, it was observed that pyrite floated well with low additions of collector.3 This phenomenon suggests that hydroxamate has a rather strong affinity for iron, and that other iron-bearing minerals should also respond to flotation with octyl hydroxamate. The object of this paper is to determine this response. The experimental work was divided into areas, the first of which involved microflotation experiments with pure goethite with an apparatus described previously.4 Goethite was selected because of the ease

Jan 1, 1968

By R. W. Balluffi, B. H. Alexander

RELATIVE diffusion rates of copper and zinc in a brass have been measured in a vapor-solid type of couple with which the amounts of copper and zinc diffusing past inert Kirkendall markers can be obtained by means of a few simple experimental measurements. If inert markers are placed on the surface of copper which is then exposed to zinc vapor from a brass chips, the particles become buried due to outward diffusion of the copper, as shown in Fig. 1. A schematic diagram of such a couple after diffusion is shown in Fig. 2. Consideration of the diffusion flow of copper and zinc shows that the entire hatched area, including the cross-hatched area, is proportional to the amount of zinc diffused inward past the markers and that the smaller cross-hatched area is proportional to the amount of copper diffused outward past the markers. These areas are completely determined by the expansion of the couple, the depth of the buried particles below the surface, and the chemical composition at the specimen surface. As Darken1 has shown, the ratio of diffusivities of copper and zinc is then given by the ratio of these two areas. Polycrystalline copper and two copper single-crystals made by the Bridgman method were prepared in the form of 1.5 cm diam disks approximately 0.5 cm thick with faces plane and parallel. Tungsten particles approximately 0.001 cm in diam were bonded to the surface of each disk by heating 5 hr at 1060°C in vacuo. Each specimen was next

Jan 1, 1953

By Friedrich Wellmer

INTRODUCTION The Ramsbeck Pb/Zn Mine is located in the northern Sauerland area of West Germany, 150 km N of Frankfurt and 120 km E of Cologne. This is a vein deposit which has been worked from the middle of the 19th century to 1974. About 15 million tons of ore were mined and milled. The ore district contains several vein deposits and is roughly 14 km in length and 4 to 5 km in width. The host rocks are strata of Lower Middle Devonian age. The strata strike 60° to 70° NE and where overturned have a dip steeper than the veins (Fig. 1). The galena-sphalerite mineralization is in quartz veins, which are mineralized where they cut the "Main Ramsbeck Quartzite" horizon, a very competent host rock. Vein structures strike at 65º to 75º, dip about 20° to 25º SE and cut the quartzite at approximately 60 m intervals. The main or "steep veins" within each vein structure dip at 10º to 80° SE with an average of 30° and are offset by thrust faults dipping 5º N to 40° S with an average of 5º S. "Flat veins" usually weakly mineralized occur in the thrust faults between the "steep veins", thus forming the overall step-like vein structure. The mineralization is very irregular and changes a- long strike and down dip. It consists of thin veins of pure sphalerite and galena with quartz and pyrite. The thicknesses of the pure sphalerite and galena veins

Jan 1, 1977

By Max Boehmer

(Pittsburg Meeting, March, 1910.) AFTER 30 years of development and after an output of $350,000,000 in value of gold, silver, lead, zinc, and copper, there has not been published a satisfactory explanation of the origin of the immense deposits of the Leadville district. The original examination find survey of Leadville by members of the U. S. Geological Survey was a most magnificent piece of work, but their attempt to explain the origin of the ores was based upon the then-accepted theory of lateral secretion, originated by Sandberger, which theory was afterwards disproved in many cases by further development in numerous districts. This theory contended that the ore in the veins had been leached by surface-waters from the eruptive rocks in the immediate vicinity, and it had its origin in the fact that the neighboring eruptive rocks all contained, to an appreciable degree, the several metals found in the ore-deposits. But the practical miner, reasoning in a simple manner from the condition of things as he found them underground, soon discovered the fallacy of this proposition. He reasoned that, in the case of the Leadville deposits, this theory could not be true, because, if the ores were leached from the overlying eruptive rocks by surface-waters, they would as a matter of necessity be controlled by the action of gravity, and the main bodies would collect in- natural depressions of the underlying limestone, and at all points where such depressions existed. But this was not in accord with the channels of ore as he found there ; and hence the theory of lateral secretion in this district was never accepted. Another objection to it consisted in the fact that large areas within the ore-bearing district contained no ores whatever, although their formation was the same, and the same limestones were covered by the same thick sheet of

Feb 1, 1910

By GEO H. DEIKE

NOT much activity has been evident during the past year in the establishment of co-operative scholarships but the interest among the coal-mining companies is more pronounced than ever. This is apparent from the replies received to a letter sent out by the Committee on the Promotion of Student Interest in Coal Mining to over 120 coalmine operating officials. With that letter was forwarded a bulletin issued by the school of mineral industries of The Pennsylvania State College entitled ?Industrial Scholarships ? a Partnership of Industry and Education.? In that circular was outlined the need for trained men in the war and postwar world, and particularly as such demands pertain to the growth of the mineral industries.

Jan 1, 1943