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By B. Ramaswami

INTERNAL oxidation occurs readily in silver due to the rapid diffusion of oxygen in silver.' It has a marked effect on creep in polycrystalline silver2 and raises the critical resolved shear stress in single crystals of silver.3 However, the effect of oxygen on the work-hardening parameters of silver is not known. It is the aim of this paper to describe the effect of internal oxidation on the work-hardening characteristics of single crystals of silver and an Ag-0.1 at. pct A1 alloy. The materials used were: 99.99 pct Ag from Handy and Harman and 99.993+ pct A1 from Alcoa. Single crystals, 6 mm by 6 mm in cross section of silver and Ag-0.1 at. pct A1 of mo.5 orientation, i.e., the orientation with the Schmidt factor m = 0.5. were grown by the Chalmers technique.4 One set of specimens, referred to herein as oxidized specimens, was annealed at 940°C for 24 hr in a muffle furnace, in air, and furnace-cooled to room temperature. Another set of specimens, referred to as nonoxidized specimens, was annealed in oxygen-free helium at 940°C for 24 hr and furnace-cooled over a period of 7 hr to room temperature. The annealed single crystals were tested at room temperature in a floor-model Instron testing machine. The results are presented in Figs. 1 and 2. A

Jan 1, 1965

D. M. Riordan has been appointed a member of the Institute Com¬mittee of the Engineers' Reserve Corps movement. Our Committee, therefore, now consists of Henry S. Drinker, Chairman, Messrs. Arthur S. Dwight, Warren A. Wilbur and D. M. Riordan.

Jan 1, 1916

By E. F. Raffo

THE design of the Chuquicamata concentrator offered an unusual combination of problems, all of which had, in one way or another, a definite effect upon the final arrangement of all the equipment and necessary facilities. First of all, a remotely located project of this magnitude required careful selection of equipment with an adequate supply of replacement parts and in some cases necessitated stand-by spare equipment ready for immediate use. Fortunately, in the course of determining the proper flowsheet, in itself a prime factor in the concentrator design, it was possible to conduct numerous grinding and flotation tests at the Anaconda and Andes concentrators. As a result of these tests made under actual operating conditions, most of the major equipment best suited for treating the Chuquicamata ore efficiently was decided upon while preliminary design layouts were still being made. The design has been based primarily on the treatment of sulphide ore crushed to about 3/4 or 1 in. However, until the new sulphide crushing plant is completed it will be necessary to handle ore crushed to 3/8 in. in the existing oxide crushing plants and to some extent a mixed ore which has had its oxide copper content removed by leaching. This mixed ore, known as leached residue, will contain a certain amount of sulphuric acid from the leaching process which necessarily requires special protective measures. Several factors influenced the final location of the Concentrator. The only established fact known during preliminary design layout was the elevation of the dumping floor over the fine ore bin. This was predetermined by the desired level railroad grade across part of the existing tailing and leached residue dumps from the oxide plant to the bin. Next it was necessary that a site be chosen that would not require an excessively long haul from either the present oxide plant or the mine and in addition provide a fairly constant natural ground slope sufficiently wide to accommodate the length of the ultimate concentrator. The site as finally chosen to meet the foregoing restrictions provided a natural ground slope of 6 to 7 pct. This was excellent, especially in a region subject to earthquakes, as it assured that foundations of heavy equipment and footings for building and crane columns would rest on cut or undisturbed ground. However, this shallow slope, although having some definite advantages in the overall consideration of plant layout, resulted in the need for extensive studies in the general arrangement of equipment. Wasteful and excessive vertical drops had to be eliminated in the

Jan 1, 1952

By R. P. Rothwell

The milling of silver ores has arrived at a great degree of perfection in the mining districts of our Western States and Territories, and I hare thought the record of the practical results obtained at the present time, in a few of the principal districts, would prove of value arid interest to many of our members, both at home and abroad. An American silver mill is composed, in descending order from where the ore is dumped, of: 1st. A rock-breaker, usually of the Blake or Alden pattern; 2d. The battery of stamps, the number of which varies from 5 to 120, generally in batteries of 5 or 10 heads, so arranged that a single battery may stand while the others are running; 3d. The tanks where the crushed ore settles (if it is a met stamping-mill), or of a drying-floor if the crushing is done dry; 4th. Amalgamating pans ; 5th. Settling pans ; 6th. Agitators or pans in which mercury escaping in the tailings is caught; 7th. Blanket sluices, over which the tailings run, and where mercury and unamalgamated sulplides are saved. A reference to the engravings (see plate), which show one of the latest forms of an 80stamp silver-mill run by a turbine water-wheel, will show clearly the arrangement of the several parts. THE ONTARIO, UTAH, SILVER MILL. One of the best examples of a silver-mill, and at the same time one of the most successful concerns in the West, is the mill of the Ontario Silver Mining Company, near Salt Lake, in Utah. This mill treats the ore from the Ontario mine, ore which at present is very base, being composed of zinc, lead, and silver sulphides and silver chloride in a quartz gangue. This ore has become baser as the mine attained greater depth, though the vein holds its own, or rather increases, both in thickness and richness. The mill is managed in a skilful and economical manner, though the necessity for

Jan 1, 1880

By W. E. Bonini, E. A. Hickok

IN the course of an investigation directed toward expanding ground-water facilities in Essex and Morris counties, New Jersey, the Board of Water Commissioners of the city of East Orange authorized a seismic-refraction survey' for the purpose of de-lineating bedrock topography below unconsolidated overburden. Results of the survey were highly satisfactory and led to the preparation of a comparatively detailed bedrock contour map. Knowledge of the bedrock depth and configuration was an important aid in selection of sites for test drilling. The portion of the East Orange Water Reserve under consideration is in the flood plain of the Pas-saic River about 10 miles west of Newark, N. J. The flood plain is about 175 ft above mean sea level and is bordered by low hills rising to elevations of approximately 250 ft. The bedrock underlying the Water Reserve consists of sandstone and shale of the Triassic Brunswick formation and is covered everywhere by deposits of unconsolidated glacial outwash sand and gravel, lacustrine clay, and recent river silt as much as 150 ft thick. Yield of wells in the sandstone and shale averages 100 to 200 gpm. Since production wells constructed in the sand and gravel aquifer in the buried river valley shown on the contour map (Fig. 1) yield 300 to 1400 gpm, it was proposed to locate additional production wells in this buried valley, where the yields per well would be maximum. In 1939 and 1946 the East Orange Water Dept. had electrical-resistivity surveys made to determine depths to bedrock. From the resistivity data the exploration company prepared a bedrock contour map. A well field expansion program begun in 1955 utilized this information to locate sites for test wells along a predicted northward extension of the buried valley in which existing production wells are located. After several test wells (wells 201-205) had been drilled, it became apparent that the resistivity information was unreliable." For example, test well 201 recorded bedrock at a depth of 72 ft, whereas the resistivity depth determination was 130 ft. As a consequence, the test drilling program was temporarily suspended and a seismic survey was under- taken to determine the topography and extent of the buried valley known from well records to underlie the existing well field. In the first phase of this study, several seismic shot point locations were placed at sites where well logs had been obtained previously. This procedure is necessary in a new area to determine whether the seismic method is applicable and what degree of accuracy is to be expected. At the East Orange Water Reserve, depths obtained from the shot points near test wells 202, 203, and 204 were within 8 to 11 pct of the depths logged (Table I). With this assurance that accurate results could be obtained, additional seismic spreads were located on the Water Reserve. Using a portable refraction seismograph, in the fall of 1955 a crew of four men shot a total of 29 reversed seismic spreads in a period equivalent to six field days. Charges as heavy as 3 1b of 40 pct dynamite were necessary at a few places to overcome ground vibrations caused by traffic on nearby highways. At most other sites, a 1-1b charge was sufficient. Travel-time plots were made for all spreads, and depths and true velocities were calculated according to formulas for multiple sloping layers by Ewing, Woollard, and Vine.' The plot of spread 7 (Fig. 2) is typical of the short spreads in which bedrock was shallow—about 50 ft in this case. Where there were not enough arrivals through the bedrock to define the high velocity bedrock line, the spreads were lengthened. This was done by placing shots on line several hundred feet away from each end of the line of geophones. It was then possible to construct complete reverse plots for both short and extended shot points (see spread 27, Fig. 3). Four individual depths were calculated from each extended spread. Three and in some cases four seismic layers were observed. The surficial layer had a velocity range of 900 to 1200 fps, the lowest velocity recorded. This seismic layer is above the water table and is interpreted as recent river silt. The bedrock had the highest velocities, which ranged from 10,600 to 16,400 fps. Intermediate velocities ranged from 4500 to 6800 fps. In every case the intermediate layer was within

Jan 1, 1959

By J. V. W. REYNDERS

IN THE remarks which I am about to make concern¬ing the safety work of the Bureau of Mines, I want first of all to disengage myself from a disposition, which is frequently in evidence, to give spectacular emphasis to the hazards of mining operations. It is of the' utmost importance to the industrial welfare of our country that the enormous annual requirement of fuel be produced and be made available in our economic activities, with a minimum of distress and hardship. The safety of coal mining is a condition with which. we are all concerned in a fundamental way. And yet we should not rush to accept hastily conceived notions that laxity among employers in respect to safety measures exists to any outstanding degree. In fact in a large number of instances, the precautionary efforts of min¬ing companies, directed to the elimination of accidents are beyond all criticism, albeit the industry suffers in reputation from the carelessness of, its less effi¬cient constituents. The Bureau of Mines has been a leading influence in disseminating the doctrines of safety, in securing the cooperation of the miners themselves, and in stirring up ' the laggards, both among the employers and the employed. It is much to the interest of well-conducted mine operations that the industry, as a whole, observe safety regulations to the utmost.

Jan 1, 1925

By C. J. McHargue, J. C. Ogle

Lightly deformed columbiun single crystals which contained only parallel hoins or purullel and intersecting trains were annealed at 1000' and 1600"C. No re-crystallizntion occurred in specimens hawing only parallel twins. Only noncoherent twin boundaries nzipated at 1000°C but both coherent and noncoherent ones moved al 1600°C. Recrystallization occurred within a few minutes at twin intersections at 1000°C. The orientation 01 the recrystallized grains differed front that of both the matrix and deformation twins, but could he derired by (110) and/or(112) rotations. ALTHOUGH twinning in metals has been extensively studied, there have been no definitive studies of the annealing behavior of crystals containing deformation twins. Some effects observed after annealing deformation twins have been summarized by Cahn1 and Hall2. Any or all of these phenomena are observed: 1) The twins may contract so that the sharp edges of the lens become blunted, and eventually the twin may disappear entirely. 2) The twins may balloon out at an edge, giving rise to a large grain having the same orientation as the twin. 3) The specimen may recrystallize; i.e., new grains are nucleated and grow at the expense of the twins and the crystal immediately adjoining the twin. Such grains have orientations which are not present before. Contraction has been observed in iron,3 titanium,3, 4 beryllium,5 zinc,8, 7 Fe-A1 alloy,' and uranium.9 Long anneals at high temperatures are required to have any appreciable effect in these metals and only thin twins are absorbed. Lens-shaped twins are absorbed from the edges: the thin, almost parallel-sided twins are usually punctured in several places and each piece contracts independently. Absorption is very gradual and no sudden cooperative jumps have been observed. The expansion of a twin into a larger grain of identical orientation is unusual, but such growth has been observed in iron,"'" zinc,6 and uranium." Crystals which have been deformed simultaneously by slip and twinning recrystallize first in the area adjacent to the twin. New grains appear faster where the twins intersect: but isolated twins, especially if thick, can also give rise to new grains. This type of recrystallization occurs in zinc.6, 7, 12, 13 and beryllium.14 Reed-Hill noted, in a single crystal of magnesium, the nucleation of a recrystallized grain at a twin intersection which had the same orientation as the second-order twin and which grew into the highly strained matrix.15 Short-time annealing has been reported to cause no change in the deformation twins in vanadium,16 columbium, 17, 18 tantalum,19 tungsten,'' and zinc.7 The purpose of this investigation was to note the effects of annealing on the coherent and noncoherent boundaries of deformation twins in columbium and to locate the nucleating sites for recrystallization. The orientation relationships, which the new recrystallized grains have with the parent crystal and the deformation twins, were also determined. EXPERIMENTAL PROCEDURE Single crystals of columbium were obtained by cutting large grains from electron-beam-melted buttons which contained 10 to 50 ppm C, 10 to 100 ppm O,, 1 to 10 ppm H2, and 10 to 15 ppm N2. The crystals were hand-ground and chemically polished until all grain boundaries were removed. The specimens were mounted in an epoxy resin and a face of each crystal was mechanically polished on a Syntron polisher using Linde A and then Linde B polishing compounds. After all faces were mechanically polished, the crystal was electrolytically polished to remove all distortion due to cutting and grinding. Laue photographs were taken of all faces of the crystals to determine the quality and orientation of each crystal. The crystals were compressed about 10 pct at -196 C in a specially constructed compression cage with an Instron tensile machine. Each crystal was separated from the top and bottom anvils by teflon films which acted as a lubricant. With the specimen crystal in position, the entire cage was cooled to -196°C by being submerged in a Dewar containing liquid nitrogen. The crystals were compressed at a rate of 0.02 in. per min and the load was recorded on a strip-chart recorder. After deformation the crystals were mechanically polished on 600-grit paper and Pellon cloth with Linde A and Linde B polishing compounds. The crystal faces were chemically polished and then etched. The twin planes were identified metallographically from an analysis of the twin traces on two surfaces. Annealing was carried out by placing each crystal in a columbium bucket made from the same electron-beam-melted material as the crystal itself and suspending the bucket by a tantalum wire in a quartz tube. After a vacuum of 10-7 Torr was attained, a furnace at 1000" or 1600 C was raised into position and the crystals held for various lengths of time. The crystals were repolished and etched after annealing to remove any surface contamination. Approximately 0.010 in. was removed during this process. The resulting surface was examined metallographically for microstructural changes due to annealing. A microbeam Laue camera mounted on a Hilger Micro-focus X-ray unit was used to determine the Orientstions of the recrystallized grains. This X-ray micro-beam camera had a 0.002-in.-diam collimator and incorporated the ideas of both and and chisWik21 and Cahn.22

Jan 1, 1967

By Joseph Gurland

EVERAL carbide-cobalt compositions were pre-^-5 pared for the purpose of determining the transverse rupture strength of various carbide-binder systems. The binder content was held at 10 and 37 volume pct Co, so as to be representative of low and high bjnder compositions. The carbides used, WC, Tic, TaC, CbC, VC and ZrC, were selected on the basis of availability, knowledge of their properties, and small solid solubilities in the binder metal at room temperature. The methods of preparation and carbon analysis of the carbides are summarized in Table I. The carbides with cobalt added were ball milled, pressed, and sintered. vacuum sintering was used throughout, except for the WC-Cs alloys, which were sintered in hydrogen. The sintering temperatures ranged from 2500" to 2750°F for the low binder alloys and from 2300" to 2550°F for the high binder alloys. Compositions and properties of the sintered com- pacts are presented in Table 11. For the transverse rupture strength, the average and range of the five best samples of each alloy are listed. Discrepancies between the actual and theoretical densities are attributed to carbon deficiencies in some samples. The theoretical densities were calculated by assuming mixtures of carbides of stoichiometric compositions and cobalt. Representative microstructures are shown in Figs. 1 to 6. The porosity was A-2 or better' in all alloys except those with ZrC. A grain size of about 3 p was

Jan 1, 1958

By J. E. Lawrence

Copper-decorated lattice disorders in silicon have been analyzed by electron transmission microscopy, chemical etching, and P-N junction reverse current measurements before and following different gettering treatments. Lattice disorders acted as the nucleating sites for copper precipitation. Copper precipitates in silicon resist chemical etching, absorb electron beams more than silicon, and cause excess reverse currents. Totally gettered disorders will chemically etch rapidly, be transparent to electron beams at extinction contrast, and not contribute to excess reverse currents. Three different gettering procedures were performed to determine the effectiveness of different EXTRANEOUS metal contamination can alter the minority carrier lifetime and resistivity of bulk silicon as well as cause excessive reverse currents in semiconductor devices. Previous workers have reported such activity for gold,1,2 copper,'-* iron,' and rnanganese.2,5 Gettering is a method employed to render these impurities electrically inactive. However, some property of the junction-degrading metals prevents gettering procedures from being wholly reliable. The comparative effectiveness of gettering with different agents has been the topic of earlier publications.2,3,6-11 Two mechanisms for gettering metallic impurities have been proposed: the distribution coefficient mechanism by Thurmond and Logan7 and the compound formation mechanism by Goetzberger and Shockley.2 Both of these models evolved from data gettering mechanisms. First, phosphorus was allowed to enter a protective SiO2 film but remain away from the Si-SiO2 interface to test the effectiveness of the compound formation gettering mechanism. Second, phosphorus was allowed to enter the backside of silicon wafers to test the effectiveness of the lattice strain gettering mechanism. Finally, nickel was diffused into the backside of silicon wafers to test the effectiveness of the distribution coefficient gettering mechanism. In each case, copper precipitates dissolved as a result of the gettering treatment. Tightly packed precipitates will resist gettering more than loosely packed copper precipitates. acquired by the electrical analyses of gettered semiconductor materials. An electrical analysis, however, cannot identify the fate of the gettered metals. The radiotracer technique has recently been applied to determine the redistribution of metals following different gettering treatments.3,9,10 The spatial resolu tion of the radiotracer technique prevented the analysis of metal precipitates which contribute to the excessive reverse currents of P-N junctions. The gettering processes employed by the earlier workers, almost without exception, allowed the gettering agent to enter the silicon lattice. This procedure makes it quite difficult to differentiate between the distribution coefficient and the compound formation mechanisms. The metallographic analysis of gettered copper precipitates discussed in this work supplements the earlier work by obtaining direct evidence of silicon lattice defects decorated with copper before and following different gettering treatments. The effectiveness of a process which restricts the gettering agent, phosphorus, to a dielectric film and thus away from the silicon lattice is discussed in addition to the ef-

Jan 1, 1969

By J. R. Long, C. E. Armantrout, A. H. Roberson, T. R. Graham, R. S. Dean

THE general program of the Federal Bureau of Mines on the study of alloys made with electrolytic manganese has been extended to copper-manganese-aluminum alloys. The initial results of the work are presented in this report and concern a determination of the mutual solubilities of these three metals to form the alpha solid solution. The principal studies of this system, reported in the literature, have been focused on the Heusler alloys containing 10 to 30 per cent Mn with 9 to 15 per cent Al. These investigations concern the ferromagnetic properties and the determination of the crystallization contours, with little emphasis on the phases present in the solid state outside of this area. Heusler1 recognized a breakdown of the beta solid solution of the magnetic alloy, which he says decomposes into the alpha, beta, and gamma phases of the copper-aluminum system, somewhat modified by the presence of manganese. Rosenhain and Lantsberry2 examined alloys ranging up to 10 per cent Mn and io per cent Al but were unable to reach definite conclusions concerning the phase boundaries in that area. Krings and Ostmann3 made magnetic studies and examined the system by thermal analysis. They present contours of the liquidus surface but do not place any of the phase boundaries. Corson4 [ ] has drawn a hypothetical boundary for the alpha field with few data to support such construction. The binary systems involved have received considerable attention by numerous investigators, and their general features are well established. The hopper-aluminum system (Fig, I) has been thoroughly examined by Stockdale,5 who places the limit of solubility of aluminum in copper at 7.4 per cent at the liquidus and 9.5 per cent at room temperature. Smiths established the eutectoid temperature at 570°C. by a study of isothermal decomposition of the beta phase. The copper-manganese system (Fig. 2) has been recently reviewed by Dean and co-workers.7 Using high-purity alloys, they place the solubility of alpha man-

Jan 1, 1946

By R. S. Dean. J. R. Long T. R. Graham, Roberson A. H., Armantrout C. E.

The general program of the Federal Bureau of Mines on the study of alloys made with electrolytic manganese has been extended to copper-manganese-aluminum alloys. The initial results of the work are presented in this report and concern a determination of the mutual solubilities of these three metals to form the alpha solid solution. The principal studies of this system, reported in the literature, have been focused on the Heusler alloys containing ro to 30 per cent Mn with 9 to 15 per cent Al. These investigations concern the ferromagnetic properties and the determination of the crystallization contours, with little emphasis on the phases present in the solid state outside of this area. Heuslerl recognized a breakdown of the beta solid solution of the magnetic alloy, which he says decomposes into the alpha, beta, and gamma phases of the copper-aluminum system, somewhat modified by the presence of manganese. Rosenhain and Lantsberry2 examined alloys ranging up to 10 per cent Mn and 10 per cent A1 but were unable to reach definite conclusions concerning the phase boundaries in that area. Krings and Ostmann3 made magnetic studies and examined the system by thermal analysis. They present contours of the liquidus surface but do not place any of the phase boundaries. Corson4 has drawn a hypothetical boundary for the alpha field with few, data to support such construction. The binary systems involved have rcceived considerable attention by numerous investigators, and their general features are well established. The copper-ahminum system (Fig. I) has been thoroughly examined by Stockdale,5 who places the limit of solubility of aluminum in copper at 7.4 per cent at the liquidus and 9.5 per cent at room temperature. Smith6 established the eutectoid temperature at 570°C. by a study of isothermal decomposition of the beta phase. The copper-manganese system (Fig' ') has been recently reviewed by Dean and CO-WorkersS.7 Using high-purity alloys,

Jan 1, 1947

By Armantrout C. E., R. S. Dean. J. R. Long T. R. Graham, Roberson A. H.

The general program of the Federal Bureau of Mines on the study of alloys made with electrolytic manganese has been extended to copper-manganese-aluminum alloys. The initial results of the work are presented in this report and concern a determination of the mutual solubilities of these three metals to form the alpha solid solution. The principal studies of this system, reported in the literature, have been focused on the Heusler alloys containing ro to 30 per cent Mn with 9 to 15 per cent Al. These investigations concern the ferromagnetic properties and the determination of the crystallization contours, with little emphasis on the phases present in the solid state outside of this area. Heuslerl recognized a breakdown of the beta solid solution of the magnetic alloy, which he says decomposes into the alpha, beta, and gamma phases of the copper-aluminum system, somewhat modified by the presence of manganese. Rosenhain and Lantsberry2 examined alloys ranging up to 10 per cent Mn and 10 per cent A1 but were unable to reach definite conclusions concerning the phase boundaries in that area. Krings and Ostmann3 made magnetic studies and examined the system by thermal analysis. They present contours of the liquidus surface but do not place any of the phase boundaries. Corson4 has drawn a hypothetical boundary for the alpha field with few, data to support such construction. The binary systems involved have rcceived considerable attention by numerous investigators, and their general features are well established. The copper-ahminum system (Fig. I) has been thoroughly examined by Stockdale,5 who places the limit of solubility of aluminum in copper at 7.4 per cent at the liquidus and 9.5 per cent at room temperature. Smith6 established the eutectoid temperature at 570°C. by a study of isothermal decomposition of the beta phase. The copper-manganese system (Fig' ') has been recently reviewed by Dean and CO-WorkersS.7 Using high-purity alloys,

Jan 1, 1947

By S. K. Basu, H. H. Kellogg

THE physical-chemical behavior of the system Pb-S-0 is of prime importance to the understanding of lead smelting processes, yet little accurate information is available on either equilibrium or kinetic behavior in this system. This paper is the first report of a program designed to fill gaps in our knowledge of this system. In the total ternary Pb-S-0, the region of greatest metallurgical interest is that bounded by the compositions Pb-PbS-PbS0,-PbO-Pb. Systems richer in sulfur, or richer in oxygen,* than those essentially pure SO2. This conclusion follows from the fact that all systems are in a highly reduced state, since either PbS or Pb is a constituent of all the equilibria. The content of 02, SO3, S2, S6, S8, and so forth, can be shown to be negligible compared to SO, in all such systems.* corresponding to this region can only be obtained at gas pressures exceeding 1 atm, a condition seldom met in lead smelting practice. Not only is the present study limited to condensed phases within this portion of the total system, but it is limited to temperatures at which all phases are pure solids, except for lead, which is liquid. In this limited system the following seven condensed phases are known to exist: Pb(l), PbS(c), PbO(c), PbSO,(c), PbSO,•PbO(c), PbSO4 • 2PbO(c), and PbSO, -4PbO(c). PbO exists in two crystal modifications,' but only the high-temperature yellow form is considered here. Schenck and co-workers2-4 reported the compound PbSO4 3Pb0 to be stable at high temperature, but the more recent work of Lander,5 and the present work, prove that the tetra-basic sulfate, rather than the tri-basic sulfate is stable. Fig. 1 shows the composition diagram for the binary PbO-PbSO2, based primarily on the work of Lander. In this study the univariant boundaries and invariant points existing among these seven condensed phases and the gas phase have been determined. In a ternary system, the phase rule indicates that an invariant point involves the simultaneous equilibrium of five phases—four condensed phases and the gas phase. A univariant relation involves four phases—three condensed phases and the gas phase. The gas phase in the systems studied is The following stable univariant equilibria between SOz and the condensed phases were identified: (a) PbS + 7PbS04 = 4(PbSO, - PbO) + 4SO2 (b) PbS + l0(PbS04 • PbO) = 7(PbSO4- 2PbO) + 4SO2 (c) PbS + 8(PbSO4 • 2PbO) = 5(PbSO4 . 4PbO) + 4SO2 (d) Pb + PbSO, • 4PbO = 6PbO + SO2 (e) 3PbS + PbSO4 . 4PbO = 8Pb + 4SO2 (f) 3PbS + 16(PbS04 PbO) = 7(PbSO4 . 4PbO)+ 12SO2 (g) 2PbS + PbSO,2PbO = 5Pb + 3SO2 (h) Pb + 3(PbSO4 . 2PbO) = 2(PbSO,. 4PbO) + SO, Of these eight univariant equilibria, five were measured in this work (a, b, c, d, and g) and the behavior of the other three (e, f, and h) was calculated by thermodynamic analysis of the measured data. Two invariant points were found corresponding to simultaneous equilibria as follows: Point 1: PbS, PbSO4PbO, PbSO4.2PbO, PbSO, - 4PbO, and SO2 Point 2: Pb, PbS, PbSO, . 2PbO, PbSO, - 4PbO, and SO2, From the measurements it was also possible to calculate the thermodynamic properties of the three basic sulfates of lead at 298.16°K. EXPERIMENTAL Apparatus—The experimental method consisted of the measurement of the gas pressure exerted by a given reaction mixture at a given temperature. An iridium crucible was used to contain the reaction mixture. There was no evidence of attack of the iridium,* but after use at high temperature for a week

Jan 1, 1961

By J. B. Newkirk

IN 1939 Bitter and Kaufmann1 suggested that iron, precipitating from a copper-rich, Cu-Fe solid solution, appears initially as coherent particles of r-Fe which transform to the body-centered-cubic form of iron when the alloy is cold worked. Since then there has been considerable discussion, supported only by indirect evidence, regarding the validity of the concept. For example, Reekie, Hutchison, and Hether-ington2 interpreted the changes in electrical resistance accompanying the aging of Cu-Fe specimens in terms of a coherent 7-Fe precipitate which transformed to the incoherent a-phase during long aging or cold working. Greninger- ound that Cu-Fe alloys which had been water quenched from 1050" and then held at 650°C for 3 hr changed from weakly to strongly ferromagnetic as the aged wire was subsequently cold worked. He also found diffraction lines corresponding to body-centered-cubic iron in Debye-Scherrer patterns given by aged and worked specimens but lines corresponding to only one face-centered-cubic phase in specimens which had been aged but not worked. Knoppwost,' and later Cech and Turnbull,5 found that aged Cu-Fe specimens showed a slight increase in ferromagnet-ism after they had be? cooled in liquid nitrogen. Very recently Denney6 followed the kinetics of the precipitation reaction as indicated by the saturation magnetization, hardness, and diffuse X-ray effects. The experimental results reported by all of the authors mentioned above are readily explained in terms of the Bitter and Kaufmann concept. However, most of the evidence is indirect when used to define the structural changes involved. It was the aim of the present investigation to determine the mechanism of precipitation of iron from a Cu-Fe solid solution in the light of available published information and with additional new and more direct experimental data. Experimental Method At 1060°C copper will contain up to 3 atomic pct Fe in equilibrium solid solution.7 The solvus slopes rapidly toward lower iron concentration, so that at 600°C only about 0.5 pct Fe remains in solution at equilibrium. Below the eutectoid temperature (850°C), the iron-rich phase in equilibrium with the copper-rich solid solution consists of body-centered-cubic a-Fe. Above 850 °C the equilibrium iron-rich phase is face-centered-cubic r-Fe. The alloy to be studied was made by melting electrolytic iron and OFHC copper by induction under vacuum in an Alundum-lined crucible. The metal was held molten for about 5 min, after which time the power was turned off and the crucible was tipped about 70" to promote directional solidification. The resulting ingot, containing 2.5 wt pct Fe by analysis, was clean, large grained, and free of gross segregation. Slices % in. thick were cut from the ingot, rolled to 1/8 in. in thickness, homogenized in hydrogen at 1060°C for 24 hr and, finally, quenched in cold water. Specimens for all subsequent tests were made from these slices. Squares measuring about 1 cm on a side were cut from the slices to make specimens for studying hardness and microstructure. Wires (0.020 in.) for the Debye-Scherrer survey were drawn from 1/8 in. sq rods which had been cut from the homogenized slices. Large crystals for observing diffuse X-ray diffraction effects were prepared by mechanically

Jan 1, 1958

HENRY A. VEZIN, Denver, Colo. (communication to the Secretary, February, 1897): I have read Mr. Austin's paper with considerable interest, more especially as the designing and study of such works have been an attractive occupation for me during the last twenty-five years. Mr. Austin says that a " plant on a terraced site has generally been considered the most advantageous," and also that " many advocate a level site," while he himself " is disposed to advocate a modification of the latter plan, utilizing an extended surface with a moderate slope."* Among the advocates of the terraced sites as against level ones, I do not recollect ever meeting a metallurgist who had even made an attempt to plan his works for level ground, or who had, in a lucid interval, figured how much he gained or lost by one or the other method. The average metallurgist starts with the assumption that it is rational to conduct his material down hill because its movement is aided by gravity, while to elevate ore or furnace-material by machinery he vaguely believes to be not alone wrong in principle, but also unnecessarily expensive. Let us look into the expense of elevating and see whether it really is prohibitory of the successful operation of smeltingworks on a level site. Hoisting or elevating material in the

Jan 1, 1897

By B. E. Eakin, A. L. Lee

Atmospheric pressure viscosity values For light hydrocarbons were calculated by a simple mixing rule based on the Sutherland constants for pure components. This method was further extended so that the atmospheric pressure viscosity of a mixture may be calculated based on the molecular weight information only. INTRODUCTION A proven method for estimating the gas-phase viscosity of a mixture is the one by Herning and zipperer.l This mixing rule has the following form: One method for calculating the pure component viscosity i is the Sutherland equation,2 which has the following form: The Sutherland constants B and S are determined from experimental data. A set of Sutherland constants for light hydrocarbons based on the data of several investigators3-5 is presented in Table 1. APPLICATION The Herning-Zipperer equation and the Sutherland equation were used to obtain an equation for calculating the gas-phase viscosity of light hydrocarbons. This equation has the form, Eq. 3 was used successfully in the study of methane-n-butane mixtures.6 Further analysis indicated that the Sutherland constants are a function of molecular weight.7 The gas-phase viscosity may be calculated based on molecular weight information only. The following equation was developed: The atmospheric pressure viscosity of ethane, propane, n-butaneand four methane-propane mixtures calculated on the basis of Eq. 6 are compared with the data of other investigators in Tables 2, 3, 4 and 5, respectively. A plot of atmospheric pressure viscosity vs molecular weight based on Eq. 6 is presented in Fig. 1.

Jan 1, 1965

By Sandford S. Cole, John S. Breitenstein

The recovery of over 80 pct of the vanadium values in titaniferous magnetite from Maclntyre Development,Tahawus, N. Y., was accomplished by an oxidizing roast with Na2O3-NaCI addition. Process description is given for leaching of roasted ore and precipitation of V2O5 and Cr2O8 from leach liquor. THE exploration and development of the Mac-Intyre orebody at Tahawus, N. Y., by the National Lead Co. provided a source of vanadium. Analyses of various composite sections of the drill cores of the MacIntyre orebody were made to establish whether or not the vanadium was constant throughout. Ten drill cores were sampled as 50 ft sections, crushed, and a portion magnetically concentrated. The head and concentrate were analyzed for total iron and vanadium. The results on the concentrates indicated that the vanadium is associated with the magnetite and maintains a close ratio to the iron content. The nominal ratio of 1:25:140 of V: TiO2:Fe was found to exist in the concentrates. Typical value for the vanadium in the magnetite both from laboratory concentration and mill production is 0.4 pct. The recovery of vanadium from the magnetite was investigated in 1942 to 1943. The research program encompassed both laboratory and pilot-plant work on sufficient scale to provide adequate data to establish the feasibility of a full scale plant. The recovery of vanadium from various ores has been reported in the literature and has been the subject of many patents. The literature dealing with recovery from titaniferous ore by roasting is quite limited. Roasting with alkaline sodium chloride, sodium chloride or alkaline earth chlorides, and sodium acid sulphate have been claimed in various processes as effective means.1-8 The reduction of the ore, followed by acid leaching, was another method proposed.'-' "he use of various pyrometallurgical processes for recovery of vanadium in the metal or in the slag has also been extensively investigated, but the results had little application to the problem."-" The separation of vanadium values from subsequent leach liquors and vanadium-bearing solution has been the subject of a considerable number of papers and patents. The most practical is by hydrolysis at a pH of 2 to 3 by acidifying a slightly alkaline solution. Data on solubility of V²O5 and V2O4 in water and in dilute sulphuric acid indicated a solubility of 10 g per liter in water.'" Laboratory Results Magnetite Analysis: Adequate stock of magnetite was provided so that the laboratory and pilot-plant operation was on ore representative of the mill production. The ore was analyzed chemically and examined by petrographic methods to ascertain whether the vanadium was present in combined state or as an interstitial component between grain boundaries. No evidence was obtained which would indicate that the vanadium was in a free state as coulsonite.15 The analysis of the ore was as follows: Fe²O³, 47.4 pct; FeO, 29.1; TiO,, 10.1; V, 0.40; and Cr, 0.2. The screen analysis of the ore on the as-received basis was: -20 +30 mesh, 28.8 pct; —30 +40, 18.9; -40 +50, 9.7; -50 +60, 15.1; -60 4-100, 5.9; -100 + 200, 11.2; -200 +325, 3.7; and -325, 7.2. Roasting Conditions: The prior practice indicated that a chloridizing roast with or without an alkaline salt had been effective on other titaniferous magnetites. On this basis roasts with additions of sodium chloride, sodium carbonate and mixtures thereof were investigated varying the roasting temperature between 800" and 1100°C. Since the ore had shown no segregation or concentration of vanadium, the influence of particle size on the freeing of vanadium by the reagents during roasting was determined. The initial work was on silica trays in an electric resistance furnace with occasional rabbling of the charge. Subsequently, the roasting was carried out in a small Herreshoff furnace to establish the influence of products of combustion on the recovery of the vanadium. The laboratory tests showed that this ore required an alkaline chloridizing roast, in conjunction with a reduction in particle size to less than 200 mesh. When roasted in air at 900 °C with 5 pct NaCl and 10 pct Na2CO³, over 80 pct recovery of the vanadium was attained as a water-soluble salt. The presence of alkaline earth elements gave detrimental effects and care had to be exercised to avoid any contamination of the ore or roast product by such materials. The solubilization of vanadium under the various conditions is given in a series of curves in Figs. 1 to

Jan 1, 1952

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 J. Gurland

The effects of variations of carbon content on the constitution and properties of sintered WC-Co alloys were studied. The grain growth of tungsten carbide during sintering was measured and it was shown that it takes place mainly by solution and reprecipitation of the carbide in and from the binder at the sintering temperature. It was found that the decomposition of W3C03C by carburization during sintering is responsible for the formation of very large grains. THE properties of sintered WC-Co alloys are critically dependent upon their final composition and structure. Slight changes of cobalt and carbon contents and small variations of grain size result in marked changes of mechanical properties and performance of products. Previous investigators have studied the microstructure as a function of composition' and have dealt with the influence of cobalt upon properties.' The present work is concerned with the effect of carbon content upon constitution, microstructure, and grain growth during sintering, as well as upon the physical properties of sintered compacts. Phase Boundaries at the Sintering Temperature The WC-Co section through the ternary diagram W-Co-C has been studied by Wyman and Kelley,' Takeda,V andford and Trent," and Rautala and Norton." Two phases, namely WC and a cobalt-rich solid solution (P), appear in the sintered structure if the carbon composition corresponds very nearly to the theoretical carbon content of WC (6.12 pct C). But small deviations from the ideal carbon content will bring about the occurrence of either graphite or the double carbide W,Co3C (7) . The 7 phase was long believed to be metastable, this conclusion being based mainly on the work of Takeda. More recent studies have shown that it is a stable phase of the ternary system,"5 but the actual phase boundaries have not been established and there has been some discussion as to whether or not the 7 phase occurs at some stage of sintering in the fully carburized alloys." In view of this uncertainty it was thought advisable to undertake an investigation of the phases present during the sintering of WC-Co alloys. Commercially available tungsten, cobalt, and carbon powders were used in the present study. A typical analysis of impurities in a sintered compact is reported in Table I. The desired carbon compositions were attained by varying the amount of carbon added to the tungsten during carburization and controlling the composition during sintering by packing the compacts into beds of mixed alundum-carbon powders of suitably selected ratios. The alloys were sintered in a hydrogen tube furnace at 1400°C, then brought to equilibrium at the temperature under investigation and quenched in water. The high temperature phases were identified by metallographic and X-ray diffraction techniques. The samples were etched with a 10 pct solution of alkaline potassium ferricyanide. The phase boundaries, established by metallo-graphic examination, are shown in Fig. 1, which is a vertical section through the ternary diagram at 16 pct Co. The temperatures of the invariant planes, at 1298" and 1357°C were established by Rautala and Norton. The vertical section shows that the three-phase field, WC + 7 + L, extends into the two-phase field, WC + L, but does not include the stoichiometric composition of WC. In practice this means that the 7

Jan 1, 1955

IN accordance with a programme arranged by a committee of the Institute, consisting of Mr. William P. Shinn, of St. Louis, chairman, and Mr. Joseph D. Weeks, of Pittsburgh, secretary, the member's of the Institute, with their ladies and invited guests, assembled in Chicago on Sunday morning, August 22d. A special train, provided by the Chicago and Northwestern Railway,. left Chicago on Monday morning at 7.50 o'clock, and conveyed the party to Marquette, arriving at 9 o'clock P.M. Here the steamer Northern Queen, which had been chartered by the committee for the accommodation of the Institute, was in waiting, and the members and ladies at once took up their quarters on the boat. EXCURSIONS IN THE MARQUETTE IRON REGION. Local Committee. EXECUTIVE. -J. C. Morse, chairman; C. Y. Osburn, secretary ; D. F. Wadsworth, treasurer; C. H. Hall, H. Merry. RECEPTION.-S. P. Ely, J. P. Pendill, E. Breitung, W. F. Swift, A. P. Swineford, J. C. Fowle, C. G. Griffey. TRANSPORTATION.-Samuel Schoch, D. Morgan, D. H.. Merritt, J. Pickands. FINANCE.-Peter White, A. W. Maitland, W D. Rees, E. R. Hall. EXCURSIONS.-W. E. Dickinson, H. A. Burt, A.. Kidder, C. E. Wright. REFRESHMENTS.-J. Q. Adams, H. H. Stafford, Joseph Kirkpatrick, D. H. Bacon. On Tuesday the iron mines in the vicinity of Negaunee and Ishpeming were visited, transportation being provided by special trains on the Marquette, Houghton and Ontonagon Railroad. In the morning the McComber, South Jackson, and Jackson mines were inspected, and in the afternoon the Cleveland, New York, Lake Superior, and Barnum mines. Dinner was provided at Negaunee, and gracefully served by, the ladies of the town. In the evening the first session of the Institute was held in the saloon of the steamer. The President, William P. Shinn, of St. Louis, congratulated the Institute on the happy consummation of the wishes of its members to have a meeting on Lake Superior. After tedious and baffling negotiations arrangements had been com-

Jan 1, 1881