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By Frank Firmstone

IN 1871, two furnaces at the Glendon Iron Works, which had been blown out on account of the "coal strike," were altered from the open-top plan with side flues for collecting the gas, to closed tops with cup and cone. In one furnace the suppression of the side flues permitted a considerable alteration in the profile, but in the other (No. 5) no change in this respect was made; the side flues were simply bricked up and new ones cut through the sides close to the top. This furnace was in blast over four years, and we can, therefore, form a pretty good idea of the effect of the alterations on the furnace process. The principal dimensions are; Height 72'; greatest diameter, 18'; diameter at tuyeres, 8'; diameter of top, 10'; diameter at stock line (point at which the top of the materials is kept), 11'; cubic contents, 11,900 cubic feet. The table below shows the average results for periods of twenty-six weeks each. 1st, of the open-topped furnace; 2d, of the furnace with the first charger used, which was an ordinary cup and cone (diameter of cone 5' 2") 3d, with the charger used ever since, a "double" cone 7' 5" diameter outside, having a central opening 3' in diameter. The diagram (Plate II) shows the daily variations, in the grade of the irons for the same periods.* * In calculating the average grade of each day's iron, each twelve hours was taken by itself whenever more than two kinds of iron were made in the 24 hours, and the diagram drawn accordingly. By counting, it will be found that there were more such days with the single cone than with the "double" cone, and more with this than with the open top. † Anthracite.

Jan 1, 1876

By H. H. Kaveler, W. R. Evans, Jack Tarner

The geological features, development history and engineering detail of the Shuler Field and the results of approximately two years of unitized operation of the Shuler Jones Sand Pool, were discussed in a prior publication.' The purpose of this paper is to present the results of pressure maintenance in the Shuler Jones Sand Pool after nine years of unit operation. GENERAL INFORMATION The Shuler Jones Sand Pool is located in and about Section 18, Township 18 South, Range 17 West, Union County, Ark. The pool was discovered .in September, 1937, unitized in February, 1941, and subjected to gas injection operations in July, 1941. Water was first returned to the reservoir in July, 1944. The reservoir is an anticlinal trap covering about 4,000 acres. The 154,000 acre-ft of sandstone initially consisted of approximately 150,000 acre-ft of productive oil zone and 4,000 acre-ft of gas-cap. The average depth of production is 7,400 ft. Maximum closure of the reservoir is 135 ft and the oil column lies between a gas-oil contact at -7,270 ft and a water-oil contact at -7,370 to -7,380 ft. The field is approximately four miles long. east and .west, and one and one-half miles wide. The sand grains are angular and vary from fine to medium size. The porosity of the sandstone averages 20.2 per cent. The specific permeability averages 400 md. Some zones have as high as 30 per cent porosity and specific permeability of 4,000 md. The reservoir rock is not uniform in character but consists of sandstone zones interspersed with shale. The variation in rock characteristics is evident in the electric log and core analyses presented in the original publication. Asphalt present in the pore space of the sandstone limited the reservoir to the southeast and apparently blocked any encroachment of water from that direction. The initial reservoir pressure at a subsea depth of 7,300 ft was 3,520 psi. The reservoir temperature was 198ºF. Initially, the solution gas volume was 765 cu ft per bbl and the reservoir volume factor was 1.45. The gas solubility and formation-volume-factors of the reservoir liquid are related with reservoir pressures above 300 psi as follows: Solution gas, cu ft per cu ft, S = 0.0334 P + 18.65 Formation volume factor of reservoir oil, FVF = 8.0 x 10 -5 P + 1.168 Gas volume factor, standard cu ft of gas equivalent to one cu ft of gas at reservoir conditions of temperature and pressure, F = .062 P - 4 Pressure (P) measured in psia. The equation for the gas volume factor presented above is based on a direct measurement of a sample of the gas and is a correction of that used in the original paper. The gravity of the oil produced is from 32 to 34" API. CALCULATION OF INITIAL OIL IN PLACE The Jones Sand production history is interesting because it lends itself to analysis by material balance. Production statistics from discovery of the Jones Sand through 1949 and material balance calculations of the initial stock tank oil in place are shown in Table I. The usual procedure in testing the application of material balance calculations is to compute the apparent initial volume of oil in place, using production and pressure information obtained at different time periods. If the apparent oil in place volumes computed increase with successive time periods, water encroachment is indicated and approximations must be mads to correct for its influence. The first requirement in utilizing such calculations is reliable reservoir pressure, accumulated gas, oil and water production, and PVT data. Calculations of apparent oil in place in the Jones Pool, based on field data

Jan 1, 1951

By W. R. Evans, H. H. Kaveler, Jack Tarner

The geological features, development history and engineering detail of the Shuler Field and the results of approximately two years of unitized operation of the Shuler Jones Sand Pool, were discussed in a prior publication.' The purpose of this paper is to present the results of pressure maintenance in the Shuler Jones Sand Pool after nine years of unit operation. GENERAL INFORMATION The Shuler Jones Sand Pool is located in and about Section 18, Township 18 South, Range 17 West, Union County, Ark. The pool was discovered .in September, 1937, unitized in February, 1941, and subjected to gas injection operations in July, 1941. Water was first returned to the reservoir in July, 1944. The reservoir is an anticlinal trap covering about 4,000 acres. The 154,000 acre-ft of sandstone initially consisted of approximately 150,000 acre-ft of productive oil zone and 4,000 acre-ft of gas-cap. The average depth of production is 7,400 ft. Maximum closure of the reservoir is 135 ft and the oil column lies between a gas-oil contact at -7,270 ft and a water-oil contact at -7,370 to -7,380 ft. The field is approximately four miles long. east and .west, and one and one-half miles wide. The sand grains are angular and vary from fine to medium size. The porosity of the sandstone averages 20.2 per cent. The specific permeability averages 400 md. Some zones have as high as 30 per cent porosity and specific permeability of 4,000 md. The reservoir rock is not uniform in character but consists of sandstone zones interspersed with shale. The variation in rock characteristics is evident in the electric log and core analyses presented in the original publication. Asphalt present in the pore space of the sandstone limited the reservoir to the southeast and apparently blocked any encroachment of water from that direction. The initial reservoir pressure at a subsea depth of 7,300 ft was 3,520 psi. The reservoir temperature was 198ºF. Initially, the solution gas volume was 765 cu ft per bbl and the reservoir volume factor was 1.45. The gas solubility and formation-volume-factors of the reservoir liquid are related with reservoir pressures above 300 psi as follows: Solution gas, cu ft per cu ft, S = 0.0334 P + 18.65 Formation volume factor of reservoir oil, FVF = 8.0 x 10 -5 P + 1.168 Gas volume factor, standard cu ft of gas equivalent to one cu ft of gas at reservoir conditions of temperature and pressure, F = .062 P - 4 Pressure (P) measured in psia. The equation for the gas volume factor presented above is based on a direct measurement of a sample of the gas and is a correction of that used in the original paper. The gravity of the oil produced is from 32 to 34" API. CALCULATION OF INITIAL OIL IN PLACE The Jones Sand production history is interesting because it lends itself to analysis by material balance. Production statistics from discovery of the Jones Sand through 1949 and material balance calculations of the initial stock tank oil in place are shown in Table I. The usual procedure in testing the application of material balance calculations is to compute the apparent initial volume of oil in place, using production and pressure information obtained at different time periods. If the apparent oil in place volumes computed increase with successive time periods, water encroachment is indicated and approximations must be mads to correct for its influence. The first requirement in utilizing such calculations is reliable reservoir pressure, accumulated gas, oil and water production, and PVT data. Calculations of apparent oil in place in the Jones Pool, based on field data

Jan 1, 1951

By F. H. Buttner, E. R. Funk, H. Udin

Gold wires, 5 mil in diam, are found to creep viscously up to approximately 5.5x106 dynes per sq cm around 1300°K. Beyond this point, an additional slip mechanism appears. The average coefficient in the viscous range at these temperatures is 18.9 ± 7x10 12 poises. This observation and other visual observations made during the experiments agree with Herring's predictions. EARLY creep studies by Chalmers on single crystals of tin produced some of the first experimental evidence to suggest that metals deform viscously under very light stresses. That is to say, over a small initial stress range up to 150 g per sq mm, the single crystals of tin elongated at a rate proportional to the stress. The proportionality constant between strain rate and stress is by definition the coefficient of viscosity. Chalmers named this range of proportionality the microcreep range. One of the first theoretical attempts to explain the microcreep phenomenon was given by Kauzman,' who applied Eyring'sQ eneral statistical mechanical theory of shear rates to creep data then available. From the rate theory, he deduced the general hyperbolic sine law for shear rate on the assumption that the distortion of the reaction path due to stress is negligible and that the system is an infinite continuum. In order to fit the available data to the equation, it was necessary to assume that creep occurs by shear of rather large blocks of material, rather than by an atomistic shear process as in diffusion. The size of the shear units was shown to increase with increasing temperatures and lower stress, or lower strain rates. In applying the hyperbolic sine law equation to the microcreep data of tin, it was shown by Kauzman that the unit shear blocks became quite small, which suggested to him that microcreep might be a self-diffusion process. Making this an assumption, Kauz- man reworked the rate theory and arrived at an equation where the shear rate is proportional to the stress. In the form of viscosity coefficient, the equation is: o- _ \LkT V = 2qAlA where u is the stress; S, the shear rate; X, the distance in shear direction moved by flow units relative to one another in the unit process; L, the distance between layers of units of flow; T, the absolute temperature; k, Boltzmann's constant; qAL, a constant proportional to the size of flow units; and kT A, the diffusion coefficient = ------kTe-Q/RT = K X2 h Kauzman applied the expression to molten lead with a fair degree of success, the calculated viscosity being low by a factor of four. For solid lead the result is 5000 times too high. Taking q = 1, and X = dA = L = 21 = nearest neighbor distance, Udin, Shaler and Wulff8 found the equation low by a factor of lo7 for solid copper. On the basis of the discrepancy in lead, Kauzman indicated that microcreep is probably not a simple diffusion process of molecular shear units, but one involving preferential diffusion paths, or even that diffusion in solids does not involve shear at all. Cottrell and Jaswon4 treat the microcreep phenomenon on the basis of slow moving dislocations and apply it to Chalmers' data on tin with fair success. Nabarro Suggested a microcreep model in which mass movement in the direction of pull is effected by the diffusion of holes. The tension on the crystal effectively creates a greater hole concentration at regions near the crystal surfaces perpendicular to

Jan 1, 1953

By M. E. Wadsworth, C. H. Pitt

Nickel corrosion in sulfuric acid solutions at elevated temperatures and oxygen wer-pressures was imestigated. Weight loss was 1inear with time and varied directly with oxygen concentration. Independent variation of the possible active species in solution indicated that the undissociated sulfuric acid molecule plays an important part in the corrosion mechanism. The rate determining step was considered to be the adsorption of oxygen on a site containing adsorbed H2SO4. THE tendency for a metal to go into solution depends on a number of factors some of which are: 1) the position of the metal in the electrochemical series; 2) the type and concentration of corroding species in solution; 3) the concentration of oxygen in solution; 4) the type of film formed at the liquid-metal interface; and 5) the physical state of the metal. The corrosion of a metal in an aqueous solution may be considered to be a heterogeneous reaction that occurs at the liquid-metal interface. The reaction is generally considered to occur as a result of electrochemical potential differences within the system. Little work has been published in the literature concerning the corrosion of pure nickel. A great deal has been publistled dealing with the experimental and theoretical aspects of the over-all corrosion process. Evans,1 Uhlig,' and recently Todt 3 and Tomashoff,4 have published books which review the results of experiments which have been conducted on corrosion, and have developed some of the basic ideas of the more widely accepted theories of corrosion. Friend5 states that. nickel does not readily discharge hydrogen from any of the common nonoxidiz-ing acids and that a supply of some oxidizing agent is necessary for appreciable rates of corrosion. He further notes that at temperatures between atmospheric and close to boiling, corrosion rates tend to vary with concentration, temperature, and aeration in acid concentrations up to 25 pct. Whitman and Russel6 studied the effect of dissolved oxygen on a number of metals in acid solutions and found that oxygen accelerates the rate of corrosion of nickel in sulfuric acid. Flowers and Kelley7 in studying the action of dissolved CO, on electroplated nickel postulated that nickel dissolves as NiHCO3 in the presence of CO, and air. It was found that oxygen was necessary for corrosion to take place and that the rate increased with increasing amounts of oxygen in solution. Flowers and Kelley attributed the oxygen effect to cathodic depolarization. MacGillavry, Rosenbaum, and wensson' determined metal solution potentials of nickel in various electrolytes. They found that nickel has no tendency to corrode in alkaline solutions in the presence or absence of air. In acid solutions in the presence of air, metal solution potential increases in the order of 1/2 v were observed. This increase was attributed to probable chemisorption of oxygen on the nickel surface and the corrosion mechanism suggested was the interaction of H+ ions with the nickel oxide formed at the surface. Delahay9 observed the reduction of oxygen on various metals. A polarograph was used to measure the course of the reaction. With some metals hydrogen peroxide was produced as an intermediate compound. However, nickel was not considered to be a hdrogen peroxide producer. Van Rysselberghe 10,11 and associates attributed the accelerating effect of carbon dioxide on the corrosion process to the presence of percarbonic acid produced in solution reacting with the hydrogen peroxide. The percarbonic acid can be reduced at less negative potentials than hydrogen peroxide and as a result accelerates the reaction. EXPERIMENTAL Since a complete description of the apparatus used can be obtained elsewhere,12'13 no attempt will be made here to describe the equipment other than to note that it consisted essentially of an autoclave unit from which samples could be withdrawn periodically without disturbing the interior state of the autoclave. A titanium autoclave liner was used to protect the autoclave from the solution.

Jan 1, 1961

Discussion of the paper of Edward Keller, presented at the Butte meeting, August, 1913, and printed in Bulletin No. 80, August, 1913, pp. 2093 to 2115. GEORGE L. HEATH, Hubbell, Mich.:-In the admirable paper quoted, is mentioned the date when the 5-g. assay was first proposed is a standard for refined metal. The author omitted, however, to mention a later paper,1 which contains a proposal for the use of a single " stock solution " of mixed acids, which has been adopted by the American Brass Co. and others. The suggestion is made that such a scheme would save time and manipulation with converter metal. Unless the low current of 0.5 ampere and the large excess of nitric acid, recommended by Mr. Keller, have been proved necessary to hold up antimony-and selenium, the use of the mixed solution which we have adopted will permit the use of 1 ampere of current per square decimeter of cathode surface, until the solutions have become colorless. At this point, we wash the covers and reduce to 0.5 ampere to prevent oxidation or contamination. The ordinary split electrodes have been used. With strong current, at least, the use of an excess of nitric acid tends to the neutralization of the solution before the end of the period, from the formation of too much ammonia., and this is detrimental. Antimony deposits more easily than arsenic, and tends to drag the latter dorm with it. There must, be some such explanation for the fact. that we have made hundreds of deposits of pure cathodes from Lake material containing no antimony, but as. high as 0.5 per cent. of arsenic. By placing an assay beaker in the Frary solenoid, or rotary device, a cathode deposit with less than 0.01 per cent. of impurity is easily obtained in one operation from 3 g. of whitneyite, carrying from 7 to 10 per cent. of arsenic. In such a case, it is necessary to test several times for end point and remove the plate as soon as no brown tint appears (at once) when hydrogen sulphide water is added to the test portion on the spot plate. Edward Keller's proportion,, of solvent figure out as 14 cc. of strong nitric to 11.4 cc. of sulphuric acid (1.84).

Jan 11, 1913

By Eric K. Albert, J. Kiusalaas

The paper presents an overview of SPASID (Kiusalaas and Albert, 1983), a new computer program developed under U.S. Bureau of Mines funding for the prediction of surface subsidence caused by under- ground mining operations. The presentation, which is illustrated with two case studies, also re-evaluates the influence function method as a tool of subsidence prediction, arriving at some rather unconventional recommendations. SPASID consists of four modules that communicate through common data bases: (1) Preprocessor. This module prepares and maintains the database for the entire site. The database contains all the information about the site and the mine operation that is necessary for the computation of subsidence. (2) Subsidence Predictor. The influence function method is used to predict the surface displacements that occur in any portion of the site that occur between two given dates. The computations take into account the time lag between extraction and displacement, and the effects of pitching seams and incomplete compaction at the edges of panels. The program contains i not he's influence function and the Green's function of transversely isotropic elasticity theory. (3) System Identification. The purpose of System Identification is to determine the optimal values of the various parameters associated with the influence functions in the Subsidence Module. System Identification requires measurements of subsidence from a site with a sirnilar overburden structure. The values of the subsidence parameters are obtained by minimizing the discrepancy between the measured and computed surface displacements. (4) Postprocessor. The Postprocessor is a graphics facility for displaying the data generated by the other program modules.

Jan 1, 1984

US 4,132,758-Leaching of copper sulfide ore using nitrogen dioxide as the oxidant A slurry of ore in sulfuric acid is contacted with a nitrogen dioxide-containing gas at a temperature below 11 5" C and a pressure of from atmospheric to 35 PSI, the slurry agitated, and the resulting nitric oxide from the slurry regenerated to nitrogen dioxide for reuse About 90% of the copper In the ore IS dissolved, and the leach solution is separated for further processing. This procedure is also useful for sulfide ores of silver, molybdenum, nickel, cobalt, and zinc T C Franklewicz and R E Lueders, assigned to Kennecott Copper Corp Jan 2, 1979 7 pp (423-27) Filed 1 1-30-77 (855,983) (Drawings below ) US 4,138,231-Wet-cleanlng of gases from the roasting of copper sulfide ore, zinc sulfide ore, pyrite, or arsenopyrite The gases are washed in dilute sulfuric acid circulating in a closed system, the wash water treated to remove arsenic, the washed gas condensed by cooling; and the condensate separated, purified of residual arsenic, and neutralized B G V Hedenas, J E Wiklund, T R H Johansson, and KA Melkersson, assigned to Boliden AB Feb 6, 1979 7 pp (55-71). Filed 3-30-77 (782,908) Priority Sweden, 4-9-76 (76/04,219) (Flow diagram at right ) US 4,148,862-In the acid-leaching of silicate-bearing calcined zinc sulfide ore, finely divided calcine is leached at elevated temperature with sulfuric acid, and additional calcine is added at an optimum rate to precipitate SI~ICIC acid in the same stage In an easily settling, readily filterable form Reactions take place at a silica concentration so low that the solution is not greatly oversaturated An anionic flocculant- may be added to the slurry immediately before the filtration step S. P Fugleberg and J T. I Poijarvi, assigned to Outokumpu Oy Apr. 10, 1979 4 pp (423-106). Filed 10-6-77 (840,041) Priority Finland, 10-8-76 (76/2880)

Jan 1, 1980

By C. G. Dunn, J. L. Walter

COULOMB' and Coulomb and Lacombe2,3 have recently discussed secondary recrystallization in soft iron (99.5 pct Fe). They found that the appearance of this phenomenon was dependent on both the presence of impurities and the thickness of sheet specimens. They concluded that impurities such as carbon, sulfur, and oxygen in the soft iron stabilized the matrix structure and allowed growth of a few grains of specific orientations. They also found that secondary recrystallization ceased when the final thickness was small and attributed this complete inhibition of growth in thin sheet to the restraining action of thermal grooves. When purer iron (99.99 pct Fe) was used, normal grain growth but not secondary recrystallization was obtained. On the other hand it is known that the necessary stabilization of the matrix structure for secondary recrystallization in high-purity silicon iron probably does not depend on impurities but more likely results from the specimen thickness effect of Beck et al.,4 according to evidence and ideas advanced by Walter and Dunn,5,6 and Detert.7 Furthermore, Mullins8 has indicated that if a gas-metal surface energy difference exists across a grain boundary equal to or greater than about 3 pct of the grain boundary energy, then such a grain boundary should not become stuck. Similarly, Walter and Dunn have estimated that any increase in restraining force due to increased thermal grooving with decrease in

Jan 1, 1962

By E. H. Rennhack

Phase equilibria of the zinc-rich portion of the Zn-Fe-A1 system containing up to 20.0 wt pct Fe and Al have been investigated at 600°C (1112°F), 450°C (842°F), and room temperature by metallographic and X-ray diffraction techniques. The phase relationships were found to involve only those phases present in the three binary systems. THE presence of small quantities of aluminum (approx. 0.2 wt pct*) in zinc galvanizing baths is known to suppress the formation of Zn-Fe alloy layers within the coating.' As part of an extended investigation of this suppression effect and the alloy reactions involved, the zinc-rich corner of the Zn-Fe-A1 equilibrium system containing up to 20.0 pct Fe and Al was determined at 600°C (1112°F), 450° F (842° F), and room temperature. The present paper reports the findings of this study. The constitution of the Zn-Fe system has been reported by Raynor2 based mainly on the work of Schramm3-3 and Truesdale et a1.6 The solid solubility of iron in zinc is extremely small and lies between 0.0009 and 0.0028 pct in the range 150° to 400°C (302°to752°F). Within the temperature and composition range of interest, a eutectic reaction involving nearly pure zinc, liquid = Zn+FeZn13, is observed at about 419°C (786° F) and 0.018 pct Fe along with a peritectic reaction, FeZn7+ liquid e FeZn13, at 530°C (986° F) and 6.2 pct Fe. The latter reaction is sluggish due to the large proportipn of solid phase involved in the transformation. Halla et al.,7 identified the compound FeZn13 as monoclinic with a = 13.68, b = 7.63, c = 5.07, and B = 128°44'. The structure of FeZn7 was reported by Bablik, et al.,8 to be of hexagonal symmetry, belonging to either the C6v = C6/m mc or D46h = C6/mc space group. Divensions of the unit cell are a = 12.81A and c = 57.6a. The Zn-A1 diagram as composed by Raynor9 and later Gebhardt10 is characterized by a eutectic decomposition, liquid 382°C (720°F) and 95.0 pct Zn and a eutectoid decomposition, at 275° (527°F) and 78.0 pct Zn. The eutectoid reaction cannot be suppressed permanently by quenching. Above 275° (527° F), a and a' co-exist in a closed miscibility gap between 31.6 and 78.0 pct Zn. Both phases are fcc and have nearly the same lattice parameter. The maximum solubility of aluminum in zinc (B) is approximately 1.0 pct at the eutectic temperature. PROCEDURE Materials. The experimental alloys were prepared from both massive and powdered material. Cast alloys were composed from three zinc-base master alloys containing 8.0 pct Fe, 16.0 pct Fe, and 50.0 pct Al which were made from C.P. zinc, Armco iron, and

Jan 1, 1962

By L. F. Coffin

Monotonic tension and controlled cyclic-strain tests have been conducted on an annealed steel at various strain rates and temperatures in the weep range. Evidence of a strain-induced precipitate reaction abozle 500°C was determined from pronounced cyclic-hardening effects, increase inflow stress, inter granular fracture, drastic decrease in low-cycle fatigue resistance, and loss in tensile fracture ductility, as well as through electron-microscopy examination. It was found that strain rate as well as temperature had a pronounced effect on these observations. A parameter of the form P = T(7.95 - log ip) was determined, which was directly related to the ductility, defined either as the true strain at fracture in the case of simple tension, or as 2N 1/2 ? E p in the case of cyclic plastic strain. A highly satisfactory comparison of the cyclic life as measured and as computed from the ductility predicted by this parameter was obtained for a range of temperatures from 400° to 650°C and for crosshead speeds of 0.002 to 0.2 in. per min. MANY metals subjected to sustained loading at elevated temperatures derive resistance to creep from solid-state reactions of various alloying constituents. These reactions can be many and varied, and occur as a consequence of time and temperature according to reaction-rate principles. Strong evidence exists that many of these reactions are influenced by plastic strain, the argument being put forth that dislocations act as sites for nucleation and growth for the new phase.' Many examples can be cited where plastic strain during transformation influences the structure, and as a consequence affects the properties.2 The low-alloy steels serve as particularly good examples for investigating the effect which aging reactions have on resulting properties. Alloying elements such as carbon and nitrogen, and carbide formers such as manganese, chromium, molybdenum, and so forth, can, by the particular aging reaction which occurs, produce strengthening effects at various temperatures, and so endow strength to the alloy over a broad range of temperatures. These effects have been systematically studied by Glen both during creep3 and for constant strain-rate tension testing.4,5 The work of Glen is of considerable interest in connection with the present study, particularly in regard to the effect of various alloying additions on the true stress-strain curve and on fracture ductility at various elevated temperatures. He has shown that strain-age hardening occurred during plastic straining, which was quite specific both to the temperature of the test and to the alloying element involved. When strain-age hardening was noted at a particular temperature, a .minimum in reduction of area was also obtained. Provided the temperature for the minimum reduction of area exceeded 300°C, all minimum ductility fractures were found to be inter-crystalline in nature. For carbon steels containing molybdenum, two minima in reduction of area were noted, one occurring at 200° to 250°C, the precise temperature depending on the percentage of molyb-

Jan 1, 1964

By W. D. Robertson, Raymond C. Boettner

A study was made of the change in density during the first (transient) and second (linear) stages of the creep curve of polycrystalline copper as a function of 1) stress, 2) temperature, 3) plastic strain, 4) impurity and atmosphere effects, and 5) structure, including single crystals. Voids were not observed in single crystals strained 15 pct at 500°C, or in a polycrystal-line aggregate produced by recrystallizing a single crystal, within the limit of sensitivity, Ae/e = 1 x 10-4. It appears that voids are heterogeneously nucleated at grain boundaries by an insoluble phase, or phases, which can be removed by directional solidification. The principal controlling mechanism of void growth appears to be condensation of vacancies at grain boundaries. Vacancies are transported to a boundary and condense as a consequence of the tensile stress component across the boundary, which depends on the orientation and configuration of the boundary plane and on boundary shear across ledges and other irregularities. The ultimate source of vacancies is the free surface and diffusional transport is by way of the boundary plane. PREVIOUS investigations have dealt with the nucle-ation of voids at grain boundaries under creep condition~'-~ and with the connection between grain boundary voids and subsequent brittle fracture.5-7 Growth of voids during the creep process, particularly in the transient and linear stages of creep, has not been studied with the same intensity. Therefore, it seems pertinent to investigate the process of void growth with respect to the related creep curve, and the morphology of growing voids with respect to the structure.

Jan 1, 1962

By W. T. Hicks

Visual observation of the oxidation of columbium shows that the protective behavior noted previously in gravimetric work in the early stages of the reaction below 600°C and throughout the reaction at 640°C is associated with an adherent oxide. The fact that the oxide is seen to move outward from the metal at temperatures from 550° to 935°C implies that the reaction takes place at the oxide-metal interface throughout this temperature range. THE work described in this paper further clarifies the complex oxidation kinetics of Cb revealed, for example, by the continuous gravimetric studies of T. L. Kolski.1 Time-lapse motion picture studies reveal details of the reaction not provided by a study of the combustion products. EXPERIMENTAL PROCEDURE Cb specimens were prepared from material with the following typical analysis: 0, 0.03 pct; N, 0.002 pct; C, 0.006 pct; Ta, 0.04 pct; Fe, 0.01 pct; Ni <0.003 pct; and Cr <0.003 pct. Arc-cast ingots were swaged and cold rolled into slabs. These slabs were machined into blocks 7/16 by 7/16 by 7/16 in; 1/16-in. holes were drilled through the large face of the blocks for suspension. The samples were then de-greased and annealed 1 hr at 1200°C in vacuum. The sample was suspended by a platinum and Pt 10 pct Rh thermocouple inside a 1-in. quartz tube in a Kanthal wound furnace (2 in. OD by 4 in. long) equipped with windows 1/2 in. sq. A Cine-Kodak Special II 16 mm motion picture camera was trained on the sample through a Spencer microscope adjusted so that a magnification of X1.5 resulted on the film. Super Anscochrome film was used to record the events in color. Argon was flushed through the furnace while the sample came to temperature. The argon was then replaced by a stream of dry oxygen at 1 atm. Pictures were taken at the rate of eight per second for about 20 sec during the change of atmosphere. Then by use of a Stevens time-lapse device pictures were taken at the rate of four per minute starting within 1 min of the initial oxygen flow. In this manner continuous visual records of the oxidation of pure Cb

Jan 1, 1962

By Clifford S. Wilson

ScReened pipe is designed with the view of restraining the fine, free-running sands of the production zone from entering oil wells. Its successful use is dependent on a number of factors. The nature and effects of some of these factors can be determined through experiment and observation, but some of the elements that have a distinct bearing on the use of screened pipe can be evaluated only by estimate. The important subsurface conditions which affect the use of screened pipe are: 1. Depth of production zone. 2. Extent of production zone. 3. Reservoir pressure. 4. Character and relative quantity of oil and gas. 5. Character of sediments: a. Cossolidation of beds. b. Variation in beds. c. Grain-size gradation of sands. d. Free-running characteristics of sand from different levels. Aside from the use of mechanical equipment and tools, the measures to be taken in the installation of screened pipe involve: 1. Size of liner. 2. Length of liner. 3. Design and mesh of screen. 4. Portion of liner to be screened. 5. Manner of setting liner. 6. Preparation of or washing of the well before or during the setting of the screen. 7. Manner of bringing in the well. 8. Manner of flowing the well. Values applicable to the actual subsurface conditions that exist at any well can only be approximated. The accuracy of the estimate will be measured by the amount and quality of the evidence at hand and the personal factor of ability to interpret the evidence fairly, whether

Jan 1, 1933

By Fred P. Dewey

IN preparing material for the exhibit of the National Museum at the New Orleans Exposition in 1881, it was decided to attempt to photograph the interior of a coal-mine, in order to get a strictly truthful representation of a thick coal-seam, and to show incidentally the methods of mining. While we have many drawings, both mechanical and artistic, illustrating the subject, they are not satisfactory for these purposes, simply because they are drawings. Aside from this, much interest attaches to pictures of inaccessible places, and the enlarged copies (30 inches by 40 inches) of the photographs we succeeded in obtaining, have attracted a large amount of attention from the visitors to the Museum. The Kohinoor colliery, Shenandoah City, Pa., was selected as most suitable for the attempt, principally on account of the fine exposure of the Mammoth bed, and the comparatively level character of the workings, in that colliery. This is one of the many anthracite-mines of the Philadelphia and Reading Coal and Iron Company. A detailed section of the fiftyfoot or Mammoth bed in this colliery is as follows: Feet. Inches. 1 0 Clod. 1 7 0 Coal. 1 0 Slate. Top Split. 8 0 Coal. 1 6 Slate divider.* 6 0 Coal. 1 0 6 Slate. 2 6 Coal. 0 5 Slate. 1 8 Coal. 1 2 Charcoal. 5 0 coal. 1 0 Bone and Coal. „ „ Coal. [ Bottom Split. 0 6 Bone and Slate. 3 0 Coal. 0 10 Bone and coal. 1 2 Coal. 0 2 Bone. 4 4 Coal. 0 1 Bone. 0 8 Coal.

Jan 1, 1888

By Alexander L. Holley

The 400-ton testing machine, ordered in June, 1875, by the United States Board appointed to test "iron, steel, and other metals," has lately been completed at the Watertown Arsenal, thoroughly proved and accepted by the Board. The excellence of the machine in every respect is more than satisfactory, and its accuracy is at first sight astonishing, although an investigation of its principles must show that if the weighing apparatus will weigh at all, it must do so with perfect accuracy, because all its movements are absolutely without friction. The proof experiments were numerous, and the effects of recoil after sudden ruptures at maximum loads, were watched with great care, but without much anxiety, because the weighing parts affected are by no means delicate in structure, and their motion is almost infinitely small. Among the tests were the following : A forged link of hard, wrought iron, 5 inches in diameter between the eyes, was slowly strained in tension, and broke short off with a loud report at 722,800 pounds. The diameter before breaking at the point of fracture was 5.04 inches; after breaking, 4.98 inches. In order to see if the weighing parts had been disturbed by the recoil, which was obviously near the greatest recoil the machine will ever suffer, a horse-hair was next tested; it was 7-1000ths of an inch in diameter; it stretched 30 per cent., and broke at 1 pound. Other horse-hairs vary in tenacity between 1 and 2 pounds. Of course, the accuracy of the machine on such delicate specimens, and indeed on specimens having some hundreds of pounds tenacity, has been checked and proved by other weighing machines. A 5-inch round bar, turned down to 38 inches diameter along the centre, was pulled apart at 430,200 pounds tension. Then some more horse-hairs were tested ; also copper wires 191/2-1000ths of an inch in diameter, which averaged 25 pounds tenacity..

Jan 1, 1879

By P. Ramachandraraa, T. R. Anantharaman

THE technique developed by Duwez, Willens and Kle-ment&apos; for rapid solidification of molten alloys in small quantities by ejecting them on to a highly conducting substrate with the aid of a shock wave has come to be known as "liquid quenching" or "splat cooling" in literature and has already been applied to alloys of many binary systems.&apos; The very high cooling rates of the order of l060 to 1080 per sec obtained in this technique and the consequent drastic undercooling of the melt have led to such striking results as formation of new amorphous and crystalline metastable phases and extension of solid-solubility limits in many alloy systems. The cooling rates in these experiments can, however, be neither accurately measured nor effectively controlled and hence the occurrence of either more than one metastable phase or appreciable differences in constitution in splat-cooled alloys of the same composition cannot be ruled out.3 In fact, workers in two laboratories have reported formation of two different cubic metastable phases in liquid-quenched Au-Si alloys containing 17 to 20 at. pct si.4,5 The present note deals with some new and interesting results obtained in a Ag-21 at. pct Ge alloy and a Au-27 at. pct Ge alloy subjected to the liquid-quenching treatment at different cooling rates. Two alloys of nearly the same composition had earlier been rapidly solidified by the standard "gun technique" in the same laboratory and shown to solidify in nonequilibrium structures, viz., an hcp phase (a = 2.987Å;c =4.718Å) in the Ag-Ge system6,7 and both hcp (a = 2.885Å; c = 4.754Å) and tetragonal (a = 11.627A; c = 22.491Å) phases in the Au-Ge system.3 Apart from different substrates (copper and stainless steel), different melt temperatures (50º to 500°C above the liquidus), and different capillary sizes (0.4 to 1.5 mm diam) in the "gun technique", slower cooling rates of the order of l050C per sec were also obtained in the present work by replacing the substrate by water at room temperature in a modification of the technique due to Olsen and Hultgren.8 No attempt was made to measure the cooling rate in any experiment. The products varied from fine powder (>40 pct by wt—200 mesh) obtained by quenching in water to thin flakes and foils (11.0 sq mm to 4.0 sq cm) produced by splat cooling. They were subjected to the Debye-Scherrer method of X-ray examination in each case. In case of the Ag-Ge alloy, in addition to the expected metastable hcp phase,6 a coexistent tetragonal phase (a = 5.093,Å; c = 7.009Å) was detected in some experiments. Eight weak X-ray reflections from this phase could be identified, two of them being the same as reported earlier.7 With increase in the cooling rate, the dominant hcp phase seems to be first accompanied by traces of silver or germanium and then either homogeneous or mixed with traces of this new tetragonal phase. The splat-cooled Au-Ge alloy showed generally the expected hcp and tetragonal phases,3 but sometimes traces of germanium were also present. Further, two new tetragonal phases with the following lattice param ters could be clearly identified in samples quenched

Jan 1, 1970

By J. M. Eldridge, P. Balk

Phosphosilicate glass films were formed, by reacting gaseous P2O5 with SiO2, over a large range of temperature (800° to 1200°C) and gas phase composition (nearly two orders of magnitude of effective P2Ospressure). The film compositions generally corresponded with the liquidus curve, delineating the maximum solubility of the tridymite Phase of SiO 2 in phosphosilicate liquid solution at the temperature of film formation. It is shown that the P2O5 concentration of the phosphosilicate liquid film tends to decrease by reaction with the underlying SiO 2 layer until the liquidus curve is reached. The validity of the thermodynamic argument used in this explanation is supported by the results of a determination of the composition of borosili-cute films, prepared by reacting gaseous B2O3 with SiO2 at different temperatures. The kinetics of phosphosilicate film formation were described by a model predicated on a steady-state diffusion of P2O5 through the film. UNDERSTANDING of the processes leading to formation of phosphosilicate and borosilicate glasses is of great importance for producing passivating layers on FET devices. Passivating films with optimum characteristics are preferably formed in a separate step, independent of the doping of the semiconductor.&apos; The results of an investigation carried out to gain improved insight into the mechanism of glass formation are presented in this paper. It would be expected that application of the known Pz05-Si02 and B 2 O 3-SiO2 phase diagrams should be useful in extending understanding of the glass-forming processes. However, the question of the propriety of treating thermally grown SiO2 in these binary oxide systems by the methods of equilibrium thermodynamics must be considered when this application is attempted. Although Sah et a1.&apos; and Allen et al. 3 investigated the kinetics of formation of phosphosilicate glass (PSG), they failed to adequately relate their diffusion models to the occurrence of experimentally observed phases in the PSG/SiO 2/Si system. Horuichi and yamaguchi4 investigated the diffusion of boron through an oxide layer and described their results in terms of a model similar to that of Sah and coworkers. More recently, Kooi 5 and Snow and Deal6 reported the compositions of PSG films formed by depositing P2 O 5 onto SiO2. These compositions apparently coincide with those at the liquidus curve delineating the maximum solubility of crystalline SiO2 in phosphosilicate liquid solutions. These authors did not discuss the thermodynamic implications of their results on the structure of thermally grown SiO2 films. The structure of thermally grown Sio2 films and that of vitreous silica are generally thought to be quite similar. Since the solubility of a substance depends on its structure, it is relevant that the solubility of vitreous silica in water7 is highly reproducible, like the solubility of thermally grown SiOz in phosphosilicate liquid. Furthermore, the vitreous silica-water system appears to be in true thermodynamic equilibrium (viz., the same solubility value can be approached from both supersaturated and under-saturated solutions). Sosman7 suggested that a type of two-dimensional lattice may form at the silica/solution interface, resulting in the observed solubility behavior that is characteristic of a crystalline solid. An alternative explanation may be that vitreous silica has a microcrystalline grain structure. Other investigators have suggested that vitreous silica has essentially the structure of B cristobalite,&apos; or is composed of microcrystals of p tridymite or cristobalite, or a mixture of both. Presumably the grain size would be sufficiently large to minimize any appreciable contribution of the grain boundaries to the solubility of the crystalline matrix. The present investigation was carried out to clarify the significance of the boundaries in the Pa,-SiO, and B2O3-SiO2 Systems in determining PSG and BSG (borosilicate) film compositions. Furthermore, the kinetic data for PSG film formation were extended, using a wider range of formation parameters than were previously reported. One model describing the kinetics of film formation will be presented that is compatible with the thermodynamics of the Pa5-Si02 system. EXPERIMENTAL PROCEDURE Glass Film Preparation. SiO2 films (1000 to 8000A thick) were obtained by oxidation of silicon substrates in dry O2 at 1100°C. PSG and BSG films were prepared by exposing these layers to gaseous oxides obtained by reacting high-purity POC13 and BBr3, respectively, with O2. A double-columned saturator was used to ensure complete saturation of the N 2 carrier

Jan 1, 1969

By S. J. Matas, R. F. Hehemann, R. H. Goodenow

The hot-stage metallographic method has been employed to determine radial growth rates of upper and lower bainite. Lower bainite appears to grow as individual plates that increase in both length and thickness while upper bainite grows as sheaves of closely spaced plates or needles. A discontinuity in the temperature dependence of the growth rate appears to be associated with the transition from upper to lower bainite and stepped quenching experiments suggest that lower bainite will not continue to grow when the temperature is raised to the upper range. Thus, a single process does not appear to control the growth of both upper and lower bainite. A tentative model based on the forces acting on a dislocation interface is proposed to account for the slow growth of bainite. It has been recognized since the early studies of Davenport and Bain that a close relationship exists between the martensite and bainite transformations in steels. However, diffusion of carbon during the transformation has lead to considerable controversy concerning the reaction mechanism.1-7 Many studies4,5,7-9 have emphasized the structura and kinetic aspects of the bainite reaction and, in particular, the difference observed between the two forms of bainite—frequently termed upper and lower bainite. A kinetic difference between the two types of bainite has been revealed in the activation energy determined from the overall reaction;4,5 however, many difficulties arise in an interpretation of these activation energies since a number of temperature dependent factors contribute to the kinetics of the overall reaction. The displacive surface relief10 accompanying the bainite reaction permits a separation of the nuclea-tion and growth contributions to the reaction and allows the kinetics of the growth process to be examined. Several investigations of this type have been conducted; however, they have been restricted to the low temperature range.3&apos;6&apos;11 Here, bainite plates are observed to grow slowly in both length and width. The present investigation extends such studies to include the upper bainite range. MATERIALS AND PROCEDURE Materials. The composition of the steels studied in this investigation are presented in Table I. The range of composition permitted a study of the effect of carbon content on the growth rate of upper bainite in the 9 pct Ni steels and consideration of both upper and lower bainite in the higher carbon steels. These steels were received as hot-rolled rounds and were forged to approximately 1/2 in. thick plates for preparation of metallographic specimens. In order to produce an essentially zero carbon steel, Steel A was decarburized in wet hydrogen at 1550°F for 15 days with the result tabulated as Steel AD. Experimental Procedure. In order to study the slow growth of the displacive transformation product, a commercially available Leitz hot stage was modified to permit heating of the specimen by its own resistance in a manner similar to that employed by other investigators.6 The furnace chamber was maintained at a pressure of 2 to 3 X 10-5 mm Hg prior to austenitizing at 2000° ± 12° F for 5 min. Samples could be cooled from the austenitizing to the transformation temperature in approximately 15 sec and the progress of transformation was recorded with a 9 cm by 12 cm single frame camera or a 16 mm movie camera. RESULTS AND DISCUSSION Growth Characteristics. The general growth characteristics observed in this investigation were analogous to those reported previously.3,6,11 Typical growth sequences for the high temperature and low temperature forms are illustrated in Figs. 1 to 5. In both temperature ranges, bainite plates increase in length at slow, temperature dependent rates until interrupted by a grain boundary, another plate, or

Jan 1, 1963

By S. S. Nosseir

INTRODUCTION General Quebec Cartier Mining Co. (QCM) , Canadian subsidiary of U . S. Steel Corporation, operates two iron ore concentrators at the North Shore of Quebec, Canada. In its own operation at Mount-Wright, over 45 million tons per year of crude ore are ground, fully autogenous in six 32&apos; x 11-1/2 Dominion Engineering mills. At Fire Lake/Lac Jeannine operation, property of Sidbec Normines Incorporated (SNI), over 11 million tons per year of crude ore are now ground, fully autogenous, in twelve 18&apos; x 5&apos; Hardinge mills. The Lac Jeannine concentrator was originally constructed by Q.C.M. in 1960 and. was since operated, in beneficiating the Lac Jeannine ore deposit until fully depleted in 1977, at an annual capacity of 18 million tons of crude per year. In 1976, the new company, Sidbec Normines, was incorporated by Sidbec Corporation, British Steel Corporation and Quebec Cartier Mining Co., in proportional holding of approximately 51 to 41 to 8 percent respectively. Since the acquisition of the Fire Lake ore deposit and Jeannine concentrator by the new company, QCM has continued managing the mine and concentrator operaions for S idbec Normines Inc . Flow-Sheet Design Jeannine concentrator comprises twelve identical mill lines grinding the ROM from 8" top size to 14 mesh nominal size range. Driven by 600 H.P. motor at 13.4 RPM corresponding to 73% critical speed, each mill is operated in a closed circuit with two 5&apos; x 12&apos; vibrating screens dressed with 2.5 x 25 mm slot opening cloth. The ground product or screen undersize at an average grade of 33.4% Fe is beneficiated by gravity separation to produce 66.5% Fe concentrate grade at 42.7% weight recovery. At the rougher stage, each mill line con-tains 128 Humphrey 13- 1/2" pitch spirals which produce a final tailing, middling and concentrate products. The rougher concentrate - so produced - is classified by 64 Humphrey pocket sizers into an underflow, which is a final concentrate product and an overflow which is further upgraded by 64 cleaner spirals. The cleaner concentrate together with the pocket sizer &apos;s underflow are dewatered on a 13&apos;[6] horizontal filter. The rougher middling together with the cleaner tailing are recycled in a closed circuit with the spirals. The rougher tailing after dewatering by hydrocyclones is disposed of by a

Jan 1, 1982