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By H. C. Fiedler

The solubility of sulfur in Si-Fe was determined by the metallographic examination of heat-treated and quenched samples. In the absence of manganese, the solubility in 3.1 pct Si-Fe was found to be about 0.010 pct at 1000o C, 0.015 pct at 11000C, and 0.020 pct at 1150°C, which is substatntially less than hitherto reported. Increasing the silicon content was found to decrease the solubility of sulfur, which is consistent with the increase in the activity coefficient of sulfur with increasing silicon content that has been reported for Fe-Si alloys. Manganese additions were studied in alloys containing 3.1 pct Si and between 0.013 and 0.015 pct S. At low manganese levels the solubility product of manganese sulfide was found to be lower than previously reported. THE solubility of sulfur in pure polycrystalline iron has been reported by Rosenquist and Dunicz1 and by Turkdogan et al.2 Samples were equilibrated in atmospheres containing different ratios of H2S/H2. Both groups of investigators found a solubility limit in y iron of 0.013 pct at 1000oC and 0.031 pct at 1200°C. In addition, Rosenquist and Dunicz1 found a solubility limit in a iron of 0.020 pct at 900°C. Ainslie, Hoffman, and seybolt3 found significantly higher sulfur contents in polycrystalline iron samples than in single-crystal samples after heating at 890°C in a sealed tube containing a mixture of powdered iron and FeS made with s35. Whereas the single crystals contained 0.013 and 0.016 pct S (± 0.005 pct), the polycrystalline samples contained between 0.016 and 0.026 pct S. Autoradiographs suggested that the excess sulfur in the polycrystalline samples was due to the segregation of sulfur in solution at grain boundaries. Ainslie and seybolt4 have reported on the solubility of sulfur in 3 pct Si-Fe. Their samples were sealed in capsules containing hydrogen and sufficient sulfur as cobalt sulfide to saturate the sample. After heat treating, the sulfur-rich phase on the surface was removed by abrading, and the sulfur content of the sample was taken as the equilibrium value for that temperature. Before the equilibrating heat treatment, the samples were heated to 1300°C to coarsen the grains. The resulting grain size, which was about 3/18 in. in diam, was considered sufficiently large to preclude a sensible increase in sulfur solubility due to grain boundary segregation. They reported the solubility to be 0.029 pct at 900oC, 0.063 pct at 1000oC, 0.076 pct at 1100°C, 0.122 pct at 1200°C, and 0.098 pct at 1300°C.

Jan 1, 1968

By Stephen G. Dardaganian

Pore volume compresibilitieu measured in the laborutory on core .samples are reported for typical reservoir .sarrrl.rtorres at reservoir pressure. These cornpressibilities ore different for each reseriloir sample and cannot be correlated to porosity. The compressihilities are a1so functions of presslire. In recent years several authors have pointed out the importance of including pore volume compressibility of the reservoir rock in certain reservoir engineering calculations. Hall' showed that in calculating the hydrocarbon volume of an undersaturated reservoir from the production per unit change in reservoir pressure, the neglect of rock compressibility could, in the extreme case of low porosity rock, lead to results in error by a factor of two. Hawkinsl' and Hobson and Mrosovsky showed that both rock and interstitial water compressibilities must be included to achieve satisfactory accuracy in this calculation. Although rock compressibility is an important reservoir property in these calculations, very few data are available. Hall' made compressibility measurements on a few samples in a small pressure range. No other direct pore volume compressibility measurements have been reported. Geertsma' discussed the elasticity of reservoir rock but did not present any new data. In this paper, rock compressibilities suitable for reservoir calculations are reported for a variety of sandstones typical of U. S. reservoirs. The measurements were made through a range of pressures which is also typical of reservoirs. EXPERIMENTAL PROCEDURE Plugs 1 in. in diameter and 2- to 3-in. long were diamond drilled, 14 from cores from seven oil-bearing or potentially oil-bearing sandstone, one from a quarried sandstone, and another from a shallow, oil-free, pure orthoquartzite. The plugs were extracted in toluene, vacuum dried, and then weighed. The plugs were then saturated with kerosene and reweighed. This gave pore volume. They were then again extracted in toluene. vacuum dried, and jacketed in 0.004-in. thick copper foil. A short length of -in high pressure tubing led from the jacket. The jacketed sample was then saturated with kerosene and placed in the hydraulic pressure cell as shown in Fig. 1. Movement of the mercury slug showed the change in pore volume of the sample under a given pressure change. Temperature was about 72" F for all measurements. Before taking any measurements, the external pressure on the sample was raised to 10,000 psig and kept there for several hours. This formed the thin copper jacket around the plug. 7-he pressure was then removed and the sample left at least overnight, during which time it recovered its original pore volume. An external pressure of 12,000 psig was then applied and held constant. The change in pore volume was noted as the internal pressure was raised in 1,000 psig increments to 10,000 psig. The internal pressure was then reduced to zero, again noting pore volume changes,

By Tell Ertl, Ernest E. Burgh

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

Jan 1, 1949

By Frederick C. Langenberg

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

Jan 1, 1957

By Robert E. Thurmond

DISCOVERY of a commercial ore deposit has resulted from a program emphasizing geophysical techniques and concentrating upon exploration of alluvial-covered areas. United Geophysical Co. selected these areas as offering the best possibility of success, for here the surface evidence of ore deposits has been hidden from the eyes of prospector and geologist alike. Pima mining district, Pima County, Arizona, was selected for initial exploration. The project was successful in that a commercial ore deposit was discovered and proved through drilling and extensive underground development. A limited region of activity was chosen and library research was begun on available economic and regional geological publications relating to the mining districts. Field reconnaissance of those districts which seemed to hold exploration possibilities provided a general picture and ascertained the existence of alluvial-covered areas of interest. At the conclusion of the reconnaissance trips all data obtained were compiled, and the district which seemed to present the best exploration possibilities was selected by statistical methods. The statistical summary was based on the following considerations: Geological Factors: 1—type of intrusive, P—presence of favorable host rocks, 3—apparent intensity of mineralization, and 4—presence of favorable structure in covered or unexplored areas. Economic Factors: 1—past production from district or mine; 2—size, shape, grade, and type of ore deposit in the district; 3—ease of acquiring mineral rights; and 4—general development facility. Exploration Favorability Factors: 1—results to be anticipated from geological methods alone; 2—application of geophysical methods, namely, topographic conditions, surface interference, depth-size relation, physical property contrasts as related to ores or controlling structural features; and 3—drilling factors. Admittedly, many of these, factors do not lend themselves to absolute evaluation, but relative evaluation, subject to inaccuracies of personal judgment, is always possible. A relative scale from 1 to 10 was established for every factor, representing varying degrees of favorability. For each district a numerical evaluation of each factor was established and a numerical total determined. The obvious advantage of this scheme is that a more concise summation can be presented by numerical means than can be achieved by descriptive means. After a district had been selected as favorable, the first step was to carry out more detailed geological and economic studies to narrow down the areas of interest. The second step was to compile all available geological data from publications and add to these data by mapping where necessary. Geological interpretation and projection of structural or other control into covered or unexplored areas was made whenever logical. To determine the possibilities of geophysical application and to select a geophysical method, physical property contrasts were related to mineral assemblages and/or structural control. If geophysics seemed applicable, trial profiles were run crossing the area normal to the strike and spaced

Jan 1, 1955

By L. E. Wilsey, W. G. Bearden

This paper presents results of analysis of the effect of fracturing on initial flow rates and on ultimate recoveries from low capacity oil formations. This analysis shows that even in formations of permeability as low as 0.1 md, large fracture treatments can yield oil recoveries and production rates approaching those of high permeability formations. Field production information is shown which supports the analytical work. INTRODUCTION Often hydrocarbon bearing formations are discovered which, while they are known to contain large quantities of oil, will not produce at commercially attractive rates without special well stimulation. Attempts to solve this problem led to the development of such techniques as underreaming, shooting, acidizing, and recently hydraulic fracturing. These methods of stimulation have been highly successful in many fields. All of these treatments, however, affect only the pay section near the well bore and therefore owe their success to circumventing and overcoming local permeability reduction about the well bore. It has been the belief that in treating wells to stimulate production in which there is no permeability reduction near the well, the maximum possible production rate increase would be of the order of two or fourfold. Hence, it has been concluded that fracture treatment of uniformly low capacity (permeability times thickness) formations could meet with but limited success. It is the purpose of this paper to show that the use of fracture treatments much larger than usually used can yield commercially attractive producing rates and high recoveries even in formations of permeability less than 0.1 of a md. PROCEDURE In order to illustrate the effects of fracturing, an analytical study of some hypothetical systems was made in which one factor at a time was varied to show what is important in recovering oil from fractured wells. It was assumed that a horizontal fracture of relatively high fluid-carrying capacity extended from a well bore. The presence of such a fracture will cause a marked influence on the flow pattern and pressure distribution in the formations, with the net effect being to reduce tremendously the resistance to flow into the well bore. A diagram of the resulting flow pattern and pressure distribution is illustrated in Fig. 1. Immediately after production commences, the principal flow of fluid is vertically from the formation flanking the fracture, into the fracture, and then into the well. After sufficient oil and gas have been produced to lower the pressure in the formation adjacent the fracture, oil and gas will begin to flow in a radial manner into the fracture from the formations beyond the end of the fracture. In calculating the performance under such conditions. the material balance or conservation of matter equation and equations of flow were solved simultaneously by a stepwise method of calculation. Flow rates were found by determining the pressure distribution, as illustrated

Jan 1, 1955

By R. R. Hartman, W. B. Agocs

IN the course of a return flight from Olympia, Wash., to Laramie, Wyo., an airborne magnetometer profile was recorded continuously. The level of flight was controlled at barometric levels along segments of the flight. Barometric altitude was changed from 3000 ft to a maximum of 12,000 ft above mean sea level to take care of topographic variations. Terrain clearance varied from 800 to 7300 ft. Horizontal positions were obtained by recording and tying to cities, towns, airports, river crossings, and other landmarks in the course of the flight. Figs. 1-6 show the course of the flight and the general geologic and tectonic features traversed. The flight line begins south of Olympia, Wash., and proceeds south across the Puget-Willemette depression to the Columbia River. Thence it proceeds eastward along the Washington-Oregon border across the Cascade Mts. and lava flows and the Umatilla basin to Pendleton, Ore. From Pendleton it traverses the Blue Mts. uplift of Oregon in a southeasterly direction, and then to the Boise basin of southwestern Idaho. The flight line swings in an easterly direction as it passes over the Snake River downwarp to the south of the Idaho batholith. It then passes over the northern portion of the Great Basin and the heavily overthrust area at the intersection of the Utah, Idaho, and Wyoming borders. The flight then assumes an easterly course to cross the series of basins and uplifts of southern Wyoming and terminates near the western flank of the Laramie uplift. It should be clearly understood that all statements in this article pertaining to the magnetics were interpreted on the assumption of elongate anomalies transverse to a single profile. Hence any theories or ideas advanced here are in line with future paths of research rather than trying to prove or disprove existing data. Magnetic Interpretation: Depth determinations were made by the slope method of Peters: which is stated as follows: "Draw a line in the maximum slope (at the point of inflection); draw a line whose slope is one-half this maximum slope; draw two lines parallel to this line tangent to the anomaly curve. The horizontal distance between the points of tangency is approximately equal to 1.6 times the depth [or the distance times 0.6251." Certain assumptions must be made for determinations of the causes of the magnetic anomalies:' 1) The anomaly is caused by a susceptibility change rather than basement relief. 2) Polarization of the basement rocks is in the same direction as the earth's inducing field. 3) The disturbing magnetic mass has a great horizontal length in comparison to its width and its sides are vertical and of great vertical extent. 4) The anomaly is unique and not affected by the anomalies from nearby sources.

Jan 1, 1957

By J. J. Casey, R. S. Busk, D. L. Leman

The mechanical properties and the phase-temperature relationships of magnesium-lithium-aluminum, magnesium-lithium-zinc, and magnesium-lithium-aluminum-zinc alloys are presented. It is shown that the strengths of some of these alloys can be tripled by heat treating and aging but that the high strength is accompanied by brittleness and lack of stability. MAGNESIUM-LITHIUM alloys are interesting because the hexagonal structure of magnesium can be changed into the more ductile and workable body-centered cubic structure by the addition of only 10 pct lithium.1 After Loonam2 determined that the ductility of the magnesium-lithium alloys is destroyed by even trace quantities of sodium, it was possible to prepare ductile alioys and study their mechanical properties. Jackson3 and coworkers have ably described their results with both the binary and polynary magnesium-lithium alloys. The present paper is a report of the mechanical properties of wrought magnesium-lithium-aluminurn, magnesium-lithium-zinc, and magnesium-lithium-aluminum-zinc alloys. Experimental Procedure The alloys were made by melting 7 lb of magnesium in a steel crucible under a molten flux of 75 pct LiCl + 25 pct LiF3 previously dried at 1600°F. The metal was heated to 1300°F for alloying aluminum and zinc and then cooled to 1250°F for adding lithium (sodium content: 0.01 to 0.04 pct). After the lithium had been alloyed, dry LiF powder was sprinkled on the melt to thicken the excess flux. After a 15 min holding period, the flux was skimmed off. Paraffin vapors were used to protect the metal as it was poured into 3 in. diam by 11 in. long magnesium molds. Billets were extruded into 3/8-in. diam rod and 1/16 x 3/4-in. strip; sheet was prepared from 1/8x 7/8-in. extruded strip, first by hot rolling and then by cold rolling 2 pct per pass. Hot rollability, or the temperature range through which the alloys could be rolled, was determined by rolling the strip two passes at 30 pct reduction per pass. Cold rollability, or the percentage of cold reduction to cause detrimental cracking, was determined on 0.064-in. hot-rolled sheet. Standard ASTM procedures were followed to obtain the mechanical properties, using 0.2 pct offset for the yield strengths. The level of properties produced with commercial magnesium alloys using the procedure described is given in a previous publication." Results Magnesium - Lithium - Aluminum System: The good workability of magnesium-lithium alloys is illustrated by the data in table I, which shows approximately how the extrusion pressure decreases as the amount of cubic phase increases. Binary magnesium-lithium alloys are soft and weak, but aluminum raises their strengths con-

Jan 1, 1951

By E. C. Tveter, R. B. Tippin

The separation of minerals by heavy liquids is a standard laboratory technique which goes back at least 50 years, but commercially economic application of this principal to ore concenfration has been prevented by problems of liquid recovery. Recent investigations which demonstrate the different types of liquid-solid systems on various ores using the two major heavy liquids - methylene bromide and tetra-bromoelhane — are discussed in this article. As a result of these studies, over-all liquid recovery, and especially desorption of heavy liquid from the mineral surface, was improved by the use of surfactants as well as both thermal and mechanical energy. The examples given in the article indicate that heavy liquids which should find major commercial use in ore concentration are now available. The sink-float process using a heavy liquid medium has long been recognized as a nearly perfect method of mineral separation based on the differences in density of the minerals. The use of heavy liquid separation (HLS) offers the potential of an ore dressing method that provides the maximum possible natural concentrate grade and high recovery. In addi- tion the process requires no water, causes no waste disposal problems, and is extremely simple — the crushed ore is merely introduced into a liquid whose density is between that of the minerals to be separated. The minerals lighter than the liquid float while those heavier than the liquid sink. As such, HLS has become a standard laboratory tool but major commercial application has been prevented by the requirement for complete recovery of the heavy liquid, imposed by economics and materials handling hazards. Investigations, both in the United States and abroad, have shown that improved liquid stability as well as improved chemical engineering techniques brighten the future for HLS in ore dressing. The available commercial heavy liquids suitable for mineral separation cost from $2.00 to $20.00 per gallon1 and on this basis alone their complete recovery is economically desirable. Possibly of even greater importance is the fact that any residual heavy liquid remaining on the products could create a serious toxicity hazard. Consequently, to make the process commercially attractive requires (1) essentially complete removal of the liquid from the ore products and (2) optimum recovery of the liquid for reuse. Until recently these two stipulations have remained as obstacles but laboratory and pilot plant research now in progress suggests that these may soon be overcome. Various heavy liquid recovery systems have been proposed to meet these requirements and might be classified into one or more of the following three general classes: Solvent Wash (Fig. 1): The dissolution of the heavy liquid from the ore with a less expensive solvent,

Jan 1, 1969

By M. S. Abrahams

Germanium has been rolled in the temperature range of 700o to 800°C. The thickness has been decreased by as much as a factor of four, from a thickness of 0.032 in. to a thickness of 0.008 in. For deformations below 60 pet, the true strain per pass is found to be a constant; from the temperature dependence of this slope, an activation energy of about 2.5 ev is obtained. This energy agrees with that for dislocation climb in germanium . For reductions greater than 60 pet, complete rings are seen in the Lave photographs, new grains are observed in the microstructure, considerable softening occurs, and the hole mobility is very low. This evidence indicates that the recrystallization of gertnanium has occurred. GERMANIUM has been deformed in many ways1 including tension, compression, torsion, and bending since Gallagher2 first described its plastic nature at elevated temperatures. All of these studies indicate that the glide plane in germanium is (111) and that the glide direction is (110). Rolled germanium specimens were used by Kolm, Warekois, and Kulin3 in their X-ray study of deformed semiconductors, but no information is given on the rolling itself. The present experiments deal with the rolling of germanium at various temperatures and for different orientations. In all previous deformation studies, the phenomenon of recrystallization (i.e., the transformation of a single crystal into a polycrystal) in germanium has not been observed4 despite relatively large deformations at elevated temperatures. The proposed reason4 for this was that sufficient energy could not be stored in the deformed germanium lattice. In contrast to the earlier studies this work will present evidence indicating that recrystallization occurs in germanium during rolling at an elevated temperature. I) EXPERIMENTAL PROCEDURE A) Test Specimens. The samples used for rolling were in the form of rectangular parallelepipeds measuring 0.3 in. long, 0.06 in. wide, and 0.035 in. high. They were cut from an undoped single-crystal ingot of p-type germanium with a resistivity of 24.4 ohm-cm, a Hall mobility of 2300 sq cm v-' sec-l, and a hole concentration of 1.1 x 1014 cm"3 at room temperature. The surfaces of the specimens were metallographically polished prior to rolling. The initial dislocation density of the samples was about 10' cm-' as determined by etching in CP4. Two different specimen orientations were used. In the first case, the direction of rolling was parallel to (251), the surfaces in contact with the rolls were of the form (1021, and the normal to the third face was parallel to (211). The corresponding di-

Jan 1, 1964

By L. J. Demer, W. W. Walker

AMONG several variables of the indentation hardness test is the effect of loading time on the measured hardness of a material. The most generally recommended duration of loading is 10sec.1-3 Although this short loading duration is undoubtedly satisfactory for harder metals, it is questionable that it is sufficient for very soft metals,4 or for certain plastics.5 The effect of duration of loading on the measured hardness of ionic crystals is largely unknown, although Onitsche and Mitsches found that the indentor (under a very low load) had not yet reached equilibrium after 60 sec in a variety of ionic crystals. To extend further the data of Onitsche and Mitsche, a systematic study was made of the effect of duration of loading for longer periods, up to 50,000 sec, on the 136 deg Dph of synthetic lithium fluoride. For comparison, less extensive tests were made on synthetic magnesium oxide and copper single crystals. The general procedure used was to indent a cleaved and polished (100) face of a lithium fluoride crystal using a Leitz Durimet microhardness tester. In certain cases, the indentor was so oriented as to align the diagonals of the 136 deg diamond pyramid indentation parallel to a (100) edge. In other cases the diagonal of the indentation was aligned at 45 deg to a (100) edge of the crystal. After indenting, the surface tested was etched in the acid etchant recommended by Gilman and Johnston.' This revealed the position of dislocation lines which intersected the surface tested. At these points of emergence were formed the usual sharp, pyramidal etch pits as shown in Fig. 1. The specific procedure used in studying duration of loading was as follows. The surface of the crystal was indented, and the load was left on the indentor for a predetermined time. This duration of loading was varied systematically from 1 to 50,000 sec. After the desired amount of time had elapsed, the indentor was removed from the crystal and the size of the resulting indentation was determined using a micrometer eyepiece. The surface was then etched to reveal the dislocation etch pit pattern around the indentation. Procedures used for lithium fluoride, magnesium oxide, and copper were similar. Preliminary studies revealed that, although an indentation was enlarged by increasing loading time, no corresponding changes occurred in the surface etch pit pattern. Since no evidence of dislocation movement was observed on the surface, it was assumed that the plastic deformation indicated by the indentor sinking into the surface was a result of dislocation movement inside the crystal. This movement was studied bf making a series of surface indentations in a crystal corresponding to various lengths of time, cleaving the crystal vertically through the indentations, etching the freshly

Jan 1, 1964

By O. Schaaber

THE existence of isothermal martensite without the presence of the athermal form thus far has been established only in a 6 pct Mn, 0.6 pct C steel' and a 23 pct Ni, 3.5 pct Mn-Fe alloy.' " Theoretical calculations, moreover, predict this phenomenon to be observable only within narrow composition limits.' In all other steels, it is generally considered that martensite inevitably forms upon cooling below the M, temperature. Even the possibility of isothermal martensite transformation has been questioned for the common steels, although Averbach and Cohen" showed that martensite formation does not stop when the cooling is arrested and that as much as 5 pct retained austenite may transform isothermally to martensite at room temperature. This note presents some observations made on a number of low alloy steels by dilatometric and inductive measurement of isothermal austenite transformation at various temperatures close to the Ms. In the dilatometer studies reported previously, austenitized specimens were immersed in a salt bath maintained at proper temperature and immediately inserted into the dilatometera8' already at thermal equilibrium with the bath. The dilation was read on a dial gage divided into 0.001 mm intervals. Induction measurements were made with a separate excitation source and a test coil, sealed together in a salt-tight case. The increase in the induced voltage caused by the transformation products was recorded at a paper speed of 4 mm per sec. The steels studied are listed in Table I. Specimens prepared from steels 1 and 2 were in the form of hollow cylinders 60 mm long, 10 mm ID, 14 to 16 mm OD, while specimens of steels 3 and 4 were in the form of notched-bar impact test specimens, DVM type. Specimens of steel 5 were in the form of strip, 7x0.3 mm. In the bainitic range, curves representing the amount of transformation vs log time have a single step appearance, as is shown by the curve of isothermal transformation at 320°C in Fig. 1.Y ransformation proceeds in accordance with the Austin-Rickett equationo P -----------= k t" 100-P where P is the percentage of transformed austenite, t is time, and k and n are constants. Near the M, temperature, however, complex curves having two steps are observed. As shown in a previous papera for steel 3 isothermally transformed at 245"C, such complex curves can be separated into two separate transformations or reactions each following the Austin-Rickett equation. The values of n in the equation for a number of such two-step transformations are listed in Table 11 for steel 1. At transformation temperatures of 250" and 235"C, evidence of a second transformation is very

Jan 1, 1956

By L. Grånäs, B. Aronsson

In a recent study of Fe-Si alloys Walter and Koch' observed pairs of dislocations in Fe-6.25 pct Si crystals rolled to reductions of 10 pct and subsequently annealed for 1 hr at 650°C. They interpreted these pairs as being due to stacking faults. From the spacing of the dislocations a stacking-fault energy of 15 to 19 ergs per sq cm was calculated. These authors did not pay any attention to the order -disorder phenomena in Fe-Si alloys. It is the purpose of this communication to report some preliminary results from a study of ordering and its influence on the plastic deformation of Fe-6.0 pct Si alloys. Our results suggest that the dislocation pairs observed by Walter and Koch may have been due to long-range order rather than to stacking faults. The alloys used in this investigation were prepared from pure electrolytic iron and silicon and were melted in argon. After hot working, strip tensile specimens were machined to a gage length of 70 mm and a thickness of 1 mm. The specimens were heat- treated for 2 hr at 1000°C, furnace-cooled, and subsequently deformed 2 pct in tension at 400°C. The strain rate was 5.6 X lo-' sec-'. Thin foils of the deformed specimens were prepared by means of the Bollman technique and examined in a Siemens Elmis-kop I at an accelerating voltage of 100 kv. In the Fe-Si system long-range ordering occurs at a silicon content of about 6 pct Si. In our alloys evidence for ordering is given by selected-area diffraction patterns which show extra reflections consistent with a super lattice of the D0 9 type. In addition, the dislocation arrangement in deformed specimens indicates that long-range order is present. A typical mi-crophotograph of a thin foil is shown in Fig. l. The dislocations are usually straight and parallel and laying in distinct directions. In the commonly observed (111) zone the projections of the dislocations are close to (113) and (oil). Observation of the image position indicates that the two dislocations in a pair have the same Burgers vector and hence constitute a superlattice dislocation.~ According to theory3 a superlattice dislocation in the DO3 structure consists of four ordinary dislocations connected by two types of antiphase boundaries as shown in Fig. 2. In our specimens only two dislocations in each pair have been observed, Fig. 1. The problem is to decide whether the area between these is a NN or a NNN antiphase boundary. Dark-field images using the (200) reflexion (the indices are defined with respect to the DO3-type superlattice) can

Jan 1, 1968

THE developments in construction and operation of the basic open-hearth furnace that have taken place in recent years have placed new emphasis on the vital influence played by regulation and control of the combustion system in both furnace production and furnace life. The several factors influencing flame development, such as regulation of fuel supply, air supply, air preheat, furnace draft, and furnace reversal, must be controlled closely if successful furnace performance is to be accomplished. Rugged instrumentation of distinctive design is required to supply dependable information concerning operating conditions, which is requisite to proper regulation of combustion. This chapter attempts to give a practical discussion of the various features of open-hearth practice and instrumentation related to the efficient heating of the furnace, control of temperature, and protection of the furnace structure from accidental overheating. The appended references will be helpful to readers wanting a more detailed treatment of individual topics. OPEN-HEARTH FUELS The most important open-hearth fuels are listed in Table 4-1 together with their compositions and other data useful for combustion calculations. A detailed discussion of open-hearth fuels is not attempted here, but certain factors peculiar to their application to this type of process are briefly indicated on the following pages. Very often an open-hearth shop is forced by economic factors to use a fuel to which its furnaces are not very well adapted, because the general fuel-allocation scheme for the works as a whole seems to demand it. Often a variable marginal supply of coke-oven gas or tar must be consumed by the open hearth, together with another fuel such as producer gas, natural gas, or oil, to fill out total requirements. Most furnaces employ more than one kind of fuel during their usefu1 life; however, the partial redesign

Jan 1, 1951

By Arthur F. Taggart, G. R. M. Del Giudice, M. Hassialis, A. M. Saddler

Flotation of sulphide minerals and native metals is no longer a practical difficulty. The underlying scientific principles of the method, although not explored in anything like complete detail, have been formulated with sufficient breadth so that the direction of attack on any specific case is clearly indicated. It has been known since the earliest days of flotation that certain of the nonsulphide nonmetal minerals—e.g., sulphur and graphite—would respond to flotation by oils as sulphides do; therefore they have been grouped with sulphides in many patents. But since the development of the chemical theory of collection,1,2,3 this similarity in action has been one of the facts cited in disproof of the theory by opponents of the hypothesis.4,5,6 Air levitation† of certain oxidized minerals, both metalliferous‡ and nonmetalliferous, and separation thereby from other oxidized minerals, is a recent development in practice, although the discovery of the method dates back 17 years7 This paper presents evidence that the principles underlying the air levita-tion of the nonsulphide nonmetal minerals are the same as those utilized in the flotation of the sulphides and native metals. It will be apparent immediately to anyone with knowledge of mineral concentration that separation of air-levitated minerals in water from minerals not so levitated is a simple matter of water-gravity concentration, the separating device employed depending solely upon the size of the particles treated and the buoyancy differences effected by the levita-tion. The usual separating means employed are: (1) a flotation machine for fine, slimy and for well aerated granular material; (2) shaking tables for granular less aerated material. By using large quantities of oil, it is possible to form substantially air-free oil-bound masses or granules of nonsiliceous minerals and to

Jan 1, 1939

By A. M. Saddler, G. R. M. Del Giudice, Arthur F. Taggart, M. Hassialis

Flotation of sulphide minerals and native metals is no longer a practical difficulty. The underlying scientific principles of the method, although not explored in anything like complete detail, have been formulated with sufficient breadth so that the direction of attack on any specific case is clearly indicated. It has been known since the earliest days of flotation that certain of the nonsulphide nonmetal minerals—e.g., sulphur and graphite—would respond to flotation by oils as sulphides do; therefore they have been grouped with sulphides in many patents. But since the development of the chemical theory of collection,1,2,3 this similarity in action has been one of the facts cited in disproof of the theory by opponents of the hypothesis.4,5,6 Air levitation† of certain oxidized minerals, both metalliferous‡ and nonmetalliferous, and separation thereby from other oxidized minerals, is a recent development in practice, although the discovery of the method dates back 17 years7 This paper presents evidence that the principles underlying the air levita-tion of the nonsulphide nonmetal minerals are the same as those utilized in the flotation of the sulphides and native metals. It will be apparent immediately to anyone with knowledge of mineral concentration that separation of air-levitated minerals in water from minerals not so levitated is a simple matter of water-gravity concentration, the separating device employed depending solely upon the size of the particles treated and the buoyancy differences effected by the levita-tion. The usual separating means employed are: (1) a flotation machine for fine, slimy and for well aerated granular material; (2) shaking tables for granular less aerated material. By using large quantities of oil, it is possible to form substantially air-free oil-bound masses or granules of nonsiliceous minerals and to

Jan 1, 1939

By O. H. Eschholz

The electrostatic process of fume precipitation is an excellent example of the successful application of scientific knowledge to an industrial operation. Originally proposed for the precipitation of sulfuric acid mists, it has been extended until at present there is practically no fume-carrying gas to which the method cannot be applied. Among the more common applications are: the recovery of non-ferrous smelter flue-dust, iron blast-furnace dust, cement dust, and potash fume. It should be borne in mind that the process is restricted to the precipitation of suspended particles, either liquid or solid, and does not separate gaseous constituents. However, by proper temperature control, mixtures of vapors having different temperatures of condensation to either solids or liquids may be selectively precipitated. The process consists essentially of subjecting suspended particles, including those too minute to be effectively acted upon by centrifugal or gravitational forces, to such an electrical force that they are driven from the gas stream, acting as a conveyer, and deposited upon a suitable receiving surface. This directional impulse is obtained from the interaction of charged particles and an electrostatic field of definite intensity gradient existing between two dissimilar electrodes, known as discharge and receiving electrodes. In principle, the equipment is equally simple. As shown diagrammatically in Fig. 1, it consists of: (1) A source of high-potential direct, current,, requiring: (a) Source of alternating-current energy. (b) Means of transforming from low voltage to high voltage. (c) Means of converting alternating to direct current. (2) Precipitation chamber having: (a) Transmission tubes for fume-laden gases. (b) Suitably designed and disposed electrodes. (c) Means for affecting removal of deposited solids. Although Hohlfeld demonstrated, in 1824, that a smoke-laden atmosphere could be cleared by applying an electrostatic field, and while Sir

Jan 1, 1919

By S. P. Kinney, A. J. Boynton

THIS paper is not the result of recent research with regard to any particular feature of iron metallurgy, blast-furnace practice or mechanical engineering. It is rather a series of notes with regard to contemporaneous progress in blast-furnace construction and operation, together with some suggestions as to changes and improvements that seem to be desirable. On April 1, 1930, a committee of the Chicago District Blast Furnace and Coke Association presented to that association a rather ambitious study of blast-furnace equipment, together with recommendations for the design of construction of a complete blast-furnace unit for the production of 1000 tons of pig iron per day. This report represented the result of months of study by members of the committee, all of whom were actively engaged in operation or design of blast-furnace plants. It is natural, therefore, that comments on the present state of the art should take this 1000-tons furnace, as recommended by the Association, as a basis for comparison with corresponding features of construction or design. See Table 1. In looking through this report at the present time, the significant difference is in the nature of the gas-washing equipment that today would be specified. In other respects, the installation would remain generally very much as it was outlined in 1930. The change in furnace dimensions would be very slight and of no especial significance, except with respect to changes in stock-line diameter, of which more will be said hereafter. The high-efficiency stove as developed by various designers is thoroughly described within this report, and few changes have taken place since. Blowing equipment shows refinement and reflects the improvement in steam engineering. Hoisting and charging equipment and ladles for the conveyance of iron and slag remain, in general, as they were in 1930. In accordance with a general tendency

Jan 1, 1935

By J. J. B. Rutherford

IT is now well known that troublesome intercrystalline corrosion may occur in austenitic stainless steels following exposure of the metal to a temperature within the range 1000° to 1500° F. (540° to 815° C.). The present paper describes a satisfactory method of estimating the extent of such corrosion, based on the measurement of the electrical resistance of a specimen before and after attack. This new method enabled us to study quantitatively the effect of several factors upon intergranular corrosion in the 18 Cr, 8 Ni type of alloy. The results show that susceptibility to this attack increases with increasing carbon content and grain size and appears to pass through a maximum for certain combinations of temperature of sensitization and period during which the alloy was maintained at that temperature; and are in complete accord with our interpretation of the mechanism of this phenomenon. The method is probably applicable to other metals or alloys subject to intercrystalline attack, such as the aluminum alloys of the duralumin type. The methods hitherto in use for estimating the degree of intergranular attack fall into three types: (1) microscopic examination,1 (2) macroscopic examination of fractures, and (3) determination of the time required for complete failure or disintegration .2 None of these lends itself very well to a measurement of the extent of corrosion. The first two are qualitative in nature and the third provides an arbitrary value largely dependent on individual judgment, since failure is a progressive phenomenon and not a sudden event. Our experience is that weight-loss determinations, although valuable in some types of corrosion investigations, bear no simple relation to intercrystalline corrosion in this type of alloy, as is to be expected since the phenomenon probably involves only the thinnest films between adjacent metallic grains.

Jan 1, 1932

By W. D. Robertson, H. Conrad

Incremental loading creep tests were conducted on magnesium single crystals in tension and direct shear at 78" to 364°K. The creep curves were transient in character and exhibited waves or periodic behavior, especially at small strain rates. A sigmoidal curve was frequently observed following the first occurrence of creep. Repeating of segments of a master curve was observed at all temperatures indicating that identical conditions for flow existed after various stress and strain histories. A logarithmic time law with a independent of temperature whs observed at 78°and 203°K, while a parabolic (power) time law was approximated at 298" and 364°K. The departure from logarithmic creep was attributed. to recovery, which was observed at 298" and 364°K. The temperature independence of a represents a serious objection to the theory of low-temperature creep based on the intersection of dislocations. IN a previous paper1 it was found that the initial creep rate of magnesium single crystals, y, following the addition of a stress increment in the range of 78° to 364°K, was given by the expression ? = C exp - {?H/kT} exp {B(T- h ?)} [1] where B and C are constants, AH is an activation energy of 10,300 cal per mole, T is the applied stress, ? is the total strain at the time of the stress increment, and h is the strain-hardening coefficient. The present paper is concerned with certain other features of creep behavior observed during this investigation; namely, the form of the creep curves, time laws for creep, recovery, and microscopic and X-ray observations of the structural manifestations of the creep flow. To the authors' knowledge the temperature range of the present investigation (0.08 Tm to 0.40 Tm) has not been covered previ-

Jan 1, 1959