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By Charles L. Mantell, James E. Hoffmann

Mechanical inclusion, electrophoretic deposition, and adsorption were studied as mechanisms for code-position of aluminas present in copper-plating electrolytes as an insoluble disperse phase. Mechanical inclusion was not a significant factor. That codeposi-tzon of aluminas by an electrophoretic mechanism was unlikely was substantiated by measurements of the potential of the aluminas. The alumina content of the deposits was studied as a function of the pH of the bath. These tests in conjunction with sedimentation studies demonstrated the absence of an isoelectric point for the alutninas over the pH range examined. Thiourea in the electrolyte (a substance known to be adsorbed on a copper cathode during electrodeposition) affected the amount of alumina in the electrodeposit. However, no adsorption of thiourea on aluminas in aqueous dispersions was detected. If it were possible to produce a dispersion-hardened alloy of copper and alumina by electrodeposition, an alloy possessing both strength and high conductivity at elevated temperatures might be anticipated. Investigation of the mechanism of codeposition of aluminas with copper was undertaken with the hope that knowledge of the mechanism would aid in the development of such an alloy. The word "codeposit" here does not necessarily imply an electrolytic phenomenon but rather that the materials codepositing, the various aluminas, are transported to and embedded in the electrodeposited copper by some means. Mechanical inclusion in electrodeposition implies a mechanism of codeposition which is wholly mechanical in nature; the only forces acting on a particle are gravity and contact forces. Such a particle is presumed to be electrically inert and incapable of any electrical interaction with electrodes in an electrolytic plating bath. Processes for matrices containing a codeposited phase by electrodeposition from a bath containing a disperse insoluble phase frequently state that code-position is caused by mechanical inclusion.10,2,12 If settling, i.e., gravity, be the controlling mechanism for codeposition of aluminas, then assumptions may be made that 1) the content of alumina in the electrodeposit should be enhanced by increasing the particle size, 2) the geometry of the system, that is, the disposition of the cathode surfaces relative to the di- rection of the falling particles, should affect the alumina content of the electrodeposit, 3) in geometrically identical systems the chemical composition of the electrolyte employed should exercise no effect on the alumina content of the deposit, that is, the alumina content should be the same in all cathode deposits irrespective of bath composition. A bent cathode19 evaluates the clarity of filter effluent in electroplating baths by comparing the roughness of the deposit on the vertical surface with that on the horizontal surface. Two difficulties are inherent in this technique: 1) the current density on the horizontal portion of the cathode would be substantially greater than that on the vertical surface; 2) should the deposit obtained be rough, projections on the vertical face could act as horizontal planes and vitiate the relationship between the vertical and horizontal surfaces. Bath composition should have no substantial effect on the alumina content of the deposit. Two different electrolytic baths were employed. They possessed variant specific conductances and substantially different pH ranges. The experimental tanks were rectangular Pyrex battery jars 6 in. wide by 3 1/4 in. long by 9 3/4 in. deep. The cathodes were stainless steel 316 sheet of 0.030 in. thickness, cut to 7.5 by 1.75 in. and bent at right angles to form an L-shaped cathode whose horizontal surfaces measured 1.75 by 3.0 in. All edges and vertical surfaces were masked with Scotch Elec-troplaters Tape No. 470. The anodes were electrolytic cathode copper 9 in. high by 2.25 in. wide by 0.5 in. thick. To eliminate inordinately high current densities on the projecting edge of the cathode, the anode was masked 1 in. above and below the projected line of intersection of the cathode with the anode. The exposed area of the anode was equal to that of the cathode, providing both with equal average current densities. The agitator in the cell was of Pyrex glass and positioned so its center line was equidistant from cathode and anode, and a plane passed horizontally through the center of the blade would be located equidistant from the bottom of the cathode and the bottom of the deposition tank. The assembled apparatus is depicted in Fig. 1. Hatched areas on anode and cathode represent the area of the electrodes wrapped with electroplaters tape. MATERIALS The chemicals were copper sulfate—CuSO4 • 5H2O— technical powder (Fisher Scientific Co.). Spectro-graphic analysis showed substantial freedom from antimony, arsenic, and iron. Traces of nickel were present.

Jan 1, 1967

By J. F. Nester, J. B. Schroeder

COMPOUNDS of rare-earth and iron-group elements are of technical interest because of their unusual magnetic properties. To date, however, all magnetic measurements1-4 have been made with polycrystalline, often polyphase, samples. For the measurement of anisotropic properties, single-crystal samples are necessary to avoid the averaging effect of randomly oriented grains. The purpose of this note is to describe a technique with which we have grown relatively large single crystals of YCo5, NdCo5, DyCo5, and "YFe9". Crystal growth of these materials is complicated because: 1) the binary equilibrium diagrams are, in general, not well-established; 2) in those cases where phase-equilibrium data are available, the compounds of interest are generally formed by peritectic reaction; 3) the molten component metals are chemically very reactive, making contaminaticn of the melts by the crucible material a serious problem. Techniques such as arc or levitation melting followed by strain annealing have been tried5)' in the past with these materials, but with little success because of the peritectic reactions and the inherently poor process control. For this reason we chose to use the zone-melting technique of Mason and cook7 for our work, since past workers8 have had some success in preparing single crystals of peritectic compounds by this method.

Jan 1, 1965

By Clyde Evarts Weed

SOME one once affirmed his great belief in luck, adding that he had found that the harder he worked the more luck he had. Clyde Weed is a firm believer in this method of courting the fugitive lady. He is at work early and late, often leaving his staff at Anaconda's offices at 25 Broadway breathless trying to keep up with the ideas teeming from a fertile brain and the actions those ideas entail. Miles ahead of his assistants much of the time, he still manages to be an agreeable fellow to work with, no small accomplishment as many can testify. Mr. Weed arrived in the world at Moorestown, Mich., on Aug. 8, 1890. Sixteen years later he entered Michigan Agricultural College, a lowly freshman. The following year, with the experience and wisdom expected of a sophomore, he transferred his studies from the reaping of a harvest on the surface of the earth to delving into the deeper, unpredictable bowels of the earth, his studies now shifted to the Michigan College of Mines. Last June his alma mater conferred upon him the degree of Doctor of Engineering.

Jan 1, 1947

By J. A. Snyder, W. L. Finlay

G. Edmunds—Solid solubility is considered to be of either the interstitial or the substitutional type. Is it possible, in a binary alloy as the simplest case, that some of the solute atoms are present in the normal lattice sites (substitutionally or filling lattice vacancies) while simultaneously others are in interstitial positionss One might even ask whether a distribution of the two types may be the normal situation. H. M. Meyer—Metastable states of interstitial atoms occupying vacant lattice sites possibly occur as well as of substitutional atoms squeezed in between regular matrix positions. However (as we know since Hume-Rothery), the solute atoms choose between the two kinds of solutions; consequently, every solute will be unequivocally either substitutional or interstitial in the equilibrium state of the solid solution. M. Balicki—In view of the fact that the authors apparently correlate the analysis of the alloys at the ingot stage with the properties exhibited at the testing stage, I would like to ask whether this is a fully justifiable procedure. In other words, how good are their determinations of solute concentration for correlating them with the mechanical properties. The answer to this question may explain some of the divergencies. Assuming good enough homogenization of the samples and exact determination of mechanical properties the position of the plotted experimental points will depend solely upon the accuracy of composition determination. If this is not accurate, say due to loss or pickup of elements during processing from the ingot to the testing stage, or due to a systematic error in the method employed for obtaining solute concentration data, the points will deviate from their true position and may align themselves along a different curve than the one expected. H. V. Kinsey—We have been studying the creep-rupture properties of titanium-base alloys at 1000°F. In the course of this work, anomalies in behavior of the alloys that would suggest that the material under test was becoming stronger as the test progressed have been observed. If this was so, the most likely explanation that we could think of was that the test bars were absorbing oxygen and nitrogen from the air during the test and were thereby becoming strengthened. In an attempt to determine the strengthening effect of absorbed oxygen and nitrogen the following experiment was conducted. A length of cold-rolled titanium was supplied by the E. I. du Pont Co. Two test bars, having a 1/4 in. diam gauge length, were prepared from this material. One bar was tested in the as-received condition. The second bar was heated in air at 1550°F for 100 hr and subsequently air cooled prior to testing. A testing temperature of 1000°F was employed. The results of these tests are tabulated in table 11. In the author's opinion, is it reasonable to assume that the bar that was exposed to air at 1550°F for 100 hr was stronger because it absorbed oxygen and nitrogen from the air during this heat treatment? W. L. Finlay (authors' reply)—Direct experimental evidence for or against Mr. Edmunds' interesting suggestion will probably never be available. It seems possible, however, that mixed interstitial-substitutional solid solution might well occur with interstitial elements. The less likely possibility of interstitial solution of a normally substitutional element like copper in aluminum was recently discussed at length by the

Jan 1, 1951

By N. N. Clark

Pachuca tanks are used widely as reactors for treating gold slimes, and for alumina digestion and uranium leaching. In some designs, slurry mixing in the tank is achieved by introducing air at the base of a draft tube, which is the full height of the tank. A buoyant air-slurry mixture rises in the draft tube and is discharged at the top. The slurry flows back through the bulk of the tank volume. Little information is available to predict the relationship between slurry flow rate in the draft tube, and the volume of air added at the base of the tube. Most current designs are based on the energy balance proposed by Lamont 25 years ago. Recent two-phase flow theory is used to develop a momentum balance for the flow in the draft tube, and a new, accurate design equation is derived. Bubble slip, frictional (wall) losses, entrance losses, and acceleration effects all contribute to the pressure gradient in the draft tube. None of these factors may be neglected under typical operating conditions. The new design equation accounts for all of these factors, and finds good agreement with Lamont's experimental example. Also, the new equation demonstrates that it is uneconomical to operate the draft tube with high airflow rates.

Jan 1, 1985

By W. A. Foster

NINETY years after the Riddle nickel deposit N was discovered in Oregon in 1864, Hanna Coal & Ore Corp. began mining operations. Until 1954 much prospecting and preliminary development work had been done on the property, but no ore had been shipped other than for metallurgical testing. The deposit is being explored by churn drilling and trenching, and a few test shafts have been put down for the purpose of studying the ore in place, determining volume and moisture factors, and gathering bulk samples for pilot plant and smelter tests. In churn drilling, 6-in. casing is driven down 2 or 3 ft behind the drill bit and bottomed at each 5-ft interval. All the sludge for each cased 5-ft interval is dumped through a splitter and one eighth is saved and analyzed. Drillholes are stopped after going through the ore zone and penetrating fresh peridotite in which the nickel content is less than 0.5 pct.

Jan 8, 1957

QUICKSILVER is a body that consists of flowing and liquid materials, almost like water with a shining whiteness; it is composed by Nature of a viscous, subtle substance with an overflowing abundance of moistness and coldness together. This composition, in the opinion of the philosophic alchemists, is a thing that is very disposed to become metal-indeed they say that it is the original seed of all metals. When it lacks the warmness and dryness or the specific time that they require, it cannot congeal and so remains in the form that we see as an imperfect thing without becoming metal. These clever investigators have also called it mercury in consideration of its properties, perhaps because of its resemblance to the planet of him whose actions place him between gods and men, according to the poets in their stories. Thus these investigators think that this has a similar place among perfect metals, since it is the primary mineral matter. It might also be that they called it so because like the god Mercury it is winged and fugitive, and by virtue of its powerful subtlety penetrates all things and can issue forth from them at will. But let it be called by any name they wish-it does not matter to us. I, like them, shall sometimes call it mercury and sometimes [23 ] quicksilver as it has been named to me, and you will understand it as such. Now I shall leave aside the disputes on whether it is the primary matter of metals or not, since I have said enough concerning this question in the first chapter of the First Book. In order to approach what the philosophers say about it, I say that it may well be material about to be converted into metal, but since it is seen to be so ill-proportioned and so badly decocted, I cannot believe that it can be disposed to the generation of all kinds of metals. Indeed, if it is, I think that if its necessary processes had not been interrupted it would be more apt to generate lead, tin, iron, or even silver rather than copper or gold. And if we wish to consider it in relation to the natural complexions [of metals] or to the power of the, planets, I think that mercury is far distant from those of gold and from the power of the sun and of the moon. Therefore I say that if it is not what I have said, it is a thing that Nature has been pleased to make as it is. I am led to say this because all of it that I have seen has had the same

Jan 1, 1942

By R. E. Cech, J. H. Hollomon

KURDJUMOV and Maksimova reported experiments with manganese steels and high carbon steels' and with an Fe-Ni-Mn alloy' in which mar-tensite was formed isothermally over a range of temperatures. They found in some cases that mar-tensite formation could be suppressed by rapid quenching to liquid nitrogen temperature. From their microstructural observations of martensite formed isothermally, they concluded that the rate controlling step is nucleation rather than growth. Kulin and Cohen,3 in an attempt to reproduce these experiments, found that with a steel having the same composition as that reported by Kurd-jumov and Maksimova, the transformation to martensite was essentially complete above the temperature range of Kurdjumov and Maksimova's isotherms. The possible reasons for this disagreement were not considered. Recent papers by Das Gupta and Lement4 and Kulin and Speich5 report the formation of isothermal martensite in a high chromium steel and in an Fe-Cr-Ni alloy, but neither paper can be considered a verification of the original Kurdjumov and Maksimova results. Further, in neither case were the authors able to suppress the formation of martensite entirely. Because of the important bearing the Kurdjumov and Maksimova results have to an understanding of the mechanism of martensite reactions it was felt that an experimental investigation directly concerned with checking the validity of their results was in order. This paper describes the results obtained on the isothermal transformation over the temperature range from —79" to —196°C of an alloy of iron, nickel, and manganese. Experimental Apparatus A 15 lb heat of an alloy containing 73.3 pct Fe, 23.0 pct Ni, and 3.7 pct Mn was melted by induction and cast under argon. The ingot was forged to 1-in. bar and a portion rolled to 1/16x1 1/2-in. strip. This strip was pack-homogenized 300 hr at 1100" in a helium-filled sealed iron tube. The composition after homogenization was 73.2 pct Fe, 22.94 pct Ni, 3.73 pct Mn, 0.05 pct C, and 0.015 pct N. The strips were cut to 1/2-in. width for dilatometer and metal-lographic specimens. Only the center portion of the 11/2-in. strip was used in the present investigation. The dilatometer employed was similar in design to one described by Flinn, Cook, and Fellows." A concentric fused auartz rod and tube assembly with hooks for holding the specimen was mounted so as to transmit the specimen dilation to a 1/10,000 in., 1/10 in. travel dial gage. The dilatometer proper was mounted by means of extension arms to a counterweighted sliding member on a vertical standard. This method of mounting permitted rapid transfer of the dilatometer from the austenitizing furnace to the quenching bath and low temperature chamber. A small electrical vibrator on the dilatometer kept frictional effects of the quartz members at a minimum. The austenitizing unit was a vertical, molybdenum-wound, hydrogen atmosphere furnace maintained at a constant temperature ±3°C by means of constant power input. A 12-in. stainless steel jacketed copper liner having 1/2-in wall thickness acted to equalize the temperature in the hot zone of the furnace. This liner, closed at the bottom end and open at the top to permit entrance of the dilatometer and specimen, was kept filled with dry nitrogen gas. A chromel-alumel thermocouple was placed inside the tube to determine the temperature. The 4-in. dilatometer specimens in the chamber varied less than 1/2° across the specimen length except for a 1 1/20 drop at the end nearest the open end of the furnace. The low temperature isothermal holding bath was a double Dewar arrangement similar to one described by Turnbull7. The outer bath was filled with a refrigerant at a temperature lower than the desired holding temperature. The inner bath was filled with Freon "11" or "12" or a mixture of both, depending upon the holding temperature. This inner bath which tended to be cooled by the outer bath was kept at a constant temperature by introducing a small amount of heat with a manually controlled electric heater. Stirring was accomplished by bubbling dry air through the bath. A Leeds and North-rup type K potentiometer was used to measure the inner bath temperature as indicated by a five element copper-constantan thermopile. The bath temperature was maintained within ±0.2°C of the desired temperature by occasionally adjusting the heater current so as to keep the Leeds and Northrup galvanometer at zero deflection with a constant setting of the potentiometer. Isothermal tests were usually continued for 300 to 400 min and another reading made at approximately 1000 min if the bath, unattended overnight, had not deviated in temperature more than 5°C. Transformation curves are drawn dashed (Fig. 1) through the time region where temperature was not controlled precisely. Experimental Procedure Dilatometer specimens of 1/2x1/16-in. strip were cut to 41/2-in. length and holes were drilled for the quartz hooks with proper spacing to give a 4-in. measured length. A thermocouple consisting of 0.012-in. diameter chrome1 and alumel wires was spot welded to the specimen and threaded between the dilatometer rods to binding posts near the dial

Jan 1, 1954

By R. W. Regehr, R. A. Burmeister

Epitaxial growth of GaAs 1-xPx on germanium substrates was achieved using an open tube vapor transport system. The compositional range of 0.3 < x < 0.4 was examined. The best results were obtained with (311) orientation of the germanium substrate. The physical and chemical properties of the resulting layers were investigated using several techniques. Spectrographic analyses of the layers indicate substantial incorporation of germanium into the GaAs t-X Px layer. Evidence is presented which indicates that this incorporation occurs via a vapor phase transport process rather than by solid phase dijfu-sion. Electrical measurements suggest that the germanium thus incorporated behaves predominantly as a deep donor in the compositional range of 0.33 < x * 0.40 and has a deleterious effect upon the luminescent properties of GaAs1-x Px. The increasing technological importance of GaAs1-xPx for use in light-emitting devices has led to an evaluation of several aspects of existing growth processes. The method most commonly used to prepare GaAs1-xPx for electroluminescent device applications is vapor phase epitaxial growth on GaAs substrates.&apos;-4 In a typical electroluminescent diode structure the active region of the diode is entirely within the epitaxial layer and thus the electrical properties of the substrate are relatively unimportant since it is effectively a simple series resistance (assuming hetero-junction effects to be negligible). The use of germanium rather than GaAs as the substrate material is of interest for several reasons. First, GaAs of reasonable structural quality has been epitaxially grown on germanium4-2 and it is reasonable to expect that GaAs1-xPx could subsequently be deposited on the GaAs layer. Second, germanium substrates are readily available with both lower dislocation densities and larger areas than GaAs. Finally, single crystals of germanium are more economical than GaAs single crystals. The principal objective of the present investigation was to test the feasibility of growing GaAs1-xPx epi-taxially on germanium substrates, and to evaluate the properties of such layers with regard to electroluminescent device requirements. The approach used was to a) demonstrate epitaxial growth of GaAs1-xPx on germanium, and b) characterize the relevant structural, electrical, and optical properties of the GaAs1-xPx layers. The possibility of germanium incorporation into the grown layers was of special interest since there was some indication of this in previous studies of GaAs growth on germanium.5&apos;11,12 Although a study of the electrical properties of germanium in GaAs1-xPx was not an intent of this investigation, several features of the electrical properties of the layers grown in the present study which appear to be due to germanium are described. EXPERIMENTAL PROCEDURE The open-tube vapor transport system used for the epitaxial growth of GaAs1-xPx is illustrated in Fig. 1. This system utilizes the GaC1-GaC13 transport reaction and is similar in most respects to the larger system described elsewhere.&apos; The germanium substrates were n-type, with a resistivity of 40 ohm-cm (Eagle-Picher Co.). These were cut to the orientations of {100), {111), and (3111, and were mechanically polished and chemically etched in CP-4 (5 min at 0°C) prior to growth. In some cases, a GaAs substrate was employed in addition to the germanium. The orientation of the latter was {loo}, and they were also mechanically polished and chemically etched prior to growth. The initial composition of the deposited layer was pure GaAs. After approximately 10 microns of GaAs was deposited on the germanium substrate, the phosphorus content of the layer was gradually increased over a distance of approximately 15 microns to the desired concentration and maintained at this value throughout the remainder of the growth. Typical operating parameters used during growth are given in Table I. Selenium was used as a n-type dopant in several runs to facilitate comparison of the electrical properties of the layers grown on germanium with those of layers grown on GaAs substrates, which are usually doped with selenium. The concentration of H2Se in the gas phase was adjusted to a value which would normally yield a carrier density of 1 to 5 x 101 7 at room temperature in layers grown on GaAs substrates. The terminal surfaces of the epitaxial layers were examined by optical microscopy for structural characteristics. Laue back-reflection photographs (Cu radi-ation) were also made on the terminal surface to verify the epitaxial nature of the deposit. After these steps

Jan 1, 1970

By R. E. Pray, M. C. Fuerstenau, J. D. Miller, B. F. Perinne

Quartz cannot be floated with potassium amyl xanthate as collector at any pH. Complete flotation is achieved with certain minimal additions of amyl xanthate and Pb from pH 5.8 to 8.5 and with amyl xanthate and Zn from pH 7.5 to 8.1. The active species of these metal ions responsible for activation are shown to be PbOH and ZnOH No flotation was effected when Cu and Mg were added as activators. Previous work1,2,3,4,5,6,7 has shown that quartz may be floated in the presence of sulfonate or soap when the following two criteria are met: 1) some portion of the added metal ion has hydro-lyzed to its first hydroxy complex, and 2) a precipitate of the metal-collector has formed. Since sulfonate and soap, two substantially different anionic collectors, conform to these criteria, this phenomenon may well be expected to be of a general nature. In this view then, it would appear that any anionic collector, including xanthates, should also float quartz when these two criteria are met. The object of this paper is to demonstrate the conditions under which quartz will respond to flotation in the presence of potassium amyl xanthate. EXPERIMENTAL MATERIALS AND TECHNIQUES Quartz was prepared by leaching the sized sample (48 x 150 mesh) with HC1 until no iron could be detected in the leach liquor. Conductivity water, made by passing distilled water through an ion exchange column, was used in the investigation. Potassium amyl xanthate was selected as collector. Purification of this reagent was effected with the following method: 1) a laboratory sample of potassium amyl xanthate was dissolved to saturation in hot ethyl alcohol and filtered several times while still hot, 2) the filtrate was cooled, during which time potassium amyl xanthate crystallized out of solution; the xanthate was then separated from the solution by filtration, 3) the amyl xanthate was dissolved in fresh hot ethyl alcohol and filtered, 4) step (2) was repeated, 5) the crystalline potassium amyl xanthate was washed with ethyl ether five times, and 6) the xanthate was dried for 24 hours under continuous vacuum. Inorganic impurities are insoluble in hot ethyl alcohol whereas dixanthogen is soluble in ethyl ether. Five-gram charges of 48x150 mesh quartz were conditioned for 3 min in 125 cc of solution containing the reagents and were floated with the small-scale cell and procedure described in previous papers.478 Reagent grade HCl and NaOH were used for pH adjustment, while reagent n-amyl alcohol was added as frother. Frother addition is necessary with this technique, but it should be mentioned that data, similar to those shown in Fig. 2 for 1 x10-4 mole per liter Pb++ and 1 X 10-4 mole per liter AX-, were also obtained with a Hallimond cell in the absence of frother. EXPERIMENTAL RESULTS Clean quartz could not be floated with amyl xanthate at any pH. Flotation was achieved under certain conditions, however, when various metal ions were added to the system. The activating ions used were lead, zinc, copper and magnesium, added as reagent grade chloride salts. Lead as Activator: The effect of Pb++ as activator was examined at five different additions of amyl xanthate (Fig. 1, 2 and 3). When 1x 10-5 mole per liter xanthate was added in the presence of 1 x 10"4 mole per liter Pb ++, no flotation was obtained at pH 6.5 or below, while a recovery of about 60% was effected at pH 7. When the pH was increased to 7.8, no flotation was again obtained, Complete depression was noted from pH 7.8 to about 10, at which point a recovery of about 30% was achieved. At about pH 11, the precipitate of lead amyl xanthate which was present below this pH dissolved and complete depression occurred. When 2.5x 10-5 mole per liter xanthate was added with the same lead addition, no flotation was obtained at pH 5.8 and below, whereas a recovery of

Jan 1, 1965

By David D. Rabb

Leaching or solution mining, a relatively simple and economical process for beneficiating metallic ores, is likely to find increasing application in the treatment of low-grade ores that are impractical to mine by any other means. This process may be carried out in two different ways: 1) dump leaching, where the ore is moved from its original location to be leached at another site; and 2) In-situ leaching, where the ore is leached in place by introducing the leach solution at the top, letting it flow down through the ore under gravity, and then recovering it plus the dissolved metals it contains. Whichever leaching method is used, it is almost always necessary to break up the ore before leaching. In this paper a study is reported which indicates that rock broken by an explosion-in particular, an underground nuclear explosion-is significantly more amenable to leaching then is rock broken by other methods. These results suggest that the leaching speed and efficiency could be increased by nuclear fracturing of the ore. Not only would the leach time be shortened, but the resulting increase in strength or richness of the solutions would decrease plant installation expense as well as reduce pumping and processing costs. A considerable fund of experience has been accumulated in the course of several hundred experimental underground nuclear explosions, so that the gross results of any given nuclear explosion can now be predicted with a fair degree of confidence.&apos; From this knowledge it seems clear that, under the proper conditions, large ore bodies can be fractured much more economically-macroscopically speaking-by nuclear explosions than by other methods. The present study concentrates on smaller scale effects that is, the cracks in the chunks of rock broken by the explosion-and shows that here too, in the microscopic domain, there are important advantages to nuclear fracturing. The intense shock produced by the very fast acting, high-brisance nuclear explosive fractures the rock in a way that should significantly improve its leachability. Experimental Procedure This study compared rocks broken by nuclear explosives with rocks produced by conventional mining, quarrying, or core drilling. The test samples, granite chunks 6 to 8 in. on a side, plus core sections, came from the area of the Hardhat*2 nuclear explosion and were taken both before and after the explosion. For comparison, several samples of quarried granite were obtained from a local gravestone monument company. The general procedure was to soak the test samples in leaching solution and then determine the extent of penetration. A standard commercial copper leaching solution was used (10 gpl Cu, 10 gpl H2SO4, 5 gpl ferric Fe, 15 gpl total Fe, pH about 1.5), to which a water-soluble penetrant dye, Zyglo 1-c, had been added. Details of the procedure were as follows: 1) Sample leached in solution containing Zyglo penetrant dye. 2) Washed with water. 3) Air-dried. 4) Cut with granite wire saw. 5) One face polished with granite monument polish. 6) Sent directly to be photographed, or heated at 110°C for 2 hr and then sent to be photographed. 7) Photographed under ultraviolet light to show crack patterns. Results After 10 days of leaching at 70-75°F, the samples were removed from the solution, washed, dried, and cut in half with a granite wire saw to study the penetration of the leach solution. Since the Zyglo dye in the leach is visible under ultraviolet light, the degree of penetration of the leach (and hence the cracks in the samples) can be studied on photographs of the crosscut samples made under ultraviolet light. The photos in [Fig. 1] show how the leach solution penetrated various representative samples. Of the 71 rock samples examined, fractures were most frequent and prominent in samples from the rubble produced by the nuclear explosion [(Fig. 1D)]. Fracturing was less apparent in shaft-mined rock [(Fig. 1B)], still less evident in drift-mined rock [(Fig. 1C)], and practically nonexistent in cored or quarried specimens [(Fig. 1A)]. The samples in [Fig. lA-C] were from the same general area as the nuclear explosion, but they were obtained before the explosion. Results of the crack studies are summarized in [Table 1]. The Zyglo-treated leach solution penetrated the test samples at the rate of about 1/2 mm during the first hour, 1 mm by the end of 4 hr, 2 to 3 mm in 12 hr, and 4 to 6 mm in 10 days, showing a progressively slower rate with time.

Jan 1, 1972

By Frank Firmstone

It is proposed to consider here only comparisons made between results obtained when the materials employed are precisely the same, two furnaces at the same works for example, or the same furnace under different conditions as respects temperature of blast, method of charging, etc. With this limitation, the most important point in the comparison is the amount of fuel consumed per ton of iron. This, in fact, is the only item in the prime cost of the iron which can properly be said to vary in consequence of changes in the furnace process; for of the other principal items, the ore used per ton of iron, and also the amount of fluxing material, will depend on its richness, which, under the assumed conditions, will be practically invariable when taken over any considerable period; the labor cost also, from its nature, should be very nearly constant when estimated on the ton of iron. Moreover, as it consists principally in handling and moving material, it is greatly affected by circumstances quite independent of

By R. K. Dann, L. W. Roberts, R. B. Benson

The mechanical properties of 300-series stainless steels were investigated in both high-pressure hydrogen and helium environments at ambient temperatures. An auslenitic steel which is unstable with respect to formation of strain-induced a (bee) and € (hcp) mar-tensile is embrittled when plastically strained in a hydrogen environment. A stable austenitic steel is not embriltled when tested under the same conditions. The presence of hydrogen causes embrittlement at the mar-lensitic structure and a definite change in the general fracture mode from a ductile to a quasicleavage type. The embrittled martensitic facets are surrounded by a more ductile type fracture which suggests that the presence of hydrogen initiates microcracks at the martensitic structure. If a steel is unstable with respecl to fortnation of strain induced martensile, plastic deformation in a hydrogen environment will produce rapid embrittlement of a notched specimen in comparison to an unnotched one. FERRITIC and martensitic steels can be embrittled by hydrogen that has been introduced into the alloys, either by thermal or cathodic charging prior to testing.1-5 However, conflicting reports exist as to whether austenitic steels that are stable or unstable with respect to formation of strain-induced martensite can be embrittled by hydrogen.8-12 A recent investigation has shown that cathodically-charged thin foils of a stable austenitic steel can be embrittled.13 An earlier investigation of a thermally charged 18-10 stainless steel revealed a significant decrease in the ductility only at the lowest test temperature of -78°C, although strain-induced bee martensite was shown to be present in one specimen tested at ambient temperatures.&apos; When martensitic steels are tested in a hydrogen atmosphere, they are embrittled.&apos;4-&apos;7 It has been observed in this Laboratory that 304L steel, which is unstable with respect to formation of strain induced martensite, forms surface cracks when plastically strained in a high-pressure hydrogen environment. Work in progress elsewhere concurrent with this investigation has also established that 304L is embrittled when tested in a high-pressure hydrogen atmosphere." The objective of this investigation was to study the effect of a high-pressure hydrogen environment on the tensile properties of a stainless steel that contained strain-induced martensite (304L) and one that did not (310). EXPERIMENTAL TECHNIQUES Notched and unnotched cylindrical specimens were machined from 304L* and 310 rods that were heat- treated at 1000°C in argon for 1 hr followed by a water quench. The chemical analyses of these steels are given in Table I. The unnotched specimens had a reduced section diameter of 0.184 & 0.001 in., a gage length of 0.7 in., and were threaded with a 0.5-in.-diam. thread on each end. The notched specimens had a reduced section diameter of 0.260 * 0.001 in. and a 0.75-in. gage length, with a 30 pct 60 deg v-notch at the center. The notch had a maximum root radius of 0.002 in. The tensile bars were fractured in a hydrogen or helium atmosphere of 104 psi at ambient temperatures. The system used for mechanically testing the specimens is to be described in detail elsewhere.19 Several specimens of each type were tested in air using an Instron testing machine. The same yield strength and ultimate tensile strength were obtained in 104 psi helium with the above system as with the conventional testing machine. Magnetic analysis was employed to determine that there was a (bee) martensite in plastically deformed 304L and that it was not present in plastically deformed 310. The magnetic technique depended on allowing the material being studied to serve as the core between a primary and secondary coil. Thus, any change in the amount of magnetic material present between the annealed and plastically deformed steels will be indicated by corresponding changes in the induced voltage in the secondary circuit." The ratio of the output signal of a nonmagnetic stainless steel to a completely magnetic maraging steel was 2000 to I. Several unnotched 304L bars tested in hydrogen were analyzed for hydrogen by vacuum fusion analysis. There was an increase in the hydrogen content to approximately 2 ppm for the specimens tested in hydrogen, as compared to less than 1 ppm for the as-received material. Several thin sections cut from notched areas of 304L specimens tested in hydrogen and containing the fracture surface contained approximately 1.5 ppm H. The accuracy of these determinations was estimated to be ± 50 pct.

Jan 1, 1969

Jan 1, 1930

By W. J. Taylor

Every one having practical experience in making heating-gas knows how much room there is for improvement,, in order to avoid not only the production of poor gas, when good gas is most wanted, but also the waste due to burning gas on top of the fuel-bed, and the loss of both time and fuel in cleaning.* The producer which I have recently designed, and with which I am now experimenting with every prospect of success, at the oreroasting kilns at Chester furnace, is intended to remove these difficulties as far as possible, and at the same time to be continuous in operation. I have not had it at work long enough to get beyond the stage of experiment; hence, I will only at this time explain it in a general way, and illustrate it with a drawing, promising a more elaborate paper if it becomes the practical success I anticipate. The features of the producer are : 1st. The round dome-shaped revolving bottom; and 2d. Metallic water-cooled walls in place of the usual brick lining. As shown in the drawing, the bottom has a sleeve, which fits over the air-admission pipe, coming up through the center of the

Jan 1, 1887

By D. R. Semmes

The possible oil territory of Alabama can be readily divided into two regions, the Paleozoic area of the north, and the Coastal Plain province of Cretaceous and younger formations lying to the south. This latter area has received much attention in the last few years and has been described by a number of writers.&apos; Although the possibilities of the Cretaceous series have been much emphasized by recent writers, the fact remains that the two, or possibly three, localities where oil or gas have been found in anything like paying quantities are confined to the area of Carboniferous rocks. Moreover, almost all of the oil seeps and a good percentage of the gas seeps are confined to this area.2 Topographically, as well as structurally, the Paleozoic area can be divided into three rather well defined provinces: (1) The broad, open Coosa Valley lying adjacent to the crystalline oldland, with comparatively little relief, except for occasional longitudinal ridges and rather intense folding; (2) the plateau region of horizontal or gently warped Pennsylvanian strata broken by occasional anticlinal valleys aligned northeast and southwest, outliers of the Coosa Valley proper, in which the older Paleozoic formations are exposed—a region of much relief (200

Jan 1, 1921

By J. D. Price, W. M. Bertholf

A. C. RICHARDSON*—First of all, [ think that the paper represents a lot more work, study, and correlation than has been indicated by the brief talk by Mr. Price. I like the way he started out and described the areas from which the samples were obtained, the locations of the washing plants, the available tonnages, and other background information with which to evaluate the data he submitted later on. Then I like the way in which he described the various types of washing plants, the tonnages handled and the difficulties of the washing problems; showing the amount of material that lies close to the specific gravity at which the washing separation is made. Later he gave figures from washing plant operations showing recoveries and cleaning efficiencies. He then discussed his own plant at Pueblo. It is the same old plant, I think, that I worked around a good many years ago. It is unusual to find a plant treating nearly 5000 tons of coal a day on tables. But this table plant is, I believe, more efficient than is indicated by the figures that Mr. Price gave. To determine the efficiency of a cleaning operation or to compare it with another it is necessary to consider the quantity and character of the material close to the specific gravity at which the separation is made. It is not fair, I believe, to penalize the table operation by something like 4 pct of out-of-place-material as he has done here. The variety and difficulty of the coals that he has to wash, the continuous shift and change in their composition make a very difficult cleaning problem and the table performance is excellent. I believe that the information in this paper will be of interest and value to anyone operating or planning to build a coal cleaning plant in this or other areas; particularly where the cleaning of fine coal is a problem. The data may be used for comparative purposes in determining the relative efficiencies of other cleaning plant separations. E. D. HAIGLER*—What is a Baum jig? J. D. PRICE (authors&apos; reply)—A Baum-type jig is one in which the pulsations of the water is secured by means of a pulsating air current applied on top of the water. I imagine you are all familiar with the old plunger-type jig which is in effect a U tube in which a plunger on one side of the U, moving up and down, causes a corresponding pulsation on the far side of the jig. In the Baum jig, the pulsating air current is applied on the surface of the water on one side of the U tube of the jig and gives a corresponding pulsation on the other. It is also commonly known as a pneumatic jig. The control of the rise and fall of the water in the jig body proper is under much better control than it is in any of the other type jigs. Mr. Richardson could enlarge on that feature, for I know that he has had considerable experience with these jigs. A. C. RICHARDSON—You have asked how to control a Baum-type jig. The pulsations in a Baum jig can be modified and regulated to a marked degree by the amount of water admitted to the jig and by the adjustments of the valve which regulates the manner in which air is admitted. The number of pulsations per minute is controlled by the number of cycles of the air valve. Thirty to forty cycles per minute is a good speed for large jigs treating coarse sizes of cod. With an air valve it is possible to modify the time-velocity curve of the pulsating water to some extent which in turn determines the action in a jig bed. Within limits the following parts of the air valve cycle may be regulated: (1) the rate and period of air admission, (2) the period of air expansion, (3) the rate and period of air exhaust, and (4) the period of air compression. The rate and period of air admission determines the acceleration of the water at the beginning of the pulsion stroke and the amplitude of the stroke. The period of air expansion, after inlet port is closed, is one in which the water has reached the desired velocity, positive acceleration reduced, and the bed held in a mobile condition. The rate and period of the air exhaust can be adjusted to modify the degree of suction and so modify the manner in which the particles in the bed stratify. The compression period, alter the exhaust port closes and before the intake port opens may be used to advantage in retarding the downward velocity of water during the suction stroke. An ideal jig stroke is one in which during the up stroke the bed is lifted slowly in a mass and opens up like an accordian with the bottom layers dropping away first. With the bed open and mobile the particles adjust themselves according to their hindered settling rates. During the down stroke, while the bed is still open the particles of high specific gravity are accelerated toward the bottom layers. It is possible to approach this stroke with all types of jigs but it is less difficult to approximate it with a Baum jig.

Jan 1, 1950

By Douglas Ashmead

In his paper Mr. Braley makes no mention of the bacteriological aspects of the problem. It is now quite well established that certain bacteria play a major role in formation of acid mine waters, and it is a simple matter in the laboratory to show that under sterile conditions the rate of acid production from a pyrites suspension is only about one quarter of that obtained from a similar suspension inoculated with drainage from a mine producing an acidic pit water. Under sterile conditions the oxidation is due to direct chemical action and, from the evidence just given and from much other evidence, this increase under nonsterile conditions is due to certain bacteria. Experiments recently completed, and shortly to be published, have shown that this bacteriological oxidation can be prevented by the maintenance of pH conditions above 4. It was found that to raise this pH above 4 at the beginning of the experiments was not sufficient but that, due to the continuing chemical oxidation, alkali had to be added daily to maintain the pH conditions above 4. The amount of alkali added, however, over a fixed period, was only about one quarter of the alkaline equivalent of the acid produced when pH conditions were not controlled over an equal period. The opinion expressed by Mr. Braley that sodium hydroxide has little or no effect on the rate of oxidation of pyrites is not substantiated by the above experiments. The writer does not claim that these results show a practical solution to the problems, especially in abandoned workings, but feels that the application of an alkaline coating, such as lime wash, to exposed accessible workings might be well worth trying. S. A. Braley (author&apos;s reply)—In 1919 Powell and Parrl suggested that bacteria, or some catalytic agent, hastened the oxidation of pyritic or marcastic sulfur in coal. Carpenter and Herndon (1933)&apos; attributed the action of Thiobacillus thiooxidans. Colmer and Hinkle (1947)3 observed an organism similar to T. thiooxidans and another organism that oxidized iron. Leathen and Braley 9rst discovered this organism in 1947 in a sample of water from the overflow of the Bradenville mine (Westmoreland County, Pennsylvania). They characterized the organism in 1954" and gave it the name Ferrobacillus ferrooxidans. Although Temple and Colmer (1951)&apos; had suggested the name Thiobacillus ferrooxidans, since they claimed it oxidized both ferrous iron and thiosulfate, we have found that pure cultures of the organism do not oxidize thiosulfate, hence the name F. ferrooxidans. In 1955 Ashmead7 isolated an organism, similar to the one called Thiobacillus ferrooxidans by Temple and Hinkle, from acid mine water in Scotland. It is probable that this organism was F. ferrooxidans. In 1954 Bryner, Beck, Davis, and Wilsonh reported microorganisms in effluents from copper mine refuse. These organisms appeared to be similar but were not in pure culture. In view of this history of bacterial investigation of acid mine water and our own ten years of experience, we do not agree with Mr. Ashmead that bacteria play a major role in acid formation. We do not find that any of these bacteria will directly oxidize pyritic material. They do, however, augment the chemical formation of sulfuric acid by atmospheric oxidation. In two papers in 1953% eathen, Braley, and McIntyre discuss the role of bacteria in acid formation and postulate the mechanism through which they operate. Mr. Ashmead in his discussion of my paper has assumed that this work was carried on in the presence of acid mine water in which bacteria would be present. This was not the case. Strictly sterile conditions were not maintained, but the organisms present in mine drainages were definitely absent in these experiments. We believe that we have demonstrated that alkalis do not inhibit the chemical oxidation of pyritic material. This is also indicated by Mr. Ashmead&apos;s discussion in which he says that alkali must be added daily due to the continuing chemical oxidation. It is interesting to note that Mr. Ashmead finds that maintenance of pH above 4.00 decreases the activity of the bacteria. We have found also that a decrease in pH below 2.8 also inhibits its activity. Table XIII of published data&apos;" illustrates the decrease in activity with increased acidity, although pH values are not given. These values are in comparison with uninoculated controls and show the marked increase in acidity up to 22 weeks but a decline at 29 weeks, at which time the experiment was terminated. It is probable that after a longer period only chemical oxidation would have continued. From our studiesv we have postulated that the iron oxidizing bacterium (Ferrobacillus ferrooxidans) oxidizes the ferrous iron, resulting from chemical oxidation, to ferric iron. The ferric iron then aids the atmospheric oxidation of the sulfuritic material and is itself reduced to ferrous iron, which in turn acts as food for the autotrophic bacteria. Study of the physiologic properties of F. ferrooxidans shows that its preferred pH is about 3.00 and its activity decreases with variation in either direction. It is extremely inactive above pH 4.00 and below 2.5. This inactivity above 4.00 is indicated by Mr. Ashmead&apos;s observations. These properties of F. ferrooxidans then correlate perfectly with our hypothesis. Ferrous iron is oxidized very slowly by atmospheric oxygen in highly acid sohtion and since the bacteria become inactive, acid is formed only by atmospheric oxidation. At a pH of 4.00 or above iron is more readily oxidized by atmospheric oxygen, but the bacterial activity is decreased. However, with a pH above 4.00 the ferric iron is removed from the field of activity since its soluble sulfate hy-drolyzes and precipitates the iron as ferric hydroxide or a basic sulfate. As we have shown in the paper under discussion, the alkali does not inhibit the chemical oxidation, and thus the acid formation continues. This

Jan 1, 1957

By C. L. T. Edwards

IN the preparation of this paper, the author has drawn upon experience with the operation of a blast furnace on 100 per cent scrap burden, which he believes was the first operation of its kind in the country. It is the writer&apos;s further belief that much of the controversy attending discussions of this subject may be obviated by the presentation of a group of facts that should be known by blast-furnace men and open-hearth men alike. The following question has been raised: "Is iron made with scrap in the blast-furnace charge as good iron as that made without scrap-made with straight ore?" This question may be answered in part by the fact that the open-hearth men of the Bethlehem Steel Co. who used pig iron from a blast furnace that operated on 100 per cent steel scrap found no difficulty in the processing of such iron other than that to be expected from the known analysis. OPERATION WITH 100 PER CENT STEEL SCRAP During World War I, there was accumulated at the Bethlehem plant of the Bethlehem Steel Co. some 22,000 tons of alloy-steel turnings and borings. This scrap material was highly corroded and, like alloy-steel turnings of that period, were as a drug on the market. There was also a small tonnage of scale, rich in valuable metal. If this scrap could be worked up into pig iron, it would become readily available for use in the open hearth. In order that the pig iron should contain the maximum percentage of nickel, permission was obtained from the Management to try a 100 per cent scrap operation. Accordingly, a blast furnace was swung over on July 25, 1919; the percentage of steel scrap increased more or less irregularly until July 29, when l00 per cent steel turnings were charged. Except for occasional charges of nickel scale as an "extra," the operation continued uninterruptedly until Aug. 27, when the furnace was swung back to the regular ore-ore and scrap-operation. During this period, the furnace production ranged from a low of 568.60 tons to a maximum of 766.07 tons. At the swing-over from i00 per cent scrap to the regular burden, the charge hung up rather severely. While the latter condition has nothing to do with the object of the paper, a brief discussion of the experience will appear later because of the interest it may have for blast-furnace operators. In Table I, results of the first and last days of the ore charge are shown, July 25 and July 29. The last column shows a summary for the period of maximum scrap charge. The furnace employed had a hearth 16 ft. 0 in., bosh 22 ft. 0 in., stock line 15 ft. 6 in., bell 11 ft. 6 in., batter ¾ in., bosh angle 73° 27&apos; and a Baker-Neuman top, with gas-engine blowers. Analyses Range of Material Charged Gravel: Si02, 64.40 to .7o.54 per cent; A1203,3-52 to 4.58; CaO, 7.27 to 9.49; M90, 5.09 to 6.14; FeO, 1.67 to 3.34, ignition loss, 9.50 to 13.83.

Jan 1, 1941

By Joseph M. Dawson

Although eight new fields were discovered along the south central fault-line district of Texas during 1938, only one can be considered as of major importance. and as a whole the year was one of no very great development. Several prospects, particularly two, were condemned through drilling, which had been considered important for probable Edwards limestone production. The oil produced was approximately the same as during 1937; namely, about 9 million harrels. This, of course, does not represent potential production but that allowed under proration. The year witnessed the very rapid decline of operations and interest in Austin chalk production. It has been found that only in rare instances mill chalk production pay for itself, because the wells decline extremely rapidly and the recovery per acre, formerly estimated at 2500 bbl., is now considered to he around 1000 barrels. There was an intent interest in the drilling arid producing of edge and abandoned properties in the three Edwards lime producing fields; namely, Luling, Salt Flat and Darst Creek. Many good wells were completed on properties formerly considered below the water level or produced beyond the economic limit The Edwards is penetrated only a few inches and a very small charge of acid is used. The results have been surprisingly

Jan 1, 1939