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By J. S. Browning

The U.S. Bureau of Mines has been experimenting with flotation processes to separate the spodumene-beryl ores mined at Kings Mountain, N.C. The success to date as well as the present status of the process is discussed. Further experimentation is underway and studies will be made on the milling costs involved in the flotation process. The pegmatites of the Kings Mountain-Lincoln ton, N.C., area constitute the largest known domestic reserve of beryl and spodumene. The reserve is estimated to contain 90 million tons of pegmatic material with 1,280,000 tons of recoverable Li,O(lithia) as spodurnene.' The pegmatites also contain 0.4 to 0.5 pct beryl disseminated throughout the orebodies. The pegmatites may contain a potential reserve of 240,-000 tons beryl, equivalent to approximately 34,000 tons of BeO. Different flotation methods for separating beryl from feldspar or quartz, or both, have been developed by various investigators.2-7 On the other hand, published information is limited on concentration of spodumene-beryl ores. As the response of beryl and spodumene to flotation is essentially the same, a successful separation of the two minerals depends upon use of a selective depressant or a selective collector for one of the minerals. Several years ago, the U.S. Bureau of Mines, recognizing the need for developing a large domestic supply of strategic beryl, undertook studies to develop improved methods of recovering this mineral. Because of the low beryl content of the pegmatites, economic production of the beryl entails its recovery as a byproduct of spodumene flotation. Thus, the development of procedures that would provide for maximum recoveries of the spodumene, as well as the beryl, was a primary objective of the studies. Tests were made on run-of-mine ore and spodumene flotation tailing from the Foote Mineral Co.'s spodumene concentrator at Kings Mountain (Fig. 1). Pet-rographic analyses of the ore and flotation tailing are given in Table I. Detailed analyses and examinations of the ore and tailings revealed that the beryllium was present in the form of a low-alkali beryl. The crystals were small, rarely larger than 14-mesh diam, and were clear and colorless. About 10 pct of the Li20 content of the ore was present in the mica and feldspar components of the pegmatite. In some weathered ores the associated clays also contained small amounts of lithia. This is typical of pegmatites in the Kings Mountain area. LABORATORY TESTS In the past, a vigorous chemical treatment of the spodumene surfaces with acid or caustic soda has been considered essential for satisfactory selective flotation of the spodumene from the other minerals in pegmatites. Many tests were made during this investigation to determine if chemical treatment of the spodumene could be eliminated in favor of a reagent combination that would depress the other minerals while selectively floating the spodumene. A simple reagent combination and process was developed that gave better spodumene recovery and grade of concentrate than the more elaborate acid or caustic treatment methods previously used. The finely ground ore pulps were conditioned with either an ammonium, alkali, or alkaline earth lignin sulfonate and sodium fluoride, and the spodumene was floated and cleaned using oleic acid as the collector. The spodumene tailing was deslimed, conditioned with sulfuric acid and coco amine acetate, and floated to reject mica. The mica tailing was thickened and conditioned with hydrofluoric acid, then washed to remove the acid. The washed pulp was conditioned with sodium hydroxide for pH control, and the beryl was floated and cleaned with oleic acid as the collector. Table II summarizes the results of the laboratory test work. About 77 pct of the spodumene and 75 pct of the beryl were recovered from the pegmatitic material. The spodumene concentrate assayed 6.1 pct Li20 and 0.01 pct BeO, and the beryl product assayed 3.0 pct Li20 and 1.57 pct BeO. Similar results were ob-

Jan 1, 1961

By Paul M. Tyler

THE winning of metals from Nature has been advanced to a degree of efficiency that commands admiration even in this Machine Age. Economy of human effort underground, in surface plants, and in treatment works, and better means of performing all manner of operations have cut costs and im¬proved products to an extent that seems far beyond the wildest imagin¬ings of those that labored in the days of hand mining and muscular metallurgy. Principles and methods borrowed from other professions and sciences - mechanical engineering, chemistry, and physics-all have con¬tributed to the rapid development of ore production and treatment, but no small part of the achievements must be credited to the free exchange of ideas within the industry itself and mass attack upon problems of mutual concern. The esprit de corps or class consciousness that has contributed so effectively to the progress of the metal industries has been less apparent among nonmetallic mineral producers. As a class they have been handicapped by inadequate contact with the metal-mining fraternity as well as among themselves.

Jan 1, 1935

By R. S. French, W. R. Hibbard

FOR tensile deformation, if the stress value is defined by the ratio of the load to the actual area, and the strain value by the natural logarithm of the ratio of the immediate length to the original gauge length of the sample, the resulting data when plotted with logarithmic coordinates result in a linear relation extending from the initial plastic yielding through the maximum load and in some cases, such as for copper and brass, to fracture'.'. The normal form of the curve, therefore, is a parabola, satisfying the following equation: S = Kem [1] where S and e represent true stress and strain, K is a constant, and m is a coefficient evaluating the slope of the curve and designated therefore as the strain hardening coefficient. Hollomon² has reported that this coefficient is a function of the yield strength as effected by grain size in alpha brass, and the carbon content and heat treatment of steel. In the case of steel, the value of the proportionality constant is a function of the carbon content. It was further shown in that paper2 and also by Low and Prater -hat, if the power relation between stress and strain remains valid, the strain hardening coefficient m, is equal to the strain at the maximum or necking load. Thus, an added significant feature is that this coefficient may serve as an index of the capacity for deformation prior to localized necking and subsequent fracture, e.g. drawability. The constant K may be defined as the strength of the material at unit strain. Together the K constant and the m coefficient describe an alloy's physical properties as far as strength and ductility are concerned for a particular yield strength and, in the case of steel, a particular carbon content. The work of Lacy and Gensamer4 gives data on alloy ferrites from which very close estimates of the strength of ternary and higher iron alloys have been made. It was the purpose of this investigation to develop similar data for commercial copper base alpha solid solution alloys. Preparation of Specimens Commercial binary alloys of copper with aluminum, beryllium, cadmium, nickel, silicon, tin and zinc were investigated. In addition, laboratory castings were made of a 1 pct silicon alloy and a 2 pct aluminum alloy to complete these particular series. Two types of copper were used, oxygen free OFHC and tough pitch FC. The analyses of these alloys are shown in table I. Standard ASTM sheet tensile specimens were used to determine the usual physical properties of each alloy and to obtain stress data at strains from 0.0005 to 0.01. Small (1/4 in. x 3 in. x tk.) samples

Jan 1, 1951

By G. W. Gross

A commercial deposit of white kaolinite clay contained in the sandy overburden of the Cambrian Gatesburg formation in Central Pennsylvania was successfully mapped by combined SP and resistivity methods and results were checked by drilling. Resistivity minima in the range between roughly 2000 and 3500 ohm-meters coupled with second-order SP maxima of 50-60 mV contrast were found to characterize commercial white kaolinite clay beneath not more than 30-40 ft. of sandy overburden in the area stdied. This investigation supports the hypothesis, established previously, that certain SP phenomena may reasonably be ascribed to diffusion and membrane potentials produced by interaction of clay lenses, sandy matrix, and ground waters. The success of this test proves that this prospecting technique can assist in locating clay deposits in sandy overburden derived from the weathering of sandstones and carbonate rocks such as the Cambrian formations of Central Pennsylvania. In a recent paper, Gross and Moore (1959) described broad self-potential minima above the outcrops of the Cambrian Gatesburg formation. These "first-order" SP anomalies, of 220-350 mV contrast (Figure 7), are related to the peculiar sandy residual soil covering the Gatesburg formation. Small positive ("second-order") peaks of 50-60 mV contrast are superposed on the bottom or flanks of the first-order troughs. They appear to be related to lenses and layers of kaolinite clays within the sandy Gatesburg overburden. Both first-order and second-order anomalies show a characteristic inverse relationship with apparent resistivity profiles in most cases. An explanation in terns of liquid-junction and shale potentials was advanced. According to this working hypothesis, shale potentials are generated: 1) at the contact of the sandy Gatesburg overburden with the more argillaceous soils of surrounding formations; 2) at the boundary of clay lenses contained in the sandy matrix of that overburden. Concentration gradients between interstitial infiltration waters and perched water tables within the Gatesburg overburden are believed to give rise to the liquid-junction potentials. In order to test this hypothesis further, a detailed study was carried out of a second-order positive anomaly on the property of the Woodbury Clay Co. at Mines (Blair County, Pa., Hollidaysburg folio of the U.S. Geological Survey). A second aim was to establish if combined SP and resistivity surveys are suitable as a practical method for delimiting favorable areas in which commercial kaolinite clay de~osits may be found by drilling. Drilling control was provided by the Woodbury Clay Co. PROCEDURES Instrumentation used for SP measurements was the same as described in the paper mentioned. For resistivity surveys, a direct-current voltmeter-ammeter device built by Georator Gorp. of Manassas (Va.) was used in combination with non-polarizing electrodes from the same manufacturer. Power was supplied by one to six 45-volt, heavy-duty B-batteries

Jan 1, 1961

By R. I. Jaffee, J. G. Dunleavy, H. R. Ogden, Webster Hodge

INTRODUCTION EARLY in 1946, at the instigation of the U. S. Army Signal Corps, the authors made an extensive survey of the available literature covering high-strength, high-conductivity alloys. For the purposes of the Signal Corps, the minimum tensile strength to be considered was 150,000 psi, together with at least 50 pct IACS conductivity. No single alloy was found to be in production, or mentioned in the literature, which had this combination of properties. The constitution diagram for the iron-copper alloys is not well established in the respect to the two-liquid region. Fig I, taken from the 1939 Ed. of the ASM Metals Handbook, shows a two-liquid system existing above the liquidus temperature, but disconnected from it. Although Ruer and Fick1 and Ruer and Goerens2 definitely established the fact that two liquid layers could occur in the system, Ruer3 was not convinced that the line off immiscibility was closed in the center. Maddocks and Claussen4 found no liquid immiscibility at temperatures up to 1570°C in alloys containing almost no carbon. Although the diagram would indicate age hardening of the copper-iron alloys is possible, Hanson and Fords found that little hardening effect could be obtained. However, Gordon and Cohen6 reported that the response is better if the quenching is very efficient. Although iron has a potent effect on the conductivity of copper, Hanson and Ford5 have shown that, when hot-rolled copper iron alloys are aged at 1200°F, the electrical conductivity decreases sharply with iron contents up to 0.2 pct Fe, and then levels off at conductivities between 60 to 70 pct IACS with compositions to 2.1 pct Fe. They also found that aging did not increase the tensile strength, although increasing iron content gave a moderate improvement in strength. High-strength copper-iron alloys, usually containing about 60 pct iron, had been reported by Smith and Palmer.7 They found that an alloy containing 56.4 pct copper, 0.21 pct magnesium, balance iron, would give a maximum tensile strength of 170,000 psi and an electrical conductivity of slightly over 35 pct IACS. The alloy could also be processed to have 150,000 psi tensile strength, and about 41 pct IACS conductivity. Decreasing the iron content increased the electrical conductivity, but the long mushy range during freezing of the alloy containing 10 to 20 pct iron made the production of good castings difficult, In spite of the difficulty encountered by Smith and Palmer with alloys of around 20 pct iron, it was decided to make a rather complete investigation 0f this type of alloy. As a result 0f this investigation, a method of alloying and fabricating copper alloys containing 10 to 15 pct iron was developed

Jan 1, 1948

By A. T. Beckwith

This paper concerns measurements of low-velocity air currents and investigations on mine ventilation by means of chemical smoke. The chemical smoke used is produced without flame and at ordinary mine temperatures, and therefore presents no ignition hazard in gaseous mines. Mining men who have worked in open-light mines are familiar with the use of tobacco smoke in determining the direction of air travel and approximately measuring low-velocity air currents. The use of chemical smoke is merely a refinement on the use of tobacco smoke and the flameless low-temperature source of chemical smoke has the additional advantage that it can be used in gaseous mines. Ventilation smoke apparatus, Fig I, is a simple device for producing dense white smoke. The apparatus as shown consists of a rubber aspirator bulb which is used to force air through a glass "smoke tube" containing a chemical substance that produces a dense white smoke on contact with air. The apparatus was developed by engineers of the U. S. Bureau of Mines.' It is inexpensive, weighs less than 3 oz, is easily carried in a pocket, and requires no skill to operate. Smoke apparatus is invaluable in practical mine ventilation work for: (I) measuring low-velocity air currents, (2) detecting air leakage, (3) observing airflow characteristics. This paper is written to show the merits of the apparatus, and is based upon findings through its extensive use, during the past six years, in mines operated by the Lehigh Navigation Coal Co. Inc. The Apparatus Certain chemicals, such as stannic chloride (SnCl4) and pyrosulphuric acid (H2S2O7) produce "white smoke" when exposed to air. Stannic chloride gives off vapors which on contact with moist air cause the formation of solid hydrates, of which SnCl4.5H20 is the most important. Pyrosulphuric acid decomposes when exposed to air with the evolution of sulphur trioxide (SO3) fumes, which become white upon contacting moisture in the air. A chemical, such as one of the above, is the active substance in a smoke tube. The glass tubes are hermetically sealed during manufacture, and are made ready for use by merely breaking off the tips at the conveniently located file cuts. When the smoke tube is connected to the aspirator, depressing the aspirator bulb forces air into contact with the chemical, and smoke discharges from the open end of the tube. A white solid (a hydrate if stannic chloride is used, or sulphur trioxide if pyrosulphuric acid is used) may occasionally form a cake in the outlet opening of a smoke tube. A small wire such as an ordinary paper clip can be conveniently employed to dislodge the cake should it seal the tube. When the assembled apparatus is not

Jan 1, 1949

By R. I. Jaffee, J. G. Dunleavy, W. Hodge, H. R. Ogden

Early in 1946, at the instigation of the U. S. Army Signal Corps, the authors made an extensive survey of the available literature covering high-strength, high-conductivity alloys. For the purposes of the Signal Corps, the minimum tensile strength to be considered was 150,000 psi, together with at least 50 pct IACS conductivity. No single alloy was found to be in production, or mentioned in the literature, which had this combination of properties. The constitution diagram for the iron-copper alloys is not well established in the respect to the two-liquid region. Fig I, taken from the 1939 Ed. of the ASM Metals Handbook, shows a two-liquid system existing above the liquidus temperature, but disconnected from it. Although Ruer and Fickl and Ruer and Goerensz definitely established the fact that two liquid layers could occur in the system, Ruer3 was not convinced that the line of immiscibility was closed in the center. Maddocks and Claussen4 found no liquid immiscibility at temperatures up to 157oOC in alloys containing almost no carbon. Although the diagram would indicate age hardening of the copper-iron alloys is possible, Hanson and Fords found that little hardening effect could be obtained. However, Gordon and Cohen6 reported that the response is better if the quenching is very efficient. Although iron has a potent effect on the conductivity of copper, Hanson and Fords have shown that, when hot-rolled copper-iron alloys are aged at 1200°F, the electrical conductivity decreases sharply with iron contents up to 0.2 pct Fe, and then levels off at conductivities between 60 to 70 pct IACS with compositions to 2.1 pct Fe. They also found that aging did not increase the tensile strength, although increasing iron content gave a moderate improvement in strength. High-strength copper-iron alloys, usually containing about 60 pct iron, had been reported by Smith and Palmer.7 They found that an alloy containing 56.4 pct copper, 0.21 pct magnesium, balance iron, would give a maximum tensile strength of 170,000 psi and an electrical conductivity of slightly over 35 pct IACS. The alloy could also be processed to have I50,000 psi tensile strength, and about 41 pct I.\CS conductivity. Decreasing the iron content increased the electrical conductivity, but the long mushy range during freezing of the alloy containing 10 to 20 pct iron made the production of good castings difficult. In spite of the difficulty encountered by Smith and Palmer with alloys of around 20 pct iron, it was decided to make a rather complete investigation of this type of alloy. As a result of this investigation, a method of alloying and fabricating copper alloys containing 10 to 15 pct iron was developed

Jan 1, 1949

By C. J. Osborn

The temperature dependence of the free energies of formation of metallurgically important oxides, sulphides, chlorides, carbonates and sulphates is presented graphically, whereby the task of deriving practical metallurgical information is greatly simplified. The diagrams have been revised according to the latest available thermodynamic data. WHILE it is true that much careful investiga-tional work remains to be done, there are already available in the literature sufficient thermo-dynamic data to enable the metallurgist to predict with reasonable confidence the equilibrium conditions to be expected in most important, and potentially important, metallurgical reactions. In this connection, the careful, critical compilations of K. K. Kelley and his collaborators in numerous U. S. Bureau of Mines Bulletins are particularly valuable. However, the translation of reliable thermo-dynamic data into metallurgical language unfortunately involves lengthy manipulations of the cumbersome formulas which can be set up from heat of formation, entropy, and heat capacity data. Many years ago, Kelley20 predicted that thermo-dynamic calculations would be made in the future "with the aid of free energy, heat content, and entropy tables, rather than by means of the algebraic methods employed at present", and where such tables are available they greatly simplify the task of deriving practical metallurgical information. However, in addition to these tables, there are also available one or two reliable graphical presentations, particularly of free energy data, which may be used in the same way as the tables, but which have the added advantages that interpolation is never necessary, and that the behavior of different metals or compounds may be compared at a glance. Some years ago Professor Robert Lepsoe, Head of the Department of Metallurgy at Norways Institute of Technology (N.T.H.), began a compilation of curves showing the temperature dependence of the heat contents of the elements, and the heat contents and heats and free energies of formation of the common metallurgical compounds. With such a compilation, the thermal and free energy requirements of a reaction may be read from curves in a matter of seconds; and this statement applies not only to the formation of compounds from their elements, and to the reverse dissociation, but to any reaction involving substances whose thermodynamic properties are available. This follows from the fact that heats and free energies of formation are completely additive. For example, the free energy change associated with the chlorination of a metallic oxide at any temperature, T, is given by the free energy of formation of the chloride at temperature T minus that of the oxide also at T; both of these quantities may be read directly from curves of the type suggested above. Since this early, unpublished work of Lepsoe, both Ellingham7 and Richardson and Jeffes46 have

Jan 1, 1951

By WILLIAM WATERS

L HISTORY. THE Pierrefitte mines, situated in the South of France, in the district of the Hautes-Pyrenees, owe their name to the fact that the first mining operations of any extent, and of comparatively recent date, were carried out in the neighborhood of the vil¬lage of Pierrefitte, which is a branch terminus of the Midi railway. The Pierrefitte mines, however, embrace a wide extent of country and several different concessions, on most of which comparatively little exploration-work has been done. The portion of the property presently to be described is a zone running roughly E-W., over a distance of about 5 miles from the valley of Cauterets to the valley of Estaing, the ridge dividing these valleys being a spur of the main chain of the Pyrenees, and running more or less at right angles to it. According to local tradition, which various indications tend to confirm, these mines are of ancient date, the first workings being attributed to the Romans, who are supposed to have sought not only the lead but also the silver which is contained in the ore. Old slags have been found in the neighborhood which might well have been produced from the cupellation of lead-ores. These old workings, while of considerable extent at times, do not seem to have extended beyond a depth of 100 ft., even this depth being somewhat exceptional. The old notarial records of the district show that mines were known to exist, and that they were even worked, in the sixteenth century, but since the mines were abandoned (by the Romans or others) considerably prior to this period, very little

Nov 1, 1908

By P. L. Weston, S. E. Khalafalla

A systematic study was made by the Bureau of Mines on the effect of so me hypothesized accelerators for the process of wustite reduction in carbon monoxide. When small concentrations of promoter materials in the order of 0.69 at. pct were added to the reducible charge, the rate of reduction to iron was increased. Promotion phenomenon prediction was made in light of a suyface reduction mechanism with the aid of Vol'kenshtein's effect regarding the propagation of crystal lattice disturbances by small amounts of relatively larger interstitial ions. The acceleration produced by a typical promotor, such as potassiunl, increases with protnoter concentration up to a maximum, beyond which the reduction rate decreases. Concentration for maximum promotion depends on the nature and physicochemical properties of the promoter. The extent of reduction rate enhancement is found to be directly proportional to the atomic volume and electronic charge of the additive. DESPITE the enormous volume of literature on iron oxide reduction, very little is reported concerning additive or impurity effects on this important metallurgical process. The beneficial effect bf calcium compound additions on the reducibility of iron oxide sinters has been reported by Tigerschiold,1 vor dem Esche,2 and Edstrom. Doi and Kasai~ found that the addition of lime or limestone to iron ores helps to break up any unreducible compounds, such as fayalite or ilmen-ite. and thus free the combined iron for reduction. Schenck et al. 5 suggested that the increased reduction rate obtained when adding lime could be accounted for by the instability of wustite in the presence of lime. Acid-base slagging reactions resulted in wustite disproportionation according to The dicalcium ferrite formed will yield iron and calcium oxide during reduction. Regenerated calcium oxide dissociates more wustite. This mechanism has been used by Seths and white7 to explain their experimental results. Recently, Strangway and ROSS' attributed the calcium carbonate acceleration of iron oxide agglomerate reduction to increased porosity, both initial as well as that developed during reduction. Aside from calcium carbonate, or oxide, no other promoter was noted in the literature, except for a brief mention by Barrett and woodg on the effect of sodium carbonate and aluminate as activators for the hydrogen reduction of magnetite at 600°C. The present investigation systematically studied a host of other promoters, including calcium and sodium, in an attempt to elucidate the mechanism by which promotion takes place and to fit the results into a simple chemical model. To attain this goal, the effect of promoter physical properties, such as atomic volume, electronic charge, and concentration are related to wustite reduction kinetics in this paper. Wustite reduction to iron, rather than the overall hematite reduction, was chosen since this reaction is known to be the slowest, and hence the rate-deter mining step for the overall iron oxide reduction process. EXPERIMENTAL PROCEDURE Raw Materials and Their Preparation. The pure or impregnated wustite pellets were prepared from minus 400-mesh chemically pure hematite powders. A known weight of hematite was thoroughly and uniformly mixed with a calculated weight of the additive. The mixed paste containing 35 wt pct water was gradually heated from 400" to 1200° C and fired at 1200°C for approximately 4 hr in an air atmosphere. After cooling, the sinter was pulverized to minus 100 mesh and pelletized into minus 4- plus 5-mesh spheres. Pellets were fired, similarly to the paste mix, air-cooled, sized, and stored. An appropriate weight of the charge (20 g) was placed in a zirconia reduction tube maintaining a uniform oxide bed height of 1 cm and a cross section of 7.1 sq cm for all of the test runs. The samples were supported in the vertical reaction tube by a bed of fragmented insulating firebrick plus 3- to 6-mesh alumina beads. The hematite was then transformed to wustite by reduction with a 30 pct CO2-70 pct CO gas mixture at 1000°C in a globar furnace. Complete conversion to wustite was ascertained by a continuous infrared gas analyzer recording the CO-CO2 content of the effluent gas until no carbon monoxide was absorbed from the inlet gas, and inlet-outlet gas analysis remained constant for 30 min. The wustite sample was then reduced with 100 pct CO at 100WC. From the recorded data, an initial rate of reduction was determined by the initial slope of the graph percent reduction vs time. In order to estimate the accuracy of the data, five separate determinations of the reduction curve of pure wustite, under otherwise identical conditions, were performed. The maximum deviation from the average reduction at 14 min amounted to 2 2 pct reduction. This deviation corresponds to 3.8 pct variation based on the percent reduction of the sample. Aiiy impurity effect below the limits of this maximum deviation was considered a spurious result. If the effect exceeded + 4 pct, then it was considered as a positive one. Considerable care was exercised in determining the initial rate from the slope of the initial segments of the curve. Each reduction curve was examined separately on large graph paper and the best tangent to the curve at zero time was drawn. The slope of this tangent was taken as a measure of the initial fractional reduction per minute. Although the time required to reach 50 pct reduction may be of special practical significance, initial rate measurements are invaluable in fundamental studies. These rates provide a measure of the process kinetics on the initial

Jan 1, 1968

By Donald Warren, J. F. Libsch

HIS investigation originated as a result of a pre-vious experimental study' of the magnetic properties of Fe-Co alloys fabricated by the powder metallurgy technique. Densities of powder compacts prepared for the magnetics investigation varied from 7.45 to 7.70 g per cu cm or from 93 to 95 pct of the experimental value of 8.08 g per cu cm for a fused alloy of the same composition.' While this range of density is considered sufficiently high for most applications, the highest possible density is to be desired for maximum magnetic properties. By applying a technique similar to the one described above to a pure electrolytic iron powder, Rostoker³ was able to achieve a density of 7.895 g per cu cm, which is the highest density ever reported for sintered iron. While Rostoker's work involved the sintering of an elemental powder rather than a mixture, it was believed that higher densities should also have been obtained for alloys using the above technique because of the recoining operation and the high sintering temperature. Consequently, it was decided to investigate the various factors affecting the density of this alloy with the idea that such a study might lead to higher densities and, as a result, powder alloys having magnetic properties identical with those of the fused alloys. It was believed that the principal reason that near-theoretical densities for the powdered alloy were not obtained was the interference of gases with the normal sintering mechanism. When present during the sintering operation, gases can exert several harmful effects: they can remain on the particle surface and interfere with surface diffusion and plastic flow; they can be released and, under certain conditions, expand the void spaces through gas pressure; or they can remain trapped in the pores and exert a hydrostatic pressure that retards elimination of the pores. Jones,4 Rhines,5 Goetzel," and others have given the effect of gases in the sintering of powder compacts an extensive treatment. Among the more important sources of gases in the sintering process are dissolved gases, adsorbed gases, air entrapped during pressing, and gaseous products of chemical reactions. During sintering adsorbed gases are partly released at a relatively low temperature, while those gases entrapped during pressing cannot escape until their pressure is increased sufficiently through increasing temperature to expand the interpartjcle openings. The remaining adsorbed gases, gaseous reduction products, and dissolved gases produce a similar effect at the higher temperatures. If, in the sintering process, gas evolution occurs after the interpore channels have been sealed, an exaggerated expansion of the void spaces results. This is particularly true if the temperature is high enough for extensive plastic flow. In his fabrication of powder bars from tantalum, Balke7 had to consider the effect of adsorbed hydrogen and provide for its escape during sintering by limiting the compacting pressure to a maximum of 50 tons per sq in. The effect of gases entrapped during pressing was first noted by Trzebiatowski8 when he found that gold and silver powders decrease in density with increasing sintering temperature if pressed at 200 tsi, while they exhibit the usual increase when pressed at 40 tsi. Recent investigators9-11 have also noted that entrapped gases have an effect on the expansion of copper compacts during sintering. Proper provision for the escape of gaseous products of reduction must be made in order to avoid deleterious effects. Myers" states that in the sintering of electrolytic tantalum powder, the temperature was gradually raised to 2600°F with a pause at 2000°F to permit reduction of the oxides. Experimental Details For the present study, 50 pct Co-50 pct Fe compacts in the form of circular disks 1½ in. in diam and 0.15 in. thick were fabricated by the pressing and sintering of a mixture of the elemental powders. It was decided to follow the sintering process by means of liquid permeability measurements, because it was thought that such measurements might serve as a measure of relative pore sizes, as well as a possible indication of the point at which most of the interpore channels become sealed. However, since the permeability as measured by the flow of a liquid, such as ethylene glycol, does not give an absolute indication of the point where the pores have become isolated, a method for determining the percentage of pores connected to the surface was set up. As an additional cross check on the permeability measurements, metallographic methods were used to study the relative pore size. Finally, the property of ultimate interest, the density, was measured. Raw Materials: The powders used consisted of an annealed, 99.9 pct pure, —150 mesh grade of electrolytic iron powder, and a 98 pct pure, —200 mesh grade of reduced and comminuted cobalt powder. The cobalt powder was not further processed either by hydrogen reduction or annealing. The screen analyses for the iron and cobalt powders are given in Table I, while the chemical analyses for each type of powder are listed in Table 11. Table 111 gives the hydrogen loss measurements for the powders according to the M.P.A. Standard Method and for a higher temperature as well. Preparation of Compacts: Equal amounts of the elemental powders were mixed by rotation for 1 hr and then pressed into compacts approximately 0.15

Jan 1, 1952

By George Krauss, Morris Cohen

NUMEROUS investigators1-4 have shown that one of the most conspicuous effects of the reverse marten-sitic transformation in Fe-Ni alloys is the stabilization of the austenite which forms on reversal. However, the present authors5 found a virtual absence of stabilization in a recent study of this subject. The purpose of this note is to account for the discrepancy.

Jan 1, 1963

By C. E Shoenfelt, Gail F. Moulton

Proven and developed oil reserves, and productive capacity increased during 1943 in the fieids of the Rocky Mountain region. Oil production during the year was nearly 45 million barrels, or slightly less than in 1942. The rate of production at the start of 1944 was slightly less than at the start of 1943. Pipe-line projects scheduled for completion during 1944 should permit a substantial increase in the rate of production. Wildcat exploration was more extensive in Montana during 1943 than in other states in the region. The results of wildcat drilling were unsatisfactory, although new oil fields were discovered on the Gebo, Little Buffalo Basin and Steamboat Butte structures of Wyoming, the Gage anticline of Montana, and the Clark Lake structure of Colorado. The area of the structures on which the discovery wells were drilled is known to be considerable, but further drilling is required to determine the importance of these fields. The most important increase in proven reserves resulted from the drilling to newly discovered deeper producing formations in the Elk Basin and other fields of the Big Horn Basin area of northern Wyoming. Lack of a market and unfavorable prices for heavy black oils had prevented complete exploration of favorable areas in the Rocky Mountain region for many years. In particular, the effect on further exploitation of the Big Horn Basin area had been quite serious. The increased demands for all oils created by the war and an increase in price in February 1943, combined later with Government approval of construction of pipe lines from the Big Horn Basin area to the Billings and the Casper districts, provided a basis for undertaking a drilling program. The important additions to reserves were made by drilling in previously discovered fields. The newly discovered fields resulted from drilling on favorable structures which had been known for several years. A continuation of the favorable results obtained during 1943 seems possible only if further testing of the newly discovered fields is satisfactory and if drilling on less favorable known structures or geophysical prospects results in the discovery of new fields. The amount of drilling in the Rocky Mountain states of Colorado, Montana and Wyoming, was about the same during 1943 as .in 1942. However, owing to the fact that a number of wells of large potential production were completed in the Elk Basin field, the total initial production of the prodicing wells was- nearly twice as great for 1943 as for 1942. Explorational activity at the end of 1943 seemed to be directed to geophysical methods, which are required to discover structures hidden beneath the rocks of Tertiary age in the Powder River and other large sedimentary basins. It is in

Jan 1, 1944

By Gail F. Moulton, C. E. Shoenfelt

Proven and developed oil reserves, and productive capacity increased during 1943 in the fieids of the Rocky Mountain region. Oil production during the year was nearly 45 million barrels, or slightly less than in 1942. The rate of production at the start of 1944 was slightly less than at the start of 1943. Pipe-line projects scheduled for completion during 1944 should permit a substantial increase in the rate of production. Wildcat exploration was more extensive in Montana during 1943 than in other states in the region. The results of wildcat drilling were unsatisfactory, although new oil fields were discovered on the Gebo, Little Buffalo Basin and Steamboat Butte structures of Wyoming, the Gage anticline of Montana, and the Clark Lake structure of Colorado. The area of the structures on which the discovery wells were drilled is known to be considerable, but further drilling is required to determine the importance of these fields. The most important increase in proven reserves resulted from the drilling to newly discovered deeper producing formations in the Elk Basin and other fields of the Big Horn Basin area of northern Wyoming. Lack of a market and unfavorable prices for heavy black oils had prevented complete exploration of favorable areas in the Rocky Mountain region for many years. In particular, the effect on further exploitation of the Big Horn Basin area had been quite serious. The increased demands for all oils created by the war and an increase in price in February 1943, combined later with Government approval of construction of pipe lines from the Big Horn Basin area to the Billings and the Casper districts, provided a basis for undertaking a drilling program. The important additions to reserves were made by drilling in previously discovered fields. The newly discovered fields resulted from drilling on favorable structures which had been known for several years. A continuation of the favorable results obtained during 1943 seems possible only if further testing of the newly discovered fields is satisfactory and if drilling on less favorable known structures or geophysical prospects results in the discovery of new fields. The amount of drilling in the Rocky Mountain states of Colorado, Montana and Wyoming, was about the same during 1943 as .in 1942. However, owing to the fact that a number of wells of large potential production were completed in the Elk Basin field, the total initial production of the prodicing wells was- nearly twice as great for 1943 as for 1942. Explorational activity at the end of 1943 seemed to be directed to geophysical methods, which are required to discover structures hidden beneath the rocks of Tertiary age in the Powder River and other large sedimentary basins. It is in

Jan 1, 1944

By K. P. Mukherjee, K. P. Gupta, J. Bandyopadhyaya

Even though a lot of work has been done in the past to establish phase equilibrium in the Cu-Si system a re cent investigation casts some doubt about the existence and crystal structure of some of the phases that form in the composition range of 15 to 25 at. pct Si in Cu. The present investigation was carried out using high temperature X-ray diffraction technique along with other standard techniques to study the phases in this composition range. The high temperature 6 phase appears to be tetragonal with parameters a,, = 8.815A, c, = 7.903A, and co/ao = 0.896. The reported bcc E phase exists at room temperature and at least up to 780°C and appears to undergo a transformation near 600°C. The phase appears to be cubic but not of the bcc type. The ? phase appears to undergo a transformation, as has been indicated by earlier investigators, and the low temperature form of .? phase is tetragonal with parameters a, = 7.267A, co = 7.8924, and co/ao = 1.086. THE Cu-Si binary system has been investigated by several investigators1" and several intermediate phases,?,e,?' at lower temperatures and ?,ß,0,e, and ? at higher temperatures, were observed between terminal solid solutions of copper and silicon. Even though the existence of the e phase and the transformation in the ? phase were reported in many early works, in a recent study of this system Nowotny and Bittner6 doubted the existence of the e phase and phase at 550°C. Among the high temperature phases, the 6 phase was reported to have a complex cubic structure with parameter a, = 8.805A.7 Nowotny and Bittner, however, suggested that the structure of the 6 phase might be of CsCl type. In order to check these contradictory reports the present study was taken up to investigate the Cu-Si binary system in the composition range of 17 to 25 at. pct Si. EXPERIMENTAL PROCEDURE Weighed amounts of copper (99.99 pct) and silicon (99.9 pct) were induction melted in recrystallized alumina crucibles under argon gas atmosphere. The alloys containing 17, 18, 20, 21, 21.2, 22, and 24 at. pct Si were annealed in evacuated and sealed quartz capsules at 700°C for 3 days and subsequently water quenched. Other than this annealing, the 21.2 at. pct Si and 24 at. pct Si alloys were annealed at 550°C for 10 days, the 17 at. pct Si alloy was annealed at 750°C for 3 days, and the 22 and 24 at. pct Si alloys were annealed at 780°C for 2 days. All annealing temperatures were controlled to within *l°C. Alloys after quenching were subjected to metallographic and X-ray diffraction investigation. A solution containing 5 g FeC13 + 10 cc HCl + 120 cc H2O diluted with six times its volume with water was used as etching reagent. A 114.6 mm diam Debye Scherrer camera was used for obtaining diffraction patterns. The 17, 21.2, and 24 at. pct Si alloys were subjected to high temperature diffractometry using a Tempress Research High temperature attachment and a GEXRD VI diffractometer. For the 6 phase (17 at. pct Si alloy) powder specimen from a 750°C annealed alloy was reheated to 750°C in the high temperature attachment for 1½ hr before taking a diffraction trace. A 550°C annealed and slowly cooled phase (24 at. pct Si) alloy was first reheated to 550°C. a diffraction trace was made after annealing it for 2 hr, and subsequently it was heated to 716OC and kept at this temperature for 2 hr before taking a diffraction trace. For the e phase (21.2 at. pct Si alloy) a 550°C annealed and slowly cooled specimen was heated first to 425°C and annealed at this temperature for 2 hr before taking a diffraction trace. Subsequently, the specimen temperature was raised to 495", 540°, 603", 635", 682", 720°, and 748°C and homogenized at each temperature for 1 hr before taking diffraction traces. The powder specimen temperature was controlled to within +2oC at each temperature and argon gas, purified by passing it at slow rate through a fused CaC12 column, hot (800°C) copper and titanium chips and finally through a P2O5 column, was used to prevent oxidation of the powder. For all X-ray work copper-radiations at 25 kv, 15 ma (for Debye Scherrer technique), and 40 kv, 20 ma (for diffractometer tech-nique) were used. RESULTS AND DISCUSSION At 700°C the alloys containing 17 to 21 at. pct Si showed two phases while the 21.2 at. pct Si alloy was found to be single phase. The X-ray diffraction patterns of the two-phase alloys were consistent with the phase (ßP-Mn type structure) and the phase (21.2 at. pct Si) patterns. The diffraction patterns of the 17 at. pct Si alloy quenched from 750" and 700°C were identical. According to the accepted Cu-Si phase dia-gram4,5,10 the 17 at. pct Si alloy at 750°C should be in the (k + 6) two-phase region and very close to the -phase boundary. The identical patterns possibly resulted from the decomposition of the 6 phase on

Jan 1, 1970

By Lucius W. Mayer

The iron-mines of the Ilsede Hütte Co. are at a town called Peine, about 20 miles east of the city of Hanover, on the railroad to Brunswick (Braunschweig). Hanover, the capital of the province, is a military city, of approximately 250,000 inhabitants, and Brunswick, 33 miles to the westward, has half this number. The mines here described are located in a hamlet called Bülten. The Ilsede Hütte Co. operates two mines, 1.5 miles apart, in this district, Gruber Bülten Adenstadt and Gruber Lengede Bodenstadt. It also operates an iron-mine north of Hanover, known as Eiserhaven, and one in the Harz mountains, the Georg Friedrich, at Grauhof. At Bülten a coarse conglomerate, a, Figs. 1 and 2, contains nodules of limonite, cemented together by calcium phosphate. The ore contains Fe, 25 to 45; Mn, 3 to 4; P, 0.6 to 1.4; S, 0.02 to 0.09; and CaCO3, 40 per cent. Directly above the conglomerate is limestone, b, followed by a mixture of clay and sand, c. Below the conglomerate is a hard clay floor, d. The ore-body, from 10 to, 12 km. long, and from 3 to 4 km. wide, has a maximum thickness of 20 m. It clips approximately 10° S.E., and strikes N. 45° E. Diamond-drill prospecting shows that the thickness diminishes to 1 m. as the end of the deposit is approached to the northward. At this point the deposit is 250 m. below the surface. In Fig. 2, the arrow, A, indicates the general direction of the work along the face, a, which is carried forward in a straight line for its entire length. At B, a train is approaching, which has come from the bench-track, shown at G, by a circuitous route, and is dumping the overburden behind the face, in the space left by the excavated rock. Formerly the work at this mine was essentially open-cut, the deposit having a very strong outcrop. Figs. 1 and 2 show also

Sep 1, 1908

By Frank Foote, E. R. Jette

In recent years the constitution of the high-silver aluminum-silver alloys has been extensively investigated. Hansenl has reviewed the literature to 1935. More recently, Obinata and Hagiya,2 Hofmann and Volk,3 Taziri4 and Tishchenko5 have confirmed the general features of the phase diagram in the region around 25 atomic per cent aluminum. In this paper we present the results of high-precision measurements of lattice constants of the silver-rich alpha solid solution in the homogeneous range and the neighboring two-phase regions. These results are used to establish the nature of the solid solution, the identity of directly measured densities with those calculated from lattice constants and the homogeneity limits of the alpha solid solution with respect to three different neighboring phases. A study of the earlier investigations indicated that the last two subjects in particular required new and accurate data. Experimental Procedure Preparation of the Alloys.—The alloys were made from high-purity silver and aluminum. The silver was "Proof Silver," 99.999 per cent pure, supplied by the U. S. Metals Refining Co. The aluminum was 99.97 per cent pure (contained Si, 0.009 per cent; Fe, 0.0016 per cent; Cu, 0.004 per cent) and was supplied by the Aluminum Company of America. The lattice constants of these two materials have been reported by Jette and Foote.6 Weighed amounts of the two metals were placed in alundum crucibles and melted in vacuo in a high-frequency induction furnace. The melts were allowed to cool in the crucible, the ingots thus obtained weighed about 10 grams. These ingots were then filed clean, hamered, again cleaned and given a homogenizing anneal in vacuo of from 6 to 15 days at temperatures ranging from 500" to 695°C. The ingots were air-cooled from the annealing temperature. Lattice-constant Measurements.—Carefully prepared filings for X-ray analysis were sealed into evacuated quartz or Pyrex tubes and annealed for various periods of time at suitable temperatures. The furnaces used were vertical, rapid-quenching furnaces, the samples being quenched by crushing the sample tube under water by means of a heavy plunger. The general X-ray technique has been previously described6 The cameras were of the symmetrical, back-reflection, focussing type. Ka, radiation from a cobait-nickel alloy target was used. The wave-length values were taken from the second edition of Siegbaum's book.7 A correction for the index of refraction was applied and the lattice constants were calculated by the method of Cohen.8, 6 The lattice constants were calculated to a common temperature of 25°C., using the value of the linear expansion coefficient of pure silver as 18.9 X 10-6. Presumably the expansion coefficient for

Jan 1, 1941

By Frank Foote, E. R. Jette

In recent years the constitution of the high-silver aluminum-silver alloys has been extensively investigated. Hansenl has reviewed the literature to 1935. More recently, Obinata and Hagiya,2 Hofmann and Volk,3 Taziri4 and Tishchenko5 have confirmed the general features of the phase diagram in the region around 25 atomic per cent aluminum. In this paper we present the results of high-precision measurements of lattice constants of the silver-rich alpha solid solution in the homogeneous range and the neighboring two-phase regions. These results are used to establish the nature of the solid solution, the identity of directly measured densities with those calculated from lattice constants and the homogeneity limits of the alpha solid solution with respect to three different neighboring phases. A study of the earlier investigations indicated that the last two subjects in particular required new and accurate data. Experimental Procedure Preparation of the Alloys.—The alloys were made from high-purity silver and aluminum. The silver was "Proof Silver," 99.999 per cent pure, supplied by the U. S. Metals Refining Co. The aluminum was 99.97 per cent pure (contained Si, 0.009 per cent; Fe, 0.0016 per cent; Cu, 0.004 per cent) and was supplied by the Aluminum Company of America. The lattice constants of these two materials have been reported by Jette and Foote.6 Weighed amounts of the two metals were placed in alundum crucibles and melted in vacuo in a high-frequency induction furnace. The melts were allowed to cool in the crucible, the ingots thus obtained weighed about 10 grams. These ingots were then filed clean, hamered, again cleaned and given a homogenizing anneal in vacuo of from 6 to 15 days at temperatures ranging from 500" to 695°C. The ingots were air-cooled from the annealing temperature. Lattice-constant Measurements.—Carefully prepared filings for X-ray analysis were sealed into evacuated quartz or Pyrex tubes and annealed for various periods of time at suitable temperatures. The furnaces used were vertical, rapid-quenching furnaces, the samples being quenched by crushing the sample tube under water by means of a heavy plunger. The general X-ray technique has been previously described6 The cameras were of the symmetrical, back-reflection, focussing type. Ka, radiation from a cobait-nickel alloy target was used. The wave-length values were taken from the second edition of Siegbaum's book.7 A correction for the index of refraction was applied and the lattice constants were calculated by the method of Cohen.8, 6 The lattice constants were calculated to a common temperature of 25°C., using the value of the linear expansion coefficient of pure silver as 18.9 X 10-6. Presumably the expansion coefficient for

Jan 1, 1941

By A. B. Kinzel

IT has often been stated that the steel industry did no research or development work in the decades preceding 1920. If restricted to organized research on the quality and field of application of structural and engineering steels, this statement may be true. But the industry did conduct a vast amount of process research during this period, although some of the projects were not carried out as separate organized research programs. Securing a low cost of tonnage production was the sole problem receiving serious attention from the industry prior to 1920, and today this is still the major problem. Those in the industry deserve much commendation for the important increase in production capacity per dollar invested and for the markedly lowered cost of production. In recent years, a distinct change may be noted in the attitude of the steel industry toward research involving its product. With the advent of high-speed machinery both in the manufacturing and transportation industries, steel as a quality engineering material has come to the fore. In the past, high-quality carbon steels and alloy steels have been introduced over a period of years, largely at the insistence of the consumer and partly prompted by research carried out by those interested in the use of the alloys. The commercial introduction of these materials made slow progress.

Jan 1, 1935

By Michael S. Koleda

Less than two years ago, the, Congress, with broad bipartisan support, passed the Energy Security Act of 1980. A decade marked by ten- fold increases in world oil prices and two major interruptions in oil flows from the Middle East had ended. An all-out national commitment to transform America's vast tar sands, oil shale and coal resources into conventional fuels had begun. The national synfuels effort was to be public-private cooperation at a scale unmatched in peace time. Private industry would own and operate the synthetic fuels facilities. Government would reduce market uncertainties to acceptable levels. The potential government commitment was substantial. Up to $88 billion would be available through the Synthetic Fuels Corporation, principally in the form of contingent financing. Billions more would be spent through Department of Energy programs. Additional incentives for alternate energy development were contained in the Energy Tax Act of 1978. The Energy Security Act clearly specified national synthetic fuels production objectives: 500,000 barrels per day by 1987 -- 2 million barrels per day by 1992. Finally, said Congress, Uncle Sam was going to do something about rapidly rising oil prices, uncertainties of energy supply, and the resulting disruption to the U. S. economy. Simply put, the purpose of the Energy Security Act of 1980 was to provide government guarantees sufficient to get synthetic fuels projects off the private sector drawing boards and into commercial production. Because of their huge cost, technological uncertainty, and lengthy pay-out period, these projects were always second place to projects of smaller size, known technology and more rapid pay-out. The Energy Security Act was the legal expression of public policy to bring the free-market synfuels timetable into line with the faster paced political timetable in the interest of national energy security.

Jan 1, 1982